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“Composition And Combination Products, And Methods For Water Purification Thereof”

Abstract: “COMPOSITION AND COMBINATION PRODUCTS, AND METHODS FOR WATER PURIFICATION THEREOF” ABSTRACT The instant disclosure is in the field of chemical sciences, more particularly towards water purification. The present disclosure relates to emulsion breaker compositions and combination products for separating impurities such as oil and tar from water, and corresponding methods thereof.

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Patent Information

Application #
Filing Date
14 August 2019
Publication Number
08/2021
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
bangalore@knspartners.com
Parent Application
Patent Number
Legal Status
Grant Date
2021-10-21
Renewal Date

Applicants

RELIANCE INDUSTRIES LIMITED
3rd Floor, Maker Chamber-IV, 222, Nariman Point, Mumbai-400 021, Maharashtra, India.

Inventors

1. Dhairyasheel Bhaskarrao Pawar
Plot no 10, Rashmi Nagar, Behind Auditor's society, Harsul, Aurangabad. Maharashtra. 431001, India.
2. Shantilal Mohanlal Modha
13-A, Sector-2, Reliance Greens, Motikhavdi, Dist-Jamnagar, Gujarat, India.

Specification

DESC:TECHNICAL FIELD
[001]. The instant disclosure is in the field of chemical sciences, more particularly towards water purification. The present disclosure relates to emulsion breaker compositions and combination products for separating impurities such as oil and tar from water, and corresponding methods thereof.

BACKGROUND OF THE DISCLOSURE
[002]. Separation of oil-water emulsion in quench/process water streams becomes key for various industrial applications including performance of various downstream processes. The factors affecting the emulsion formation is also governed by upstream processes. For instance, in a typical gas cracker plant, the emulsion of oil in water needs to be separated prior to using said water for dilution steam generation. In gas cracker plant, poor run length of sour ‘water filtration system’ (comprising pre-filter, filter and coalescer) has been an area of concern. Water filtration systems’ underperformance not only affects the run length of ‘process diluent (steam) generator’, but it also adds on extra maintenance cost owing to frequent requirement of filter elements. During maintenance of process diluent generator, sour water is routed to Effluent Treatment Plant (ETP) continuously increasing load on effluent treatment process. In addition to consumption of filter elements, sour water filtration system demands additional costs due to frequent filter elements change over. Further, at one point in time, for many days, entire sour water filtration system and process diluent generator would need to be bypassed requiring this water continuously to be sent to ETP for treatment.

[003]. Therefore, for the improvement of water filtration system run length, attempts were made to ascertain the reasons for frequent clogging of the filter/coalescer elements. Total solid load (measured as TSS) was observed to be consistently < 10 ppm while the effectiveness of oil removal system seemed to be poor and inconsistent. The turbidity of water at the outlet of oil water separator was observed to be consistently higher than 1500-2000 NTU. The microscopic analysis of clogged coalescer elements indicated presence of sticky slimy layer. The formation of such slimy layer with interference of various hydrocarbon species with different dosing chemicals such as amine for pH control etc. could not be clearly established. Additionally, the tar which is expected to get separated from the oily water was also not being removed effectively.

[004]. Despite using currently available emulsion breaker (EB) formulations, the effectiveness and repeatability of separating oil and other impurities such as tar from quench water stream, especially quench water stream of cracker plant cannot be sustained. Therefore, there is a need to develop a simple, implementable, cost-effective and improved/efficient formulation for separating impurities such as oil and tar from water stream. The present disclosure addresses said need.

SUMMARY OF THE DISCLOSURE
[005]. The present disclosure relates to an emulsion breaker (EB) composition comprising phosphate, glycol and amine.

[006]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), tetra ethylene glycol (TeEG), Triethanol amine (TEA) and water.

[007]. The present disclosure particularly provides a combination product comprising:
a) the composition as defined above, and
b) a solvent,
for separating impurities including oil and/or tar from water.

[008]. In some embodiments, the present disclosure provides a combination product comprising:
a) a composition comprising phosphate, glycol and amine, and
b) a solvent,
for removal of hydrocarbon impurities such as oil and tar from quench water stream.

[009]. The present disclosure further provides methods for preparing the above defined composition and combination product and methods for purifying/separating impurities in a water sample by employing said composition/combination product.

[0010]. In some embodiments, the present disclosure provides a method to purify quench water stream in a thermal cracker plant comprising step of injecting the above described combination product to the quench water pipeline, to purify said quench water stream.

DESCRIPTION OF THE DISCLOSURE
[0011]. As used herein, the terms ‘composition’ and ‘formulation’ are employed interchangeably in the present disclosure.

[0012]. As used herein, the term ‘combination product’ refers to a combination of separate components as a single product. In some embodiments, the ‘combination product’ of the present disclosure comprises component A and component B, wherein the component A is a composition and the component B is a chemical compound, and said component A and component B exist separately. In some embodiments, the ‘combination product’ of the present disclosure comprises: a) an emulsion breaker (EB) composition, and b) a solvent. In embodiments of the present disclosure, the ‘combination product’ is an emulsion breaker (EB) product.

[0013]. As used herein, the term ‘quench water’ refers to the water generated through the quench tower during the process of quenching (immediate cooling) furnace effluent gases. In some embodiments, the furnace effluent gases in the thermal cracker plant are very hot (about 800 to 850?) and requires immediate cooling (quenching) in the quench water tower to minimize further propagation of polymerization. Water generated through said quench water tower is called quench water. In some embodiments, the quench water comprises impurities selected from oil, tar, coke particle, slime, or any combination thereof.

[0014]. As used herein, the term ‘process water’ and ‘sour water’ are employed interchangeably and refer to the water obtained after removal of oil and/or tar in the oil separator and removal of coke particles in the coke removal unit of a thermal cracker plant.

[0015]. As used herein, the terms ‘thermal cracker plant’ refers to process equipment used in petroleum refining which employ cracking of ‘refinery off gases’ comprising preferably ethane, propane or mixture thereof by using heat energy to obtain ethylene, propylene or mixture thereof.
[0016]. The present disclosure aims at providing compositions/products for separating impurities in water. Particularly, the present disclosure aims at improving the efficiency of separating hydrocarbon impurities such as oil and tar from water. The disclosure focusses on efficient separation of hydrocarbon impurities - oil and tar slimy material, from quench water of a thermal cracker plant. Such efficient separation of impurities such as oil and tar would avoid frequent clogging of pre-filter/filter/coalescer elements of the water filtration system and would help in improved run length of water filtration system and the subsequent process diluent generator (also known as Dilution Steam Generator or DSG) of the thermal cracker plant once the process water/sour water is fed into the process diluent generator.

[0017]. The present disclosure invention particularly tries to achieve improved efficiency of oil and tar separation from quench water stream of a thermal cracker plant. The quench water is treated for solids and residual oil removal followed by sour gases removal before it is fed to process diluent generator. However, the effectiveness of separating impurities such as oil and tar from quench water affects the performance of water filtration system (pre-filter, filters and coalescer) and process diluent generator which thereby impacts maintenance cost, manpower cost and additional load on effluent treatment unit. Additionally, the frequent outage of process diluent generator affects the overall operating cost of the thermal cracker plant.

[0018]. Despite employing currently available emulsion breaker formulations, the effectiveness and repeatability of separating impurities such as oil and tar from quench water stream cannot be sustained. In the gas cracker plant, the process diluent generator can underperform and the main contributing factor for the same has been attributed to the poor run length of water filtration system (pre-filter, filter and coalescer). Said problem including high maintenance and operational costs were the compelling reasons for the present inventors to study this problem with greater insight to identify implementable solution for separating impurities including oil and tar from a water stream.

[0019]. Therefore, a detailed analysis of quench water was done by the present inventors to understand the pattern of oil-water emulsion formation in quench water along with various operating conditions of the plant such as feed type, feed mix ratio, furnaces conversion, pH of quench water etc. After generating operating data which covers majority of plant operating conditions, extensive and burdensome trials were conducted to formulate a chemical base which would help to effectively separate hydrocarbon impurities including oil and tar from water.

[0020]. Accordingly, the present disclosure provides an emulsion breaker (EB) composition and a combination product for separating impurities from water. The emulsion breaker (EB) composition comprises phosphate, glycol and amine, and the combination product comprises: a) the composition comprising phosphate, glycol and amine; and b) a solvent. The emulsion breaker (EB) composition and the combination product are employed for removal of impurities such as oil and tar from water.

[0021]. In embodiments of the present disclosure, an emulsion breaker (EB) composition comprising phosphate, glycol and amine is provided.

[0022]. In some embodiments of the present disclosure, the composition comprises phosphate selected from a group comprising disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), dipotassium phosphate (K2HPO4), monopotassium phosphate (KH2PO4) and combinations thereof.

[0023]. In some embodiments, the phosphate is a combination of disodium phosphate (Na2HPO4) and monosodium phosphate (NaH2PO4).

[0024]. In some embodiments of the present disclosure, the composition comprises glycol selected from a group comprising polyethylene glycol (PEG), tetra ethylene glycol (TeEG), diethylene glycol (DEG) and combinations thereof.

[0025]. In some embodiments, the glycol is Tetraethylene glycol (TeEG).

[0026]. In some embodiments of the present disclosure, the composition comprises an amine which is triethanol amine (TEA).

[0027]. In some embodiments of the present disclosure, the composition comprises water.

[0028]. In some embodiments, the composition comprises phosphate at a concentration ranging from about 1 wt% to 15 wt%.
[0029]. In some embodiments, the composition comprises phosphate selected from a group comprising disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), dipotassium phosphate (K2HPO4), monopotassium phosphate (KH2PO4) and combinations thereof, at a concentration ranging from about 1 wt% to 15 wt%.

[0030]. In some embodiments, the composition comprises phosphate at a concentration ranging from about 2 wt% to 9 wt%.

[0031]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) and monosodium phosphate (NaH2PO4) at a concentration ranging from about 1 wt% to 15 wt%.

[0032]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration ranging from about 1 wt% to 5 wt%, and monosodium phosphate (NaH2PO4) at a concentration ranging from about 1 wt% to 10 wt%.

[0033]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration ranging from about 2 wt% to 3 wt%, and monosodium phosphate (NaH2PO4) at a concentration ranging from about 5 wt% to 6 wt%.

[0034]. In some embodiments of the present disclosure, the composition comprises glycol at a concentration ranging from about 1 wt% to 10 wt%.

[0035]. In some embodiments, the composition comprises glycol selected from a group comprising polyethylene glycol (PEG), tetra ethylene glycol (TeEG), diethylene glycol (DEG) and combinations thereof, at a concentration ranging from about 1 wt% to 10 wt%.

[0036]. In some embodiments, the composition comprises glycol at a concentration ranging from about 4 wt% to 6 wt%.

[0037]. In some embodiments, the composition comprises Tetra ethylene glycol (TeEG) at a concentration ranging from about 1 wt% to 10 wt%.

[0038]. In some embodiments, the composition comprises tetra ethylene glycol (TeEG) at a concentration ranging from about 4 wt% to 6 wt%.

[0039]. In some embodiments of the present disclosure, the composition comprises amine at a concentration ranging from about 1 wt% to 10 wt%.

[0040]. In some embodiments, the composition comprises amine at a concentration ranging from about 4 wt% to 6 wt%.

[0041]. In some embodiments, the composition comprises Triethanol amine (TEA) at a concentration ranging from about 1 wt% to 10 wt%.

[0042]. In some embodiments, the composition comprises Triethanol amine (TEA) at a concentration ranging from about 4 wt% to 6 wt%.

[0043]. In some embodiments of the present disclosure, the composition comprises water at a concentration ranging from about 70 wt% to 90 wt%.

[0044]. In some embodiments, the composition comprises water at a concentration ranging from about 80 wt% to 90 wt%.

[0045]. In some embodiments, the water in the composition can be replaced with any alternate component or solvent capable of dissolving phosphate, glycol and amine compounds described herein.

[0046]. In some embodiments of the present disclosure, the emulsion breaker (EB) composition comprises disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), tetra ethylene glycol (TeEG), triethanol amine (TEA) and water.

[0047]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration ranging from about 1 wt% to 15 wt%, monosodium phosphate (NaH2PO4) at a concentration ranging from about 1 wt% to 15 wt%, tetra ethylene glycol (TeEG) at a concentration ranging from about 1 wt% to 10 wt%, Triethanol amine (TEA) at a concentration ranging from about 1 wt% to 10 wt%, and water at a concentration ranging from about 70 wt% to 90 wt%.

[0048]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration ranging from about 2 wt% to 3 wt%, monosodium phosphate (NaH2PO4) at a concentration ranging from about 5 wt% to 6 wt%, Tetra ethylene glycol (TeEG) at a concentration ranging from about 4 wt% to 6 wt%, Triethanol amine (TEA) at a concentration ranging from about 4 wt% to 6 wt%, and water at a concentration ranging from about 80 wt% to 90 wt%.

[0049]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration of about 0.47 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 1.15 wt%, tetra ethylene glycol (TeEG) at a concentration of about 1.0 wt%, triethanol amine (TEA) at a concentration of about 1.0 wt%, and water at a concentration of about 96.38 wt%.

[0050]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration of about 1.41 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 3.35 wt%, tetra ethylene glycol (TeEG) at a concentration of about 3.0 wt%, triethanol amine (TEA) at a concentration of about 3.0 wt%, and water at a concentration of about 89.24 wt%.

[0051]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration of about 2.35 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 5.75 wt%, tetra ethylene glycol (TeEG) at a concentration of about 5.0 wt%, triethanol amine (TEA) at a concentration of about 5.0 wt%, and water at a concentration of about 81.9 wt%.

[0052]. In some embodiments, the composition comprises disodium phosphate (Na2HPO4) at a concentration of about 2.35 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 5.75 wt%, tetra ethylene glycol (TeEG) at a concentration of about 1.0 wt%, triethanol amine (TEA) at a concentration of about 1.0 wt%, and water at a concentration of about 89.9 wt%.
[0053]. The present disclosure further relates to a method for preparing the emulsion breaker (EB) composition as defined above, comprising mixing phosphate, glycol and amine in water.

[0054]. In some embodiments, the method for preparing the emulsion breaker (EB) composition as defined above comprises:
a) adding water to the phosphate and dissolving the mixture; and
b) adding glycol and amine to the mixture, and optionally mixing and addition of water to prepare the composition.

[0055]. In some embodiments, the method for preparing the emulsion breaker (EB) composition as defined above comprises:
a) adding water to disodium phosphate (Na2HPO4) and monosodium phosphate (NaH2PO4), and dissolving the mixture; and
b) adding tetra ethylene glycol (TeEG) and Triethanol amine (TEA) to the mixture followed by mixing and addition of water to prepare the composition.

[0056]. In some embodiments, the method for preparing the emulsion breaker (EB) composition as defined above comprises:
a) adding water to disodium phosphate (Na2HPO4) and monosodium phosphate (NaH2PO4), and dissolving the mixture by mechanical stirring;
b) adding tetra ethylene glycol (TeEG) and Triethanol amine (TEA) to the mixture followed by addition of water to make up the final volume of the composition.

[0057]. In some embodiments, the composition is prepared by taking exact quantity of the phosphate in a vessel followed by adding water and dissolving it by mechanical stirring. Thereafter, weighed quantities of glycol and amine are added and mixed well. The whole content is made up with water to the prescribed volume to obtain the composition.

[0058]. In some embodiments, the composition is prepared by taking exact quantities of disodium phosphate (Na2HPO4) and monosodium phosphate (NaH2PO4) in a vessel, adding about 60% water and dissolving it by mechanical stirring. Thereafter, weighed quantities of Triethylene glycol (TeEG) and Triethanol amine (TEA) are added and mixed well. The whole content is made up with water to the prescribed volume to obtain the composition.

[0059]. In some embodiments, the composition described above may additionally comprise a solvent selected from a group comprising aromatic or aryl hydrocarbon, paraffinic hydrocarbon, naphthenic hydrocarbon, aliphatic or alkyl hydrocarbon, and combinations thereof. In some embodiments, the aromatic or aryl hydrocarbon is a C6 to C8 aromatic or aryl hydrocarbon selected from a group comprising toluene, xylene, benzene, para-xylene, o-xylene and combinations thereof. In some embodiments, the aromatic or aryl hydrocarbon is a combination of toluene and xylene. Accordingly, in some embodiments, the composition of the disclosure comprises phosphate, glycol, amine, water and an additional solvent as defined above.

[0060]. The present disclosure further provides a combination product comprising:
a) the emulsion breaker (EB) composition as described above; and
b) a solvent.

[0061]. In some embodiments, the combination product comprises:
a) a composition comprising phosphate, glycol, amine and water; and
b) a solvent.

[0062]. In some embodiments, the combination product comprises component a) (i.e. the composition) and component b) (i.e. the solvent) as separate components.

[0063]. In some embodiments, the combination product comprises component a) (i.e. the composition) and component b) (i.e. the solvent) as separate components, and not together as a single composition/formulation.

[0064]. In some embodiments of the present disclosure, the solvent in the combination product is selected from a group comprising aromatic or aryl hydrocarbon, paraffinic hydrocarbon, naphthenic hydrocarbon, aliphatic or alkyl hydrocarbon, and combinations thereof.
[0065]. In some embodiments, the aromatic or aryl hydrocarbon is a C6 to C8 aromatic or aryl hydrocarbon.

[0066]. In some embodiments, the C6 to C8 aromatic or aryl hydrocarbon solvent is selected from a group comprising toluene, xylene, benzene, para-xylene, o-xylene and combinations thereof.

[0067]. In some embodiments, the paraffinic hydrocarbon is selected from a group comprising decane, dodecane, hexadecane and combinations thereof.

[0068]. In some embodiments, the naphthenic hydrocarbon is selected from a group comprising straight run naphtha, platformer feed, kerosene and combinations thereof.

[0069]. In some embodiments, the aliphatic or alkyl hydrocarbon is selected from a group comprising n-hexane, n-heptane & n-octane and combinations thereof.

[0070]. In some embodiments, the solvent in the combination product is a C7 and a C8 aromatic or aryl hydrocarbon.

[0071]. In some embodiments, the solvent in the combination product is toluene and xylene.

[0072]. In some embodiments, the solvent in the combination product is two or more hydrocarbons selected from xylene, para-xylene and o-xylene.

[0073]. In some embodiments, the solvent in the combination product is xylene, para-xylene and o-xylene.

[0074]. In some embodiments, the solvent in the combination product is a paraffinic hydrocarbon and a naphthenic hydrocarbon.

[0075]. In some embodiments, the solvent in the combination product is an aromatic/aryl hydrocarbon and a naphthenic hydrocarbon.

[0076]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio ranging from about 2833 : 1 to about 17000 : 1 (EB composition : Solvent).

[0077]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio ranging from about 2833 : 1 to about 4250 : 1.

[0078]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio of about 2833 : 1.

[0079]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio of about 3400 : 1.

[0080]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio of about 4250 : 1.

[0081]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio of about 5667 : 1.

[0082]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio of about 8500 : 1.

[0083]. In some embodiments, the combination product comprises: the emulsion breaker (EB) composition and the solvent at a ratio of about 17000 : 1.

[0084]. In some embodiments, the combination product comprises solvent at a concentration ranging from about 1 wt% to 10 wt%. In some embodiments, the combination product comprises solvent at a concentration ranging from about 1 wt% to 3 wt%.

[0085]. In some embodiments, the combination product comprises a mixture of C7 aryl hydrocarbon and C8 aryl hydrocarbon at a concentration ranging from about 1 wt% to 10 wt%.

[0086]. In some embodiments, the combination product comprises a mixture of C7 aryl hydrocarbon and C8 aryl hydrocarbon at a concentration ranging from about 1 wt% to 3 wt%.

[0087]. In some embodiments, the combination product comprises: a) a composition comprising phosphate at a concentration ranging from about 1 wt% to 15 wt%, glycol at a concentration ranging from about 1 wt% to 10 wt%, amine at a concentration ranging from about 1 wt% to 10 wt% and water at a concentration ranging from about 70 wt% to 90 wt%; and b) the solvent at a concentration ranging from about 1 wt% to 10 wt%.

[0088]. In some embodiments, the combination product comprises: a) a composition comprising phosphate at a concentration ranging from about 2 wt% to 9 wt%, glycol at a concentration ranging from about 4 wt% to 6 wt%, amine at a concentration ranging from about 4 wt% to 6 wt%, water at a concentration ranging from about 80 wt% to 90 wt%; and b) solvent at a concentration ranging from about 1 wt% to 3 wt%.

[0089]. In some embodiments of the present disclosure, the combination product comprises:
a) a composition comprising disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), tetra ethylene glycol (TeEG), Triethanol amine (TEA), water; and
b) a C7 to C8 aromatic or aryl hydrocarbon.

[0090]. In some embodiments of the present disclosure, the combination product comprises:
a) a composition comprising disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), tetra ethylene glycol (TeEG), Triethanol amine (TEA), water; and
b) a mixture of toluene and xylene.

[0091]. In some embodiments, the combination product comprises: a) a composition comprising disodium phosphate (Na2HPO4) at a concentration ranging from about 1 wt% to 15 wt%, monosodium phosphate (NaH2PO4) at a concentration ranging from about 1 wt% to 15 wt%, tetra ethylene glycol (TeEG) at a concentration ranging from about 1 wt% to 10 wt%, Triethanol amine (TEA) at a concentration ranging from about 1 wt% to 10 wt%, water at a concentration ranging from about 70 wt% to 90 wt%; and b) a mixture of toluene and xylene at a concentration ranging from about 1 wt% to 10 wt%.

[0092]. In some embodiments, the combination product comprises: a) a composition comprising disodium phosphate (Na2HPO4) at a concentration ranging from about 2 wt% to 3 wt%, monosodium phosphate (NaH2PO4) at a concentration ranging from about 5 wt% to 6 wt%, tetra ethylene glycol (TeEG) at a concentration ranging from about 4 wt% to 6 wt%, Triethanol amine (TEA) at a concentration ranging from about 4 wt% to 6 wt%, water at a concentration ranging from about 80 wt% to 90 wt%; and b) a mixture of toluene and xylene at a concentration ranging from about 1 wt% to 3 wt%.

[0093]. In some embodiments, the combination product comprises: a) a composition comprising disodium phosphate (Na2HPO4) at a concentration of about 0.47 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 1.15 wt%, tetra ethylene glycol (TeEG) at a concentration of about 1.0 wt%, triethanol amine (TEA) at a concentration of about 1.0 wt%, and water at a concentration of about 96.38 wt%; and b) a mixture of toluene and xylene at a concentration of about 2.0 wt%.

[0094]. In some embodiments, the combination product comprises: a) a composition comprising disodium phosphate (Na2HPO4) at a concentration of about 1.41 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 3.35 wt%, tetra ethylene glycol (TeEG) at a concentration of about 3.0 wt%, Triethanol amine (TEA) at a concentration of about 3.0 wt%, and water at a concentration of about 89.24 wt%; and b) a mixture of toluene and xylene at a concentration of about 2.0 wt%.

[0095]. In some embodiments, the combination product comprises: a) a composition comprising disodium phosphate (Na2HPO4) at a concentration of about 2.35 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 5.75 wt%, tetra ethylene glycol (TeEG) at a concentration of about 5.0 wt%, triethanol amine (TEA) at a concentration of about 5.0 wt%, and water at a concentration of about 81.9 wt%; and b) a mixture of toluene and xylene at a concentration of about 2.0 wt%.

[0096]. In some embodiments, the combination product comprises: a) a composition comprising disodium phosphate (Na2HPO4) at a concentration of about 2.35 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 5.75 wt%, tetra ethylene glycol (TeEG) at a concentration of about 1.0 wt%, Triethanol amine (TEA) at a concentration of about 1.0 wt%, and water at a concentration of about 89.9 wt%; and b) a mixture of toluene and xylene at a concentration of about 2.0 wt%.

[0097]. In embodiments of the present disclosure, the wt% of solvent in the combination product refers to the concentration of solvent with respect to the water sample used for treatment/purification. For instance, a combination product comprising 2 wt% of mixture of toluene and xylene means employing a concentration of 2% toluene and xylene mixture for a given quantity of quench water sample, for example, 100 ml of quench water sample. In some embodiments, a combination product comprising 1.7 wt% of mixture of toluene and xylene means employing a concentration of 1.7% (or 2 ml) toluene and xylene mixture for 100 ml quench water sample. In some embodiments of the present disclosure, the water sample used for treatment/purification is quench water.

[0098]. In embodiments of the present disclosure, the wt% of the components of the emulsion breaker (EB) composition in the combination product is employed such that the total wt% of the composition (phosphate, glycol, amine and water) adds up to 100 wt%.

[0099]. The present disclosure also relates to a method for preparation of the above described combination product comprising: a) a composition and b) a solvent, wherein the composition comprises phosphate, glycol, amine and water. The method of preparing said combination product comprises preparing the composition and the solvent separately.

[00100]. In some embodiments, the preparation of the composition is as described above. In some embodiments, the preparation of the composition comprises adding water to the phosphate and dissolving the mixture. Thereafter, glycol and amine are added to said mixture followed by optional mixing and addition of water to make up the final volume of the composition.

[00101]. In some embodiments, the composition is prepared by taking exact quantity of the phosphate in a vessel followed by adding water and dissolving it by mechanical stirring. Thereafter, weighed quantities of glycol and amine are added and mixed well. The whole content is made up with water to the prescribed volume to obtain the composition.

[00102]. In some embodiments, the composition is prepared by taking exact quantities of disodium phosphate (Na2HPO4) and monosodium phosphate (NaH2PO4) in a vessel, adding about 60% water and dissolving it by mechanical stirring. Thereafter, weighed quantities of Triethylene glycol (TeEG) and triethanol amine (TEA) are added and mixed well. The whole content is made up with water to the prescribed volume to obtain the composition.

[00103]. In some embodiments of the present disclosure, the concentrations of the components of the emulsion breaker composition or the combination product is employed such that the total wt% in the final composition/combination product adds up to 100 wt%.

[00104]. The invention described herein thus tries to solve the most complex and tedious problem of separation of oil-water and other impurities such as tar from processed/quench water stream which has further industrial application(s). As described above, the problem which originates from ineffective oil and tar separation from water makes the further downstream industrial processes very difficult/challenging. Further, the designing of vessel(s) for quench water purification is based on initial assumptions of oil/tar quality in the water stream. Thus, the ineffectiveness of oil and tar separation from quench water stream also affects the selection of associated equipment, pipelines, pumps, instruments etc. very difficult, thereby severely affecting the day-to-day operation of plant. Thus, the present invention would not only help in efficient and faster separation of oil and tar from water, but it would also help to reduce the associated maintenance with unit operation.

[00105]. The chemistry of the emulsion breaker composition and the combination product described herein is based on various trails to demonstrate the suitability and efficacy for better and faster oil/tar separation from water. Extensive attempts were made to identify the suitable chemistry which helps to effectively separate oil and tar from quench water.

[00106]. The key for better and faster separation of oil from water in industrial applications lie in lowering the surface tension in the most effective way without affecting other process functions. There are numerous parameters that contribute to break the tight emulsion of oil with water, such as pH, temperature, ionic strength of water and size of the colloidal particles. The tight emulsion of quench water could be due to the poly nucleus aromatics (tar) with water. Therefore, the first priority is to break the tight emulsion, to separate tar from water. Second, resultant tar must be taken out from water. Third, the chemicals/composition required for this task should be economical and easily available.

[00107]. By keeping all the above analysis and factors in mind, the present inventors were able to develop the emulsion breaker (EB) composition and the combination product described herein. In embodiments of the present disclosure, the components of the present emulsion breaker composition and the combination product perform the following functions to achieve improved efficiency in removing hydrocarbon impurities such as oil and tar from water:
(a) Phosphate is highly aggressive and provides better separation. The phosphate component in the present composition also helps to maintain the pH of quench water and thereby reducing the need/requirement of additional chemicals which helps in avoiding lower pH conditions and thereby potential corrosion issues.
(b) Amine helps to control the aggressiveness and thus the pH control is better.
(c) Glycol helps in enhancing the hydrophilicity of amine.
The composition comprising phosphate, glycol and amine thus breaks the tight emulsions in water to separate oil, tar and other impurities from water.
(d) Solvent used in the combination product helps to dissolve the tar substances due to better solubility and therefore helps in effective separation of tar impurities from water. It attracts the tar impurities and separates the resultant tar from water.

[00108]. The present disclosure also provides a method to purify water or separate impurities in water, said method comprising step of contacting the above described composition or the combination product with the water.

[00109]. In some embodiments, the water subjected to a method of purification comprises hydrocarbon impurities.

[00110]. In some embodiments, the water subjected to a method of purification comprises impurities selected from oil, tar, coke particles, slime, or any combination thereof.

[00111]. In some embodiments, the water subjected to a method of purification comprises oil and tar impurities.

[00112]. In some embodiments, the water subjected to a method of purification is quench water stream of a thermal cracker plant. In some embodiments, the water subjected to a method of purification is process water stream or sour water stream of a thermal cracker plant.

[00113]. Thus, in some embodiments, the present disclosure provides a method for purifying or separating oil and tar impurities in a quench water stream of a thermal cracker plant, the method comprising injecting the emulsion breaker composition or the combination product described herein to the quench water pipeline.

[00114]. The present disclosure also provides a method to purify quench water stream in a thermal cracker plant comprising step of injecting the above described combination product to the quench water pipeline, to purify the quench water stream. In some embodiments, the quench water stream comprises impurities including oil and tar. In some embodiments, the combination product comprises:
a) a composition comprising phosphate, glycol, amine and water; and
b) a solvent.

[00115]. In some embodiments, the thermal cracker plant comprises a dosing system which primarily consists of a tank, a metering pump and an injecting device, in the main quench water pipeline.

[00116]. In some embodiments, the solvent and the composition of the present combination product are added/injected separately into the quench water pipeline.

[00117]. In some embodiments, the composition comprising phosphate, glycol, amine and water is injected into the quench water stream via. the dosing system.

[00118]. In some embodiments, the solvent is injected into the quench water stream at a point which is just before the injection point of the composition.

[00119]. In some embodiments, the method to purify quench water stream comprises injecting the composition or the combination product at a dose ranging from about 1 ppm to 150 ppm.

[00120]. In some embodiments, the method to purify quench water stream comprises injecting the composition or the combination product at a dose ranging from about 10 ppm to 25 ppm.

[00121]. In some embodiments, the method to purify quench water stream comprises injecting the composition or the combination product at a dose ranging from about 6 ppm to 18 ppm.

[00122]. In some embodiments, the method to purify quench water stream comprises injecting the composition or the combination product at a dose ranging of from about 4 ppm to 6 ppm.

[00123]. In some embodiments, the present disclosure provides a method to purify quench water stream in a thermal cracker plant by employing the combination product as described above, comprising:
a) injecting the solvent into the quench water pipeline; and
b) injecting the composition comprising phosphate, glycol, amine and water into the quench water pipeline, wherein said composition is injected into the quench water pipeline at a point which is after the injection point of the solvent.

[00124]. The present disclosure further provides a method of breaking an emulsion, comprising: contacting an effective amount of the emulsion breaker (EB) composition or the combination product described above, with the emulsion.

[00125]. In some embodiments, the method of breaking an emulsion comprises: bringing an effective amount of the emulsion breaker (EB) composition or the combination product described above, in contact with the emulsion.

[00126]. In some embodiments, the method of breaking an emulsion comprises: contacting the emulsion breaker (EB) composition or the combination product described above at a dose ranging of from about 1 ppm to 150 ppm, with the emulsion.

[00127]. In some embodiments, the method of breaking an emulsion comprises: contacting the emulsion breaker (EB) composition or the combination product described above at a dose ranging of from about 10 ppm to 25 ppm, with the emulsion.

[00128]. In some embodiments, the method of breaking an emulsion comprises: contacting the emulsion breaker (EB) composition or the combination product described above at a dose ranging of from about 6 ppm to 18 ppm, with the emulsion.

[00129]. In some embodiments, the method of breaking an emulsion comprises: contacting the emulsion breaker (EB) composition or the combination product described above at a dose ranging of from about 4 ppm to 6 ppm, with the emulsion.

[00130]. In some embodiments, the emulsion is an oil-water emulsion present in quench water stream of a thermal cracker plant.

[00131]. The present disclosure also provides a kit comprising the combination product described herein. In some embodiments, the kit contains: a) a composition comprising phosphate, glycol, amine and water; and b) a solvent. In some embodiments, the kit contains phosphate, glycol, amine, water and solvent.

[00132]. ADVANTAGES/BENEFITS: The present disclosure provides advantages including but not limiting to the following:
1) The products of the present disclosure are successful in breaking tight emulsions in water (eg. quench water) to separate hydrocarbon impurities including oil and tar from water.
2) The products of the present disclosure show efficient and faster separation of impurities including oil and tar from water stream. In some embodiments, separation of impurities from quench water was achieved within 30 minutes to 1 hour of residence time which is much lesser than the originally designed/conventional vessel employed for separation (residence time was around 1 hour 20 minutes).
3) Improved run length of water filtration system (pre-filters, filters and coalescers) thereby reduction of revenue cost incurred for replacement of elements by a minimum 60-80% annually.
4) Improved run length of dilution steam generators (DSG) by at least 50%, thereby savings in operating costs.
5) Improved run length of water filtration system and DSG would reduce the manpower and therefore there is less potential of human injury and also reduces vulnerability of being in hazardous area during operation.
6) Oil-water separator vessel can be sized/designed without considering inclusion of any additional chemical to aid better and faster separation. Effectiveness of the present products would help in even reducing the size of vessel used for oil water separation. Further, during revamp of the same/existing plant, the existing/conventional vessel may even be used at higher throughput with minimum (or without) modifications.

[00133]. Additional embodiments and features of the present disclosure will be apparent to one of ordinary skill in art based upon description provided herein. The embodiments herein provide various features and advantageous details thereof in the description. Descriptions of well-known/conventional methods/steps and techniques are omitted so as to not unnecessarily obscure the embodiments herein. Further, the disclosure herein provides for examples illustrating the above described embodiments, and in order to illustrate the embodiments of the present disclosure certain aspects have been employed. The examples used herein for such illustration are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the following examples should not be construed as limiting the scope of the embodiments herein.

EXAMPLES
Example 1
Preparation and testing of efficiency of the products of present disclosure
[00134]. Experiments were performed to prepare and test the efficiency of the present compositions/combination products on purification of water.

Chemicals used to prepare the compositions/combination products were:
1. Tetra ethylene glycol (TeEG)
2. Triethanol amine (TEA)
3. Disodium phosphate (Na2HPO4)
4. Monosodium phosphate (NaH2PO4)
5. C7-C8 solvent (mixture of toluene and xylene)

TeEG, TEA, Na2HPO4 and NaH2PO4 were procured commercially, and C7-C8 solvent (mixture of toluene and xylene) is one of the products of the gas cracker plant.

Preparation:
First, the phosphate salts (Na2HPO4 and NaH2PO4) were dissolved in 60 ml of DM water (demineralized water) by mechanical stirring. TeEG and TEA were added to it and a final volume of 100 ml was made up with DM water (demineralized water). Thus, a composition comprising TeEG, TEA, Na2HPO4 and NaH2PO4 was prepared in DM water.

The following products were prepared:

Product 1 -
a) TeEG: 1 gm / 100 ml (about 1 wt%)
b) TEA: 1 gm / 100 ml (about 1 wt%)
c) Na2HPO4: 0.47 gm / 100 ml (about 0.47 wt%)
d) NaH2PO4: 1.15 gm / 100 ml (about 1.15 wt%)
e) DM Water : Balance (about 96.38 wt%)
and
f) C7-C8 solvent (toluene:xylene at 40:60) : 2 ml / 100 ml of quench water (about 1.7 wt%)

Product 2 -
a) TeEG: 3 gm / 100 ml (about 3 wt%)
b) TEA: 3 gm / 100 ml (about 3 wt%)
c) Na2HPO4: 1.41 gm / 100 ml (about 1.41 wt%)
d) NaH2PO4: 3.35 gm / 100 ml (about 3.35 wt%)
e) DM Water : Balance (about 89.24 wt%)
and
f) C7-C8 solvent (toluene:xylene at 40:60): 2 ml / 100 ml of quench water (about 1.7 wt%)

Product 3 -
a) TeEG: 5 gm / 100 ml (about 5 wt%)
b) TEA: 5 gm / 100 ml (about 5 wt%)
c) Na2HPO4: 2.35 gm / 100 ml (about 2.35 wt%)
d) NaH2PO4: 5.75 gm / 100 ml (about 5.75 wt%)
e) DM Water : Balance (about 81.9 wt%)
and
f) C7-C8 solvent (toluene:xylene at 40:60): 2 ml / 100 ml of quench water (about 1.7 wt%)

Product 4 -
a) TeEG: 1 gm / 100 ml (about 1 wt%)
b) TEA: 1 gm / 100 ml (about 1 wt%)
c) Na2HPO4: 2.35 gm / 100 ml (about 2.35 wt%)
d) NaH2PO4: 5.75 gm / 100 ml (about 5.75 wt%)
e) DM Water : Balance (about 89.9 wt%)
and
f) C7-C8 solvent (Toluene: xylene at 40:60): 2 ml / 100 ml of quench water (about 1.7 wt%)

The above combination products 1, 2, 3 and 4 comprised: 1) the composition having TeEG, TEA, Na2HPO4, NaH2PO4 and DM water; and 2) C7-C8 solvent.

Trial description:
a) About 100 ml of quench water (QW) sample was measured in a stoppered glass cylinder. Two different quench water stream samples were selected, one having high turbidity, and another having a comparatively lower turbidity.
b) C7-C8 solvent (toluene:xylene mixture) was added and shaken for about 10 seconds.
c) Different amounts/dosages of the compositions comprising TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, was added. The amount/dosage of the mentioned compositions comprising TeEG, TEA, Na2HPO4, NaH2PO4 and DM water were employed ranging from 0 ppm to 150 ppm.
d) The entire mixture was shaken well and allowed to settle for about 1 hour.

Trial Results:
Product 1 experimental results
(pilot run with two types of water samples having low and high turbidity)

Low Turbidity QW:
Base Sample : Quench Water from Coke Removal Unit (CRU)
Initial pH: 5.4
Initial Turbidity: ~ 8000 Nephelometric Turbidity Unit (NTU)
Test temperature: Room temperature (about 23? to 26?)

Turbidity of the water separated at bottom is measured after 1 hour of settling and the results are shown in Table 1.

Table 1: Turbidity Results of Product 1
Sample Details Product 1
doped 0.0 ppm Product 1
doped 5.0 ppm Product 1
doped 10.0 ppm Product 1
doped 20.0 ppm Product 1
doped 25.0 ppm Product 1
doped 50.0 ppm Product 1
doped 75.0 ppm Product 1
doped 100 ppm Product 1
doped 150 ppm
Turbidity 6820 5450 2280 1400 1240 3660 4210 4400 5500
% Reduction 15 32 72 83 85 54 47 45 31

Note: In all the experiments of Table 1, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 5 ppm, 10 ppm, 20 ppm, 25 ppm, 50 ppm, 75 ppm, 100 ppm and 150 ppm).

High Turbidity QW:
Base Sample : Quench Water from CRU
Initial pH: 5.8
Initial Turbidity: ~ 25000 NTU
Test temperature: Room temperature (about 23? to 26?)

Turbidity of the water separated at bottom is measured after 1 hour of settling and the results are shown in Table 2.

Table 2: Turbidity Results of Product 1
Sample Details Product 1
doped 0.0 ppm Product 1
doped 5.0 ppm Product 1
doped 10.0 ppm Product 1
doped 20.0 ppm Product 1
doped 25.0 ppm Product 1
doped 50.0 ppm Product 1
doped 75.0 ppm Product 1
doped 100 ppm Product 1
doped 150 ppm
Turbidity 22800 13250 7280 4680 4740 10200 12800 14000 14800
% Reduction 9 47 71 81 81 59 49 44 41

Note: In all the experiments of Table 2, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 5 ppm, 10 ppm, 20 ppm, 25 ppm, 50 ppm, 75 ppm, 100 ppm and 150 ppm).

Observations/Discussion:
1. Product 1 at different dosages was found to be effective in reduction of turbidity in both high and low turbidity samples.
3. Separation of impurities took place within half an hour.
4. Separated tar accumulated at solvent and colour changed from colorless to dark brown.

Based on the above trial, the concentration of product 1 was increased to three-fold to obtain product 2 and the trial was carried out again.

Product 2 experimental results (pilot run with water sample having high turbidity)

High Turbidity QW:
Base Sample : Quench Water from CRU
Initial pH: 6.2
Initial Turbidity: ~ 12000 NTU
Test temperature: Room temperature (about 23? to 26?)

Turbidity of the water separated at bottom is measured after 1 hour of settling and the results are shown in Table 3.

Table 3: Turbidity Results of Product 2
Sample Details Product 2
doped 0.0 ppm Product 2
doped 6.0 ppm Product 2
doped 12.0 ppm Product 2
doped 18.0 ppm Product 2
doped 24.0 ppm
Turbidity 5050 3560 2400 3480 5350
% Reduction 58 70 80 71 55

Note: In all the experiments of Table 3, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 6 ppm, 12 ppm, 18 ppm and 24 ppm).

Observations/Discussion:
1. Product 2 at different dosages was found to be very effective in reduction of turbidity.
3. Separation of impurities took place within half an hour.
4. Separated tar accumulated at solvent and colour changed from colorless to dark brown.

The concentrations of product 1 was increased five-fold to obtain product 3 and the trial was carried out again.

Product 3 experimental results (pilot run with water samples having high and low turbidity)

High Turbidity QW:
Base Sample : Quench Water from CRU
Initial pH: 6.5
Initial Turbidity: ~ 9500 NTU
Test temperature: Room temperature (about 23? to 26?)

Turbidity of the water separated at bottom is measured after 1 hour of settling and the results are shown in Table 4.

Table 4: Turbidity Results of Product 3
Sample Details Product 3
doped 0.0 ppm Product 3
doped 3.0 ppm Product 3
doped 4.0 ppm Product 3
doped 5.0 ppm Product 3
doped 6.0 ppm
Turbidity 5920 3050 1800 1750 1980
% Reduction 38 68 81 82 79

Note: In all the experiments of Table 4, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm).

Low Turbidity QW:
Base Sample : Quench Water from CRU
Initial pH: 5.2
Initial Turbidity: ~ 4600 NTU
Test temperature: Room temperature (about 23? to 26?)

Turbidity of the water separated at bottom is measured after 1 hour of settling and the results are shown in Table 5.

Table 5: Turbidity Results of Product 3
Sample Details Product 3
doped 0.0 ppm Product 3
doped 3.0 ppm Product 3
doped 4.0 ppm Product 3
doped 5.0 ppm Product 3
doped 6.0 ppm
Turbidity 2200 1650 902 850 980
% Reduction 52 64 80 82 78

Note: In all the experiments of Table 5, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm).

The efficiency of Product 3 was tested in another set of highly turbid QW sample as follows:

High Turbidity QW:
Base Sample: Quench Water from CRU
Initial pH: 5.7
Initial Turbidity: 13180 NTU (measured by diluting sample 10 times)
Test Temp: Room Temperature (23-26?)

Table 6: Turbidity Results of Product 3
Sample Details Product 3
doped 0.0 ppm Product 3
doped 2.0 ppm Product 3
doped 3.0 ppm Product 3
doped 4.0 ppm Product 3
doped 5.0 ppm Product 3
doped 6.0 ppm
Turbidity 9050 6550 4580 2560 2680 4350
% Reduction 31 50 65 81 80 67

Note: In all the experiments of Table 6, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm).

Observations/Discussion:
1. Product 3 at different dosages were found to be very effective in reduction of turbidity in both high and low turbidity samples.
2. Separated tar accumulated at solvent and colour changed from colorless to dark brown.

Product 4 experimental results
Base Sample : Quench Water from Coke Removal Unit (CRU)
Initial pH: 6.4
Initial Turbidity: ~ 8800 NTU
Test temperature: Room temperature (about 23? to 26?)

Turbidity of the water separated at bottom is measured after 1 hour of settling. The turbidity of the water sample was lowered to < 1000 NTU (90 % reduction) by employing Product 4.

Observations/Discussion:
1. Product 4 was found to be effective in reducing turbidity of quench water.
2. Separated tar accumulated at solvent and colour changed from colorless to dark brown.

Additionally, the following composition (product 5) comprising glycol, phosphate, amine and water was also prepared and tested for reduction in turbidity of QW sample, as follows:

Product 5 -
a) TeEG: 5 wt%
b) TEA: 5 wt%
c) Na2HPO4: 2.35 wt%
d) NaH2PO4: 5.75 wt%
e) DM Water : 81.9 wt%

Preparation:
First, the phosphate salts (Na2HPO4 and NaH2PO4) were dissolved in water by mechanical stirring. TeEG and TEA were added to it and a final volume of 100 ml was made up with DM water (demineralized water).

Trial description:
a) About 100 ml of quench water (QW) sample was measured in a stoppered glass cylinder. Quench water stream sample with high turbidity was employed.
b) Different dosages of product 5 was added to the QW samples.
c) The entire mixture was shaken well and allowed to settle for about 1 hour.

Trial Results:
High Turbidity QW:
Base Sample: Quench Water from CRU
Initial pH: 5.7
Initial Turbidity: 13180 NTU (measured by diluting sample 10 times)
Test Temp: Room Temperature (23-26?)

Table 7: Turbidity Results of Product 5
Sample Details Product 5
doped 0.0 ppm Product 5
doped 2.0 ppm Product 5
doped 3.0 ppm Product 5
doped 4.0 ppm Product 5
doped 5.0 ppm Product 5
doped 6.0 ppm
Turbidity 9790 8770 8750 8460 8400 8800
%Reduction 26 33 34 36 36 33

Note: In all the experiments of Table 7, the C7-C8 solvent and the composition TeEG, TEA, Na2HPO4, NaH2PO4 and DM water, were employed according to the trial description provided above. Particularly, about 1.7 wt% of C7-C8 solvent was initially added to the quench water sample followed by the addition of the composition at different dosages (i.e. 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm).

Observations/Discussion:
Product 5 was able to reduce turbidity of highly turbid quench water sample.

[00135]. The above results based on the emulsion breaker compositions/combination products of the present disclosure additionally indicate that it was ideal to maintain a pH of about 5.0 to 7.0 of the water sample. Further, the present emulsion breaker compositions/combination products were successful in accelerating the rate of flocculation and coagulation leading to faster separation of the water phase and the tar/oil phase. In particular, emulsion breaker compositions/ combination products efficiently facilitated the breaking of the tight emulsion of water and tar. The separated oil/tar were dissolved in solvents (such as C7-C8 aryl hydrocarbons) which can be easily removed by oil decantation in the oil separation vessel.

[00136]. The above results also indicate that when higher concentrations of the components of the emulsion breaker composition/combination product is employed, less dosage (ppm) of said composition/combination product is sufficient to achieve effective/desired reduction in turbidity.

[00137]. While the above results are based on Na2HPO4, NaH2PO4 (phosphates), TeEG (glycol), TEA (amine), DM water and C7 to C8 aromatic or aryl hydrocarbons (solvent), emulsion breaker compositions/combination products employing alternative compounds under phosphate, glycol, amine, water and solvent can be developed by a person skilled in the art based on the reading of present disclosure/examples. Further, results of said emulsion breaker compositions/combination products employing alternative components of phosphate, glycol, amine, water and solvent are expected to be similar and are within the purview of the present disclosure. For instance, the phosphates K2HPO4 and KH2PO4 are of the same class as Na2HPO4 and NaH2PO4 and are expected to behave similarly because both are cationic surfactants and have similar function; the glycols PEG and DEG are similar to TeEG and are expected to behave similarly because they are used for enhancing hydrophilicity of resultant solution; the solvents C7 to C8 aryl hydrocarbons are light solvents and similar light solvents such as benzene, toluene and xylenes as described in the present disclosure are expected to behave similarly because they are used to extract the oil/tar which gets separated by the action of the composition comprising glycol, phosphate and amine.

Example 2
Comparative Examples
[00138]. The following different formulations were developed and employed for testing their efficiency in reducing turbidity of quench water (QW) samples.

i. Formulation comprising glycols, amine, alcohols and solvents:
Trials were conducted by doping various concentrations of prepared formulations comprising glycols, amine, alcohols and solvents wherein different formulations with varying components were employed.

Results: No improvement in the turbidity of the QW sample was seen. The test QW samples showed almost the same/similar turbidity as the initial QW sample and there was no visual improvement.

ii. Formulation comprising glycols, amine and surfactants
Trials were conducted by doping various concentrations of prepared formulations comprising glycols, amine, alcohols and solvents wherein different formulations with varying components were employed.

Results: No improvement in the turbidity of the QW sample was seen. The test QW samples showed almost the same/similar turbidity as the initial QW sample and there was no visual improvement.

iii. Formulation comprising glycols, amine, borax salts and solvent
Trials were conducted by doping various concentrations of prepared formulations comprising glycols, amine, alcohols and solvents wherein different formulations with varying components were employed.

Results: No improvement in the turbidity of the QW sample was seen. The test QW samples showed almost the same/similar turbidity as the initial QW sample and there was no visual improvement.

[00139]. In the following experiments, compositions and combination products were employed by removing at least one ingredient/component in each of said composition and combination product to understand the efficiency in reducing turbidity of quench water (QW) samples.

High Turbidity QW:
Base Sample: Quench Water from CRU
Initial pH: 5.7
Initial Turbidity: 13180 NTU (measured by diluting sample 10 times)
Test Temp: Room Temperature (23-26?)

a) Composition comprising glycol and amine
Trials were conducted by doping a formulation comprising glycol (TeEG) at 5 wt% and amine (TEA) at 5 wt%. About 90 wt% DM water was added to prepare the formulation. The formulation was doped at 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm.

Results: No desired result/visual improvement in turbidity was observed.

b) Composition comprising glycol and phosphate
Trials were conducted by doping a formulation comprising glycol (TeEG) at 5 wt%, disodium phosphate (Na2HPO4) at 2.35 wt% and monosodium phosphate (NaH2PO4) at 2.35 wt%. About 86.9 wt% DM water was added to prepare the formulation. The formulation was doped at 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm.

Results: No desired result/visual improvement in turbidity was observed.

c) Composition comprising amine and phosphate
Trials were conducted by doping a formulation comprising amine (TEA) at 5 wt%, disodium phosphate (Na2HPO4) at 2.35 wt% and monosodium phosphate (NaH2PO4) at 2.35 wt%. About 86.9 wt%. DM water was added to prepare the formulation. The formulation was doped at 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm.

Results: No desired result/visual improvement in turbidity was observed.

d) Product comprising glycol, phosphate and solvent
Trials were conducted by doping a combination product comprising: a) glycol (TeEG) at 5 wt%, disodium phosphate (Na2HPO4) at 2.35 wt%, monosodium phosphate (NaH2PO4) at 5.75 wt%, and about 86.9 wt% DM water; and b) C7-C8 Solvent at about 1.7 wt%. The product was doped at 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm.

Results: No significant reduction/visual improvement in turbidity was observed.

e) Product comprising amine, phosphate and solvent
Trials were conducted by doping a combination product comprising: a) amine (TEA) at 5 wt%, disodium phosphate (Na2HPO4) at 2.35 wt%, monosodium phosphate (NaH2PO4) at 5.75 wt%, and about 86.9 wt% DM water; and b) C7-C8 Solvent at about 1.7 wt%. The product was doped at 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm.

Results: No significant reduction/visual improvement in turbidity was observed.

f) Product comprising glycol, amine and solvent
Trials were conducted by doping a combination product comprising: a) glycol (TeEG) at 5 wt%, amine (TEA) at 5 wt%, and about 90 wt% DM water; and b) C7-C8 Solvent at about 1.7 wt%. The product was doped at 0 ppm, 2 ppm, 3 ppm, 4 ppm, 5 ppm and 6 ppm.

Results: No significant reduction/visual improvement in turbidity was observed.

[00140]. The above experimental results indicate that addition or employment of alternate chemical components such as alcohols, surfactants, borax salts etc. did not yield desired results as there was either no or insignificant reduction in turbidity of the tested QW samples. This fact shows the importance/significance of the emulsion breaker compositions/products of the present disclosure in successful reduction of quench water turbidity, thereby purifying or separating the impurities such as oil and tar in the water sample. The above experimental results, for instance, the comparison of results of present products 1, 2, 3, 4 and 5 (Example 1) and compositions/products under a), b), c), d), e) and f) (Example 2), additionally highlight the synergistic interaction of each of the components of the present emulsion breaker composition/combination product leading to desired results. In particular, it is demonstrated that if any of the components are lacking in the present emulsion breaker composition/combination product, successful or desired results in breaking tight emulsion are not achieved.

[00141]. As regards all the embodiments/examples characterized in this specification, in particular in the claims, it is intended that each embodiment mentioned in a dependent claim is combined with each embodiment of each claim (independent or dependent) said dependent claim depends from. As an example, in case of an independent claim 1 reciting 3 alternatives A, B and C, a dependent claim 2 reciting 3 alternatives D, E and F and a claim 3 depending from claims 1 and 2 and reciting 3 alternatives G, H and I, it is to be understood that the specification unambiguously discloses embodiments corresponding to combinations: A, D, G; A, D, H; A, D, I; A, E, G; A, E, H; A, E, I; A, F, G; A, F, H; A, F, I; B, D, G; B, D, H; B, D, I; B, E, G; B, E, H; B, E, I; B, F, G; B, F, H; B, F, I; C, D, G; C, D, H; C, D, I; C, E, G; C, E, H; C, E, I; C, F, G; C, F, H; and C, F, I, unless specifically mentioned otherwise.

[00142]. Similarly, and also in those cases where independent and/or dependent claims do not recite alternatives, it is understood that if dependent claims refer back to a plurality of preceding claims or plurality of embodiments, any combination of subject-matter covered thereby is considered to be explicitly disclosed. For example, in case of an independent claim 1, a dependent claim 2 referring back to claim 1, and a dependent claim 3 referring back to both claims 2 and 1, it follows that the combination of the subject-matter of claims 3 and 1 is clearly and unambiguously disclosed as is the combination of the subject-matter of claims 3, 2 and 1. In case a further dependent claim 4 is present which refers to anyone of claims 1 to 3, it follows that the combination of the subject-matter of claims 4 and 1, of claims 4, 2 and 1, of claims 4, 3 and 1, as well as of claims 4, 3, 2 and 1 is clearly and unambiguously disclosed.

[00143]. The above considerations apply mutatis mutandis to all claims and embodiments of the present specification. To give a few examples, the combination of claims 2, 3, 4 and 5 is clearly and unambiguously envisaged in view of the claim structure/claimed subject-matter. The same applies for the combinations of claims 13, 14, 15 and 16, and, to give a few further examples which are not limiting, the combination of claims 18, 19 and 20 and the combination of claims 20, 21 and 22.

[00144]. The foregoing description of the specific embodiments and examples reveal the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments in this disclosure have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein.

[00145]. Throughout this specification, the word “comprise”, or variations such as “comprises” or “comprising” or “including” wherever used, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps. Additionally, throughout the specification, “a group comprising” of a particular stated element, integer or step, or group of elements, integers or steps also envisages “a group consisting” of said stated element, integer or step, or group of elements, integers or steps without inclusion of any other element, integer or step, or group of elements, integers or steps.

[00146]. With respect to the use of substantially any plural and/or singular terms herein, those having skill in the art can translate from the plural to the singular and/or from the singular to the plural as is appropriate to the context and/or application. The various singular/plural permutations may be expressly set forth herein for sake of clarity.

[00147]. Any discussion of documents, acts, materials, devices, articles and the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.

[00148]. While considerable emphasis has been placed herein on the particular features of this disclosure, it will be appreciated that various modifications can be made, and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. These and other modifications in the nature of the disclosure or the preferred embodiments will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
,CLAIMS:We Claim:

1) An emulsion breaker (EB) composition comprising phosphate, glycol and amine.

2) The composition as claimed in claim 1, wherein the phosphate is selected from a group comprising disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), dipotassium phosphate (K2HPO4), monopotassium phosphate (KH2PO4) and combinations thereof; the glycol is selected from a group comprising polyethylene glycol (PEG), tetra ethylene glycol (TeEG), diethylene glycol (DEG) and combinations thereof; and the amine is triethanol amine (TEA); and wherein the composition comprises water.

3) The composition as claimed in claim 1 or claim 2, wherein the phosphate is at a concentration ranging from about 1 wt% to 15 wt%, preferably about 2 wt% to 9 wt%; the glycol is at a concentration ranging from about 1 wt% to 10 wt%, preferably about 4 wt% to 6 wt%; the amine is at a concentration ranging from about 1 wt% to 10 wt%, preferably about 4 wt% to 6 wt%, and the water is at a concentration ranging from about 70 wt% to 90 wt%, preferably about 80 wt% to 90 wt%.

4) The composition as claimed in any of the claims 1 to 3, wherein the composition comprises disodium phosphate (Na2HPO4) at a concentration ranging from about 1 wt% to 15 wt%, monosodium phosphate (NaH2PO4) at a concentration ranging from about 1 wt% to 15 wt%, tetra ethylene glycol (TeEG) at a concentration ranging from about 1 wt% to 10 wt%, triethanol amine (TEA) at a concentration ranging from about 1 wt% to 10 wt%, and water at a concentration ranging from about 70 wt% to 90 wt%.

5) The composition as claimed in any of the claims 1 to 4, wherein the composition comprises
disodium phosphate (Na2HPO4) at a concentration of about 0.47 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 1.15 wt%, tetra ethylene glycol (TeEG) at a concentration of about 1.0 wt%, triethanol amine (TEA) at a concentration of about 1.0 wt%, and water at a concentration of about 96.38 wt%; or
disodium phosphate (Na2HPO4) at a concentration of about 1.41 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 3.35 wt%, tetra ethylene glycol (TeEG) at a concentration of about 3.0 wt%, triethanol amine (TEA) at a concentration of about 3.0 wt%, and water at a concentration of about 89.24 wt%; or
disodium phosphate (Na2HPO4) at a concentration of about 2.35 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 5.75 wt%, tetra ethylene glycol (TeEG) at a concentration of about 5.0 wt%, triethanol amine (TEA) at a concentration of about 5.0 wt%, and water at a concentration of about 81.9 wt%; or
disodium phosphate (Na2HPO4) at a concentration of about 2.35 wt%, monosodium phosphate (NaH2PO4) at a concentration of about 5.75 wt%, tetra ethylene glycol (TeEG) at a concentration of about 1.0 wt%, triethanol amine (TEA) at a concentration of about 1.0 wt%, and water at a concentration of about 89.9 wt%.

6) A combination product comprising:
a) the emulsion breaker (EB) composition of any of the claims 1 to 5; and
b) a solvent.

7) The combination product as claimed in claim 6, wherein the combination product comprises:
a) phosphate, glycol, amine and water; and
b) a solvent.

8) The combination product as claimed in claim 6 or claim 7, wherein the solvent is selected from a group comprising aliphatic or alkyl hydrocarbon, aromatic or aryl hydrocarbon, paraffinic hydrocarbon, naphthenic hydrocarbon and combinations thereof;
and wherein the aromatic or aryl hydrocarbon is a C6 to C8 aromatic or aryl hydrocarbon, said C6 to C8 aromatic or aryl hydrocarbon selected from a group comprising toluene, xylene, benzene, para-xylene, o-xylene and combinations thereof,
the paraffinic hydrocarbon is selected from a group comprising decane, dodecane, hexadecane and combinations thereof,
the naphthenic hydrocarbon is selected from a group comprising straight run naphtha, platformer feed naphtha, kerosene and combinations thereof, and
the aliphatic or alkyl hydrocarbon is selected from a group comprising n-hexane, n-heptane, n-octane and combinations thereof.

9) The combination product as claimed in any of the claims 6 to 8, wherein the solvent is:
a) a mixture of C7 and C8 aromatic or aryl hydrocarbon;
b) a mixture of toluene and xylene;
c) a mixture of two or more hydrocarbons selected from xylene, para-xylene and o-xylene;
d) a mixture of a paraffinic hydrocarbon and a naphthenic hydrocarbon; or
e) a mixture of an aromatic hydrocarbon and a naphthenic hydrocarbon.

10) The combination product as claimed in any of the claims 6 to 9, wherein the combination product comprises the emulsion breaker (EB) composition and the solvent at a ratio ranging from about 2833 : 1 to about 17000 : 1 (EB composition : Solvent), preferably about
2833 : 1 to about 4250 : 1.

11) The combination product as claimed in any of the claims 6 to 10, wherein the combination product comprises:
a) a composition comprising phosphate at a concentration ranging from about 1 wt% to 15 wt%, preferably about 2 wt% to 9 wt%, glycol is at a concentration ranging from about 1 wt% to 10 wt%, preferably about 2 wt% to 9 wt%, amine at a concentration ranging from about 1 wt% to 10 wt%, preferably about 2 wt% to 9 wt%, and water at a concentration ranging from about 70 wt% to 90 wt%, preferably about 80 wt% to 90 wt%; and
b) solvent at a concentration ranging from about 1 wt% to 10 wt%, preferably about 1 wt% to 3 wt%.

12) The combination product as claimed in any of the claims 6 to 11, wherein the product comprises:
a) a composition comprising disodium phosphate (Na2HPO4), monosodium phosphate (NaH2PO4), tetra ethylene glycol (TeEG), triethanol amine (TEA) and water; and
b) a C7 to C8 aromatic or aryl hydrocarbon, preferably a mixture of toluene and xylene.

13) The combination product as claimed in any of the claims 6 to 12, wherein the product comprises:
the composition (Na2HPO4, NaH2PO4, TeEG, TEA and water) and the solvent at a ratio ranging from about 2833 : 1 to about 17000 : 1 (composition : solvent), preferably about 2833 : 1 to about 4250 : 1;
or,
the product comprises:
a) a composition comprising disodium phosphate (Na2HPO4) at a concentration ranging from about 1 wt% to 15 wt%, preferably about 2 wt% to 3 wt%, monosodium phosphate (NaH2PO4) at a concentration ranging from about 1 wt% to 15 wt%, preferably about 5 wt% to 6 wt%, tetra ethylene glycol (TeEG) at a concentration ranging from about 1 wt% to 10 wt%, preferably about 4 wt% to 6 wt%, triethanol amine (TEA) at a concentration ranging from about 1 wt% to 10 wt%, preferably about 4 wt% to 6 wt%, water at a concentration ranging from about 70 wt% to 90 wt%, preferably about 80 wt% to 90 wt%, and
b) a mixture of toluene and xylene at a concentration ranging from about 1 wt% to 10 wt%, preferably about 1 wt% to 3 wt%.

14) A method for preparing the emulsion breaker (EB) composition as defined in any of the claims 1 to 5, comprising mixing phosphate, glycol and amine in water.

15) The method as claimed in claim 14, wherein the method comprises:
a) adding water to the phosphate and dissolving the mixture;
b) adding glycol and amine to the mixture followed by optional mixing and addition of water to prepare the composition.

16) A method for purifying water containing impurities, said method comprising contacting the emulsion breaker (EB) composition or the combination product as claimed in any of the claims 1 to 13 with the water to separate the impurities.

17) The method as claimed in claim 16, wherein the water comprises impurities selected from oil, tar, coke particle, slime, or any combination thereof; and wherein the water is quench water stream of a thermal cracker plant.

18) The method as claimed in claim 16 or claim 17, wherein the method comprises separating oil and tar impurities in a quench water stream of a thermal cracker plant by injecting the emulsion breaker (EB) composition or the combination product of any of the claims 1 to 13 to the quench water pipeline;
and wherein the composition or the combination product is injected at a dose ranging from about 1 ppm to 150 ppm.

19) The method as claimed in any of the claims 16 to 18, wherein said method comprises purifying quench water stream in a thermal cracker plant by employing the combination product, the method comprising:
a) injecting the solvent into the quench water pipeline;
b) injecting the composition comprising phosphate, glycol, amine and water into the quench water pipeline, wherein said composition is injected at a point which is after the injection point of the solvent.

20) A method of breaking an emulsion, comprising: contacting an effective amount of the emulsion breaker (EB) composition or the combination product of any of the claims 1 to 13 with the emulsion, wherein the emulsion is an oil-water emulsion present in quench water stream of a thermal cracker plant.

Documents

Application Documents

# Name Date
1 201921032843-STATEMENT OF UNDERTAKING (FORM 3) [14-08-2019(online)].pdf 2019-08-14
2 201921032843-PROVISIONAL SPECIFICATION [14-08-2019(online)].pdf 2019-08-14
3 201921032843-POWER OF AUTHORITY [14-08-2019(online)].pdf 2019-08-14
4 201921032843-FORM 1 [14-08-2019(online)].pdf 2019-08-14
5 201921032843-DECLARATION OF INVENTORSHIP (FORM 5) [14-08-2019(online)].pdf 2019-08-14
6 201921032843-Proof of Right (MANDATORY) [10-01-2020(online)].pdf 2020-01-10
7 201921032843-FORM 18 [14-08-2020(online)].pdf 2020-08-14
8 201921032843-COMPLETE SPECIFICATION [14-08-2020(online)].pdf 2020-08-14
9 201921032843-OTHERS [30-08-2021(online)].pdf 2021-08-30
10 201921032843-FER_SER_REPLY [30-08-2021(online)].pdf 2021-08-30
11 201921032843-CLAIMS [30-08-2021(online)].pdf 2021-08-30
12 201921032843-FER.pdf 2021-10-19
13 201921032843-PatentCertificate21-10-2021.pdf 2021-10-21
14 201921032843-RELEVANT DOCUMENTS [28-09-2022(online)].pdf 2022-09-28
15 201921032843-RELEVANT DOCUMENTS [30-09-2023(online)].pdf 2023-09-30

Search Strategy

1 IntellectualPropertyIndiaE_03-03-2021.pdf

ERegister / Renewals

3rd: 20 Dec 2021

From 14/08/2021 - To 14/08/2022

4th: 31 Jul 2022

From 14/08/2022 - To 14/08/2023

5th: 31 Jul 2023

From 14/08/2023 - To 14/08/2024

6th: 07 Aug 2024

From 14/08/2024 - To 14/08/2025

7th: 30 Jul 2025

From 14/08/2025 - To 14/08/2026