Method for preparing acrylic copolymer aqueous dispersion for pressure-sensitive glues

FIELD: chemistry of polymers.

SUBSTANCE: invention relates to emulsion method for co-polymerization of acrylic monomers. Invention proposes a method involving preliminary emulsification of mixture of butyl acrylate with (meth)acrylic and/or vinyl monomer in water in the following mass ratio co-monomer : water = 1:(0.2-0.3) in the presence of 3.4-4.0 wt.-% of sulfooxyethylated alkylphenol ammonium salt wherein (C8-C10)-alkyl has the alkylation degree 18-26 wt.-%, the following emulsion co-polymerization at temperature 78-82°C for 3-10 h at continuous dosing of preliminary prepared co-monomers emulsion and 0.3-0.6 wt.-% of ammonium or potassium persulfate in the total ratio to the reaction mass co-monomer : water = 1:(0.4-0.5) followed by additional polymerization of the reaction mixture in addition of 0.1 wt.-% of ammonium or potassium persulfate after keeping the reaction mixture for 0.5 and 1.5 h and its final temperature keeping for 2 h. Invention provides increasing concentration of acrylic copolymer aqueous dispersion at low content of coagulum and improving its adhesion properties. Invention provides the development of a method for preparing highly concentrated aqueous dispersion with the content of acrylic copolymer 60 wt.-%, not less, for glues showing sensitivity to pressure.

EFFECT: improved preparing method, improved and valuable properties of dispersion.

2 cl, 1 tbl, 13 ex

 

The invention relates to the chemistry of polymers, namely, the emulsion polymerization method of the acrylic monomers, which allows to obtain a highly concentrated aqueous dispersions for adhesives, pressure-sensitive, used in the manufacture of self-adhesive materials.

The concept of self-adhesive materials include various polymer films, textile, foamed polymeric materials, paper products, on one or two sides of which are covered with an adhesive layer protected by the adhesive coating. They are used as decorative coatings, labels and marking signs, heat, noise, vibration insulating materials, packaging adhesive tapes, medical tapes, etc.

The use of such materials based on the preliminary removal of the protective release material, if any, and bonding to the surface due to light briefly pressing or rolling, resulting in a strong bond between the material and the surface. Such conditions are "instant bonding" is provided by a special group of adhesives that are called adhesives with a permanent tack or adhesives, pressure-sensitive. They do not provide structural strength, however, stick together virtually all materials, including those having low surface - polyethylene, polypropylen, fluoropolymers.

Significant advantages of adhesive compositions based on aqueous dispersions are determined by the absence of toxic, flammable and expensive organic solvents. However, the use of adhesives with a water content of about 50% increases the energy consumption during processing, reduces the performance of the equipment, which is not always compensate for their lower cost. Reducing these costs is possible with the production of highly concentrated aqueous dispersions. In this case also reduced transportation costs adhesives and their storage.

The authors of the invention the objective was to obtain a highly concentrated aqueous dispersion of acrylic copolymer (the content of the copolymer is not less than 60 wt.%) for the adhesive, pressure-sensitive, with low content of coagulum and improved adhesive properties.

A method of obtaining an acrylic copolymer for adhesive tapes for medical purposes (USSR author's certificate No. 1171470, C08F 220/18, 1985), including radical emulsion copolymerization of butyl acrylate and acrylic acid, and treating the reaction mixture with an aqueous solution of ammonia. The method includes separate injection into the reactor monomers, aqueous solution of sulfated ethoxylated Nonylphenol, ammonium persulfate, and then heated to 65-70°and, when the achievements the Institute of 4-10% conversion of the monomers, adding an aqueous solution of ammonia in quantities of 0.5-1.0 equivalent relative to acrylic acid. At the end of the dosing monomers the polymerization continued for 4 hours with continuous stirring and purging with nitrogen. The finished dispersion has a dry matter content 59-60 wt.%, the viscosity of 4.0-8.7 PA·C. the content of the coagulum in the description is missing. Reproduction of this author's evidence shows that the dispersion has a content of the coagulum from 5 to 8 wt.%. In addition, based adhesive dispersions obtained in this way does not provide sufficient adhesive properties.

The closest in technical essence of the present invention is a method of obtaining a water dispersion (co)polymers according to the patent of Russian Federation №2076109, C08F 2/24, 1997 - prototype. The method of obtaining aqueous dispersions of (meth)acrylic or (meth)akriliniu polymers prototype includes radical emulsion polymerization of a pre-emulsified (meth)acrylic monomers or mixtures thereof with vinyl monomers. At the stage of preliminary emulsification to prepare an emulsion when the mass ratio of monomer:water of 1:(0.1 to 0.7)and as an emulsifier use of ionic compound of the formula R-O(CH2CH2O)n-XO3Me (1), where X Is S, P, Me=Na, K, NH4when R is alkyl n=1-13, R - alkylphenyl, dialkylphenol n=6-30 is whether its mixture with nonionic compound of General formula: R-O(CH 2CH2O)n-N (2)where R is alkylphenyl, dialkylphenol n=6-100, containing at least 0.4% by weight of monomers of the compounds of formula (1) in General the content of the emulsifier is not less than 0.5% by weight of monomers. The prepared emulsion of monomers is metered into the reactor for 1.5 to 2.0 hours and simultaneously carry out the dosing of the total amount of the polymerization initiator. As an initiator of polymerization using potassium persulfate or ammonium. The temperature of polymerization 75-80°C. After the dosage of the monomers, the reaction mass was incubated for 30 min at a temperature of 80±2°and zakolerovat. As acrylic monomers using a methacrylate, acrylate, butyl acrylate, 2-ethyl hexyl acrylate, acrylic acid, as methacrylic monomers: methyl methacrylate, methacrylic acid. As vinyl monomers: styrene, vinyl acetate.

The main drawback received on the prototype of a water dispersion of a (meth)acrylic copolymer is a low concentration of the copolymer. The concentration of copolymer in the patent is not given. It is obtained by calculation from the above description and examples is 50-55 wt.%. The description also provides data on the content of the coagulum in the dispersion and adhesion characteristics. Was reproduced in the method according to example 10 of the description of the prototype, which is the closest in composition to polymerize the mixture to declare, and obtained the necessary data for comparison. The content of the coagulum upon receipt dispersion was 0.1 wt.%, and strength when peeling the adhesive on the basis of GOST 289666.2-91 - of 0.51 kN/m

The aim of the invention is to increase the concentration of aqueous dispersion of acrylic copolymer with a low content of the coagulum and improve its adhesion properties.

To achieve this goal, we propose the following method of obtaining a water dispersion of acrylic copolymer.

The previously prepared emulsion of comonomers in water at a mass ratio comonomer:water of 1:(0,2-0,3), in the presence of 3.4 to 4.0 wt.% ammonium salt sulphoxidation alkylphenol, where the alkyl, C8-C10, co degree of sulfation 17-26 wt.%. As comonomers use butyl acrylate, vinyl acetate, acrylic and methacrylic acid.

The finished emulsion of monomers is metered into the reactor within 3-10 hours and parallel to submit to 0.3-0.6 wt.% of ammonium persulfate or potassium when the total mass ratio in the reaction mass comonomer: water of 1:(0.4 to 0.5). Polymerization occurs at a temperature of 78-82°C.

After dispensing the emulsion and polymerization initiator are depolymerization residual monomers by filing 0.1 wt.% of potassium persulfate or ammonium after holding the reaction is second mass within 0.5 and 1.5 hours at a temperature of 78-82° C. Further maintain the reaction mass at a temperature of 78-80°C for 2 hours and cooled.

The result is a dispersion of acrylic copolymer containing copolymer 69,5-to 70.2 wt.%.

The essence of the invention is illustrated by the following examples.

Example 1

In a reactor equipped with reflux condenser, stirrer and a funnel for dispensing components, load 30 g of water and raise the temperature to 80±2°C. the Previously prepared emulsion of monomers with water and an emulsifier, as follows: into a glass placed 114 g of water, 31 g 79% ammonium salt sulphoxidation of Nonylphenol with a degree of sulfation 26 wt.% (3.4 wt.%) and the whole monomer mixture 465,5 g (64,0%) of butyl acrylate (TU 2435-002-52460063-2003) and 24.5 g (3.4 wt.%) methacrylic acid (TU 6-02-59-89). After stirring for 30 minutes was formed white viscous mass. Next, prepare a solution of the initiator in 60 g of water was dissolved 2,94 g of ammonium persulfate (GOST 20478) (0.4 wt.%). At the dosage used 50 g of the solution of the initiator.

The total water content in the reactor is of 28.8 wt.%.

When the temperature reached 80±2°C reactor start dosing emulsion and initiator solution within three hours. At the end of the dosing emulsions give exposure for 0.5 hours, then add a solution of initiator - 5 grams a half hour the extracts add the remaining initiator solution - 5, Maintain the reaction mass at 78-80°two hours and cooled to 20-30°C, filtered through a nylon sieve and pour into clean, dry container.

Next, determine the properties of the resulting dispersions.

The concentration of the copolymer determined through a mass fraction of solids according to GOST 17537. To do this, take out a portion of the dispersion by weight of 0.5-1.0,

Drying of the sample produce over 3 hours at a temperature of (110±2)°in a drying Cabinet to constant weight.

The content of the coagulum obtained in the polymerization process, determine dry from the total amount of coagulum, remaining on the filter walls of the reactor and the stirrer.

The grain size dispersion is determined visually. This dispersion is applied in a thin layer (˜20-30 microns dry) on a glass plate or a polymer film and light to determine the grain size on a scale from 0 (very good, no microcoagulation) to 10 (very bad, many microcausality).

Neutralization of the resulting dispersion is carried out by introducing ammonia to a pH of 6.5-7.5. Get a homogeneous adhesive composition, which is used to evaluate adhesion properties.

Adhesive properties characterize a measure of the strength at breaking PET-gr. steel, which is determined according to GOST 28966.2-91. The thickness of the adhesive layer was 60 μm.

The degree sulfation the Oia ethoxylated alkylphenol (OP-10) (mass fraction of ammonium salt of the sulfated material) was determined by titrimetric method in the environment of acetone with the indicator thymol blue method developed by the Federal state unitary enterprise "Institute of polymers".

The test results obtained dispersion is given in the table.

Examples No. 2-4

The polymerization is conducted as in example No. 1, except that use ammonium salt sulphoxidation of Nonylphenol with varying degrees of sulfation: example No. 2 - 17 wt.%; example No. 3 - 19 wt.%; example No. 4 - 21 wt.%. Properties of the resulting dispersions are given in the table.

Example No. 5

The polymerization is conducted as in example No. 1 with the difference that the monomer mixture used 420,4 g (57,4 wt.%) of butyl acrylate, 70,0 g (9.6 wt.%) vinyl acetate, 9,8 g (1.3 wt.%) methacrylic acid, and as an emulsifier - 32,9 g 82% ammonium salt sulphoxidation of Nonylphenol with a degree of sulfation 19 wt.% (3.7 wt.%). The amount of initiator was 4.9 g of ammonium persulfate (0.7 wt.%). Properties of the resulting dispersions are given in the table.

Example No. 6

The polymerization is conducted as in example No. 1 with the difference that the monomer mixture used 445,0 g (60,7 wt.%) of butyl acrylate, and 11.5 g (1.6 wt.%) acrylic acid and 11.5 g (1.6 wt.%) methacrylic acid, 35,3 g 79% ammonium salt sulphoxidation of Nonylphenol with a degree of sulfation 17 wt.% (3.8 wt.%). Properties of the resulting dispersions are given in the table.

Example No. 7 (prototype)

Mix 168 g (40,7 wt.%) of butyl acrylate, 28 g (of 6.8 wt.%) is enolacetate, 4 g (1.0 wt.%) of methacrylic acid, 80 g of water, 10 g (2.6 wt.%) ammonium salt sulphoxidation of Nonylphenol. Since the degree of sulfation was not specified, we used the emulsifier with the degree of sulfation 17 wt.%. Stirred until the formation of a stable homogeneous emulsion. The resulting emulsion is metered into the reactor containing 100 g of water for 1.5 h at 75°With, at the same time submit the ammonium persulfate in an amount of 2.0 g (0.5 wt.%), dissolved in 20 g of water. At the end of dosing the mixture was incubated for 30 min at 80±2°and zakolerovat. Properties of the resulting dispersions are given in the table.

The total water content in the reactor 48.4 wt.%.

Examples No. 8-13 (for comparison)

Conditions of formation and properties of the dispersions are shown in table.

11.
Table
Conditions of formation and properties of the dispersions used as adhesives, pressure-sensitive
no PPThe reaction mixture composition, wt.%Conditions for obtaining varianceThe properties of the dispersions and adhesives based on it
Monomeric mixtureWaterEmulsifier - ammonium salt sulfo-oxyethylene the data alkylphenol degree of sulfation) InitiatorThe ratio of the phases, the monomer/waterThe dosing time of the emulsion, hTime-temperature exposure, hMass fraction of non-volatiles, wt.%The content of the coagulum, wt.%Grain, pointsStrength when peeling, kN/m
123456789101112
1.BA 64,0 MAC 3,428,83,4 (26)the ammonium persulfate and 0.41:0,433of 0.5, 1.5, and 2.069,50,10-20,70
2.BA 63,7 MAC 3,428,83,7 (17)the ammonium persulfate and 0.41:0,4330.5, 1.5, and 2.069,8040,74
3.BA 63,7 MAC 3,428.83,7 (19)the ammonium persulfate and 0.41:0,433of 0.5, 1.5, and 2.0to 70.20 30,70
4.BA 63,7 MAC 3,428,83,7 (21)the potassium persulfate and 0.41:0,4310of 0.5, 1.5, and 2.070,000-20,67
5.BA 57,4 VAC 9.6 MAC 1,327,33,7 (19)the ammonium persulfate 0,71:0,43of 0.5, 1.5, and 2.069,50,430,67
6.BA 60,7 MAC 1,6 AK 1,631,74,0 (17)the ammonium persulfate and 0.41:0,55of 0.5, 1.5, and 2.069,61,340,60
To compare
The placeholderthe persulfate
7.BA 40,748,42,6ammonium1:0,431,50,550,0 0,160,51
VÁC 6,8(17)0,5
MAC 1,0
8.BA 63,728,83,7the persulfate1:0,433of 0.5, 1.563,528,680,43
MAC 3,4(15)ammoniumand 2.0
0,4Ȁ
9.BA 63.728,83.7the persulfate1:0,433of 0.5, 1.570,32,340,52
POPPY 3.4(28)ammoniumand 2.0
0.4
10.BA 64.429,12,7the persulfate1:0,433of 0.5, 1.5100% coagulum
POPPY 3.4(17)ammoniumand 2.0
0,4
BA 63.128,5the 4.7the persulfate1:0,433of 0.5, 1.571,01,140,55
MAC 3.3(17)ammoniumand 2.0
0,4
12.BA 69.822,04,1the persulfate1:0,33of 0.5, 1.573,112,150,54
MAC 3.7(17)ammoniumand 2.0
0.4
13.BA 63.739,83,1the persulfate1:0,730,5 and 2,041,2000,34
POPPY 3.4(17)ammonium
0.4

From the table it follows that the proposed method of obtaining a water dispersion of acrylic copolymer allows to obtain a dispersion having a concentration of the copolymer 69,5-to 70.2 wt.%, with the content of the coagulum 0-1,3 wt.% and strength when peeling the adhesive on its basis 0,60-to 0.74 kN/m (see examples No. 1 to 6). These figures are significantly higher than the prototype, which has a concentration of the copolymer 50-55 wt.% and rocheste when peeling ˜ of 0.51 kN/m the content of the coagulum in the prototype is ˜0.1 wt.% (see example No. 7).

Changing the terms of the proposed method of obtaining dispersion leads to deterioration of the quality of dispersion.

Data presented in table shows that only the use of ammonium salts sulphoxidation alkylphenol, where the alkyl, C8-C10with a degree of sulfation 17-26 wt.% allows you to obtain a dispersion with improved properties. Use sulphoxidation alkylphenol with a degree of sulfation outside the claimed, for example, 15 wt.% and 28 wt.% results in dispersions with a high content of coagulum (28,6 wt.%) and low adhesion (0,43-0,52 kN/m) (see examples No. 8-9).

The use of ammonium salts sulphoxidation alkylphenol with a degree of sulfation 17-26 wt.% the number outside the claimed increases the content of the coagulum and to reduce adhesion properties (see examples No. 10-11).

The polymerization of the monomers in the present method is carried out with continuous dosing of the emulsion of the monomers and initiator within 3-10 hours. Reducing the time of dispensing, for example, up to 2 hours leads to an increase of the content of the coagulum to ˜2-3% and reduce the adhesion properties to 0,4-0,5 kN/m Rise time dispensing reduces its adhesive is TBA dispersion ˜ 0,5 kN/m

The claimed method of pre-emulsification is carried out at a mass ratio comonomer:water of 1: (0.2 and 0.3). Beyond these ratios degrades the quality of the water dispersion.

The implementation of the polymerization at a mass ratio in the reaction mass comonomer: water of 1:(0.4 to 0.5), is also the essential feature of the proposed method. Beyond the claimed ratios, for example 1:0.3 or 1:0.7 and increases the content of the coagulum in the dispersion and reduces its adhesive properties (see examples No. 12-13).

Increase the exposure time on the stage of depolymerization compared to the prototype is required to complete depletion of residual monomers for obtaining highly concentrated copolymer.

Thus, only the combination of all the above essential features of the proposed method allows to obtain a water dispersion of acrylic copolymer for adhesive, pressure-sensitive, with a high concentration of polymer with a low content of coagulum and high adhesive properties. Exclusion of any of the above features of the proposed method significantly affects the quality of the water dispersion and limits its use as an adhesive, pressure-sensitive.

1. A method of obtaining a water dispersion of AllowOverride for adhesives, pressure-sensitive, by pre-emulsification mixture of butyl acrylate with (meth)acrylic and/or vinyl monomer with water and emulsifier - ammonium salt sulphoxidation alkylphenol, subsequent emulsion copolymerization at a temperature of 78-82°in the presence of a radical initiator and temperature exposure of the dispersion, wherein the pre-emulsification of the comonomers in water is carried out at a mass ratio comonomer: water of 1:(0,2-0,3), in the presence of 3.4 to 4.0 wt.% ammonium salt sulphoxidation alkylphenol, where the alkyl, C8-C10with a degree of sulfation 17-26 wt.%, and emulsion polymerization is carried out for 3-10 h with continuous dosing of pre-obtained emulsion of comonomers and 0.3-0.6 wt.% of ammonium persulfate or potassium when the total mass ratio in the reaction mass comonomer:water of 1:(0.4 to 0.5), followed by depolymerization reaction mixture with the introduction of 0.1 wt.% of ammonium persulfate or potassium by 0.5 and 1.5 h exposure of the reaction mixture and the final temperature exposure for 2 hours

2. The method according to claim 1, wherein the depolymerization reaction mixture and the final extract obtained dispersion is carried out at a temperature of 78-82°C.



 

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2 cl, 1 tbl, 24 ex

FIELD: polymer production.

SUBSTANCE: invention relates to processes of producing lacquer acrylic filming agents used in manufacture of masonry, road-line, and other paints. Process of invention is realized by two-step polymerization of butyl acrylate, methyl methacrylate, styrene, and methacrylic acid at ratio (40-5):(40-45):(10-14):(1-5) in toluene-ethyl acetate mixture, while portionwise feeding monomers/initiator mixture and repeatedly ageing reaction mixture. When conversion of monomers attains 82-85%, solution of butyl acrylate/styrene/methacrylic acid copolymer is additionally charged at ratio 42:57:1 dissolved in toluene/butanol (or ethanol) mixture or toluene/acetone mixture, or in toluene/ethyl acetate/ethanol/butanol mixture. Butyl acrylate/styrene/methacrylic acid copolymer is added in amount 1.77-4.0% based on concentration of principal substance. Toluene and ethyl acetate are used in proportion (0.1-1.0):1. In the first stage, 20-30% of butyl acrylate/methyl methacrylate/styrene/methacrylic acid mixture is added and, in the second stage, 70-90%. Thus obtained filming agent is characterized by high content of nonvolatile substances at rather low viscosity, high adhesion, good strength and film drying rate, low moisture absorption, high water and wear resistance.

EFFECT: improved performance characteristics of agent.

9 cl, 4 tbl, 7 ex

FIELD: polymer production.

SUBSTANCE: invention relates to a method for production of high-molecular weight water-soluble polymers used as flocculant at enterprises of water conditioning, petroleum processing, petrochemistry, iron and nonferrous metallurgy, paper-and-pulp, varnish-and-paint, chemical, and other industries. In particular, invention provides a method for production of high-molecular weight (meth)acrylic anionic flocculant via copolymerization of water-soluble anionic ethylenically unsaturated monomer with nonionic ethylenically unsaturated monomer, the former being salt of (meth)acrylic acids and the latter (meth)acrylic acid amide and ester at salt/amide/ester ratio 100:10:(1-6) or 100:(1-6):10. Proposed method leads to production of high-molecular weight (meth)acrylic anionic flocculant in the form of powder with nearly 100% content of principal substance, which is well dissolved in water.

EFFECT: enhanced efficiency in treatment of various disperse systems (industrial effluents).

3 cl, 4 tbl, 4 ex

FIELD: chemical industry, chemical technology, polymers.

SUBSTANCE: invention relates to a method for preparing aqueous polymer dispersions of the multipurpose designation. Method for preparing an aqueous dispersion of styrene-acryl copolymer is carried out by preliminary emulsifying a mixture of acrylic monomers with styrene in the presence of emulsifying agent and the following aqueous-emulsion co-polymerization of the reaction mixture in the presence of initiating agent. Monomer mixture comprises additionally acrylamide, and method involves using ammonium persulfate and hydrogen peroxide as an initiating agent. Method involves the successive fractionally dosing feeding ammonium persulfate for two stages followed by addition of a mixture of polymethylsiloxane of molecular mass 55-1000 Da and iron sulfate in their mass ratio = (25-35):1 to the reaction mixture at stirring, cooling the reaction mass and its neutralization to pH = 5-6. Invention provides preparing the stable aqueous polymeric dispersion with diminished size of particles. Invention provides enhancing strength and water resistance of film prepared on its base.

EFFECT: improved preparing method.

1 tbl, 3 ex

FIELD: polymer materials.

SUBSTANCE: sheet organic glass is obtained by way of bulk (co)polymerization of (meth)acrylic acid esters in presence of UV absorber, radical polymerization initiator, and light-absorbing additive. Process involves monomer prepolymerization and subsequent final polymerization if mixture in flat-parallel mold. Methacrylic acid esters utilized are, in particular, methyl methacrylate or its mixtures with (meth)acrylic acid or (meth)acrylic acid esters. Light-absorbing additive is methane decomposition product obtained in high-voltage discharge plasma at atmospheric pressure and characterized by loose density 0.65-0.85 g/cm3 and specific pore volume 0.40-0.50 cm/cm3. Additive, taken in amount 0.001-0.01 wt parts per 100 wt parts monomer, is mixed with prepolymer. Resulting mixture is affected by ultrasound and then polymerized in mold until conversion is completed. Sheets manufactured according to invention are suitable for neutral light filters employed in instrumentation engineering, in personal protection devices, and in sporting airplane glazing operations.

EFFECT: improved optical characteristics of glass due to more uniform light transmission in visible spectrum region.

1 tbl, 15 ex

The invention relates to the production of aqueous latexes with podyma polymer particles

FIELD: polymer materials.

SUBSTANCE: sheet organic glass is obtained by way of bulk (co)polymerization of (meth)acrylic acid esters in presence of UV absorber, radical polymerization initiator, and light-absorbing additive. Process involves monomer prepolymerization and subsequent final polymerization if mixture in flat-parallel mold. Methacrylic acid esters utilized are, in particular, methyl methacrylate or its mixtures with (meth)acrylic acid or (meth)acrylic acid esters. Light-absorbing additive is methane decomposition product obtained in high-voltage discharge plasma at atmospheric pressure and characterized by loose density 0.65-0.85 g/cm3 and specific pore volume 0.40-0.50 cm/cm3. Additive, taken in amount 0.001-0.01 wt parts per 100 wt parts monomer, is mixed with prepolymer. Resulting mixture is affected by ultrasound and then polymerized in mold until conversion is completed. Sheets manufactured according to invention are suitable for neutral light filters employed in instrumentation engineering, in personal protection devices, and in sporting airplane glazing operations.

EFFECT: improved optical characteristics of glass due to more uniform light transmission in visible spectrum region.

1 tbl, 15 ex

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