Claims:1. An allyl acetate based copolymer composition, comprising:
an allyl acetate monomer 101;
at least one of a vinyl acetate monomer 102 and an acrylic monomer 103;
at least one of a colloid and surfactant;
a redox initiator;
wherein the copolymer composition has
a molecular weight greater than 55000,
a viscosity within a predefined range of 0.1 to 1000 poise,
a pH value within a predefined range of 4.0 to 6.0 and
a glass transition temperature within a predefined range of -20 to 40°C.

2. The copolymer composition of claim 1, wherein the allyl acetate monomer 101 is 15% of the total copolymer composition.

3. The copolymer composition of claim 2, wherein ratio of the vinyl acetate monomer 102 to the allyl acetate monomer 101, or the acrylic monomer 103 to the allyl acetate monomer 101, or combination of the vinyl acetate monomer 102 and the acrylic monomer 103to the allyl acetate monomer 101 is 99:1 to 75:25.

4. The copolymer composition of claim 3, wherein the acrylic monomer 103 is at least one of butyl acrylate, methyl acrylate, methyl methacrylate, Ethylhexyl Acrylate (EHA), styrene and a combination thereof.

5. The copolymer composition of claim 1, wherein the colloid is in a predefined range of 3 to 15% weight of the total copolymer composition, and wherein the surfactant is in a predefined range of 0.1 to 6% weight of total copolymer composition.

6. The copolymer composition of claim 1, wherein the redox initiator comprises a reducing agent and an oxidising agent,
wherein the reducing agent is at least one of tartaric acid, ascorbic acid, sodium bisulphite, sodium metabisulphite and a combination thereof,
wherein the oxidising agent is at least one of alkali metal persulphate, alkali metal peroxide and a combination thereof,
wherein the alkali metal persulphate and the alkali metal peroxide is at least one of ammonium persulphate, potassium persulphate, sodium persulphate, hydrogen peroxide, t-butyl hydrogen peroxide and a combination thereof.

7. The copolymer composition of claim 6, wherein the redox initiator further comprises a metal salt, wherein the metal salt is used with or without metal complexing agents, wherein the metal salt is at least one of iron, copper, manganese, silver, vanadium, nickel, cobalt and a combination thereof.

8. The copolymer composition of claim 1, wherein the copolymer composition is a milky white composition containing at least 50% solid content, and wherein the copolymer composition is tack-free and clear or transparent.

9. The copolymer composition of claim 1, wherein a free monomer content in the copolymer composition is less than or equal to 0.3% of the total weight of the copolymer composition.

10. A method of forming a copolymer composition, the method comprising:
forming a monomer mixture comprising an allyl acetate monomer 101 and at least one of a vinyl acetate monomer 102 and an acrylic monomer 103 in a predefined ratio;
forming a solution of water at least one of a colloid and a surfactant;
feeding a redox initiator to a reactor 109 via one or more feed points;
stirring, via an agitator 110, the monomer mixture and the solution in the reactor 109 in order to facilitate reaction of the monomers for a time period, maintaining an equilibrium between the feed rate and rate of reaction, thereby avoiding flooding conditions of the monomer mixture;

adding at least one of the vinyl acetate monomer 102 and the acrylic monomer 103 to the reactor in order to consume residual allyl monomer thereby obtaining an allyl acetate based copolymer composition, wherein the copolymer composition has
molecular weight greater than 55000,
viscosity within a predefined range of 0.1 to 1000 poise,
pH value within a predefined range of 4.0 to 6.0 and
glass transition temperature within a predefined range of -20 to 40°C.

11. The method of claim 10, wherein the solution is a colloidal solution or a surfactant solution formed by,

feeding the water and at least one of the colloid and the surfactant,
stirring the mixture of the water and at least one of the colloid and the surfactant and
heating the mixture stirred at a predefined temperature in order to form the solution.

12. The method of claim 11, wherein the solution is maintained at a predefined temperature in a range of 50 to 90 °C.

13. The method of claim 10, wherein the solution is a colloidal solution or a surfactant solution formed by,
feeding the water and at least one of the colloid and the surfactant,
stirring the mixture of the water and at least one of the colloid and the surfactant, in order to form the solution.
, Description:FORM 2

THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENT RULES, 2003

COMPLETE SPECIFICATION

(See Section 10 and Rule 13)

Title of invention:

ALLYL ACETATE COPOLYMER COMPOSITION

APPLICANT:

PIDILITE INDUSTRIES LIMITED
A company incorporated as per laws of India and having address as
Regent Chambers, 7th floor,
Jamnalal Bajaj Marg, 208,
Nariman point, Mumbai-400021 (India).

The following specification describes the invention and the manner in which it is to be performed.

CROSS-REFERENCE TO RELATED APPLICATIONS AND PRIORITY
[001] The present application does not claim priority from any patent application.
TECHNICAL FIELD
[002] The present disclosure in general, relates to field of polymers. More particularly, the disclosure relates to method and system of copolymerization of allyl acetate to obtain an allyl acetate copolymer composition with improved/enhanced characteristics.
BACKGROUND
[003] Allyl polymerization have received much less emphasis as compared to vinyl polymerization because of the difficulty of allyl compounds to polymerize and due to their availability. It is evident that chain transfer reaction in most of the monomers has much lower impact on polymerization as compared to allyl polymerization. The chain transfer between active growing chain and allyl monomer can lead to termination of growing chain and also lead to termination of the chain reaction. The monomer radical produced is resonance stabilised and is consequently less active. The allyl radicals have lower tendency to initiate a new polymer chain. This "degradative chain transfer" leads to produce low molecular weight compounds. Even small amount of allyl acetate inhibits or retards the polymerization of other monomers.
[004] Higher dosage of catalyst is required for allyl polymerization compared to the other monomers due to the "degradative chain transfer" caused by allyl radicals. The allyl radicals do not respond to heat and light and therefore catalyst are the preferred way of carrying out the reaction. The available allyl copolymers usually have low molecular weight. Considering the existing art, it is found that thermal system as well as lower dosage of catalyst is used in conventional VAM polymerization which is insufficient to have the desired kinetics of reaction. The reaction temperature drops as the addition of monomer continues. By using higher dosage of catalyst, the stability of copolymer composition gets affected.
SUMMARY
[005] This summary is provided to introduce concepts related to methods and systems for copolymerization of allyl acetate thereby generating an allyl acetate based copolymer composition and the concepts are further described below in the detailed description. This summary is not intended to identify essential features of the claimed subject matter nor it is intended for use in determining or limiting the scope of the claimed subject matter.
[006] In one embodiment, an allyl acetate based copolymer composition is disclosed. The copolymer composition may comprise an allyl acetate monomer and at least one of a vinyl acetate monomer and an acrylic monomer. The copolymer composition may further comprise at least a colloid or a surfactant. The copolymer composition may further comprise a redox initiator. In one aspect, molecular weight of the copolymer composition may be greater than 55000. Further, viscosity of the copolymer composition may be within a predefined range of 0.1 to 1000 poise. Further, a pH value of the copolymer composition may be within a predefined range of 4.0 to 6.0. Furthermore, a glass transition temperature (Tg) of the copolymer composition may be within a predefined range of -20 to 40°C.
[007] In another embodiment, a method of forming an allyl acetate based copolymer composition is disclosed. The method may comprise forming a monomer mixture comprising the allyl acetate monomer and at least one of the vinyl acetate monomer and the acrylic monomer in a predefined ratio. The method may comprise forming a solution of water and at least one of the colloid and the surfactant. The method may comprise feeding a redox initiator to a reactor via one or more feed points. The method may further comprise stirring, via an agitator, the monomer mixture and the solution in the reactor in order to facilitate reaction of the monomers for a time period, maintaining an equilibrium between the feed rate and rate of reaction, thereby avoiding flooding conditions of the monomer mixture. The method may comprise adding at least one of the vinyl acetate monomer and the acrylic monomer to the reactor in order to consume residual allyl monomer thereby obtaining an allyl acetate based copolymer composition. The molecular weight of the copolymer composition may be greater than 55000. The viscosity of the copolymer composition may be within the predefined range of 0.1 to 1000 poise. The pH value of the copolymer composition may be within the predefined range of 4.0 to 6.0. The glass transition temperature of the copolymer composition may be within the predefined range of -20 to 40°C.

BRIEF DESCRIPTION OF THE DRAWINGS
[008] The detailed description is described with reference to the accompanying Figures. In the Figures, the left-most digit(s) of a reference number identifies the Figure in which the reference number first appears. The same numbers are used throughout the drawings to refer like features and components.

[009] Figure 1 illustrates a system 100 facilitating allyl acetate copolymer composition, in accordance with embodiments of the present disclosure.

DETAILED DESCRIPTION
[0010] Some embodiments of this invention, illustrating all its features, will now be discussed in detail.

[0011] The words "comprising," "having," "containing," and "including," and other forms thereof, are intended to be equivalent in meaning and be open ended in that an item or items following any one of these words is not meant to be an exhaustive listing of such item or items, or meant to be limited to only the listed item or items.

[0012] It must also be noted that as used herein and in the appended claims, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise. Although any systems and methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present invention, the preferred, systems and methods are now described. The disclosed embodiments are merely exemplary of the invention, which may be embodied in various forms.

[0013] Various modifications to the embodiment will be readily apparent to those skilled in the art and the generic principles herein may be applied to other embodiments. However, one of ordinary skill in the art will readily recognize that the present disclosure is not intended to be limited to the embodiments illustrated, but is to be accorded the widest scope consistent with the principles and features described herein.

[0014] The present disclosure describes an allyl acetate copolymer composition and method of preparing the allyl acetate copolymer composition. Figure 1 illustrates the system 100 enabling production of the allyl acetate copolymer composition, in accordance with embodiments of the present disclosure. The system 100 may comprise a monomer mixture of an allyl acetate monomer 101 and at least one of vinyl acetate monomer 102 and an acrylic monomer 103, a reactor 109 with one or more feed points, one or more pumps (112 a, 112 b), a pump 112, a pump 115, a reservoir tank 105, reservoir tank 106, reservoir tank 107, an agitator 110, thermocouple 111 and a reflux condenser 113. The monomer mixture may be stored in one of the reservoir tank 105. Water 104 may be supplied to the one or more reservoir tanks (105,106,107) respectively. Further, redox initiator may be stored in one or more reservoir tank (106 a, 106 b). Colloid or surfactant may be stored in a reservoir tank 107. The monomer mixture comprising the allyl acetate monomer 101 and at least one of the vinyl acetate monomer 102 and the acrylic monomer 103, may have ratio by weight or by volume. The monomer mixture, wherein the ratio of at least one of the vinyl acetate monomer 102 and the acrylic monomer 103 to the allyl acetate monomer 101, may be in a ratio varying from 99:1 to 75:25. The monomer mixture may be a homogeneous mixture. The colloid or the surfactant may be fed, via the pump 115, to the reservoir tank 105 wherein the monomer mixture is stored. Sometimes, the colloid may be fed, via the one or more feed points, directly to the reactor 109. The monomer mixture may be fed from the reservoir tank 105, via feed pump 108, to the reactor 109. The pumps (108,112,115) may be a positive displacement pump. In one embodiment, the pumps (108,112,115) may be a peristaltic pump. The feeding of the monomer mixture to the reactor 109 may be continuous or intermittent/at any frequency. The redox initiator may be added to the reactor 109 via the pump 112. The feed rates of the monomer mixture and sufficient additional time may be optimised maintaining an equilibrium, thereby avoiding flooding conditions of the monomers. The equilibrium between feed rate and rate of reaction may help in maintaining the chemical composition of the polymer chain (chemical composition drift), eventually providing adequate reaction kinetics.

[0015] One of the strategy may be such that addition of the monomers may be done in two stages. The monomer mixture may be added to the reactor 109 (stage 1), followed by addition of at least one of the vinyl acetate monomer 102 and the acrylic monomer 103 (stage 2), in order to consume residual allyl acetate monomer. The reaction of at least one of the vinyl acetate monomer 102 and the acrylic monomer 103 and the allyl acetate monomer 101 may leave some residual allyl acetate monomer in the reactor 109. In order to react with the residual allyl acetate monomer, at least one of the vinyl acetate monomer 102 and the acrylic monomer 103 may further be fed, via the feed pump 108, to the reactor 109. The free monomer may be less than 0.3% weight of the total copolymer composition.

[0016] The addition of monomers (stage 2) may result in observable difference in properties of copolymer composition like improved water resistance, good film integrity, transparency of the film and flexibility. The ratio of the monomer mixture may be kept constant throughout the supply to the reactor 109. The feed rate of the monomer mixture may be varied, depending on the rate of reaction of the monomers, facilitating the copolymer composition.

[0017] A solution may be formed comprising water and at least one of the colloid and the surfactant. The solution may be a colloidal solution or a surfactant solution, comprising colloid and surfactant respectively. In one aspect, a method of forming the colloidal solution is described. The method may comprise feeding the water and the colloid. The method may comprise stirring the mixture of the water and the colloid. The method may further comprise heating and stirring the mixture at a predefined temperature in order to form the colloidal solution. The method may further comprise the surfactant to form the colloidal solution. The colloidal solution and the monomer mixture are further mixed together in the reactor 109.

[0018] In another aspect, a method of forming the surfactant solution is described. The method may comprise feeding the water and the surfactant. The method may comprise stirring the mixture of the water and the surfactant. The monomer mixture may be further stirred with the mixture of the water and the surfactant thereby forming the surfactant solution. The surfactant solution may be a pre-emulsion. The monomer mixture may be added neat (without use of water) or as a pre-emulsion in water. The solution may be further fed to the reactor 109.

[0019] The redox initiator may comprise a reducing agent and an oxidising agent. The reducing agent may be at least one of tartaric acid, ascorbic acid, sodium bisulphite, sodium metabisulphite and a combination thereof. The oxidising agent may be at least one of alkali metal persulphates and alkali metal peroxides and a combination thereof, wherein the alkali metal persulphates and alkali metal peroxides may be at least one of ammonium persulphate, potassium persulphate, sodium persulphate, hydrogen peroxide, t-butyl hydrogen peroxide and a combination thereof. The redox initiator may further comprise a metal salt. The metal salt may be used with or without metal complexing agents. The metal salt may be at least one of iron, copper, manganese, silver, vanadium, nickel, cobalt and a combination thereof.

[0020] The colloid may be polyvinyl alcohol. The choice of polyvinyl alcohol (PVOH) may determine the properties of latex and thus the copolymer obtained, especially rheological properties such as viscosity and shear thinning, or setting speed and grab. The rheology properties of the copolymer may depend on molecular weight, distribution and degree of hydrolysis of PVOH used. Various suitable polyvinyl alcohol may be used, preferably the PVOH having the degree of hydrolysis of 60-99 mole%. The most commonly used PVOH in the emulsion polymerization, having an intermediate degree of hydrolysis (85-92%), may generate good balance between hydrophobic and hydrophilic properties of the colloid. However, in order to achieve the desired viscosity level of the polymer latex and to allow for good adhesion performance of the bond, blends of PVOH having different molecular weight and degree of hydrolysis may be used together. The colloidal stabilizer PVOH may be used in a predefined range of 3-15 % by weight of the composition, preferably 2-8 % by weight of composition.

[0021] The copolymer latex may be co-stabilized by use of surfactants, if needed, to further control the rheological properties. Nonionic emulsifiers may be fatty alcohol ethoxylates, modified fatty alcohol ethoxlates, alkyl phenol ethoxylates, alkyl polyglycol ethers, EO/PO block copolymers may be used. The emulsifiers may be used in the predefined range of 0.1 to 1 % by weight based on total monomer content.

[0022] For surfactant stabilized emulsions (no colloid) such as vinyl acetate-allyl acetate-acrylic emulsions or vinyl acetate-allyl acetate emulsions, surfactants such as anionic emulsifiers and/or nonionic emulsifiers may be used. The anionic emulsifiers may be at least one of alkali metal or ammonium salts of alkyl, aryl or alkyl-aryl sulfates, sulfonates or phosphates, alkyl sulfonic acids, sulfosuccinate salts, fatty acids, the nonionic emulsifiers and a combination thereof. The surfactant may be used in the predefined range of 0.1 to 6 % by weight of total monomer content.

[0023] The presence of monomer mixture, the redox initiator and the solution (either colloidal solution or the surfactant solution) may be stirred by the agitator 110 in the reactor 109. The agitator 110 may be anchor type, turbine impeller, propeller agitator and the like. The agitator 110 may be coupled to a motor 114. The motor 114 may be a Variable Frequency Drive (VFD). The stirring action by the agitator 110 may enhance the rate of reaction of the monomer mixture. An efficient stirring by the agitator 109 may be critical in order to ensure the proper mixing of the monomer mixture, the redox initiator and the solution which may improve the rate of reaction. The agitator action may further help in avoiding monomer phase segregation during the copolymerization. Additionally, steam may be supplied, via an inlet, to the reactor 109 in order to facilitate the reaction. Further, the reflux condenser 113 may pull in vapour generated during the reaction of the monomers, then condensate the vapour and return the condensate to the reactor 109. Water is supplied via an external source to the reflex condenser 113 in order to facilitate the cooling of the vapour present in the reflex condenser 113. The thermocouple 111 may be used for measuring the temperature of the reaction in the reactor 109. Hereinafter the formed copolymer composition comprising the colloidal solution or the surfactant solution may also be referred as “colloid based copolymer composition” or “surfactant stabilized copolymer composition” respectively. An opening may be provided to the reactor 109 in order to remove the formed copolymer composition. A pump may be used to transfer the formed copolymer composition from the opening of the reactor 109 to the blender tank 116. Additives may be further added to the formed copolymer composition. The blender tank 116 may comprise a blender/stirrer, used for blending of the formed copolymer composition.

[0024] Additionally, the dosage of the colloid or the surfactant may be optimised in order to achieve properties like flow, good emulsion stability and resistance to water. The redox initiator may also be optimised in order to minimise amount of grits generated in the reaction due to poor reactivity of allyl acetate monomer. The grits may arise due to instability of the polymer particles being formed during the polymerization. The oxidizing agent and the reducing agent may be added to the reaction in separate streams, preferably simultaneously with the monomer mixture at a predefined rate. The reaction may be maintained at a predefined temperature in a range of 50 to 90°C, preferably 70 to 80°C, in order to maintain high rate of radical generation.

[0025] In another embodiment, an allyl acetate based copolymer composition is described in accordance to the present disclosure. The copolymer composition may have molecular weight greater than 55000. The copolymer composition may have viscosity within a predefined range of 0.1 to 1000 poise. The copolymer composition may have pH value within a predefined range of 4.0 to 6.0. The copolymer composition may have glass transition temperature within a predefined range of -20 to 40°C. The appearance of the copolymer composition is milky white. There are some additional parameters which are also considered during manufacturing of the copolymer compositions such as Minimum Film Forming Temperature (MFFT), aaccelerated stability, freeze thaw, tackiness, etc.

[0026] The present disclosure may include surfactant stabilized copolymer compositions which are used in application like paints, construction and adhesives. The white glue may be primarily used in the wood working applications. The copolymer compositions may have properties like good film formation without use of external plasticizers, very good film integrity under water compared to vinyl acetate based homopolymers, clear or transparent film which may make difficult to see any glue line at joints and flexibility of film.

[0027] The viscosity of the copolymer composition may be an important parameter and is necessary to obtain the same in most desirable range to maintain suitability in wood working application. The colloid based copolymer composition based on VAM-allyl acetate may have very high tendency to resist flow. The colloid selection may be crucial in order to meet the application requirements. The copolymer composition may have the Brookfield viscosity in the range of 0.1–1000 poise. For wood working application, the viscosity may be in the range of 50-1000 poise, more preferably 150-500 poise. For surfactant stabilized systems, the viscosity may be in the range of 0.05 poise to 100 poise, more preferably 0.5-20 poise.

[0028] In yet another embodiment, acrylic monomer may be incorporated in surfactant stabilized copolymer composition. In some embodiments containing VAM and allyl acetate monomer, in the ratio varying from 75:25 to 99:1, vinyl acetate monomer may be partially replaced with any of the above said acrylic monomers without affecting conversion into the copolymer composition. The acrylic monomer may be at least one of butyl acrylate, methyl methacrylate, acrylonitrile, acrylic acid, methacrylic acid, n-methylol acrylamide and a combination thereof. However, the use of hydrophobic monomers like Ethylhexyl Acrylate (EHA), Styrene etc. may be difficult which may further lead to poor reaction kinetics and copolymer conversion. Using these hydrophobic monomers may result in flooding conditions during the reaction and may leave very large free monomer quantities after the batch of copolymer composition is processed.

[0029] The allyl copolymer composition may also be carried out with many acrylic monomers (not all) in absence of vinyl acetate monomer. The ratio of quantities of acrylic monomers to allyl acetate monomer may be varied in the same range from 99:1 to 75:25. It may be observed that higher the allyl acetate, the molecular weight of the copolymer composition reduces drastically and the copolymer composition obtained may not be useful for the mentioned applications. The monomer addition time may also increase significantly with the increasing amount of allyl acetate used in the monomer mixture. It is observed that the addition of certain acrylic monomers like butyl acrylate, methyl acrylate, methyl methacrylate provides good reaction kinetics while the hydrophobic monomers like EHA and Styrene lead to extremely poor reaction and low conversion.

[0030] It is observed that pH plays an important role in the reaction kinetics of the copolymer composition. Based on the experimental results, it is found that when the pH of the dispersion drops below the pH value of 3, the rate of reaction becomes extremely low. The pH of the reaction should be kept between 3 to 9, more particularly between 5 -7, throughout the course of reaction in order to achieve good kinetics and complete copolymer conversion. Therefore, buffers may be used that keep the pH well above 3. Some of the buffer examples may be at least one of sodium bicarbonate, sodium acetate, sodium citrate, diammonium phosphate, trisodium phosphate and a combination thereof.

[0031] The concentration range of total amount of the surfactants may be from 0.5 to 10 weight %, preferably 1 to 6 weight %, based on total copolymer composition. Various anionic and nonionic surfactants and their combinations may be used. In the preparation of the polymer dispersions, polymer content of the dispersion may vary from 40 to 65 weight % and particularly from 45 to 55 weight % of the total copolymer composition.

[0032] Various batches were processed at 5Kg and 100Kg scale are considered for the performance analysis. The batches having satisfactory processing conditions but with limitations like inferior freeze thaw and accelerated heat stability (55OC for 30 days). The results of the same are discussed below. Further, it was required to refine the overall process and ingredients which resulted in overcoming limitations of the earlier reported batches. Some of the batch examples of copolymer composition along with the results obtained are discussed below:

[0033] Example 1: Colloid based copolymers of vinyl acetate and allyl acetate.

Ingredients Parts
Vinyl Acetate 40
Allyl Acetate 7.5
Water 49
Polyvinyl alcohol 2.5
Hydrogen peroxide
(35 % solution) 0.6
Tartaric Acid 0.3
Sodium Bicarbonate 0.1

[0034] An aqueous solution is prepared by dispersing in a reaction vessel distilled deionized water and polyvinyl alcohol. The aqueous solution in the reaction vessel is then stirred with impellers at a speed of 30 rpm. The mixture is stirred at room temperature for 30 minutes, followed by heating the mixture at 85-90oC for 2 hours to prepare the aqueous solution. The reaction is started at 78 ±2°C and is maintained throughout the reaction. A monomer mixture is prepared separately using the vinyl acetate monomer (VAM) and the allyl acetate monomer in a separate tank. VAM seed is prepared using 125 gm VAM followed by addition of hydrogen peroxide and tartaric acid respectively. The monomer addition is done in two stages. The monomer mixture of VAM and allyl acetate (Stage 1) is added to the mixture of aqueous colloid solution using a dosing pump in a controlled manner over a period of time. This is followed by addition of VAM (Stage 2). The monomer is added to the stirred aqueous solution in the reaction vessel. The stirring of the reaction mixture continues, by means of the impellers, until the monomers, both Stage 1 and Stage 2 additions are done. The heating of the reaction mixture continues along with stirring for over a period of 6 hours using metering pump. Two additional pumps are used in order to add oxidizing and reducing catalyst throughout the reaction. After the addition of monomer is done, the reactor is kept for next 1 hour at the reaction temperature and is then cooled to temperature of 40°C.

[0035] The resulting dispersion is milky white viscose copolymer composition which has very low free monomer content (less than 0.5%) and 50% solids with viscosity within the range of 500-750 poise. The produced copolymer composition has poor flow contrary to polyvinyl acetate copolymer composition. The film formed by the copolymer composition is clear after drying, retain considerable strength and resistance to rubbing after immersion in water. This copolymer composition can be used as a replacement for application where vinyl acetate copolymer compositions are used. The results obtained are tabulated below. Table 1 shows physical parameters of the bench pilot batch done in 5Kg and of the plant batch done in 100Kg scale respectively.

COPOLYMER COMPOSITION PARAMETERS
Sr. No. Properties Observed Results Specification Range
1 Appearance Milky White Milky White
2 % Solid Content 50.41% 49.0-51.0
3 Viscosity on Brookfield RVT @ 20 RPM (30°C) 250 poise 150-500
5 pH 4.6 4.0-6.0
6 Film Clarity (Glass Plate) Clear Clear
7 Particle size (nm) 742 ---
8 % Free Monomer 0.09% Less than 0.3%
9 MFFT (°C) 13.1 ---
10 Accelerated Stability
(30 days at 55°C) Pass Pass
11 Freeze Thaw
(3 cycles at -10°C to 25°C) Pass Pass
12 Tack Non Tacky Non Tacky
13 Molecular Weight (Mw) 81540 >55000
14 Glass Transition Temp.
[Tg (°C)] 36.4 33-37
Table 1

[0036] Example 2: Surfactant stabilized copolymer composition of vinyl acetate and allyl acetate.
Ingredients Parts
Vinyl Acetate 44.4
Acrylic Acid 0.22
Allyl Acetate 7.9
Water 42.67
Rhodoline WA40 1.7
Pluronic F-68 2.1
Hydrogen peroxide
(35 % solution) 0.6
Tartaric Acid 0.3
Sodium Bicarbonate 0.1

[0037] In the process similar to that explained in example 1, a surfactant is used in place of colloids to stabilize the particles. A pre-copolymer composition is prepared by addition of a mixture of VAM and allyl acetate to the surfactant/aqueous solution. The pre-copolymer composition is then added to the reactor containing water and surfactant(s). Table 2 shows the physical parameters of the plant batch done in 5 Kg scale.

COPOLYMER COMPOSITION PARAMETERS
Sr. No. Properties Observed Results
1 Appearance Milky White
2 % Solid Content 55.9
3 Viscosity on Brookfield RVT
@ 20 RPM (30°C) 3 poise
5 pH 4.5
6 Film Clarity (Glass Plate) Clear
7 Particle size (nm) 238
8 % Free Monomer 0.01
9 MFFT (°C) ---
10 Accelerated Stability (30 days at 55 °C) Pass
11 Freeze Thaw (3 cycles at -10 C to 25 °C) Pass
12 Tack Non Tacky
13 Molecular Weight (Mw) 82210
14 Glass Transition Temp. [Tg (°C)] 25.4

Table 2

[0038] Example 3: Surfactant stabilized copolymer composition of vinyl acetate, allyl acetate and acrylate.
Ingredients Parts
Butyl Acrylate 15
Vinyl Acetate 23.7
Allyl Acetate 7.5
N-methylol acrylamide 1
Acrylic Acid 0.5
Water 50
Calfax DB 45 0.8
Laffonics MB 400 0.8
t-BHP (70 % solution) 0.6
Sodium Metabisulphite 0.3
Sodium Bicarbonate 0.1

[0039] In a process similar to that shown in example 2, the acrylic monomers are used by further replacing a part of the vinyl acetate monomer. The dispersion produced are surfactant stabilized rather than colloids. In place of mixing the monomers, a pre-copolymer composition is formed by pouring the monomer mixture in the surfactant and water solution. Rest of the process and temperature are similar to the one stated in example 1. Table 3 shows the physical parameters of the plant batch done in 5 Kg scale.

COPOLYMER COMPOSITION PARAMETERS
Sr. No. Properties Observed Results
1 Appearance Milky White
2 % Solid Content 28.00%
3 Viscosity on Brookfield RVT @ 20 RPM (30°C) 0.5 poise
5 pH 5.35
6 Film Clarity (Glass Plate) Clear
7 Particle size (nm) 85
8 % Free Monomer 0.35
9 MFFT (°C) ---
10 Accelerated Stability (30 days at 55 °C) Pass
11 Freeze Thaw (3 cycles at -10 C to 25 °C) Pass
12 Tack Slightly Tacky
13 Molecular Weight (Mw) 55548
14 Glass Transition Temp. [Tg (°C)] 13.1

Table 3

[0040] Example 4 Surfactant stabilized copolymer composition of vinyl acetate and acrylate.

Ingredients Parts
Butyl Acrylate 20.0
Methyl Methacrylate 19.0
Allyl Acetate 7.1
Acrylamide 0.9
2-Acrylamido-2-methylpropane sulfonic acid 0.45
Water 50.75
Calfax DB 45 (45 % sol.) 0.46
Disponil AFX 3070 (70 % sol.) 0.50
t-BHP (70 % solution) 0.3
Sodium Metabisulphite 0.3
Sodium Bicarbonate 0.24

[0041] The process is similar to example 2 and example 3, as explained above. The results obtained for the example 4 are also within the specification range of the above stated examples.

[0042] In accordance with embodiments of the present disclosure, the copolymer compositions described above may be used in multiple applications including but not limited to:
• adhesives
• construction
• paints.

[0043] The embodiments, examples and alternatives of the preceding paragraphs or the description and drawings, including any of their various aspects or respective individual features, may be taken independently or in any combination. Features described in connection with one embodiment are applicable to all embodiments, unless such features are incompatible.