DESC:FORM – 2

THE PATENTS ACT, 1970
(39 OF 1970)

COMPLETE SPECIFICATION
(Section 10, rule 13)

“A COMPOSITION AND PROCESS FOR PREPARATION OF PCR BOPET FILM”

SUMILON POLYESTER LIMITED
A Company Incorporated under the Indian Companies Act
Having address at
43 & 46/2, Village Versana, N.H.no-8A,
Gandhidham 370201, Gujarat, India

The following specification particularly describes the nature of these inventions:
FIELD OF INVENTION:
The present invention relates to a composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film. More particularly, the invention relates to improved a composition and process for preparation of PCR (post consumed recycle) biaxial oriented polyester film (BOPET) film using recycle material which is efficient and is eco-friendly.
BACKGROUND OF THE INVENTION
The widespread use of polymer-based products ("plastics") in consumer goods have lead to a corresponding interest in suitable methods for reclaiming or recycling as much of these products as is practical. The use of plastic products has increased significantly in the recent past, with many enterprises joining the industry and many more varieties of plastics being made. Companies consider plastics easier and cheaper to manufacture as compared to other materials such as metals and stones because they're produced from byproducts of crude oil and can be recycled. However, the wide use of plastic products has shortfalls and loss.
Disposable plastics used in packaging foodstuff meant for human consumption contain harmful compounds. Improper disposal of these packaging products leads to these harmful compounds finding their way to water bodies, where they dissolve over a long time due to their non-biodegradable nature. Most of these chemicals have not undergone an ecological risk appraisal, and their impact on human well-being and the environment is presently vague. One example is phthalates, which are used in the manufacture of PVC.
Said polymer-based products (plastic), packaging foils/ films/ containers, and paper that are used by the consumers and which are diverted from the landfill and utilized in the production of other commodities. Said waste of materials can be used for recycling process which is known as Post-Consumer recycled materials. The Post-Consumer recycled content is content created by consumers after a product has reached the end of its use. The benefit of using post-consumer content is it reuses refuse in the manufacture of goods, preventing items from ending up in the landfill or needing to rely on raw materials. An example of post-consumer content is aluminum cans. After a can has been bought at the store and has served its use, it is put in a recycling bin for collection. Once the can has been separated from the refuse along with other aluminum materials, it is then sent to a manufacturer where it is melted down and used in the creation of other aluminum products.
There are number of effort are been done of reduce the carbon foot print to protects the environment from the use of post consumed recycle material. The efforts of reducing the environmental effect of disposable plastics, many studies are been done. In more recent years, however, polyester chemistry and the techniques for using polyester have developed to the point at which polyester has become widely used as a material for "disposable" beverage bottles. Accordingly, these polyester bottles, once disposed of, present a significant opportunity for economical and efficient recycling, provided appropriate techniques can be developed. One of the fast growing types of plastic material for recycling is Polyethylene terephthalate (PET) flakes originating from post–consumer PET bottles as described above.
The PET recycling is the process of recovering different types of collected post-consumer PET container in order to reprocess them into varied other products. Before any post-consumer recycle PET waste is recycled, and it need to go through different stages so that it can be further used for making various types of recycled pet products that is sufficiently meet the appropriate standards for packing food products.
PRIOR ART OF THE INVENTION:
US patent application US5876644Arelates toa method of recycling post-consumer polyester to obtain recycled polyester of sufficiently high purity to meet food packaging requirements is disclosed. The method includes cleaning comminuted pieces of post-consumer polyester to remove surface contaminants; melting the surface-cleaned post-consumer polyester pieces; extruding the post-consumer melt; blending the melt of post-consumer polyester with a melt of virgin polyester prepolymer; solidifying and pelletizing the blended melt while the virgin polyester prepolymer remains as prepolymer; and polymerizing the solid blended pellets in the solid state.
However, the above patent application uses 25% of PCR material instead of using 50% PCR for reducing the carbon foot prints. Thus the above patent application fails to provide decreased carbon foot prints in 25% PCR materials. Said above patent application uses virgin polymer which must be used in range of 5-10 %, because it is crude source of petrochemical. Wherein said patent application used 75% of virgin polymers for producing PCR materials, which is not ecofriendly. Therefore said application fails to provide a process for preparation of PCR biaxial oriented polyester film (BOPET) film using recycle material which is efficient and is eco-friendly.
Klockner Pentaplast Publication in Plastic Today (article- November 30, 2012) relates to Pentaform Smart Cycle TH-ES100 films are made from 100% PCR material from beverage bottles, unlike standard PCR films, which combine PCR content and virgin resin. Pentaform Smart Cycle films help customers meet their sustainability goals for visual packaging applications. Suitable for face-seal, tray, and trapped blister thermoformed applications, Pentaform Smart Cycle films offer clarity, and process ability on standard thermoforming and form/fill/seal equipment.
However, the above patent application provides a cast (Amorphous-polyethylene terephthalate (APet)) film sheets rather than the thin BOPET film for using the PCR film in thermoforming box and tray applications. Hence, above application fails to provide the process for preparation of BOPET film. Said patent application produce the thin film which cannot used for thin packaging application; wherein the present invention provides an PCRBOPET film which are suitable for thin packaging application. Therefore said above patent application fails to provide process for preparation of PCR biaxial oriented polyester film (BOPET) film using recycle material which is efficient and is eco-friendly.
DISADVANTAGES OF PRIOR ART:
Said prior art suffers from at least all or any of the following disadvantages:
1. The conventional composition and process used higher range of virgin polymer (in the range of 75%) using the crude source of petrochemical during the processing of PCR chips, which is less eco-friendly against the chips used with more than % of PCR material.
2. The conventional process fails to provide decreased carbon foot prints in by using PCR materials, due to low consumption of post consumed material in the polymer or film.
3. In conventional process of making film, additives are used to enhance the property, which may lead to low environment friendly.

Thus, there is an unmet urge to provide the invention that obviates the disadvantages of prior art and provides a solution to the problems yet unaddressed.

OBJECTS OF INVENTION:
The primary object of the present invention is to provide a composition and process for preparation of PCR BOPET (Biaxial oriented polyethylene terephthalate) film.
Another object of the present invention is to provide a composition and process for preparation of PCR BOPET film by using post consumes recycle materials.
Yet another object of the present invention is to provide a composition and process for preparation of PCR BOPET film which decreased carbon foot prints in by using minimum virgin polymers.
Yet another object of the present invention is to provide a composition and process for preparation of PCR BOPET film by mechanical process which reduces the concentration of oligomers and improves surface properties of PET films and enhances the usage of the PCR BOPET film.
Yet another object of the present invention is to provide a composition and process for preparation of PCR BOPET film in which PCR is in the range of 50-98%.
Yet another object of the present invention is to provide a film with DEG (Diethylene Glycol) content reduces the melting point of the polymer and thereby it reduces the heat required for processing of the polymer.
Yet another object of the present invention is to provide a composition and process for preparation of PCR BOPET film which use minimum amount of additives, thus enhances the property of the PCR BOPET film and thereby became ecofriendly.
Yet another object of the present invention is to provide a composition and process for preparation of PCR BOPET film by using post consume recycle materials it contains high % of transmittance, clarity and glossiness thereby is it suitable packing film.
Yet another object of the present invention is to provide a composition and process for preparation of PCR BOPET film by using post consume recycle materials it contains good quality of printability and lamination strength which is suitable for the packing film.
SUMMARY OF THE INVENTION;
The present invention provides an improved composition and process for preparation of PCR BOPET (Biaxial oriented polyethylene terephthalate) film. Wherein said composition of the PCR BOPET film comprises of;
• % PCR resin,
• DEG,
• virgin polymers (PET copolymer),
• Additives.
SAID improved process for preparation of PCR BOPET (Biaxial oriented polyethylene terephthalate) film; wherein said process comprises the steps:
• Producing Post Consumed (PCR) Flakes;
• Producing of PCR BOPET film wherein first and the third layer of the film is the skin layer.
• Preparing the middle layer of the present BOPET film.
• Extruding said skin layer and the middle layer of the BOPET film mixing in a proportion forming a melt.
• Melting and removing the contamination and transferring into mold die.
• Molding and casting and stabilizing PCR BOPET film.

DETAILED DESCRIPTION OF INVENTION:
The present invention provides a composition and process for preparation of PCR BOPET (Biaxial oriented polyethylene terephthalate) film. Said PCR BOPET film is prepared by using post consume recycle materials which make the film environmental friendly, cost effective and efficient. Said invention provides the use of recovered PET (polyethylene terephthalate) polymers which is used as a raw material for preparing BOPET film. Said present invention provide an composition and process for preparation of PCR BOPET film which decreased carbon foot prints in by using minimum virgin polymers. Said PCR BOPET film provides minimum amount of additives, thus enhances the property of the PCR BOPET film and thereby became ecofriendly. Said invention reduces the generation of oligomer in film and provides low oligomer content within the range of 0.02 to 4 % in final PCR chips which contribute to maintain the low oligomer presence in the final PCR BOPET film.
Said composition of the PCR BOPET film which comprises of;
• % PCR resin,
• DEG,
• virgin polymers,
• Additives.
Wherein, said PCR BOPET film consists of PCR (post consumed recycle) resin for bottles, cups, containers etc. Said PCR (post consumed recycle) material are selected herein but limited to food containers and bottles that have been disposed of after their initial use. Said invention also provides mixed polymer recycle stream containing a very high proportion of PET contents. Said PCR (post consumed recycle) resin is in the range of 50-98%.
Said oligomer in PCR resin chips improves surface properties of PET films and enhances the usage of the PCR BOPET film.
Said DEG reduces melting point of the polymer and also to reduce the heat required for processing of the polymer. Said DEG improves the flow ability of the melt if it is present in above said limits. Said DEG used in very low contains which is in the range of 0.5-3.0 mol %.
Said virgin polymers are provided for smooth runability of polymer which helps in maintaining the strength, thermal stability, dimensional and stability. Said virgin polymers are selected as but not limited to PET resin, polyethylene terephthalate in form of bright chips, comprise of Pet copolymer. Said virgin polymers are in the range of 0-5%.
Said additives are provided for maintaining the surface properties, color, haze, transparency, aesthetics, winding, and printability. Said additives are selected as but not limited to silica, barium and titanium dioxide (tio2). Said additives are added with combination of various ratios like a ration of between 50:50 and 99:1, between 50:50 and 98:2, between 70:30 and 90:10, between 80:20 and 85:15.
Said process provides mechanical recycling process to make PCR chips for preparation of BOPET film; which comprises;
Comprises of following steps:
A. Producing Post Consumed (PCR) Flakes:
B. Producing PCR BOPET film.
Wherein;
I. Step A: Producing Post Consumed (PCR) Flakes;
For producing Post Consumed (PCR) Flakes comprise further the following steps:
a) Firstly, collecting the post consumed material which is not limited to food containers and bottles that have been disposed of after their initial use. After collection, recovery of the polyester flakes were occurred;
b) Further above recovered polyester flakes in step (a) undergoes isolation process which form polyester chips with 100% recycle content.
c) Mechanically recycle and convert the flakes into post consumed recycled chips through solid state polymerization (SSP) process. Wherein the mechanical process includes mechanical operations such as but not limited to sorting, washing, sizing, pelletizing. Said present PCR BOPET film is produce through the mechanical recycling process which provides PET chips of IV in the range of 0.65- 0.85 dl/gm.

II. Step B: Production of PCR BOPET film:

Said PCR BOPET film is prepared by using said mechanical process for preparing PCR chips produced in step A. Said film comprises of three layers, wherein first and the third layer of the film is the skin layer and the middle or the second layer is the main layer. The thickness of the main layer is more than the thickness of skin (1st and 3rd layers) for formation of said PCR BOPET film. Further, the materials will be transferred from the two different sections, first from the middle layer of final film and second from the skin layer (1st and 3rd layer) in the final film.

1. For the preparation of the skin layer (1st and 3rdlayer) of the present PCR BOPET film, following steps are included:

i. Said mechanically recycled post consumed recycled (PCR) chips/ flakes through solid state polymerization (SSP) process from above step (C) is further transferred into the existing hopper.
ii. In other hopper, additives and virgin polymer and PCR was fed.
iii. Said post consumed recycled (PCR) chips/ flakes and additives, virgin polymer in the hopper in above step (i & ii) were further transferred through high pressure vacuum blower system to loss and weight feeder
iv. Said additives, virgin polymer and PCR chips (i & ii) were fed in extruder are mixed.
v. Said above mixture is transferred to the existing extruder, screen changer, gear pump and filter and then sent to Die where skin layers was formed during extrusion process. Said bright chips (virgin chips), PCR Chips and silica are conveyed by hopper by vacuum blower system.
2. For the preparation of the middle layer of the present BOPET film, following steps are included:

i. Said above recovered PCR chips are conceded through the existing continuous fluid bed pre-crystallize. Said PCR chips were heated in the air, simultaneously higher degree of agitation taken place to prevent the formation of any agglomerates as the material is heated through the amorphous/crystalline phase.
ii. Said PCR chips are further passes through existing pre-crystallizer to column dryer. Said column dryer dry’s the heat for removal of internal moisture of said PCR chips. Said process takes place in the range of 4-5 hours.
iii. Said above dried chips are transferred to the existing extruder hopper by rotary valve and vibro-feeder. Further, said dried PCR chips are transferred to the melting extruder for molten flow of PCR chips to the metering extruder which is used to homogenize the melt.
iv. Said above melt transferred through the filtration process for removal of any contamination source in film. After filtration process said melt flow transferred to the die.

3. Further at the Die, said skin layer and the middle layer of the present BOPET film are mixed in a proportion forming a melt. Said Melt is than passed through screen changer followed by melt pump to filter, removing the contamination if any and is transferred to mold die.

4. Further the process of casting in BOPET film consist of Hot melt which is from the main section (Middle layer) and co-extruder section which from skin layer (1st and 3rd layer) is die and cast on the casting roller. The temperature of said casting roller is kept at very low temperature by inner water cooling system of the casting roller. Further the quenching process on the cast roll occurred which converted the melt in form of thick cast layer and this cat layer is taken off from the casting roller using take off roll.

5. After casting the film, said film transferred to the pinning system which pins the cast film with the electrostatic field into the cast roll. Said cast film is threaded towards the machine direction orientation (MDO). Said film is also stretched by stretching roll in machine direction for machine direction orientation of film.

6. After machine direction orientation of film, said film further transferred to the transverse direction orientation section where again film get stretched up to the maximum width.

Said film after molding and casting is crystallized and is stabilized in the crystallization zone to produce Stable PCR BOPET film. Said Stable PCR BOPET film thickness is in the range of 8 micron to 200 micron. Said improved process of PCR BOPET film by using post consume recycle materials it contains high % of transmittance, clarity and glossiness thereby is it suitable packing. Also said PCR BOPET film contains good quality of printability and lamination strength. Said present PCR BOPET film is produce through the mechanical recycling process which provides PET chips in the range of 0.65- 0.85 dl/gm.
Said invented PCR BOPET films are used in various packaging and industrial applications where high thermal, mechanical, optical, other ant functional properties are required. Said PCR BOPET films have a property of shrinkage which can vary according to the final application requirement. However, normal shrinkage is in range of 0 to 2.4 % at 150C / 30 minutes.
Examples:
Said improved process for preparation of PCR biaxial oriented polyester film (BOPET) film is performed and illustrate in the table 1 according to the said process for the preparation of PCR BOPET film. Said process conditions are kept in the disclosed ration as discussed above detailed process. Said % PCR resin composition are kept in the range of 80-100%, Oligomer PCR resin chips are kept in the range of 0.02 to 4 % and also kept low content of DEG.
Table 1: The process is performed in different Process conditions
Process condition
Film Production condition Example 1 Example 2 Example 3 Example 4 Example 5
Crystallizer temperature 175 174 174 175 174
Dryer temp 168 168 168 168 168
Melting extruder temp 286 285 285 286 285
MD stretching temperature in the first stage (ºC) 85 85 85 85 85
MD stretching ratio in the first stage 105 105 105 105 105
MD stretching ratio in the second stage 324 317 317 324 317
TD stretch ratio 4.26 4.23 4.23 4.26 4.23
Residence time from crystallization to cooling 3.2 3.2 3.2 3.2 3.2
Resin composition (PET/PCR/Silica)
% PCR resin composition 98 80 85 95 90
Oligomer in PCR resin chips 0.0425 0.0952 0.0512 0.0465 0.074
Content of DEG 0.5 1 0.5 2 1
Virgin polymer 2 10 5 0 5
Silica or other additive 0 10 10 5 5

Table 2: Quality evaluation result of the experimental data:
Quality evaluation result
Nominal thickness (Micron) 12 12 12 12 12
Transmittance (%) 88.2 88.6 88 88.2 88.2
Clarity (%) 96.4 93.5 93.1 95.2 96.1
Gloss (%) 126-128 124-127 122-125 126-128 126-128
Printability Good Good Good Good Good
Lamination strength Good Good Good Good Good
Oligomer in final film 1.12 0.97 0.54 0.66 0.81

Said above table 2, contain quality evaluation result data of PCR BOPET film which provides thickness of the film 12 micron with 88.2 % of transmittance, 93.1 – 96.4 % of clarity and 122- 128 % of glossy thereby is it suitable packing material. Also said PCR BOPET film provides good quality of printability and lamination strength with less amount of oligomer in final film in the range of 0.50-1.20.
ADVANTAGES OF THE PRESENT INVENTION:
1. The present invention provides an improved process for preparation of PCRBOPET (Biaxial oriented polyethylene terephthalate) film.
2. The invention provides an improved process for preparation of PCRBOPET film by using post consume recycle materials.
3. It provides PCR BOPET film which decreased carbon foot prints in by using minimum virgin polymers.
4. It provides a mechanical process for preparation of PCR BOPET film for improving surface properties of PET films by reducing the concentration of oligomers polymers and thus enhances the usage of the PCR BOPET film.
5. It provides an improved process for preparation of PCR BOPET film which is in the range of 50-98%.
6. The invention provides a film with DEG content in the range of 0.5-3.0 mol % to reduce the melting point of polymer and reduce heat required during extrusion in an improved process for preparation of PCR BOPET film.
7. It provides process for preparation of PCR BOPET film with minimum amount of additives for enhancing the property of PCR BOPET film and thus became ecofriendly.
8. It provides process for preparation of PCR BOPET film by using post consume recycle materials it contains high % of transmittance, clarity and glossiness thereby is it suitable packing film.
9. It provides process for preparation of PCR BOPET film by using post consumes recycle materials it contains good quality of printability and lamination strength which is suitable for the packing film.
10. It provides process for preparation of PCR BOPET film by using post consumed recycle material used for various type of coatings like acylic, Polyurethane, copolyester, antistatic, hard coating and other functional coating like PVDC, EVOH, PVOH, Barrier coatings etc., applied by inline or offline coating processes by means of different coating rollers.
11. It provides process for preparation of PCR BOPET film by using post consumed recycle material can be treated using corona treatment to provide the suitable surface tension on surface of film used for various application of packaging such as printing, lamination , metal adhesion etc.
,CLAIMS:We Claim:
1. A composition and process for preparation of PCR (post consumed recycle) biaxial oriented polyester film (BOPET); wherein said composition of the PCR BOPET film comprises;
o % PCR resin,
o DEG,
o virgin polymers,
o Additives;

Wherein said process comprises the steps:

• Producing Post Consumed (PCR) Flakes;
• Producing of PCR BOPET film wherein first and the third layer of the film is the skin layer;
• Preparing the middle layer of the present BOPET film;
• Extruding said skin layer and the middle layer of the BOPET film mixing in a proportion forming a melt;
• Melting and removing the contamination and transferring into mold die;
• Molding and casting and stabilizing PCR BOPET film.

2. A composition for the preparation of PCR (post consumed recycle) biaxial oriented polyester film (BOPET) as claimed in claim 1; wherein said composition comprises of;
o % PCR resin,
o DEG,
o virgin polymers,
o Additives;
Said PCR BOPET film consists of PCR (post consumed recycle) resin for bottles, cups, containers; said PCR (post consumed recycle) material are food containers and bottles that have been disposed of after their initial use; said polymer recycle stream containing high proportion of PET contents; said oligomer in PCR resin chips improves surface properties of PET films and enhances the usage of the PCR BOPET film; said DEG reduces melting point of the polymer and heat required for processing of the polymer; wherein said DEG improves the flow ability; said virgin polymers provide smooth runability of polymer maintaining the strength, thermal stability, dimensional and stability; said virgin polymers are selected as but not limited to PET resin, polyethylene terephthalate in form of bright chips, comprise of Pet copolymer; said additives are provided for maintaining the surface properties, color, haze, transparency, aesthetics, winding, and printability; said additives are selected as but not limited to silica barium and titanium dioxide (tio2).
3. The composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film as claimed in claim 1; wherein the concentration of oligomers content in the BOPET film is in range of 0.02 to 4 %.

4. The composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film as claimed in claim 1; wherein said DEG is in the range of 0.5-3.0 mol %.

5. The composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film as claimed in claim 1; wherein said PCR resin composition in the PCR BOPET film is in the range of 50-98%.

6. The composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film as claimed in claim 1; wherein said virgin polymers are in range of 0-50%.

7. The composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film as claimed in claim 1; wherein said PCR BOPET films have a shrinkage in the range of 0 to 2.4 % at 150C / 30 mins.

8. The composition and process for preparation of PCR biaxial oriented polyester film (BOPET) film as claimed in claim 1; wherein said additive is in the ratio of 50:50 and 99:1, 50:50 and 98:2, 70:30 and 90:10, 80:20 and 85:15.

Dated this 15th day of July 2020,

________________________
GOPI J. TRIVEDI (Ms)
IN/PA 993
Authorized Agent of the Applicant

To,
The Controller of Patents,
Patent Office,
Mumbai