FI64384C - FOERFARANDE FOER FRAMSTAELLNING AV DISPERGERBARA DISPERSIONSPULVER SAMT DERAS ANVAENDNING - Google Patents

Description

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Patent and Registration Office .... ... , . ,,,. , · (44) Date of issue and date of publication. -

Patent and Registration Office of the United Kingdom of Great Britain and Northern Ireland 29.07.8 (32) (33) (31) Request for Privilege — Begird prlorltet 02. Cl.76

Federal Republic of Germany-Förbundsrepuhliken iyskiand (DE) P 26ll26l.O

(71) Hoechst Aktiengesellschaft, 6230 Frankfurt (Main) 80, Federal Republic of Germany-Förbundsrepubliken (DE) (72) Detlev Seip, Kelkheim, Wolfgang Zimmermann, Kelkheim, Federal Republic of Germany-Förbundsrepubliken lyskland (DE) (7l) Oy Kolster Ab (5 * 0 Method for the preparation and use of dispersible dispersion powders - Förfarande för framställning av dispergerbara disp-persionspulver samt deras användning

The invention relates to a process for the preparation of dispersible vinyl acetate copolymer dispersion powders and to the use of these powders in the field of application of coating and construction.

More specifically, the invention relates to a process for the preparation of water-dispersible dispersion powders suitable for use as a binder in plastic plasters and plasters by emulsion copolymerization with a straight chain of vinyl acetate having 3 to 18 carbon atoms. or branched esters of branched carbosyl acids, acrylic, methacrylic, maleic or fumaric acid esters of aliphatic alcohols having 1 to 18 carbon atoms, vinyl chloride or * -olefins and / or ethylene having 1 to 12 carbon atoms and, optionally, monovalently active possibly using external plasticizers in the presence of a radical initiator and in the presence of 2 64384 additional emulsifiers as well as 5 to 20% by weight of the copolymer. at least one polyvinyl alcohol having a viscosity in a 3% aqueous solution at 20 ° C of 3 to 5 mPas and an ester number of 90 to 215 mg KOH / g followed by a spray-dried copolymer dispersion with simultaneous but different addition of 2 to 2% by weight - #, based on the dry matter content of the aqueous dispersion, anti-caking agents having a particle size of 0.01 to 0.5. This process is characterized in that the emulsion copolymerization of the monomers is carried out at a temperature of TC-1 ° C in the presence of a) 0.02-1.0 wt.% Emulsifier, based on the copolymer, and h) 0.05-2.0 wt.%. an ionic emulsifier containing oxyethylene groups, calculated on the copolymer.

Water-dispersible vinyl acetate homopolymer and copolymer dispersion powders are known. Homopolymer dispersion powders have a use mainly in the adhesive industry, while copolymer dispersion powders have a use mainly in the coating and building material industry. In addition to the general requirements for a dispersion powder, such as high storage stability, good readiness and good dispersibility in water, there are special requirements when used in the coating and building material field. Thus, for dispersions obtained from dispersion powders with water, the minimum film r. Formation temperature should be about ° ° C and the polymers should have good stability against bases. In combinations with hydraulically binding binders, the dispersion powders should be well compatible and provide improved tensile and compressive strength of the specimens. For surface coating layers, such as asbestos cement, wood and masonry in so-called plastic-bound mortars, the sole binder used is required to have a particularly high adhesion and abrasion resistance of the mortar mixtures bound by the dispersion powders on all substrates, especially when wet.

DE 1 719 317 describes a process for the preparation of non-agglomerated, dispersible powders from vinyl acetate polymers and copolymers by drying the dispersions. Dispersions are prepared using polyvinyl alcohols as a protective colloid, and with a change in monomers of 80-90 #, 0.5 parts by weight of polyvinyl alcohols are added with a viscosity of the dispersion of 3-13.

II

3 64384 mPas (k% solution at 20 ° C) and a degree of hydrolysis of 75-95 mol%. Dispersion powders prepared according to German bulletin 1 7-9 317 do not meet the conditions for the production of sufficiently water-resistant plastic-bonded mortars.

DS-A-2 013 2U3 discloses a process which is not similar to the process according to the present application, but the said DE-publication a does not disclose an essential feature of the invention according to the application, namely the use of a large amount of polyvinyl alcohol. On the contrary, that publication literally warns against the addition of a large amount of polyvinyl alcohol, since, according to its example 7, the use of a large amount of protective colloid does not give a stable dispersion.

DE-A-2 214 1010 describes a process for preparing a redispersible vinyl acetate / ethylene copolymer dispersion powder by flake-drying a vinyl acetate / ethylene-soda polymer dispersion. Dispersions are prepared at ethylene pressures up to 100 atmospheres and preferably at polymerization temperatures of 50-7 ° C with the addition of small amounts of ionic pig emulsifiers and polyvinyl alcohol as a protective colloid. Plastic mortars made using these dispersion powders are very water resistant. However, if the vinyl acetate / ethylene i-s copapolymer i-d is dispersions are prepared at polymerization temperatures above 70 ° C in order to shorten the polymerization time, then the plastic-bonded mortars made from the dispersion powders obtained are no longer sufficiently water-resistant. However, when using a vinyl acetate / ethylene copolymer dispersion, polymerization temperatures above 70 ° C are desirable because dispersions with shorter monomer dosing times can be prepared more economically.

The polymerization temperature of 20 to 100 ° C, preferably 50 to 7 ° C, must be used in the process according to DE application publication 2 2hh10. This information should be understood as a recommendation to work at temperatures below 7C ° C. In the process according to the invention, on the other hand, a polymerization temperature of 70 to 100 ° C is used, since it is preferable to carry out the polymerization at a higher temperature.

6 4 3 8 4

A copolymer dispersant prepared by the process of the invention. the vinyl acetate content is preferably greater than 00% by weight. Suitable mixed monomers for vinyl acetate are vinyl esters of straight-chain and branched carboxylic acids having 3 to 18 carbon atoms, acrylic, methacrylic, maleic alcohols of aliphatic alcohols having 1 to 1 carbon atoms. or fumaric acid esters, v-nyl chloride or β-olefins containing h-12 C atoms, such as isobutylene and / or ethylene. Suitable monomer combinations include vinyl acetate / 2-ethylhexanoic acid vinyl ester, vinyl acetate / vinyl laurate, vinyl acetate / vinyl ester of 10 C-branched carboxylic acids, vinyl ethylene, vinyl acetate aat ti / vir.ylpi valat ti / ethylene and vinyl asat aat ti / vi nyyl ik Lori di / ethylene.

Monomer combinations with a minimum film-forming temperature of about 0 ° C for the corresponding dispersions are preferred. But vinyl acetate monomer combinations with a minimum film-forming temperature for the corresponding dispersions above 0 ° C and further reduction to about 0 ° C are also preferred. long chain Adipic and fatal acid esters, trialkyl and triaryl phosphoric acid esters or glycerol esters of Sten carboxylic acids. In addition to the monomers mentioned, other monomers which stabilize the dispersion can also be added, such as, for example, monom.ee containing carboxyl groups, such as acrylic, methacrylic, crotonic or itacenic acid. mono styrene acids, the alcoholic components of which may contain from 1 to 18 carbon atoms, acrylamide or methacrylamide in concentrations up to 5% by weight of the total polymer. In addition, crosslinking components can also be used, for example compounds containing ethylene groups, such as N-methylolacrylic amide, or monomers containing two or more unsaturated double bonds, such as diallyl maleate, tetraallyloxyethane or adipic acid vinyl ester.

The palatable emulsifier / protective colloidal system of the invention, which is formed by the copolymer dispersions of vinyl acetate used in the required dispersion powders, consists of ionic and non-ionic polyvinyl alcohol emulsions. Jor.isia emulsifiers Tor are not used, calculated as the amount of 0, OP-1 O'ino%, cd · relative to the polymer; lii r.esti 0.0 Ö ~ 0.1 L by weight ?, otiull iu <'s ti added

II

5 64384 charge of alkyl sulphate type emulsifiers containing 1C-J.6 C atoms. Nonionic oxyethylated emulsifiers are added to the charge relative to the polymer in amounts of 0.05 to 2% by weight, preferably 0.1 to 1% by weight. Preferred emulsifiers of this type include oxyethylated aliphatic alcohols, oxyethylated alkylthenols and oxyethylated polypropylene glycols. One or more types of polyvinyl alcohol are used in amounts of 5 to 20% by weight, preferably 7 to 15% by weight, based on the polymer, with an ester number of 90 to 215 mg XOH / g, in particular 90 to 160 mg KOH / g and a viscosity of a% aqueous solution. at 20 ° C 3-30 mPas, especially b-20 mPas. For the preparation of the dispersion powder according to the invention, it is advantageous if 50 to 90% by weight of the batch polyvinyl alcohol is included in the polymerization solution at the beginning of the dispersion and 10 to 50% by weight is subsequently added to the aqueous solution of the finished dispersion. The pH of the dispersion solution is adjusted to U-7.5. A suitable buffering agent such as sodium acetate, sodium phosphate or sodium bicarbonate may be added to adjust the pH of the dispersion solution.

o

The emulsifier / protective colloid system allows for particularly preferred polymerization temperatures above 70-100 ° C. The higher the polymerization temperature, the more economical the method, because the higher the polymerization temperature, the polymerization heat can be more easily dissipated and thus the monomer dosing time and thus the total preparation time of the dispersion can be shortened.

With the polymerization initiators a, the usual radical initiators of the charge are added, in particular water-soluble basic compounds, but also monomer-soluble compounds.

The solids content of the vinyl acetate copolymer dispersions is about 30 ~ βθ by weight. After completion of the polymerization, a solids content of about 30-30% by weight suitable for flake drying is adjusted by adding water or an aqueous solution of polyvinyl alcohol.

Aqueous plastic dispersions are prepared according to the invention. . . . . . . .., o di sper s xopulver it hiutaiekui stake. If the contribution to Iisana is about 0 C ·. In order to ensure good storage stability of the dispersion powder, anti-caking agents must be used in the flake drying in order to ensure a good storage stability of the dispersion powder. Suitable anti-caking agents include aluminosilicates having an average particle size of about 0.01 to 0.5, as well as carbonate acids or n-i 646384 acids. Particularly preferred anti-caking agents are silicic acids and aluminosilicates, with preferred amounts being from 2 to 20% by weight based on the solids content of the aqueous plastic dispersion. The anti-caking agent is fed simultaneously but separately from the aqueous dispersion to the flake drying tower. This way of adding an anti-caking agent largely prevents the formation of an undesired wall cover of the dryer.

The dispersion powders prepared according to the invention have good storage stability, are very ready-to-use and can be mixed with water rapidly into homogeneous dispersions which are stable in viscosity and storage. They are well suited for the manufacture of adhesives, glues and coatings. They are particularly useful for the dry production of plastic bonded mortars. These plastic-bonded mortars are prepared by carefully mixing various granular mineral additives with the vinyl acetate mixed polymer powders of the invention. At the construction site, these dry powders are mixed with water and applied in a suitable manner to the wall or masonry. After drying, these plastic-bonded mortars largely meet the requirements imposed on them, such as good wet and dry adhesion and good water resistance.

Example 1 1. Preparation of vinyl acetate / ethylene copolymer dispersion A solution adjusted to pK 6.0 consisting of 7 parts by weight of sodium lauryl sulfate, 76 parts by weight of ethanol is introduced into a 30-volume pressure reactor equipped with a temperature control apparatus and a stirrer. of oxyethylated nonylphenol α, 6 8 0 parts by weight at 20 ° C as a 4% aqueous solution of polyvinyl alcohol having a viscosity of about 8 mPas and an ester number of 1 * 0 mg KOH./g, 139 parts by weight at 20 ° C: as a U% aqueous solution having a viscosity of about 18 mPas and an ester number of li + 0 mg KOH / g, 15.3 parts by weight of anhydrous sodium acetate and 7700 parts by weight of water. The reactor is purged with nitrogen and ethylene to thoroughly remove all oxygen. The stirrer is then set at 150 rpm, 70% by weight of vinyl acetate is added, the contents of the reactor are heated to 60 ° C, a solution of 6 parts by weight of ammonium persulphate in 500 parts by weight of water at 60 ° C is added and the contents of the vessel are further heated. 80 ° C. During the heating operation, ethylene τ 64384 is added until the pressure is 20 bar. When the internal temperature of 80 ° C is reached, a five-hour dosing of 6830 parts by weight of vinyl acetate and 4.2 parts by weight of 350 parts by weight of aqueous ammonium persulphate is started at an interior temperature of 80 ° C and an ethylene pressure of 20 bar. After the additional addition has been stopped, the solution is subjected to an exchange reaction with a solution of 1.8 parts by weight of ammonium persulfate in 155 parts by weight of water and reheated for 1.5 hours at an external temperature of 85 ° C. The ethylene import is then stopped and the dispersion is cooled to room temperature. A solution of 220 parts by weight of kneyl alcohol of 1280 parts by weight, having a viscosity of a 4% aqueous solution of polyvinyl alcohol at 20 ° C and about 4 nPas and an ester number of 1 mg mg KOH / g, is then added to the dispersion. After that, pi s run at 50 percent. the vinyl acetate / ethylene copolymer dispersion has an ethylene content of about 14% by weight, a residual monomer content of 0.5% by weight, a latex viscose bond (Ξρρ-rechtreometn C / II, at 25 ° C) 5> L Pas <] a minimum film melting temperature-la k 0 ° 0.

2. Vinyl acetate / ethylene sekapolymeeripulverir. manufacturing

The vinyl acetate / ethylene copolymer dispersion prepared in Example 1, 1 is diluted with water to a solids content of 3% by weight before drying the flakes. A sprayer is used as the drying device, the cylindrical part having a diameter of 1.6 m and a length of 4 m and a conical part having a length of 2 m. The dispersion is fed into the nozzle by spraying two substances with a flow opening of 0 mm with an eccentric screw pump. Drying takes place downstream, the drying gas is nitrogen with a consumption of 7 5 5 irt '/ h. The temperature of the drying gas at the weather point s a is 115 ° C and sv> 1 o .: at 65 ° C. The spray air consumption of the product nozzle is 70 parts by weight at a pre-player pressure of 5 bar and a temperature of 23 ° C. Through the second two nozzles, located close to the tower wall just below the product nozzle, a finely divided silicic acid powder with a SiO 2 content of 93%, B2T-p .: r.ta-area O, is dispensed into the flake drying tower simultaneously with the dispersion as an anti-caking agent. , 250 m / g and the average size of the primary particles δ, 0.1 μm, in an amount of 5% ve si di sper si is calculated relative to the amount of solids. The resulting dispersion powder is very flowable and very storage stable, sr is, β 64384 powder sample is also 2 ^ hour at its 50 ° C *. easily fluffed after storage at 2 ° C / cm 2. The bulk density of the powder is 330 g / liter, the shaking density is 3% and the bulk density is 70 g / liter. The powder is easily miscible with water to give a stable dispersion with a viscosity of 7.3 Pas, measured with a 50% dispersion (3 pprecht rheomer C / II, at 25 ° C).

In addition to the suitability of adhesives, glues and coatings for lighting, this powder can be used as the sole binder in plastic dry mortars with excellent properties. manufacturing. The table below provides a selection of different instructions for making nucleosides. The mortars are prepared by vigorously mixing the solid ingredients together, then adding water, mixing again and applying the mortars with a scraper or a mortar to the asb cement test plates under a layer of about> mm. Dryer mortars are characterized by very good water resistance and very good adhesion to the substrate. After storage of the boards in water, the mortars remain virtually unchanged. Their adhesion to asbestos cement in is very good and wet abrasion is insignificant.

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Comparative Example I

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According to the procedure described in Example I, a vinyl acetate / ethylene copolymer dispersion is prepared at a polymer temperature of 6 ° C at 20 bar and an ethylene pressure of 20 bar, with the change from Example 1 that the polymerization solution does not contain oxyethylated nonyl phenol. The low polymerization temperature of 60 ° C and the associated polymerization temperature. Due to the inconvenience, the monomer dosing time must be added to Example 1 Repeat from five to eight hours. As described in Example 1, the resulting 50% vinyl acetate / ethylene copolymer dispersion can be flake-dried in the presence of the anti-caking agents described therein to a stable dispersion powder suitable for the production of plastic-bonded mortars with good water resistance.

Comparative Example II

In the preparation of the vinyl acetate / ethylene copolymer di spers ion, the procedure is as in Comparative Example I, but proceeding as in Example I at the desired high polymerization temperature of 80 ° C. The monomer addition time was (as in Example 1) 5 hours. The obtained vinyl acetate / ethylene copolymer dispersion could be flake-dried in the presence of an anti-caking agent silicic acid into a dispersion powder according to the procedure described in Example I. However, Once the dried mortars have been stored in water, the mortar can be easily separated from the substrate and rubbed off the surface. Comparative Examples I and II show that, in order to achieve the goal of low and economically unfavorable polymerization times with low polymerization temperatures, the mixing of the emulsifier / protective colloid system according to the invention can be dispensed with. However, at economically favorable high polymerization temperatures, the desired goal is achieved only by using the emulsifier / protective colloid system according to the invention.

Example II

In a 100-volume polymerization vessel equipped with an anchor stirrer and a reflux condenser, a copolymer dispersion of vinyl acetate is prepared at a polynerization temperature of 80 ° C at 80 ° C and a monomer addition time of 2.5 hours using a polymerization solution of 30,800 The viscosity of a 4% aqueous solution at 20 ° C is 8 ns and the ester number is 1 to 0 mg KOH / g, 150 parts by weight of oxyethylated polypropylene glycol having a molecular weight of about 2000 with an ethylene oxide content of about 40% by weight. parts by weight of sodium sulphate sulphate and 53 parts by weight of anhydrous sodium acetate, a monomer mixture consisting of 18C parts by weight of vinyl acetate and 12000 parts by weight of 1C carbon-branched craboxylic acids an ester and a catalyst solution consisting of 55 parts by weight of ammonium persulfate and 800 parts by weight of water. After preparation, the dispersion is subjected to an exchange reaction of 990 parts by weight of phthalododibutyl ester with a solution of 750 parts by weight of polyvinyl alcohol in 3000 parts by weight of a water having a viscosity of 2% aqueous polyvinyl alcohol at 2 ° C and h mPas and ester number iUc mg KOH . The resulting copolymer copolymer of about 50% vinyl acetate has a minimum film-forming temperature of 0 ° C and a latex viscosity of 2.5 Pas measured in an Epprecht rheometer C / II 25C at 1C.

Flake drying of a dispersion diluted with water to a solids content of 2% by weight, carried out according to the values of Example I, 2, with 8% of the solids of the dispersion and a 93% SiO2 content of synthetic silica as anti-caking agent, ΒΞΤ 230 m / g and a primary particle size of 0.018 microns, resulting in a highly shear-resistant and flowable dispersion powder which was excellent for the production of water-resistant mortars.

Example III

According to the procedure described in Example I, 1, a vinyl acetate / vinyl chloride / ethylene terpolymer dispersion was prepared at a polymerization temperature of 80 ° C and an ethylene pressure of b bar by the change from Example I, 1 to give a batch of vinyl acetate instead of 76% by weight. a mixture of 5350 parts by weight of vinyl acetate and 2290 parts by weight of vinyl chloride and, instead of 76 parts by weight of oxyethylated nonylphenol, 57 parts by weight of oxyethylated stearyl alcohol α with 20 moles / ethylene oxide per mole of stearyl alcohol. The vinyl acetate / 12 64384 vinyl chloride / ethylene-polymer polymer dispersion could be flak-dried after a second dilution by flocculation according to the instructions described in Example I, 2.

Example IV

According to the procedure described in Example II, a vinyl acetate / 2-ethylhexanoic acid vinyl ester copolymer dispersion is prepared with the difference from Example II that instead of the monomer mixture given in Example II, 2100% by weight of viryl acetate and 9000 parts by weight of mixture and no phthalic acid dibutyl ester is subsequently added to the dispersion. The dispersion can, as described in Example II, be flake-dried in stock to a stable, flowable dispersion powder which is excellently suitable for the preparation of water-resistant plastic mortars. Example V

According to the instructions given in Example II, a vinyl acetate / dibutyl maleate copolymer dispersion was prepared with the difference from Example II that 20100 parts by weight of vinyl acetate and 9900 parts by weight of dibutyl maleate were used instead of the monomer mixture in Example II and 9900 parts by weight of polypropylene ••• polypropylene glycol with thenium oxide content. A dispersion powder made from this dispersion with a flake-like scale is also excellently suitable for the production of water-resistant plastic mortars.

Claims (3)

13 64384 Claims v ^ A process for the preparation of water-dispersible dispersion powders suitable as binders for plastic binders and plasters by emulsion copolymerization of vinyl acetate with straight-chain or branched carboxylic acid esters of acyl alcohols containing 1 to 13 carbon atoms, 1 to 18 carbons. maleic or fumaric acid esters, vinyl chloride or olefins 11a and / or ethylene having 1 to 12 carbon atoms and, if appropriate, other morphomers and possibly using external plasticizers in the presence of a radical imitator and in the presence of additional emulsifiers and from 5 to 20% by weight of at least one polyvinyl alcohol, based on the cappolymer, having a viscosity in a 4% aqueous solution? C 'C has a mass of 3 to 5 and an ester number of 90 to 215 mg KOH / g followed by a copolymer dispersion obtained by spray-drying at the same time but at a different point from 2 to 2% by weight, based on the dry matter content of the aqueous dispersion. 0.01-aine.5 μm anti-caking agents, characterized in that the emulsion polymerization of the nonomers is carried out at a temperature of 70-100 ° C in the presence of a) 0.02-1.0 wt. an emulsifier, based on the copolymer, and b) an O5, 2.0 wt.% nonionic emulsifier containing oxyethylene groups, based on the copolymer. Process according to Claim 1, characterized in that oxyethylated alkylphenols, oxyethylated alcohols and oxyethyl-strong polypropylglycols are used as nonionic oxyethylated emulsifiers. Use of dispersion openings prepared according to Claims 1 and 2 as binders for the production of plastic-bound plasters in dry mixes.