Abstract: ABSTRACT HYDROPHOBIC CARBONACEOUS MATERIAL AND A PROCESS FOR PREPARATION THEREOF The present disclosure relates to hydrophobic carbonaceous material and a process for preparation thereof. The hydrophobic carbonaceous material has desired characteristics such as relatively high hydrophobicity without the need for an additional step of halogenation, as required conventionally. The process of the present disclosure converts chlorinated hydrocarbon, obtained from industrial plant waste, particularly vinyl chloride monomer plant, into highly valuable hydrophobic carbonaceous material, thereby making the process environment friendly and economical.
DESC:FIELD
The present disclosure relates to hydrophobic carbonaceous material and a process for preparation thereof.
DEFINITIONS
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used to indicate otherwise.
Hydrophobicity refers to the physical property of a molecule (known as a hydrophobe) that is seemingly repelled (does not attract) from a mass of water.
Dehydrochlorination refers to a process of eliminating hydrogen chloride from an organic compound/substance/material.
Contact angle with water refers to the determination of hydrophobicity/hydrophilicity of the surface of a material. Generally, if the contact angle is smaller than 90°, the solid surface is considered hydrophilic and if the water contact angle is larger than 90°, the solid surface is considered hydrophobic.
Carbonization refers to a process that produces carbonaceous residue by thermal decomposition of an organic substance.
Carbonaceous material refers to a wide variety of carbonaceous forms, mainly obtained by carbonization, including carbon, graphite, diamond, highly oriented pyrolytic graphite (HOPG), fibers such as thermal graph, carbon foam, and carbon nanotubes (CNTs), which are generally black in color.
Crystallinity refers to the degree of structural order in a solid. In a crystal, the atoms or molecules are arranged in a regular, periodic manner.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
The preparation of carbon black or carbonaceous material involves cracking of petroleum hydrocarbons at high temperature. However, such processes do not impart the desired hydrophobicity to the carbonaceous material. Rather, the hydrophobicity is induced through post chemical modification by reacting the carbonaceous material with halogen namely chlorine, bromine, or fluorine, or also by reacting with hypochlorous acid. Further, such procedures are energy intensive, require a large land footprint, generate relatively higher amount of effluent, incur a high equipment cost, including both CAPEX and OPEX, making it economically unattractive and also detrimental to the environment.
Therefore, there is a need for a process to prepare hydrophobic carbonaceous material that mitigates the drawbacks mentioned hereinabove.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows.
It is an object of the present disclosure to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a hydrophobic carbonaceous material.
Still another object of the present disclosure is to provide a process for preparing the hydrophobic carbonaceous material.
Yet another object of the present disclosure is to provide a simple, energy efficient and environment friendly process for the preparation of carbonaceous material from industrial waste.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure provides a process for preparing a hydrophobic carbonaceous material from chlorinated hydrocarbon. The process comprises a step of introducing a chlorinated hydrocarbon in a reactor. The chlorinated hydrocarbon is heated to a temperature in the range of 140 °C to 150 °C, at a first predetermined rate, to obtain a heated mixture. A catalyst is added to the heated mixture to obtain a reaction mixture. The reaction mixture is heated to a temperature in the range of 240 °C to 260 °C, at a second predetermined rate, to obtain gaseous hydrochloric acid and a crude solid product. The crude solid product is purified to obtain hydrophobic carbonaceous material.
The present disclosure further provides a hydrophobic carbonaceous material, characterized by having chlorine content in the range of 20 wt.% to 30 wt.%, contact angle with water in the range of 95° to 120°, surface area in the range of 150 m2/g to 400 m2/g, pore volume in the range of 0.15 cm3/g to 0.30 cm3/g, and pore diameter in the range of 2.5 nm to 4.5 nm.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
The present disclosure will now be described with the help of the accompanying drawing, in which:
Figure 1 illustrates a graphical representation of the contact angle versus the chlorine content of the carbonaceous material of the present disclosure;
Figure 2 illustrates an FTIR spectrum of the hydrophobic carbonaceous material (sample 1) in accordance with the present disclosure; and
Figure 3 illustrates a graphical representation of DMA (Dynamic Mechanical Analysis) curve of the hydrophobic carbonaceous material (sample 1) in accordance with the present disclosure.
DETAILED DESCRIPTION
Embodiments, of the present disclosure, will now be described with reference to the accompanying drawing.
Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
Carbon black/carbonaceous material is prepared by the cracking of petroleum hydrocarbons at high temperature. However, such processes do not impart the desired hydrophobicity to the carbonaceous material. Rather, the hydrophobicity is induced through post chemical modification by reacting the carbonaceous material with halogen namely chlorine, bromine, or fluorine, or also by reacting with hypochlorous acid. Such procedures are not only energy intensive, but also require a large land footprint, generate higher amount of effluent, and incur high equipment cost, including both CAPEX and OPEX, making it economically unattractive and also detrimental to the environment.
Further, vinyl chloride monomer (VCM) plants generate a huge amount of chlorinated hydrocarbon as a waste due to uncontrolled radical chlorination of ethylene. Conventionally, the chlorinated hydrocarbon is incinerated, after the recovery of a reasonable amount of light chlorinated hydrocarbon liquid which can be reused as solvent. The conventional incineration of the chlorinated hydrocarbon, is performed at relatively high temperatures of around 1450 °C, to yield carbon dioxide and hydrochloric acid. Not only does the incineration process consume high energy but it is also responsible for environmental pollution due to emission of carbon dioxide and volatile organic compounds (VOCs) namely dioxane.
The present disclosure provides a hydrophobic carbonaceous material and the process for its preparation. The process is simple, environment-friendly and economical that provides hydrophobic carbonaceous material with desired hydrophobicity and physical characteristics. The process also converts effluent waste to a highly valuable material.
In an aspect, the present disclosure provides a process for preparing a hydrophobic carbonaceous material from chlorinated hydrocarbon. The process comprises introducing a chlorinated hydrocarbon in a reactor.
The chlorinated hydrocarbon has chlorine content in the range of 45 wt.% to 55 wt. %. In an embodiment, the chlorinated hydrocarbon has chlorine content of 53.4 wt.%.
In an embodiment, the chlorinated hydrocarbon is obtained from an industrial plant waste.
In an exemplary embodiment, the chlorinated hydrocarbon is obtained from vinyl chloride monomer plant. The chlorinated hydrocarbon is generated as a waste in vinyl chloride monomer plant, due to uncontrolled radical chlorination of ethylene. The conventional method of treating this waste involves high temperature incineration to carbon dioxide and hydrochloric acid, which not only requires high energy but also poses environmental hazards. The present method avoids high temperature incineration as well as generation of CO2, and converts effluent waste to a highly valuable product.
The chlorinated hydrocarbon is at least one selected from the group consisting of ethylene dichloride, 1,1,2-trichloroethane, 1,1,2,2,-tetrachloroethane and 1,1,1,2,2-pentachloroethane. In an embodiment, the chlorinated hydrocarbon contains ethylene dichloride, 1,1,2-trichloroethane, 1,1,2,2,-tetrachloroethane and 1,1,1,2,2-pentachloroethane.
In an embodiment, the chlorinated hydrocarbon comprises ethylene dichloride in an amount in the range of 5 wt.% to 15 wt.%, 1,1,2- trichloro ethane in an amount in the range of 5 wt.% to 10 wt.%, 1,1,2,2-tetrachloroethane in an amount in the range of 1 wt.% to 10 wt.% and 1,1,1,2,2-pentachloroethane in an amount in the range of 0.5 wt.% to 5 wt.%. In an exemplary embodiment, the chlorinated hydrocarbon comprises ethylene dichloride in an amount of 10 wt.%, 1,1,2- trichloro ethane in an amount of 7 wt.%, 1,1,2,2-tetrachloroethane in an amount of 4 wt.% and 1,1,1,2,2-pentachloroethane in an amount of 1 wt.%.
In an embodiment, the chlorinated hydrocarbon further comprises long-chain chlorinated hydrocarbons.
The reactor is any one selected from continuous type reactor, fixed bed type reactor, autoclave, rotary scraper type reactor, rotary cone type reactor with fixed scraper, kneader type reactor and multiple vessel type reactor.
The chlorinated hydrocarbon is heated to a temperature in the range of 140 °C to 150 °C, at a first predetermined rate, to obtain a heated mixture. A catalyst is added to the heated mixture to obtain a reaction mixture.
The first predetermined rate of heating is in the range of 1 °C/min to 5 °C/min. In an embodiment, the first predetermined rate of heating is 2 °C/min.
The catalyst is a Lewis acid selected from the group consisting of AlCl3, GaCl3, InCl3, FeCl3, CrCl3, ZrCl2, MoCl6, and SnCl4. In an embodiment, the catalyst is AlCl3.
The catalyst is added in an amount in the range of 1 wt.% to 5 wt.% with respect to the chlorinated hydrocarbon. In an embodiment, the catalyst is added in an amount of 3 wt.% with respect to the chlorinated hydrocarbon.
Further, the reaction mixture is heated to a temperature in the range of 240 °C to 260 °C, at a second predetermined rate, to obtain gaseous hydrogen chloride (HCl) and a crude solid product.
The second predetermined rate of heating is in the range of 1 °C/min to 5 °C/min. In an embodiment, the second predetermined rate of heating is 4 °C/min.
The step of heating the reaction mixture is carried out for a time period in the range of 60 minutes to 300 minutes. In one embodiment, the time period is 90 minutes. In another embodiment, the time period is 240 minutes.
The addition of the catalyst to the heated mixture ensures effective catalytic activity.
The reaction mixture when heated, in the presence of the catalyst, at the second predetermined rate leads to dehydrochlorination of chlorinated hydrocarbon, as evident by the liberation of HCl gas. The HCl gas also catalyzes the dehydrochlorination reaction. The chlorinated hydrocarbon, post dehydrochlorination, undergoes carbonization via subsequent increase in the chain length, followed by cyclization and/or aromatization, to form the hydrophobic carbonaceous material.
Further, the crude solid product is purified to obtain the hydrophobic carbonaceous material.
The step of purification comprises cooling the crude solid product to a temperature in the range of 80 °C to 100 °C, and mixing with at least one fluid medium at a temperature in the range of 80 °C to 100 °C, for a time period in the range of 5 minutes to 50 minutes, followed by filtration to obtain the hydrophobic carbonaceous material.
The step of purification of the crude solid product enables to remove the organic impurities present therein.
In an exemplary embodiment, the crude solid product is cooled to 90 °C, and mixed with a fluid medium at 90 °C, for 30 minutes, followed by filtration to obtain the hydrophobic carbonaceous material.
The fluid medium is selected from the group consisting of toluene, dichloromethane, water and mixtures thereof.
In an embodiment, the step of purification is reiterated for effective removal of soluble organic impurities present in the crude solid product. In an exemplary embodiment, the step of purification is carried out by cooling the crude solid product to 90 °C, and mixing with toluene at 90 °C for 5 minutes, followed by filtration, wherein this step is repeated three times with toluene and then three times with water, to obtain the hydrophobic carbonaceous material.
The hydrophobic carbonaceous material is dried at a temperature in the range of 90 °C to 120 °C, for a time period in the range of 1 hour to 5 hours. In an exemplary embodiment, the hydrophobic carbonaceous material is dried in an oven at 110 °C, for 4 hours.
The gaseous hydrogen chloride (HCl) is separated from the solid product, prior to the step of purification. In an embodiment, the separated hydrogen chloride is recycled to a vinyl chloride monomer plant.
In an exemplary embodiment, a chlorinated hydrocarbon is introduced in a reactor. The chlorinated hydrocarbon is heated to 150 °C, at 2 °C/min, to obtain a heated mixture. Aluminium chloride is added as catalyst to the heated mixture to obtain a reaction mixture. The reaction mixture is heated to 250 °C, at 4°C/min, to obtain gaseous hydrochloric acid and a crude solid product. The crude solid product is purified by cooling to 90 °C, and mixing with at least one fluid medium at 90 °C, for 30 minutes, followed by filtration to obtain hydrophobic carbonaceous material.
In another aspect, the present disclosure provides a hydrophobic carbonaceous material, characterized by having chlorine content in the range of 20 wt.% to 30 wt.%, contact angle with water in the range of 95° to 120°, surface area in the range of 150 m2/g to 400 m2/g, pore volume in the range of 0.15 cm3/g to 0.30 cm3/g, and pore diameter in the range of 2.5 nm to 4.5 nm.
In an exemplary embodiment, the hydrophobic carbonaceous material is characterized by having chlorine content of 29 wt.%, surface contact angle of 115°, surface area of 161 m2/g, pore volume of 0.16 cm3/g, and pore diameter of 2.9 nm.
The hydrophobic carbonaceous material has a storage modulus in the range of 9.5 x109 Pa to 9.9 x109 Pa. The storage modulus of the hydrophobic carbonaceous material of the present disclosure is comparable to carbon nanotubes.
The hydrophobic carbonaceous material has potential applications in many significant areas such as a polymer additive with relatively better corrosion resistivity, fire retardant properties, antismoke properties, relatively lower bacterial growth and high barrier properties. Further, the hydrophobic carbonaceous material is also suited for electrical applications including capacitors (super/pseudo), electrical double layers (EDL) or as adsorbing agents for chemical components from bulk mixture, for water purification by removal of contaminants, as transport barriers for drug delivery or as a solid support or binder to a catalyst.
In an embodiment, the hydrophobic carbonaceous material has an ability to adsorb organic compounds selected from the group consisting of 1,2-dichloroethane, n-nonane, ethyl benzene, monoethylene glycol, acetic acid, benzoic acid, phenol and toluene.
The adsorption capacity of the hydrophobic carbonaceous material for the organic compound is in the range of 0.01 to 4 g/g of the organic compound with respect to the carbonaceous material. In an exemplary embodiment, the adsorption capacity is 3g/g of the organic compound with respect to the carbonaceous material.
The present disclosure thus provides a simple and economical process to obtain the hydrophobic carbonaceous material. The hydrophobic carbonaceous material has desired characteristics such as relatively high hydrophobicity without the need for an additional step of halogenation as required conventionally. Further, the process of the present disclosure converts the chlorinated hydrocarbon, obtained as a byproduct or waste from industrial processes, particularly vinyl chloride monomer plant, into highly valuable hydrophobic carbonaceous material, thereby making the process environment friendly and economical.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment, but, are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following laboratory scale experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. These laboratory scale experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial/commercial scale.
Experimental Details
Example 1: Preparation of hydrophobic carbonaceous material (Sample 1)
Chlorinated hydrocarbon (100 g) having chlorine content of 53.4 wt%, obtained from vinyl chloride monomer plant was taken in a vessel container equipped with a heater. The chlorinated hydrocarbon was heated to 150 °C, at a rate of 2 °C/min, to obtain a heated mixture. Aluminium chloride (AlCl3) catalyst (3 g) was slowly added to the heated mixture to obtain a reaction mixture. The reaction mixture was heated to attain a temperature upto 250 °C, at a rate of 4°C/min, to obtain gaseous hydrochloric acid and a crude solid product. The total reaction time was 90 minutes. Hydrogen chloride gas was liberated initially slowly and then faster which finally diminished gradually. The liberation of HCl gas was confirmed by ammonia torch and Congo red paper test. The gaseous HCl was separated from the crude solid product. The crude solid product was purified by cooling to 90 °C and mixing with toluene (60 mL) at 90 °C, for 5 minutes, followed by filtration. This step of purification (mixing with solvent and filtration) was repeated two more times with toluene (120 mL), and then three times with water (180 mL) to obtain hydrophobic carbonaceous material, wherein it was observed that the color of the toluene layer becomes brown to colorless. The hydrophobic carbonaceous material was dried in an oven at 110?C for 4 hours.
Example 2: Preparation of hydrophobic carbonaceous material (Sample 2)
The procedure as given in Example 1 was repeated, except that the reaction time was 240 minutes instead of 90 minutes, wherein the rate of heating the reaction mixture, to attain a temperature upto 250 °C, was maintained at 3°C/min.
Example 3: Preparation of hydrophobic carbonaceous material (Sample 3)
The procedure as given in Example 1 was repeated, except that the experiment was performed in an autoclave, for 25 g of chlorinated hydrocarbon, and the heating was done at 200?C for 4 hours.
The chlorinated hydrocarbon used in each of the examples (1-3) contains the components as provided in Table 1.
Table 1: Composition of the chlorinated hydrocarbon used in Examples 1-3
Sr. No. Chlorinated hydrocarbon Amount of each component (in wt.%)
1 Ethylene dichloride 10
2 1,1,2- trichloro ethane 7
3 1,1,2,2-tetrachloroethane 4
4 1,1,1,2,2-pentachloroethane 1
5 Unknown heavy hydrocarbons (mixtures of long chain hydrocarbons containing chlorine) 78
Characterization and measurement of physical properties:
The samples 1-3, as obtained from examples 1-3 respectively, were subjected to measurement of chlorine content, contact angle with water, surface area, pore volume and pore diameter, as illustrated in Table 2. Chlorine content was measured by Oxygen flask method IS 15778-2007, contact angle was measured by water contact angle measurement as per ASTM D5946 and surface area, pore volume and pore diameter were measured as per standard BET method.
Table 2: Measurement of physical properties
Sample number Chlorine content (Wt%) Contact Angle (oC) Surface Area (BET) (m2/g) Pore Volume (cm3/g) Pore diameter (nm)
Sample 1 29.74 115 161.6467 0.164 2.9
Sample 2 26.96 101 380.3068 0.281 3.6
Sample 3 26.24 98 331.7382 0.245 4.2
As observed in Table 2, the sample 1 has relatively higher chlorine content than samples 2 and 3 that leads to increase in hydrophobicity which is evident from the increase in the contact angle. A direct relation between the contact angle and the chlorine content is as illustrated in Figure 1. With increase in the number of halogen atoms attached with the carbon, a relatively greater surface negative charge is also generated. The negative nature of water dipole causes repulsion with the carbonaceous material, thus making the material to be hydrophobic in nature. This primarily indicates that the increased chlorine content could be the reason for hydrophobicity. The process of the present disclosure thus provides a scope to obtain a carbonaceous material with desired hydrophobicity that is controlled by adjusting the chlorine content of the respective samples.
Fourier Transform Infra-red spectroscopy (FTIR)
The sample 1 was subjected to FTIR measurements, and the corresponding FTIR spectrum obtained (in transmittance mode) is as shown in Figure 2. The FTIR spectrum of the sample 1 exhibits bands at 1437 and 1596 cm-1, which correspond to the aromatic ring C-C stretching vibration bands. The presence of aromatic C-C stretching bands indicates that aromatic structures are formed by cyclization of unsaturated hydrocarbon chain formed by repeated addition of carbon units via carbonization.
Dynamic mechanical analysis
The sample 1 was subjected to dynamic mechanical analysis (DMA), and the resulting data is as shown in Figure 3. The DMA curve of sample 1 exhibits a storage modulus values 9.86 x109 Pa. This value of storage modulus is characteristic of carbon nanotube material.
Adsorption capacity:
The adsorption capacity of the sample 2 was tested. 110 mg of sample 2 having 27 wt.% chlorine content, was taken in 5 mL of the organic compound (liquid) and stirred for 3 hours to obtain a mixture. The mixture was filtered through Whatman 42 followed by suction drying to obtain sample 1 with the adsorbed organic compound. The adsorption capacity of the carbonaceous material for different organic compounds, as tested in individual experiments, is as illustrated in Table 3.
The adsorption capacity (Qs) was calculated using the following equation:
wherein Qs is the adsorption capacity (g/g);
mst is the weight of fully saturated carbonaceous material (after adsorption); and
mo is the weight of the dry carbonaceous material (before adsorption).
Table 3: Adsorption capacity of hydrophobic carbonaceous material (sample 2)
Sr. No. Component Absorption capacity (g/ g of carbon)
1 1,2-Dichloro ethane (EDC) 1.05
2 n-Nonane 1.8
3 Ethyl Benzene 3.15
4 Mono ethylene glycol(MEG) 3.31
5 Acetic acid 3.58
6 Benzoic acid 0.3
7 Phenol 0.03
8 Toluene 1.38
As observed in Table 3, the carbonaceous material (sample 2) shows relatively high absorptivity for aromatic hydrocarbons such as ethyl benzene as well as glycols/carboxylic acid derivatives.
The present disclosure relates to a simple and economical process to obtain a hydrophobic carbonaceous material having desired characteristics such as relatively high hydrophobicity without the need for an additional step of halogenation as required conventionally. Further, the process of the present disclosure converts chlorinated hydrocarbons obtained from industrial waste, particularly vinyl chloride monomer plant, into highly valuable hydrophobic carbonaceous material, thereby making the process environment friendly and economical.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of a process for preparing a hydrophobic carbonaceous material, wherein the process:
• is simple and economical;
• provides hydrophobic carbonaceous material with relatively high hydrophobicity without the need for an additional step of halogenation; and
• converts chlorinated hydrocarbons obtained from industrial waste, particularly vinyl chloride monomer plant waste into highly valuable hydrophobic carbonaceous material, thus making the process environment friendly.
The embodiments herein and the various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein 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 examples should not be construed as limiting the scope of the embodiments herein.
The foregoing description of the specific embodiments so fully 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 herein 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.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results.
Any discussion of documents, acts, materials, devices, articles or 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.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the disclosure, unless there is a statement in the specification specific to the contrary.
While considerable emphasis has been placed herein on the components and component parts of the preferred embodiments, it will be appreciated that many embodiments 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 changes in the preferred embodiment as well as other embodiments of the disclosure 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. A process for preparing hydrophobic carbonaceous material from chlorinated hydrocarbon, said process comprising the following steps:
(i) introducing chlorinated hydrocarbon in a reactor;
(ii) heating the chlorinated hydrocarbon to a temperature in the range of 140 °C to 150 °C, at a first predetermined rate, to obtain a heated mixture;
(iii) adding a catalyst to the heated mixture to obtain a reaction mixture;
(iv) heating the reaction mixture to a temperature in the range of 240 °C to 260 °C, at a second predetermined rate, to obtain gaseous hydrogen chloride (HCl) and a crude solid product; and
(v) purifying the crude solid product to obtain hydrophobic carbonaceous material.
2. The process as claimed in claim 1, wherein the chlorinated hydrocarbon is at least one selected from the group consisting of ethylene dichloride, 1,1,2-trichloroethane, 1,1,2,2,-tetrachloroethane and 1,1,1,2,2-pentachloroethane.
3. The process as claimed in claim 1, wherein the chlorinated hydrocarbon has chlorine content in the range of 45 wt.% to 55 wt. %.
4. The process as claimed in claim 1, wherein the chlorinated hydrocarbon is obtained from an industrial plant waste, particularly vinyl chloride monomer plant.
5. The process as claimed in claim 1, wherein the catalyst is a Lewis acid selected from the group consisting of AlCl3, GaCl3, InCl3, FeCl3, CrCl3, ZrCl2, MoCl6, and SnCl4.
6. The process as claimed in claim 1, wherein the catalyst is added in an amount in the range of 1 wt.% to 5 wt.% with respect to the chlorinated hydrocarbon.
7. The process as claimed in claim 1, wherein the first predetermined rate of heating and the second predetermined rate of heating are independently in the range of 1 °C/min to 5 °C/min.
8. The process as claimed in claim 1, wherein the step (iv) of heating the reaction mixture is carried out for a time period in the range of 60 minutes to 300 minutes.
9. The process as claimed in claim 1, wherein the step (v) of purification comprises cooling the crude solid product to a temperature in the range of 80 °C to 100 °C, and mixing with at least one fluid medium at a temperature in the range of 80 °C to 100 °C, for a time period in the range of 5 minutes to 50 minutes, followed by filtration to obtain the hydrophobic carbonaceous material.
10. The process as claimed in claim 9, wherein the fluid medium is selected from the group consisting of toluene, dichloromethane, water and mixtures thereof.
11. The process as claimed in claim 1, wherein the step (v) of purification is reiterated.
12. The process as claimed in claim 1, wherein the gaseous hydrogen chloride is separated from the crude solid product, prior to step (v) of purification.
13. The process as claimed in claim 1, wherein the hydrophobic carbonaceous material is dried at a temperature in the range of 90 °C to 120 °C, for a time period in the range of 1 hour to 5 hours.
14. A hydrophobic carbonaceous material, characterized by having chlorine content in the range of 20 wt.% to 30 wt.%, contact angle with water in the range of 95° to 120°, surface area in the range of 150 m2/g to 400 m2/g, pore volume in the range of 0.15 cm3/g to 0.30 cm3/g, and pore diameter in the range of 2.5 nm to 4.5 nm.
15. The material as claimed in claim 14, characterized by having chlorine content of 29 wt.%, contact angle with water of 115°, surface area of 161 m2/g, pore volume of 0.16 cm3/g, and pore diameter of 2.9 nm.
16. The material as claimed in claim 14, having an ability to adsorb organic compounds selected from the group consisting of 1,2-dichloroethane, n-nonane, ethyl benzene, monoethylene glycol, acetic acid, benzoic acid, phenol and toluene.
17. The material as claimed in claim 16, having an adsorption capacity in the range of 0.01 to 4 g/g of said organic compound with respect to the material.
| # | Name | Date |
|---|---|---|
| 1 | 201821032400-STATEMENT OF UNDERTAKING (FORM 3) [29-08-2018(online)].pdf | 2018-08-29 |
| 2 | 201821032400-PROVISIONAL SPECIFICATION [29-08-2018(online)].pdf | 2018-08-29 |
| 3 | 201821032400-PROOF OF RIGHT [29-08-2018(online)].pdf | 2018-08-29 |
| 4 | 201821032400-POWER OF AUTHORITY [29-08-2018(online)].pdf | 2018-08-29 |
| 5 | 201821032400-FORM 1 [29-08-2018(online)].pdf | 2018-08-29 |
| 6 | 201821032400-DRAWINGS [29-08-2018(online)].pdf | 2018-08-29 |
| 7 | 201821032400-DECLARATION OF INVENTORSHIP (FORM 5) [29-08-2018(online)].pdf | 2018-08-29 |
| 8 | 201821032400-Proof of Right (MANDATORY) [23-03-2019(online)].pdf | 2019-03-23 |
| 9 | 201821032400-ENDORSEMENT BY INVENTORS [29-08-2019(online)].pdf | 2019-08-29 |
| 10 | 201821032400-DRAWING [29-08-2019(online)].pdf | 2019-08-29 |
| 11 | 201821032400-COMPLETE SPECIFICATION [29-08-2019(online)].pdf | 2019-08-29 |
| 12 | 201821032400-FORM 18 [03-09-2019(online)].pdf | 2019-09-03 |
| 13 | 201821032400-REQUEST FOR CERTIFIED COPY [30-09-2019(online)].pdf | 2019-09-30 |
| 14 | 201821032400-Annexure [01-10-2019(online)].pdf | 2019-10-01 |
| 15 | 201821032400-FORM 3 [04-10-2019(online)].pdf | 2019-10-04 |
| 16 | 201821032400-CORRESPONDENCE(IPO)-(CERTIFIED COPY)-(4-10-2019).pdf | 2019-10-07 |
| 17 | 201821032400-ORIGINAL UR 6(1A) FORM 1-250319.pdf | 2020-01-07 |
| 18 | 201821032400-Information under section 8(2) [11-12-2020(online)].pdf | 2020-12-11 |
| 19 | 201821032400-FORM 3 [11-12-2020(online)].pdf | 2020-12-11 |
| 20 | 201821032400-PETITION UNDER RULE 137 [02-03-2021(online)].pdf | 2021-03-02 |
| 21 | 201821032400-FER_SER_REPLY [02-03-2021(online)].pdf | 2021-03-02 |
| 22 | 201821032400-CLAIMS [02-03-2021(online)].pdf | 2021-03-02 |
| 23 | 201821032400-PatentCertificate19-03-2021.pdf | 2021-03-19 |
| 24 | 201821032400-IntimationOfGrant19-03-2021.pdf | 2021-03-19 |
| 25 | 201821032400-RELEVANT DOCUMENTS [30-09-2021(online)].pdf | 2021-09-30 |
| 26 | 201821032400-FER.pdf | 2021-10-18 |
| 27 | 201821032400-RELEVANT DOCUMENTS [27-09-2022(online)].pdf | 2022-09-27 |
| 28 | 201821032400-RELEVANT DOCUMENTS [22-09-2023(online)].pdf | 2023-09-22 |
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