FORM-2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See Section 10; rule 13)
POLYMERIZATION OF HYDROCARBONS
RELIANCE INDUSTRIES LIMITED
an Indian Company
of 3rd Floor, Maker Chamber-IV, 222, Nariman Point,
Mumbi-400 021, Maharashtra, India.
Inventors (l)JASRA RAKSHVIR; (2) INGLE NINAD DEEPAK (3) KAPADIA PRADEEP PARESH; (4) MUNSHI PRADIP
THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE NATURE OF THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED.
This application is a Divisional Patent Application to the Indian Patent Application No.3049/MUM/2012 filed on 18th October, 2012 the entire contents of which are specifically incorporated herein by reference.
FIELD OF THE DISCLOSURE
The present invention relates to polymerization of hydrocarbons.
BACKGROUND:
Polymerization is a process of reacting monomer molecules together in a chemical reaction
to form linear chains or a three-dimensional network of polymer chains. Conventional
processes for the polymerization includes radical polymerization, cationic polymerization,
anionic polymerization, photo-irradiation polymerization and coordination catalytic
polymerization
In general, photo-irradiation polymerization process utilizes UV light emitted by various sources such as a filament-based lamp, vapor/gas-based lamp and the like. However, the filament-based or vapor/gas-based lamp used as a source of UV light emits defused or multi- r directional UV light that exhibits a high rate of intensity decay with distance. Therefore, these lamps are incapable of inducing effective reactions which further lead to consumption of high amount of electrical power. Additionally, these lamps are bulky and have a short life period (8000-15000 hours).
Further, the use of such light sources may cause short and long term health hazards by way of scattered UV radiations in the immediate environment. Furthermore, reaction vessels made of quartz make the chemical process and its apparatus expensive.
Thus, there is a need for a novel and economic process for polymerization of hydrocarbons. Further, there is also a need for an apparatus which will utilize low-intensity solid state lights for polymerization of hydrocarbons. OBJECTS
Some of the objects of the system of the present disclosure, which at least one embodiment discussed herein satisfies, are as follows:
It is an object of the present disclosure to ameliorate one or more problems of the state-of-the-art or at least provide a useful alternative.
•It is an object of the present disclosure to provide a process for polymerization of hydrocarbons which is economic.
It is another object of the present disclosure to provide a process for polymerization of hydrocarbons which is environmentally safe.
It is a still another object of the present disclosure to provide a process for polymerization of hydrocarbons which utilizes light emitting diodes as a source of visible light. It is a still another object of the present invention to provide a process for polymerization of hydrocarbons without addition of an additive like swelling and dispersing agents. It is a further object of the present disclosure to provide an apparatus for polymerization of hydrocarbons.
It is still a further object of the present disclosure to provide an apparatus for polymerization of hydrocarbons which is energy efficient and economic.
It is even a further object of the present disclosure to provide an apparatus for polymerization of hydrocarbons which is easy to handle.
SUMMARY
In accordance with one aspect of the present disclosure there is provided a process for polymerization of a hydrocarbon; said process comprising the following steps: i. introducing the hydrocarbon in a reaction vessel; ii. introducing at least one photo-initiator in the reaction vessel; iii. agitating the hydrocarbon and the photo-initiator in the reaction vessel for a
predetermined time period; iv. establishing an inert atmosphere in the reaction vessel in which the hydrocarbon
and the photo-initiator is being agitated; and v. passing visible light emitted by a light source into the reaction vessel for a predetermined time period to obtain a polymerized hydrocarbon.
Typically, the hydrocarbon is at least one monomer selected from the group consisting of
isoprene, acrylic acid alcohol, epoxide, hydroxyacid, lactum and vinyl monomers.
Typically, the hydrocarbon is introduced in the reaction vessel in the form of a slurry or a
solution.
Typically, the method step of agitation is carried out with the help of a rotating stirrer at speeds ranging from 200 to 850 rpm for a time period of 5 to 60 minutes.
Typically, the photo-initiator is at least one peroxide selected from the group consisting of hydrogen peroxide, benzoyl peroxide t-butylhydroperoxide, per-benzoic acid and per-acetic acid.
Typically, the light source is at least one solid state light emitting device selected from the group consisting of Light Emitting Diodes (LEDs), LASER, Organic Electroluminescence material, T Inorganic Electroluminescence, Organic Light Emitting Diodes and Inorganic Light emitting ^ Diodes. (
Typically, the amount of the photo-initiator is in the range of 20 to 800 ppm.
Typically, the visible light is characterized by wavelength of 390 to 780 nm and said light is passed into the reaction vessel for a time period of 2 to 12 hours.
Typically, a light source from which light is passed is placed on at least one location selected -from the group consisting of outside the reaction vessel, inside the reaction vessel and embedded on the walls of the reaction vessel.
Typically, the light source from which light is passed is placed outside the reaction vessel at a distance of 0.2 to 12 cm from the exterior wall of the reaction vessel, preferably at a distance of 0.5 to 4 cm.
Typically, the step of passing light includes guiding the beam, of light to a reaction zone in the reaction vessel in which the process is taking place.
The process of the present disclosure also includes the step of heating the agitating hydrocarbon in the inert atmosphere at a temperature in the range of 40 to 90°C before executing step (v).
In accordance with another aspect of the present disclosure there is provided an apparatus for polymerization of a hydrocarbon, said apparatus comprising a reaction vessel, a purging means to purge fluid into said reaction vessel, a centrally mounted stirrer and a light source.
The apparatus of the present disclosure further includes guiding means to guide the light to a reaction zone of the reaction vessel.
Typically, the light source is at least one solid state light emitting device selected from the group consisting of Light Emitting Diodes (LEDs), LASER, Organic Electroluminescence material, Inorganic Electroluminescence, Organic Light Emitting Diodes and Inorganic Light emitting Diodes.
Typically, the light source from which the light having wavelength of 390 to 780 nm is passed, is placed on at least one location selected from the group consisting of outside the reaction vessel, inside the reaction vessel and embedded on the walls of the reaction vessel.
Typically, the light source is placed at a distance of 0.2 to 12 cm from the exterior wall of the reaction vessel, preferably at a distance of 0.5 to 4cm.
Typically, the reaction vessel is glass walled and transparent.
DETAILED DESCRIPTION:
In accordance with the present disclosure there is provided a process for polymerization of a hydrocarbon. The process involves the, following steps:
In the initial step, a hydrocarbon and a photo-initiator is introduced into a reaction vessel and then agitated for a predetermined period of time. Non limiting examples for hydrocarbons used in accordance with the present disclosure include isoprene, acrylic acid alcohol, epoxide, hydroxyacid, lactum and vinyl monomers.
Typically, photo-initiator includes one or more peroxides selected from the group consisting of hydrogen peroxide, benzoyl peroxide t-butylhydroperoxide, perbenzoic acid and peracetic acid
In accordance with the present disclosure the method step of agitation is carried out at a speed ranging from 200 to 850 rpm for a period of 5 to 60 minutes.
In accordance with one embodiment of the present disclosure hydrocarbon is in the form of slurry.
In the next step, an inert atmosphere is established in the reaction vessel by purging an inert gas and subsequently, a visible light is passed for a period of 2 to 12 hours into the reaction vessel to obtain the polymerized hydrocarbon. In accordance with one embodiment, nitrogen gas is purged to establish the inert atmosphere in the reaction vessel.
In accordance with the present disclosure the hydrocarbon is heated at a temperature of 40 to 90°C before passing the visible light into the reaction vessel.
The light source, from which the visible light of wavelength 390 to 780 nm is emitted, is a bank of solid state light emitting devices. Non limiting examples of the solid state light emitting devices includes Light Emitting Diodes (LEDs), LASER, Organic Electroluminescence material, Inorganic Electroluminescence, Organic Light Emitting Diodes and Inorganic Light emitting Diodes.
The light source is placed on at least one location selected from the group consisting of outside the reaction vessel, inside the reaction vessel and embedded on the walls of the reaction vessel. The distance between the exterior wall of the reaction vessel and the light source, placed outside the reaction vessel is in the range of 0.2 to 12 cm, preferably at a distance of 0.5 to 4cm The step of passing light from light source placed outside the reaction vessel includes guiding the beam of light to a reaction zone of reaction vessel in which the process is taking place. In accordance with the present disclosure there is also provided an apparatus for polymerization of hydrocarbons. The apparatus includes a reaction vessel, purging means to purge fluid into the reaction vessel, a centrally mounted stirrer and a light source. The apparatus of the present discloser also includes guiding means to guidcthe light from the light source to a reaction zone in the reaction vessel. The guiding means includes but is not limited to waveguide, lens and set of lenses.
The light source, from which the visible light of wavelength 390 to 780 nm is emitted, is a bank of solid state light emitting devices. Non limiting examples of the solid state light emitting devices includes Light Emitting Diodes (LEDs), LASER, Organic Electroluminescence material,
Inorganic Electroluminescence, Organic Light Emitting Diodes, Inorganic Light emitting Diodes and combinations thereof.
In accordance with the present disclosure the light source is placed on at least one location selected from the group consisting of outside the reaction vessel, inside the reaction vessel and embedded on the walls of the reaction vessel.
The distance between the exterior wall of the reaction vessel and the bank of LEDs placed outside the reaction vessel is in the range of 0.2 to 12 cm, preferably at a distance of 0.5 to 4cm. Typically, the reaction vessel is glass walled and transparent.
Hereinafter, the present disclosure will be described in more detail with reference to the following examples, but the scope of the present disclosure is not limited thereto.
Example 1: Radical-initiated Polymerization Monomer
An aqueous solution of 10 ml of partially neutralized acrylic acid and 1.6g of benzoyl peroxide were added to a round bottom flask and continuously stirred using a magnetic stirrer. The temperature of the mixture was maintained at 50°C. Nitrogen gas was then purged in the round bottom flask for removing air or oxygen. Subsequently, the mixture was exposed to light emitted by one or more light emitting devices. The start time of reaction was noted from the time the mixture was exposed to the LED light having wavelength of 405nm. At the end of 4 hours, formation of polyacrylic acid was confirmed by Nuclear Magnetic Resonance (NMR) and Gel Permeation Chromatography (GPC).
Example 2: Radical-initiated Polymerization of an Unsaturated Hydrocarbon 10ml of isoprene, 50ml toluene and 1ml hydrogen peroxide were added to a round bottom flask and continuously stirred using a magnetic stirrer. The temperature of the mixture was maintained at 50°C. Nitrogen gas was then purged in the round bottom flask for removing air or oxygen. The mixture was exposed to light emitted by one or more light emitting devices. The start time of the reaction was noted from the time the mixture was exposed to the LED light having wavelength of 405nm. At the end of 4 hours, formation of poly-isoprene was confirmed.
Throughout this specification the word "comprise", or variations such as "comprises" or "comprising", 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.
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 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 pf the disclosure, unless there is a statement in the specification specific to the contrary.
We Claim:
1. A process for polymerization of a hydrocarbon; said process comprising the following steps:
i. introducing the hydrocarbon in a reaction vessel; ii. introducing at least one photo-initiator in the reaction vessel; iii. agitating the hydrocarbon and the photo-initiator in the reaction vessel for a
predetermined time period; iv. establishing an inert atmosphere in the reaction vessel in which the hydrocarbon and the photo-initiator is being agitated; and v. passing visible light emitted by a light source into the reaction vessel for a predetermined time period to obtain a polymerized hydrocarbon.
2. The process as claimed in claim 1, wherein the hydrocarbon is at least one monomer selected from the group consisting of isoprene, acrylic acid alcohol, epoxide, hydroxyacid, lactum and vinyl monomers.
3. The process as claimed in claim 1, wherein the hydrocarbon is introduced in the reaction vessel in the form of a slurry or a solution. .
4. The process as claimed in claim 1, wherein the method step of agitation is carried out with the help of a rotating stirrer at speeds ranging from 200 to 850 rpm for a time period of 5 to 60 minutes.
5. The process as claimed in claim 1, wherein the photo-initiator is at least one peroxide
selected from the group consisting of hydrogen peroxide, benzoyl peroxide t-
butylhydroperoxide, per-benzoic acid and per-acetic acid.
6. The process as claimed in claim 1, wherein the amount of the photo-initiator is in the range of 20 to 800 ppm.
7. The process as claimed in claim 1, wherein the light source is at least one solid state light emitting device selected from the group consisting of Light Emitting Diodes (LEDs), LASER, Organic Electroluminescence material, Inorganic Electroluminescence, Organic Light Emitting Diodes and Inorganic Light emitting Diodes.
8. The process as claimed in claim 1, wherein the visible light is characterized by wavelength of 390 to 780 nm and said light is passed into the reaction vessel for a time period of 2 to 12 hours.
9. The process as claimed in claim 1, wherein the light source from which light is passed is placed on at least one location selected from the group consisting of outside the reaction vessel, inside the reaction vessel and embedded on the walls of the reaction vessel.
10. The process as claimed in claim 1, wherein the light source from which light is passed is placed outside the reaction vessel at a distance of 0.2 to 12 cm from the exterior wall of the reaction vessel, preferably at a distance of 0.5 to 4 cm.
11. The process as claimed in claim 1, wherein the step of passing light includes guiding the beam of light to a reaction zone in the reaction vessel in which the process is taking place.
12. The process as claimed in claim 1, which includes the step of heating the agitating hydrocarbon in the inert atmosphere at a temperature in the range of 40 to 90°C before executing step (v).
13. An apparatus for polymerization of a hydrocarbon, said apparatus comprising a reaction vessel, a purging means to purge fluid into said reaction vessel, a centrally mounted stirrer and a light source.
14. The apparatus as claimed in claim 13, further includes guiding means to guide the light to a reaction zone of the reaction vessel.
15. The apparatus as claimed in claim 13, wherein the light source is at least one solid state light emitting device selected from the group consisting of Light Emitting Diodes (LEDs), LASER, Organic Electroluminescence material, Inorganic Electroluminescence, Organic Light Emitting Diodes and Inorganic Light emitting Diodes.
16. The apparatus as claimed in claim 13, wherein the light source from which the light having wavelength of 390 to 780 nm is passed placed on at least one location selected from the group consisting of outside the reaction vessel, inside the reaction vessel and embedded on the walls of the reaction vessel.
17. The apparatus as claimed in claim 13, wherein the light source is placed at a distance of 0.2 to 12 cm from the exterior wall of the reaction vessel, preferably at a distance of 0.5 to 4 cm.
18. The apparatus as claimed in claim 13, wherein the reaction vessel is glass walled and transparent.