DK143760B - PROCEDURE FOR MANUFACTURING AQUESTIC DISTRIBUTIONS - Google Patents

Description

(19) DENMARK fw, p.a

»(A) PROCEDURE WRITING on 11 + 3760 B

DIRECTORATE OF THE PATENT AND TRADEMARKET SYSTEM

(21) Application No. 3560/76 (51) int.CI.3 C 08 F 218/04 (22) Submission day 6, Aug · 1976 // C 09 D 3/74 (24) Running day 6 Aug. 1976 (41) Aim. available Feb. 9 1977 (44) Submitted 5 · Oct · 1 9 $ 1 (86) International Application no.

(86) International filing day (85) Continuation day "(62) Master application no."

(30) Priority Aug. 8 1975, 2535374, DE

(71) Applicant H0ECHST AKTIENGESELLSCRAFT, 6230 Is Ankfur t / Mai n 80, DE.

(72) Inventor Helmut Braun, DE: Helmut Rinno, DE: Wepner Stelze], DE.

(74) Associate Engineer Budde, Schou & Cq.

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(54) Process for preparing aqueous drug dispersions.

The problem of dispersion dye wet adhesion on smooth, non-absorbent substrates has for a long time limited the use of certain dispersion dyes, low pigmented dispersion dyes, and among these, especially those which dry up to shiny or silky matte films, are poorly adhered to smooth, non-absorbent substrates when the smears moisten again after drying. Particularly bad is the wet adhesion of fresh smears that are not yet aged.

BO Low pigmented dispersion paints are selected in those cases where the smear should be washable · Due to the high binder-> agent content of these colors, a closed, washable film is formed.

Ό _j. Shiny or silky matte dispersion paints also have a pigment volume concentration of less than 40% and usually of approx. 10 - 25%.

£ 3

2 U37 $ Q

For enhancement of gloss, flowability and open time (the time when the film surface is still moist, i.e. where a closed film has not yet formed on the surface) and as a film consolidation agent (agent which helps to firm the film after ironing) moreover, they contain organic solvents in greater quantity, approx. between 3 and 20%. Gloss, flowability and open time are affected e.g. using polyhydric water miscible alcohols with up to 6 carbon atoms, especially ethylene and propylene glycol or monomethyl, ethyl, - propyl or butyl ethers thereof. To improve the film consolidation, limited water-soluble solvents such as the monoglycol ethers of carboxylic acids and especially esters of carboxylic acids with monoalkyl ethers of glycols or oligoglycols are used. Butyldiglycol acetate is one of the most widespread representatives of this group. The combination of low pigmentation and higher solvent content has a particularly negative effect on the wet adhesion of the dispersion dyes.

Defective wet adhesion means that the smears intended to be washable are no longer in possession of this property when applied to smooth, non-absorbent substrates, e.g. on old alkyd resin or oil paint smears.

In damp rooms, such as kitchens or bathrooms and many industrial premises, where condensation water is to be expected, the new wipe can detach from the substrate when insufficient wet adhesion is provided. Finally, a defective wet stitching makes the ironing work difficult. For example, The plinth and the top half or wall and ceiling are done in different colors, it may happen that the first coat is soiled with a different color due to inaccurate brushing. In principle, these dirt can be removed with a damp cloth or sponge. However, in the case of defective wet stitching, the first stripping is easily damaged or pushed off completely.

For these reasons, attempts have not been made to modify plastic dispersions such that the dispersion dyes produced with these dispersion colors have the desired wet adhesion. From German Publication No. 1,595,501 it is e.g. known in the manufacture of plastic dispersions by polymerization of suitable monomers in aqueous emulsion to incorporate from 0.2 to 15% by weight, based on the total amount of the monomers, compounds with oxirane groups as comonomers in the polymerate and then allowing ammonia 3 or amines to act on copolymer in sate t at room temperature. Suitable oxirane compounds are primarily glycidyl esters of acrylic or methacrylic acid, but also allyl glycidyl ether or vinyl glycidyl ether.

Dispersion colors made with such plastic dispersions already have a fairly good wet adhesion. For many purposes in practice, the wet adhesive tip is nevertheless far from adequate.

It has now been found that aqueous plastic dispersions suitable for the production of high wet adhesive dispersion paints can be produced which impart a particularly good wet adhesion to the non-absorbent or non-absorbent substrate thus produced.

This is done by the process of copolymerization under current conditions in aqueous system of the following monomers: A) 5-50% by weight, based on the total amount of the monomeric vinyl esters of saturated branched monocarboxylic acids having 5-20 carbon atoms whose carboxyl group is bonded directly to a tertiary or quaternary carbon atom, B) 40-94.5% by weight based on the total amount of the monomers, vinyl acetate / vinyl propionate, vinyl butyrate and / or vinyl isobutyrate, C) optionally 0-30% by weight, based on the total amount of the monomeric, α, β-ureaacetic acids or derivatives thereof which can be copolymerized with the said monomers, the process of the present invention being characterized in that during the polymerization, % by weight, calculated on the total amount of the monomer, of an acetic acetic ester of the general formula 0 ORR 'ch3-c-ch2-cxc = ch where X means -0-, -Q-CH - or -O-CH -CH9-0-C-, and R and R 'each Δ 2. £ ft

ISLAND

means H or CH 3, or an acetic acetic acid ester of hydroxypropyl acrylate, methacrylate or crotonate.

Compounds of the kind described under D are e.g. acetic acetic acid vinyl ester, acetic acetic acid allylic ester or acetic acid ester of β-hydroxyethyl acrylate or methacrylate or crotonate or hydroxy propyl acrylate or methacrylate or crotonate. Preferably acetic acetic acid allyl ester is used because the best results are obtained with it. Also preferably 1-5% by weight of component D is used, because this range has proved particularly suitable for achieving the desired effect.

4 143760

Examples of vinyl esters of saturated monocarboxylic acids, whose carboxyl groups are bonded directly to a tertiary or quaternary carbon atom, are pivalic acid vinyl ester, isononanoic acid vinyl ester or preferably versatinic acid vinyl ester such as e.g. is disclosed in British Patent Specification No. 993,470. Versatin 10-acid vinyl ester is particularly preferred. Mixtures of such monomers can also be used.

Speaking as in B), vinyl esters come vinyl acetate, vinyl propionate, vinyl butyrate or vinyl isobutyrate or mixtures of these compounds. Preferably, vinyl acetate is used.

Examples of α, β-unsaturated compounds of the kind mentioned in C) are e.g. acrylic acid, methacrylic acid, crotonic acid, maleic or fumaric acid or esters of acrylic acid, methacrylic acid or crotonic acid, di- or monoesters of maleic or fumaric acid, wherever they are. present alcohol groups contain 1-30, preferably 1-20 carbon atoms, or other derivatives of these acids, e.g. (meth-) acrylamide, (meth-) acrylonitrile or maleic anhydride. If copolymerization of such monomers is desired, the selection of the species and the amount should be made according to the generally accepted views for the preparation of smear dispersions. In particular, care must be taken that polymers are formed which, under the established drying conditions for the color, form a film and the choice of the monomers for the production of copolymers must be made so that, according to the position of the polymerization parameters, the formation of copolymers with the present invention can be expected. keto group-containing monomers.

If desired, several of the compounds mentioned under C) may also be used simultaneously.

In copolymerization of monomers which homopolymerized to give water-soluble polymers, only such quantities should be used so that the water sensitivity of the dispersion films or of the smear films does not become excessively high. (Meth-) acrylic acid, crotonic acid, maleic or fumaric acid, (meth-) acrylamide or maleic anhydride should e.g. are not copolymerized in amounts greater than 5%, based on the total amount of the monomers.

The aqueous plastic dispersions are prepared with a solids content of between 20 and 70%, preferably between 40 and 60%.

In addition, the aqueous plastic dispersions are commonly produced by methods known to those skilled in the art.

Plastic dispersions are extremely complex systems. The preparation of the present invention of the very valuable dispersions requires the use of the experience of the field of emulsion polymerization, although not specifically described herein. Ignoring the rules known to one of ordinary skill in the art of emulsion polymerization can therefore affect important properties, e.g. the water resistance, in the dispersion films or the smear films in an unfavorable direction. Therefore, based on the polymer content, the dispersions should not exceed the commonly used amounts of up to 3%, preferably up to 2%, ionic emulsifiers or up to 6%, preferably up to 4%, non-ionic emulsifiers.

As nonionic emulsifiers, e.g. alkyl polyglycol ethers, e.g. the ethoxylation products of lauryl, oleyl or stearyl alcohol or of mixtures such as coconut fatty alcohol, alkylphenol polyglycol ethers, such as the ethoxylation products of octyl or nonylphenol, diisopropylphenol, triisopropylphenol or of di- or tri-tertylene or tert-butylphenol

Speaking as ionic emulsifiers comes primarily anionic emulsifiers. These may be the alkali metal or ammonium salts of alkyl, aryl or alkyl aryl sulfonates, sulfates, phosphates, phosphonates or compounds with other anionic end groups, as there may also be oligo or polyethylene oxide units between the hydrocarbon group and the anionic group. Typical examples are sodium lauryl sulfate, sodium octylphenol glycol ether sulfate, sodium dodecylbenzenesulfonate, sodium lauryl diglycol sulfate, ammonium tri-tert.butylphenol penta or octaglycol sulfate.

As protective colloids, natural substances such as gum arabic, starch, alginates or modified natural substances such as methyl, ethyl, hydroxyalkyl or carboxymethyl cellulose or synthetic compounds such as polyvinyl alcohol, polyvinylpyrrolidone or mixtures of such compounds are optionally used. Preferably, modified cellulose derivatives and synthetic protective colloids may be used.

To initiate and continue the polymerization, oil and / or preferably water-soluble radical formers or redox systems are used. Suitable are e.g. hydrogen peroxide, potassium or ammonium peroxide disulfate, dibenzoyl peroxide, lauryl peroxide, tert-butyl peroxide, bis-azodiisobutyronitrile, alone or together with reducing components, e.g. sodium bisulfite, rongalite, glucose, ascorbic acid and other compounds having a reducing effect.

The dispersions prepared according to the invention have the particular advantage that they are both suitable for producing dispersion gloss colors with good wet adhesion on non-absorbent substrates and that they have a high saponification resistance.

Example 1 In a 2 liter three-neck flask, which is in a heating bath, equipped with a stirrer, reflux, drip funnel and thermometer, a stirring barrel of 709 parts by weight of water is heated with stirring.

12 parts by weight of polyvinyl alcohol with the degree of hydrolysis 88 mole percent and a viscosity of the 4% aqueous solution at 20 ° C at 18 cP

0.9 parts by weight of sodium vinyl sulfonate 1.1 parts by weight of sodium dodecylbenzenesulfonate 15 parts by weight of nonylphenol polyglycol ether with approx. 30 parts ethylene oxide 0.72 parts by weight Nal 2 PO 2 · 2H 2 O 1.67 parts by weight Na 2 HPO 4 · 12 H2O 1.5 parts by weight of ammonium peroxide disulfate and 60 parts by weight of a monomer mixture taken from a mixture of 300 parts by weight of vinyl acetate, 150 parts by weight of 2-ethylhexyl acrylate , 150 parts by weight of pivalic acid vinyl ester and 18 parts by weight of acetic acetic acid allyl ester, thereby initiating polymerization. When the temperature has risen to 70 ° C, dosing of the remaining monomer mixture is started.

Immediately upon completion of the monomer addition, a solution of 0.3 parts by weight of ammonium peroxide disulfate in 15 parts by weight of water is added. Reheat for 2 hours at the polymerization temperature (70 ° C) with continued stirring and the mixture is cooled. The solids content is approx. 47.5%.

7

Example 2 (Comparative Example) 143760

Proceed in exactly the same manner as described in Example 1, but no acetic acetic acid allyl ester is used during polymerization.

Example 3 In an apparatus such as that described in Example 1, a dispersion float consisting of 618 parts by weight of water 18 parts by weight of oleyl polyglycol ether is heated by approx. 25 parts by weight of ethylene oxide 0.2 parts by weight of sodium dodecylbenzenesulfonate 12 parts by weight of hydroxyethyl cellulose with an average degree of polymerization of approx. About 400 parts by weight (about 100,000) 1.5 parts by weight of sodium acetate 2.5 parts by weight of ammonium peroxydlsulfate and 63 parts by weight of a monomer mixture taken from a mixture of 450 parts by weight of vinyl acetate, 150 parts by weight of iso-nonanoic acid vinyl ester and 12 parts by weight of acetic acid allyl ester at 70 ° C. temperature, the remaining monomer mixture (549 parts by weight) is dosed over 3 hours. After the dosing, 0.5 parts by weight of ammonium peroxide disulfate is added in 15 parts by weight of water and then heated for 2 hours. The solids content is approx. 50%.

Example 4 (concatenation example)

The procedure is exactly the same as described in Example 3, except that acetic acetic acid allyl ester is not used during polymerization.

Example 5 In an apparatus such as that described in Example 1, a dispersion float consisting of 657 parts by weight of water 18 parts by weight of nonylphenol polyglycol ether is heated by approx. 30 ethylene oxide units

12 parts by weight of polyvinyl alcohol with the degree of hydrolysis 88 mole percent and a viscosity of the 4% aqueous solution at 20 ° C at 18 cP

0.9 parts by weight sodium vinyl sulfonate 1.5 parts by weight sodium acetate 2.5 parts by weight ammonium peroxide disulfate 48 parts by weight vinyl acetate and 12 parts by weight versatin-10-acid vinyl ester to 70 ° C, and at this temperature a mixture of 432 parts by weight vinyl acetate, 108 parts by weight is added at this temperature. versatin - 10-acid vinyl ester and 9 parts by weight of acetic acetic acid ester After dosing, 0.5 parts by weight of ammonium peroxide disulfate is added in 15 parts by weight of water and then heated for 2 hours. The solids content is approx. 49%.

Example 6 (Comparative Example)

Proceed exactly in the same manner as described in Example 5, except that acetic acetic acid allyl ester is not used during polymerization.

Example 7 In an apparatus such as that described in Example 1, a dispersion float consisting of 622 parts by weight of water 18 parts by weight of nonylphenol polyglycol ether is heated by approx. 30 parts ethylene oxide 1.5 parts by weight sodium acetate 12 parts by weight hydroxyethyl cellulose with an average degree of polymerization of approx. 400 (molar weight approx. 100,000) 2.5 parts by weight of ammonium peroxide disulfate and 60 parts by weight of a mixture prepared from 369 parts by weight of vinyl acetate, 150 parts by weight of versatine - 10-acid vinyl ester, 48 parts by weight of butyl acrylate, 18 parts by weight of acetic acid allylic ester and 6 parts by weight of crotonic acid at 70 ° C and at this temperature the remaining monomer mixture (558 parts by weight) is dosed over 3 hours. After dosing, 0.5 parts by weight of ammonium peroxide disulfate is added in 15 parts by weight of water and then heated for 2 hours. The solids content is approx. 50%.

Example 8 (Comparative Example) 9

The procedure is exactly the same as described in Example 7, except that acetic acetic acid allyl ester is not used during polymerization.

To prepare the high wet adhesion dispersion dyes, the dispersions are mixed with a pigment slurry. Such pigment slurries, also called pigment doughs or pigment pastes, which are suitable for use in low pigmented dispersion colors and especially gloss colors, consist e.g. of titanium dioxide uniformly dispersed in water. They usually contain protective colloids such as cellulose derivatives, e.g. hydroxyethyl cellulose, and dispersants, e.g. salts of poly (meth) acrylic acid or sodium polyphosphate. Furthermore, common ingredients in the pigment slurry are antimicrobial preservatives, antifoam agents, pH value stabilizers and fillers. Particularly suitable titanium dioxide pigments are rutile and anatase. For gloss colors, it is important that the average particle diameter of the pigment is close to the lower gram of the wavelength of light, ie. know from approx. 0.4 to 0.2 µ. For the manufacture of low pigmented matte colors, for example, while using special surface-rich silicate pigments. Binder-rich matte colors provide scents that are easy to clean. Of course, the pigment paste may also contain colored pigments, but the desired tint can be adjusted just as well by fading the dispersion color of white pigment.

The pigment slurry can be prepared by the known methods, e.g. by dispersing pigment in a dissolver or on ball or sand mills. For use in gloss colors, the pigment slurry must not contain significant amounts of pigment aggregates because these adversely affect the gloss.

For either the dispersion or the finished dispersion color, adjuvants, e.g. plasticizers, cross-linking agents, buffering agents, thickeners, thixotropic agents, anti-rust agents, alkyd resins or drying oils. Softeners are not the solvents initially referred to as film consolidation agents with only temporary effect, but compounds such as dibutyl phthalate which lower the film formation temperature and remain in the polymer for a long time.

For testing the wet adhesion, gloss colors are prepared according to the recipes below.

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Recipe I

1. Water 41.0 parts by weight 3¾1 aqueous solution of 15.6 parts by weight "Tvlose H 20, r® / S \" Calgon N "(solid) 0.4 parts by weight

Dispersant PA 30 3.0 parts by weight

Ammonia, 25% 1.0 weight percent

Preservative 2.0 parts by weight

Anti-foaming agent 3.0 parts by weight

Titanium dioxide 175.0 parts by weight of grain size 0.2 - 0.4 µ 1.2- Propylene glycol 10.0 parts by weight is dispersed and then the second dispersion (at 50% solids - 710.0 parts by weight content) to which 2.0 parts by weight 25% is added ammonia if the pH does not exceed approx. 7th

With stirring, a mixture of 3. Butyldiglycol acetate 10.0 parts by weight 1.2- Propylene glycol 27.0 parts by weight is then slowly added.

The liquid or soluble constituents listed below, with the exception of the 1,2-propylene glycol, are first placed in a stirrer in the order in which the pigment is dispersed with a dissolver. Next, 1,2-propylene glycol is added. Of this pigment paste, a greater amount is produced to ensure the same conditions, e.g. with respect to the pigment dispersion, for the mixture with the various dispersions to be tested.

Recipe II

Prescription II differs from Prescription I in a higher proportion of organic solvents, to the color of which is added a mixture of 53 parts by weight of 1,2-propylene glycol and 17 parts by weight of butyldiglycol acetate.

Recipe III

Prescription III differs from Prescriptions I and II in an even higher proportion of organic solvents, to the otherwise finished color namely a mixture of 68.7 parts by weight of 1,2-propylene glycol and 21.3 parts by weight of butyl diglycol acetate.

Recipe IV

Prescription IV differs from Prescription I in a different composition of the solvent mixture added to the otherwise completed color (process step 3 in the color preparation), namely, a mixture of 12.4 parts by weight of 1,2-propylene glycol, 4.6 parts by weight of butyldiglycol acetate and 20 parts by weight of 2,2,4-trimethyl-pentanediol-1,3-monoisobutyrate-1 (trade name "Texanol").

For the preparation of the individual colors, a corresponding proportion is extracted from the pigment paste, which in the method mentioned in the above recipe is mixed with the approx. 1 day old dispersions under a slow stirrer. Next, the solvents mentioned in 3. are added. Once finished, the colors are sieved.

After one day's stand, these gloss colors are applied to glass plates and to steel plates on which is already sprayed an air-drying, pigmented, glossy alkyd resin varnish which has been aged at 100 ° C for 24 hours after drying. A film applicator with a gap height of 200 µ is used. After 24 hours drying time for the gloss colors, these are tested for wet adhesion by the two methods described below. 1

Wear Test On such a mechanical wear machine, such as is described in German Publication No. 2,262,956, which is similar to Gardner's washable and abrasive machine, though with an approx.

1.20 m long running distance, the prepared glass sheets are placed in such a way that the applied dispersion color films are perpendicular to the brush direction of travel. Due to the length of the run, approx. 15 colors are examined simultaneously in the same experiment. A pig hairbrush is used, which is moistened with distilled water at the beginning of the test. During the test, distilled water is also dripped onto the running distance of the brush, so that the brush path is constantly covered with a water film. In case of insufficient wet adhesion, after a few brushing steps, the dispersion color is pushed away from the base of the brush and goes off at the boundary between moist and dry film. The wet adhesion is the better the longer the brush runs before the film is pushed off. Optimal wet adhesion is available when the film after 5000

14376O

12 brush strokes (1 brush streak is a back and forth flow) have not yet been pushed off in the damp brush path.

2) Condensation experiments

Here is used a right-angle thermostat, which is half filled with water at a temperature of 50 ° C, and in whose gas space above the water surface a fan is mounted. The top opening is coated with the prepared steel sheets - with the test surface facing down - and thereby closed. The thermostat is in a room maintained at 23 ° C.

At the temperature difference, water vapor condenses on the underside of the plates and affects the glossy color films. After 15 minutes in each case, the plates are picked up and evaluated.

Insufficient wet adhesion appears in the formation of blisters between the dispersion color and the alkyd resin lacquer and in the film's easy peelability, e.g. with your fingertip. With good wet adhesion, the film is still blister-free and does not peel even after 4 hours. The test results are given in Table I.

Table I

Compilation of trial results

Example Recipe Rubbing test Resistance to No._ No. number of double brush strokes Condensation test 1 II 25000> 6 hours IV 23000> 6 hours 2+ II 500 30 min.

IV 450 25 min.

3 II> 5000> 6 hours III> 5000> 6 hours 4+ II 250 <15 min.

5 I> 5000> 6 hours 6+ I 120 30 min.

7 I> 5000> 6 hours 8 * I 500 2 hours + comparative examples, not according to the invention

Example 9 13 In an apparatus such as that described in Example 1, a dispersion float consisting of 607 parts by weight of water and 18 parts by weight of oleyl polyglycol ether is heated by approx. 25 ethylene oxide units, 0.2 parts by weight of sodium dodecylbenzene sulfonate, 12 parts by weight of hydroxyethyl cellulose with an average degree of polymerization of about 400 (molecular weight approx. 100,000), 1.5 parts by weight of sodium acetate, 2.5 parts by weight of ammonium peroxide disulfate, and 60 parts by weight of a monomer addition prepared from 450, 150 parts by weight isononanoic acid vinyl ester and 12 parts by weight 2-i (acetoacetyl) oxyethyl methacrylate, to 70 ° C. At this temperature, the remaining monomer mixture (552 wt. Parts) is then dosed over 3 hours. After completion of the dosing, the reaction mixture is mixed with 0.5 parts by weight of ammonium peroxy disulfate in 15 parts by weight of water and post-heated for 2 hours. The solids content of the resulting dispersion amounts to. 50%.

Example 10 In an apparatus such as that described in Example 1, a dispersion float consisting of 636 parts by weight of water, 18 parts by weight of nonylphenyl polyglycol ether with about 30 ethylene oxide units, 12 parts by weight of polyvinyl alcohol having a degree of hydrolysis of 88 mole percent and a viscosity of ep 4% aqueous solution is heated. 18 cP at 25 ° C, 0.9 parts by weight sodium vinyl sulfonate, 1.5 parts by weight sodium acetate, 2.5 parts by weight ammonium peroxydisulfate, 48 parts by weight vinyl acetate, 12 parts by weight versatin-10-acid vinyl ester and 1.2 parts by weight 2- (acetoacetyl) -cycloppylcrotonate at 70 ° C . At this temperature, a mixture is then dispensed over 3 hours from 432 parts by weight of vinyl acetate, 108 parts by weight versatin-10-acid vinyl ester and 18 parts by weight of 2- (acetoacetyl) propylcrotonate. After completion of the dosing, the reaction mixture is mixed with 0.5 parts by weight of ammonium peroxide disulfate in 15 parts by weight of water and re-heated for 2 hours. The solids content of the resulting dispersion is approx. 50%.

Example 11

Example 9 is repeated except that 2- (acetoacetyl) ethyl methacrylate is used instead of 2- (acetoacetyl) oxypronyl acrylate. The solids content of the resulting dispersion is approx. 50%.

Example 12

Example 10 is repeated, however, instead of 2- (acetoacetyl) propylcrotonate, 2- (acetoacetyl) oxyethyl acrylate is used. The solids content of the resulting dispersion is approx. 50%.

Example 13

Example 9 is repeated except that 2- (acetoacetyl) ethyl methacrylate is used instead of 2- (acetoacetyl) oxypropyl methacrylate. The solids content of the resulting dispersion is approx. 50%.

Example 14

Example 10 is repeated, however, instead of 2- (acetoacetyl) propylcrotonate, 2- (acetoacetyl) oxyethylcrotonate is used. The solids content of the resulting dispersion is approx. 50%.

Test results In the manner described in Example 8, dispersion colors are prepared and tested from the dispersions prepared according to Examples 9-14. The results of the test are summarized in Table II.

lc 143760 lb

Table II

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Ex. Recipe Testing Test, Resistance at No. No. of Double Brush Stroke Condensation Test 9 II> 5000> 6 hours 10 I> 5000> 6 hours 11 II> 5000> 6 hours 12 III> 5000> 6 hours 13 iv> 5000> 6 hours 14 I> 5000> 6 hours

comparison Tests

Plastic dispersions are prepared according to Examples 1 and 2 of DE Publication No. 15 95 501. From these dispersions, gloss colors are prepared and tested according to recipe I of Example 8. The test results are shown in Table III.

Table in DE Publication Writing Of Rubbing Tests, Resistance at No. 15 95 501, Number of Double Brush Strokes Condensation Trial Example No. _____________ 1,250 90 minutes 2 110 30 minutes