Title of Invention

IMPROVED PROCESS FOR MANUFACTURE OF FLUORINATED POLYETHYLENE

Abstract An 'improved process for manufacture of fluorinated polyethylene' in which the surface of hydrocarbon polymer is converted to fluorocarbon polymer by a process, which comprises of mixture of fluorine with inert gas nitrogen into reaction with solid polyethylene, firstly the polyethylene is cleaned so that it is free from lint and oil, the cleaned material is introduced into the chamber then this chamber is evacuated, thereafter, the fluorine and nitrogen gas is introduced into the chamber and this continued till the desired quality of the fluorination is obtained at the temperature of -10°c to 120°c, at last the chamber is purged with nitrogen to remove the traces of fluorine and 4 HF gas, the reaction of fluorination is as follows :-
Full Text FORM - 2
COMPLETE SPECIFICATION
1) "IMPROVED PROCESS FOR MANUFACTURE OF FLUORINATED POLYETHYLENE".
2) M/S. BLOOM PACKAGING PRIVATE LIMITED, (An Indian Joint Stock Company Registered under the companies Act, 1956) having its registered office at Readymoney Terrrace, 167 Dr. A.B. Road, Worll, MUMBAI- 400 018, Maharashtra, India.
The following specification particularly describes the nature of this invention & the manner In which It is performed:

The present invention relates to an 'Improved process for manufacture of fluorinated polyethylene'.
Presently the various containers used for packing of agrochemicals, petroleum oils, solvents and similar materials are conventionally made up of LDPE (Low Density Polyethylene ), HDPE (High Density Polyethylene), HMHDPE, PET (Polyethylene terephthalene), PTFE (Polytetrafluoroethylene) and other suitable and easily available materials. These containers are used for storing and packing of agrochemical formulations with or without hydrocarbon solvents. The various solvents commonly known as Xylene, C-9, Aromex, Benzene, Toluene, Cyclohexanone, Isopropyl alcohol (IPA), Renine, etc. are used in the preparation of finished goods which are used in household and agricultural purposes.
However, observation shows that these conventional containers have several disadvantages, some of which are mentioned below.
These containers, when filled with the required, chemicals or solvents, allow the solvent vapours to penetrate through them, in turn causing the permeation of solvents from the chemicals. This is due to permeability of solvent vapours and presence of non barrier properties of polyethylene.
Further, the above stated problem develops deficiency of wall buckling which later on results in leakage. This might even cause the chemical composition to change, In worst cases.

In conventional containers, the penetration of the solvents through the containers causes container softening and/or swelling.
The net weight of the product when packed does not remain the same after storage of the containers for a certain amount of time, due to the weight toss of the product on account of the leakage.
Moreover, active ingredients are lost and there is also a considerable amount of odour emission.
The present invention 'Improved process for manufacture of fluorinated polyethylene' has been developed with a goal to overcome the disadvantages of the conventional system and provide a better alternative.
The first objective of the present process is to make it impermeable to hydrocarbon solvent vapours, which should make the polyethylene containers suitable, safe and fit for use.
The second objective is to evade the development of deficiency of wall buckling which usually later on results In leakage.
Another objective is to maintain the hardness of the container and prevent softening and swelling of the container. .
The net weight of the product should also be maintained the same after storage of the containers even for a long time.

The loss of active ingredients as well as odour emission should be eliminated.
The present invention 'Improved process for manufacture of fluorinated polyethylene' will now be explained in detail as follows.
Fluorine is known to be a highly reactive gas. Fluorinating the compounds, materials and containers helps to form a good surface coating for polymer containers for Individual raw materials, synthetic substances, surfaces of synthetic substances and consumer goods.
in the present invention the surface of hydrocarbon polymer is converted to fiuorocarbon polymer by a process which comprises of bringing a mixture of fluorine with inert gas (N2) nitrogen into reaction with solid polyethylene. The fiuorocarbon polymers having chemical composition and physical properties very similar to those of PTFE can also be produced from the reaction of fluorine with polyethylene.
Nitrogen is the most suitable medium for the fluorinatlon with a fluorine source. It is economic and equally advantageous from the technical point of view.
In the present invention, fluorine concentration and reaction temperature are
two main factors. The chemical reaction can be accelerated by increasing the
concentration of reacting gas or by increasing the reaction temperature. The
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fluorinatlon of polyethylene is carried out by first cleaning the polyethylene material so that It is free from lint and oil. Thereafter the cleaned material Is introduced into the chamber, then this chamber is evacuated, thereafter the fluorine gas and nitrogen gas is Introduced Into the chamber and this Is

continued till the desired quality of the fluorlnation is obtained. The polymer surface has to be thoroughly cleaned otherwise during treatment with fluorine, above room temperature the polyethylene will ignite. The time of the treatment of surface will depend on the equipment used, surface to be treated, the concentration of the fluorine! used and the temperature. The level of fluorination depends on the reaction time of the container in the chamber or reactor in contact with fluorine and nitrogen gas. At last the chamber Is purged with nitrogen to remove the traces of fluorine and HF gas.
The reaction of fluorination is as given below:

The reaction between the fluorine and the polyethylene is accompanied by strict control of the heat if process is to be successfully operated. If the temperature Is not kept under control (maintained within the desired band), the reaction progresses in an uncontrolled manner and instead of an orderly simple substitution of fluorine for hydrogen, many other undesired reactions might occur. As a result the polymer will be degraded. An increasing proportion of short chain polyfluoroaikanes is formed, in the extreme case the polymer is observed to burn in the fluorine and excessive local heating may lead to charring.

The reaction must be carried out under sub-atmospheric condition. This Is done so that in case of any leak occurred it would be from outside in instead of inside out, therefore handling of process is safe.
The fiuorination can take place between temperature range - 10 to 120 ° C. The temperature range mentioned is, of course, the general temperature prevailing In the reaction vessel, the local temperature at the actual points of reaction will temporarily be much higher. The proper reaction temperature must be selected to have better fiuorination. Therefore the present invention is to ensure the manufacture of a uniform fluorinated polyethylene material, blanks, synthetic substances and surfaces of synthetic substances. The penetration depth of the fluorinated surface layer must be controlled by correct selection of suitable process variables.
The fiuorination process Includes the circulation of gases in the reactor through heat exchanger. The controlling media used in the heat exchanger is water at 75 to 100 ° C. The advantage of circulation is that fluorine goes to all corners of the reactor and reacts with both inside and outside surfaces.
The present invention 'Improved process for manufacture of fluorinated polyethylene' has many advantages some of which are mentioned in the paragraphs that follow.
The fiuorocarbon coating produced In the container Increases the thermal stability of the surface of the container.

It aiso increases the resistance of the poiymer surfaces to soivents and corrosive chemicais.
The present process improves friction and wear properties of the poiymer surfaces.
The polyethylene obtained by following the said process is solvent resistant and permeation resistant coating on poiymer surface which also exhibit a high barrier for solvent vapours permeability, it also gives uniform and beautiful fluorination of materials and blanks.
The present process reduces the permeation of solvents from the chemicais.
It also avoids container softening and / or swelling.
The present process reduces product weight loss, so the net weight of the product remains almost the same even after a long storage time.
It also reduces odour emission and active ingredient loss.
Aggressive chemicals such as petrochemicals, solvents, Industrial formulations can be packed in fiuorinatad containers and still retain their original composition.

WE CLAIM :-
1) An 'improved process for manufacture of fluorinated polyethylene' in which the
surface of hydrocarbon polymer is converted to fluorocarbon polymer by a
process, which comprises of mixture of fluorine with inert gas nitrogen into
reaction with solid polyethylene, firstly the polyethylene is cleaned so that it is
free from lint and oil, the cleaned material is introduced into the chamber then
this chamber is evacuated, thereafter, the fluorine and nitrogen gas is introduced
into the chamber and this continued till the desired quality of the fluorination is
obtained at the temperature of -10°c to 120°c, at last the chamber is purged with
nitrogen to remove the traces of fluorine and 4 HF gas, the reaction of
fluorination is as follows :-

2) The process as claimed in claim (1) in which the fluorine concentration and reaction temperature are two main factors. The reaction can accelerated by increasing the concentration or reaction temperature;
3) The process as claimed in claim 1 and 2 in which time of reaction depend upon the equipment used, surface to be treated concentration of fluorine used and temperatures;
4) The process as claimed in claim 1, 2 and 3 which is accompanied by strict control of the heat otherwise many other undesired reaction might occur as result polymer will be degraded;
5) The process claimed in claim 1 to 4 in which the reaction must be carried out under sub-atmospheric condition. This is done so that in case of any leak occurred it would be from outside in instead of inside out, therefore handling of process is safe,

6) The process claimed in claim 1 to 6 in which the fluorination can take place between temperature ranges 100°c to 120 ° C, the temperature range mentioned is the general temperature prevailing in the reaction vessel, the local temperature at the actual points of reaction will temporarily be much higher;
7) The process claimed in claim 1 to 7 in which the fluorination process includes the circulation of gases in the reactor through heat exchanger, the controlling media used in the said heat exchanger is water at 75 to 100 o C.
Dated 30TH DAY OF JUNE 2003,
Signature
MR. JOSEPH VARIKASERY OF VARIKASERY & VARIKASERY
Agent for the applicant

Documents:

728-mum-2003-cancelled pages(17-12-2004).pdf

728-mum-2003-claims(granted)-(17-12-2004).doc

728-mum-2003-claims(granted)-(17-12-2004).pdf

728-mum-2003-correspondence(18-12-2004).pdf

728-mum-2003-correspondence(ipo)-(23-01-2004).pdf

728-mum-2003-form 1(05-11-2004).pdf

728-mum-2003-form 19(21-07-2003).pdf

728-mum-2003-form 2(granted)-(17-12-2004).doc

728-mum-2003-form 2(granted)-(17-12-2004).pdf

728-mum-2003-form 3(25-08-2003).pdf

728-mum-2003-power of attorney(21-07-2003).pdf


Patent Number 207050
Indian Patent Application Number 728/MUM/2003
PG Journal Number 30/2007
Publication Date 27-Jul-2007
Grant Date 21-May-2007
Date of Filing 21-Jul-2003
Name of Patentee M/S. BLOOM PACKAGING PRIVATE LIMITED
Applicant Address READYMONEY TERRACE, 167 DR. A.B. ROAD, WORLI, MUMBAI - 400 018, MAHARASHTRA, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 PRADEEP SAGAR READYMONEY TERRACE, 167 DR. A.B. ROAD, WORLI, MUMBAI - 400 018, MAHARASHTRA, INDIA
PCT International Classification Number N/A
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA