DE2200743A1 - Method and preparation for improving the properties of cement concrete - Google Patents

Description

PATENT LAWYERS 8 MUNICH 8O. MAUERKIRCHERSTR. 48

Dr. Berg Dipl.-Ing. Stopf ,, 8 Munich 80, Mauerkircherstraße 45 · Your reference Your letter Our reference Date I ^ f _t J <H "l · 197 *

Attorney's file 2 2 011
Be / Ro

Esso Research and Engineering Company Linden / USA

"Process and preparation; to improve the properties of cement concrete"

The present invention relates to a method of improvement the properties of cement concrete, and in particular a preparation suitable for this process is.

Cement-concrete are mixtures of cement, granular material and water that are generally poured into formwork

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the. This Formge practice method makes it necessary that the concrete is sufficiently fluid. This fluidity is in the generally obtained by diluting the concrete with a much larger amount of water than to ensure it the setting of the cement is required. However, this excess water is harmful in many ways.

Part of the excess water migrates into the interior of the concrete mass and carries the cement with it. This leads to soakings and to the formation of a network of capillaries, which affects both the resistance of the material to the atmosphere and its mechanical strength after drying to decrease the compressive strength of approximately Vfi,

Aids are known which have the effect of improving the plasticity of the concrete into which they are incorporated and which therefore make it possible to introduce less water into the concrete during the mixing process. Be used generally solutions of lignosulfonates with 15 40? o solid material, in the ratio of 2-5 kg per ton of cement "

The iignosulfonates, the by-products of the cellulose and pulp industries are actually complex mixtures,

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whose composition and properties are extremely variable. You also need to get by the sugar that they have contain, as this has the effect of delaying or even preventing the setting of the cement

Attempts have also been made to use various surfactants in the manufacture of cement concrete to use. These compounds are generally wetting agents or foaming agents. Promote the wetting agents the dispersion of the cement particles in the mixed water, while the foam-forming agents furthermore the formation and retention of air bubbles in the mortar or concrete mass support. These two effects appear to improve the plasticity of green concrete. However it is quite difficult to properly control the introduction of air into the mix. When the volume of air introduced is very considerable, it is possible that after drying one obtains a concrete of the cell type which, although interesting Has properties for many special purposes, but its mechanical strength is relatively low.

The present invention relates to a method which, in detail, makes it possible to obtain a moderately stable concrete in the concrete and maintain reproducible amounts of trapped air ten, which has the effect of improving the plasticity of the concrete without affecting the setting of the cement or the mechanical strength of the final material

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to decrease.

This procedure consists of getting into the concrete or slinging Mortar per 1000 parts by weight of cement, a parts by weight of one Product A and B are weight parts of one. Introduces product B, where the products A and 3 are still defined below and the numbers a and Td correspond to the following ratios:

0 ^ C a /.0.2
0.05a <b ^ l 0.25a

The product A is a solution of an alkaryl sulfonate, ζ.Δ. an alkylbenzenesulfonate in a concentration of 50 70 G-ewo / j. The alkaryl sulphonates are the salts of an alkali metal or alkaline earth metal with alkarylsulphonic acid in which each molecule contains at least 1b carbon atoms and the average number of carbon atoms per molecule is at least 19. The hydrocarbon oil in which these alkaryl sulfonates are dissolved has a start of distillation above 25O ⁰ O and a viscosity of 10 to 100 cSt at approximately 20 ⁰ O ₀

The product B is a salt, ^{liquid at 20 0} O, of an aluminum alcohol and of carboxylic acids, the latter having at least 7 carbon atoms per molecule.

The alkaryl sulfonates are preferably sodium alkaryl sulfonates. The sulfonic acids of which these bulfonato stain-

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inen, preferably have 19-21 carbon atoms per molecule " It can be such acids, for example, that one by an alkylation reaction between an olefin with an average of 11-13 carbon atoms per molecule and a benzene-containing hydrocarbon with 8 carbon atoms per molecule. The alkylation and sulfonation can be carried out according to generally known methods »

The hydrocarbon oil used to dilute the alkaryl sulfonates A liquid mineral oil or a mixture of hydrocarbons can be used and thus forms solution A be that has the desired properties in terms of volatility and viscosity. ICs is possible in particular Use alkylbenzenes with an average of 17-19 carbon atoms per molecule, which is obtained as a result be, aass one alkylated benzene with a propylene tetramer, whereby these are commercially (imprecisely called) "detergent alkylates" or "dodecylbenzenes" are called,

Preferably, the amino alcohols contained in the salt B have the general formula HHx (R-OH) y, in which χ and; / are integers which correspond to the conditions 1 ^ y ^ 3 and x. + y ₌ 5, v / orin R is a divalent hydrocarbon radical with 2-4 carbon atoms. These amino alcohols are preferably monoethanolamine, diethanolamine and / or triethanolamine

• -6-

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The acids from which dr, s derived product ± i are preferably acids which are uei 2O ⁰ U liquid. These include, in particular oleic acid, the dimer of oleic acid, aliphatic acids with branched, saturated chain, as obtained by the oxo synthesis of oligomers of propylene or isobutylene, mixtures of acids which are known as "Naphtensäureri ^1, the paraffin ( Petroleum), liquid acid by-products known as "tall oils" - which come from the paper pulp industry etc. "

It is possible to use, for example, monoethanolamine oleate as product B.

The area of discovery is obviously not restricted by that further useful additives are also introduced into the xieton. In particular, it can be beneficial be to incorporate a common antifoam agent into the concrete or mortar.

According to a preferred method of the present invention, one puts in a cement concrete or mortar per 1000 parts by weight Cement from 0.03 to 0.1 parts by weight of a solution, the 30-70 $ of their weight is a sodium alkylbenzenesulfonate, wherein the solvent is "detergent alkylate", monoethanolamine oleate in an amount between 1/20 and 1/4 the amount of alkylbenzenesulfonate solution and approximately 0.0005-0.002 parts by weight of a common antifoam.

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It is very useful to the concrete or cement mortar the products A and B in the form of a more or less diluted To supply solution prepared in advance.

In addition to the method just described, the present invention also relates to a preparation which can be used to carry out this method, ie _o an additive which improves the properties of concrete and cement mortar.

According to the present invention, this additive is a preparation which is essentially characterized in that it contains concentrations a ¹ or b ¹ of products A and B, as defined above, preferably diluted with water or with a solvent or a mixture of solvents which are miscible with water, where the numbers for a 'and b ¹ correspond to the following ratio?

0.05 a ¹ ^ b ^! ^ 0.25 a ¹

In the preparation according to the present invention, the products A and B can advantageously be in water or in dispersed or dissolved in a mixture of water and one or more organic water-miscible solvents be. Solvents that can be used include in particular methyl, ethyl, isopropyl, isobutyl alcohols, monomethyl, monoethyl or monobutylethylene glycol or -diethylene glycol ethers, ethylene glycol, propylene-

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glycol, diethylene glycol and technically equivalent solvents.

Although not essential, the dilution of drug components A and B aids in the present Preparation of their use. The presence of organic solvents in the preparation has the effect of to promote the later homogeneity and to support the dispersion of the active ingredients A and B in the mixed water «

It should be pointed out that it is impossible to be precise Limits with regard to the dilution of the active ingredients "A and B" within the preparation are given, beyond that is left to one's own discretion.

At most it can be stated that, for example, a preparation of 100 parts by weight contains 5 parts of products A and B total and contains 95 parts of water, is easy to use. However, it is also possible to use a preparation to give preference with a higher concentration of active substance, for example a preparation whose 100 parts by weight 50 parts of products A and B in total, Contains 20 parts of a water-miscible organic solvent and 50 parts of water.

According to the invention, the preparation is added to concrete or Iuörtel the invention in such a relationship that

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the resulting mixture up to 0.225 parts by weight, preferably Contains 0.03 to 0.13 parts by weight of products A and B per 1000 parts of cement.

The scope of the invention is not limited to the introduction of the preparation described above, since it is in addition to the products A and B and possibly vpn solvents, others useful additives can be introduced. So it can be particularly advantageous to use this preparation as a product incorporated, as they are currently used as antifoam agents.

Accordingly, there is an advantageous method of implementation of the present invention in that the preparation as an additive to improve the properties of cement mortar and concrete is used, in addition, for example, for each! part of product A from 0.01 - 0.05 parts Antifoam agents of the usual type, from 0.5-1 part organic, water-miscible solvent and up to Contains 200 parts of water

According to the present invention, concrete and mortar are obtained which, when green, have better plasticity and which, when they have set, have a higher mechanical strength.

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example 1

100 parts by weight of an additive I according to the invention were the one made by mixing:

4 parts of solution (a1) of sodium sulfonate 0.5 parts of monoethanolamine oleate
0.1 part of conventional anti-foaming agent 95.4 parts of water

Solution A1 contained 40% sodium alkaryl sulfonate, where the solvent "dodecylbenzene" is «the sulfonic acid, contained in this salt was obtained by treating the alkylation product of orthoxylene with propylene tetramer sulfonated "

A concrete was then produced in which 0.1 part of additive I was browned per 100 parts of cement. Farther a control concrete was produced without an additive. Using the appropriate amount of mixed water, the plasticity was determined of the two concretes so set, this being determined by means of the Abrams funnel method (standard ΪΠ? -Ρ-18.451) became that sinking in the concrete thong in both Cases was practically the same.

The preparation in kg / m and the plasticity in mm of the two Concretes are given in the following table

Tabel

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Concrete xnit additive control concrete

cement 350 350 Granules 5-25 μ 1099 . 1099 Granules 0-5 dim 714 714 water 184 200 Additive I. 0.35 iiil plasticity 10 8th

Test pieces were made with each concrete that accelerated setting in a water bath at 60 0 for a predetermined period of time. The compressive strength of the dried samples was according to standard IP-P-18.305 determined. The results obtained are in summarized in the following table:

Concrete with additive I control concrete

Average density 2.32 2.34

Compressive strength (bar)

after H hours 170 175

after 19 hours 210 185

after 24 hours 235 200

The additive I makes it possible to reduce the amount of mixed water required to obtain the same plasticity by 8 io and to increase the compressive strength after 24 hours of accelerated setting by 17.5 ⁰ A »

• Example 2

Two samples of mortar under the reference numbers A and B were prepared using 0.5 and 2 parts by weight of Additive I, respectively

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contained cement per 1000 Gewi clit, and these were with a control mortar ve rf], ic Ji en, which is produced without an additive became.

These mortars were made with sand with a modulus of fineness of 1.36 and with 300 kr of cement per ni ^ Concrete was made «

The amount of washing water was adjusted so that the plasticity of the mortar obtained, determined by the A'brams funnel method (French Standard NF-P-I8451) thereby determined is that you let the concrete funnel sink by 6 cm.

The possibility of handling the concrete was determined by the "Plasticlmeter" of the Highways Department Laboratory, according to two methods by U ₀ Duriez and J. Arrainbide ("l \ ouveau Traite des Materiaux de Construction", Dunon, editor, edition I, pages 1219 and 1330) certainly. This method consists in measuring the time, in seconds, required for the vibrated mortar to flow through a calibrated nozzle to in turn reach three fixed marks. The shorter the times measured, the easier the mortar is to handle.

With each of the concrete mixes, cylindrical test pieces were made with a diameter of 16 mm and a height of

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32 cm, after allowing a certain period of time to set, the density of the test pieces was determined and then their compressive strength was determined according to the standard NF-P-18.305. The volume of the enclosed air was calculated from the density of the test pieces - this being given as a percentage of the volume of the test piece ₀

The results obtained are shown in the table below refer to;

Control mortar Mortar A Mortar B

Mixed water
(Liter / m ^) O 210 200 132 included
Air {'/ o) (Bar) - 1.5 2.5 Handling (sec 18-20-30 16-18-27 10-12-13 Compressive strength after 7 days 180 170 180 after 28 days 275 295 295

It can be seen from the table that the invention makes it possible to achieve a considerable improvement in handling without To achieve a weakening of the mechanical strength

In the following examples, the mortar samples without additives were used as controls according to standard method MT-P-15403 manufactured. According to this standard, a mortar approach consists of 1350 g of normal dry sand and 450 g of cement and 225 g of water. The mortar samples and an additive were made made in the same way except that the

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225 g of water were replaced by 205-215 g of water and the additive. The plasticity and the sweating respectively Welding each of the samples of fresh or »green mortar, as well as the air content and mechanical strength each sample after allowing it to set for a certain period of time.

The plasticity of the mortar samples was determined by that the expansion is determined under certain conditions by the method described by M. Duriez and J. Arrambide ("No u ve au 'üraite des kateriaux de Construction", Volume I, Pages 1085 and 1086).

A blunt cone of fresh iuörtel is on a table formed, which in turn is capable of delivering vertical impacts to a reproducible extent by means of a suitable squat (Machine Standard MF-P-I5.412) “The used The form is given in the standard HF-P-15.414.

The result is expressed as a percentage of the increase in the 3 durometer determined at the base of the truncated cone after 15 standardized impacts.

The welding measurement is carried out as follows: A testing tube (internal diameter 48 mm _? Internal height 200 mm) is attached to a shaping machine, standard WP-F-15 »412. The Versuohsröhre is filled to three quarters with the mortar that is being tried. She then becomes one

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Cycle with 60 thrusts suspended «The test tube is suspended until topped up and again subjected to a cycle of 60 thrusts. The test tube is then removed from the table, covered with a watch glass and left to stand at ordinary temperature. "Two hours later this is under test standing piece weighed, the floating water layer on top removed with filter paper and the weight loss ■ lust measured in grams with an accuracy of 0.1 g »

The air content of the set mortar is determined from the weight of the test pieces by comparing the mortar with and found without an additive

The mechanical strength is according to the standard U] P-P-15 = 451 measured"

Example 3

A number of additives II-VI were produced, whereby they differ from the additive of Example 1 only by the Differentiate between the sodium sulfonate concentration in solution A,

To produce the additives II-VI, the A1 solution from Example 1 was replaced by the solutions A2, A3 "A4, A5 and A6, the 60 or". 55 "» 50, 45 and 40 fo sodium sulfonate contained ο

The properties of the types of concrete to which the additives II VI have been incorporated are shown in the table below summarized: - _ifi_

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-46 -

Welding used expansion air pressure strength additive g 5 & halt <$> speed (bar) ' ^x

II 1.5 44 6th 495 III 1.5 4 5 5.5 508 IV 1.4 45 5.0 540 V 1.4 41 4.5 590 VI 1.3 41 4th 574 Footnote:

χ set after 75 days

Example 4

An additive VII was made with the same composition as Additive I produced, except that the monoethanolamine oleate was replaced by an equal weight of triethanolamine oleate. The concrete to which the additive VII was incorporated has the following property:

Welding (g) 1.25

Expansion ($) 33
Air content (> b) 4

Compressive strength (bar) 452

The compressive strength was after 75 days of setting ./einesson.

Example 5

An additive VIII and an additive IX were produced in the same composition as additive I, with the exception of that the Honoethanolaminoleate by an equal length of a salt of lonoethanolamine and isomeric acids of

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Carrinic acid and replaced by the salt of monoethanolamine and the dirner of oleic acid »

The isomeric acids of capric acid (decanoic vinegar) are commercially available products made by oxo-synthesis Prop; / lentrimer were produced «

Examples of Iüörtel were made, being 0.1 0.2 Parts of additives VIII or IX contained per 100 parts of cement, and these examples of körtel were on the one hand i ^ it a sample without additive and on the other hand with 2 samples which contained 0.1 and 0.2 parts of Additive I per 100 parts of cement, respectively.

The properties of the concrete samples thus obtained are the
The table below shows the additive ratios expressed as a percentage of cement by weight:

Mixed water used welding spreading air

Additive Additive IX (ß) (r) (*) stop (° / o) without Additive IX 225 ' 2.4 44 control viii Additive I. 215 ^^ 46 /in Additive I. 215 ,., 51 3.5 0.1 ^ Additive 215 1.9 45 <£ 1 0.2 # Additive 215 2.0 45 2.5 0.196 Additive 215 1.8 38 ■ 1 0 296 215 1.7 50 3.5

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■ ueisyiel 6

100 parts by weight of additive "Ä" were made by mixing:

40 parts of solution A from Example 1 4 parts of iuonoäthanolaminoleate 1 part of antifoam
20 parts isobutanol
34 parts of water
The additive X is immediately mixed with the water.

An additive 11 was produced by diluting additive X with 10 fo in water and this was applied to two mortar samples in a ratio of 0.1 and 0.2 fi in relation to the cement The properties of these mortar samples compared can be found in the following table, in which the proportions of additive are expressed as a weight percentage of cement.

Proportion of mixed welding spreading air content additive XI water (g) (κ) (%) (° / q)

0.0 225 2.4 44 control 0.1 # 215 2.5 45 <ϊ 0.1 / 210 2.1 59 < 1 $ 0.2 215 2.2 • 56 4th 0.2 per cent 210 1.9 47 4th 0.2 ° / 205 1.7 55 4 ■

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The same results were obtained with additive X, v / hen you add it directly to the liquor of the solder all in one admitted ten times lower ratio.

Example 7

This example shows the advantages of the preparations according to the invention in comparison & u solutions of alkaryl sulfonates, v / hen used alone with regard to the particular i,.: e chanical stability of the through these ueiden adüitivearten improved concrete.

Samples of mortar were prepared, modified by the addition of 0.1 parts by weight of Additive I or Additive III per 100 parts by weight of cement. The additives I and III, which were defined in the preceding examples, contained 4% by weight of the solutions A1 and A3 of the sulfonates., As they have already been defined _o

Furthermore iaörtelbeispiele were produced, whereby they through the solutions A1 and A3 were modified, whereby these were used separately in proportions of 0.004 and 0.008 parts by weight per 100 parts of cement "

Test pieces were produced, with the air content and the mechanical strength after 21 days (R1) and after 28 days (R2) setting. Ea were get the following results:

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- 20 experiments - used spread air - JM Il2

Mr. Additive ( 44 stop (7 =) (Bar) (] 3ar) 1 0.1 '; y additive I. 42 _ 510 2 0.1 ^ additive HI 4 5 6th - 450 0.004 / o λ1 4: 3.6 419 460 4th 0.004> Aj 50 'j ° y> \ - ^ 75 5 0.006 / 0 λ1 ■ • -1 4.5 XRQ 6th 0.006 ', j α3 L2.5 y, c 26 y ^ 4 O without additive 0.0 4o5

Whether the solutions of the alkyl sulfonates are used as such or whether they are used in additive form according to the invention; in an equal jüiteil in relation to cement used ν ground, they give a fresh or _"t reen -ortel the same plasticity and., prukticch öerx same percentage of air content. If However oulfonate ./endet as such ver ^7, ibt observed, d.-.- ß ctie laeohanische strength of the mortar is weakened "

By increasing the proportion of ouli'onate to whom; she ice cream such has been used, the Tl:, oti :: ität is now actually used and the amount of trapped air increases, however the loss of mechanical strength increases significantly ο

It is well known that between the luechanisehen jtewti., keit des Iuörte * ls after the tie off and. α em share of included Air consists of the subsequent relationship known as Fe ret's relationship (Hevue des uiteriaux J .. υ

20983 0/10 Λ 5th

Const-ruction, 1961, ITr. 5.4 &, direct 265-282)

(1) H, --- K / G \ 2

^t ic + -B ■ + TJ

-.ν or in

IL ₊ the compressive strength of the mortar after setting IC is a coefficient that depends on the units used for the application or use performance of the mortar and the setting time, Q, E and -V are the volumes which are ingested from the cement or water and the "enclosed air" for a given volume of fresh mortar after this has been placed in the mold used to manufacture the test piece.

If the theoretical mechanical strength R + of the test pieces is determined by means of the JTer & t ¹ s ratio, it can be determined that the experimentally measured strength is higher in the case of mortars made with additives i or III as the theoretical resistance or strength, while the measured resistance is practically the same as the calculated resistance in the case of the mortar samples which were modified ala by means of the sulfonate solutions. In fact, the ratios £ 1 = Ri / Rt 'and £ 2 = R2 / Rt ² the measured and the calculated resistance "or" strength after 21 or 28 days of setting, if you take them off

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the test results 1 - 6 given above are calculated using the following values:

Number of attempts C \

2 3 4 5 6

To calculate the theoretical Y / iderotability or strength shown as the denominator in this ratio, it is believed that the measured mechanical strength Ro of the control test piece is in the FerSt's ratio can be introduced in such a way that one accepts

(2) V = 0

V ^K ( Q ) ²

⁰ VC + E /

If one now removes K from the ratios (1) and (2), one obtains the equation:

- 1.16 - • 1.15 1.03 1.04 0.95 0.98 0.90 0.92 0.85 0.87

(3)

^B ) + V /

V C ■■ + E

The value of the sum (O + E) is obtained by experiment. With a normal mixture it is 360 ocm and this corresponds to a total volume of 905 ecm if it contains practically no enclosed air.

The volume of air V which is brought into a batch is determined from the proportion of that which is trapped as measured by experiment

Air rises. -23-

2 0 9 8 3 0/1 0 A 5

Claims (1)

- 23 pat en tan sayings: [i . '} A method for improving the properties of cement mortar or cement concrete, characterized in that one in the Leton or mortar, per 100 weight of steep cement, a. Parts by weight of product A and parts by weight of product B according to the ratio, 0 Ca C 0.2 and 0.5a <b <0.25a
and in what the product A is a solution of alkar / isulphonates of an alkali metal or alkaline earth metal, each molecule of these sulphonates contains at least 1d carbon atoms, the average number of carbon atoms per molecule is at least 19, and the sulphonates in a concentration of 30-70 wt./6 in the Hydrocarbon oil are dissolved that a start of distillation of at least. 250 ⁰ C and a viscosity of 10-100 cSt at 20 ⁰ C, and the product B is a salt which ^{is liquid at 20 °} C., of an amino alcohol and a carboxylic acid, the carboxylic acid containing at least 7 carbon atoms per molecule 2 .. The method according to claim 1, characterized in that dai. ' liatrium alkarylsulfonates are used as alkarylsulfonates "
. ■ ■ ■ ■. -24- 209830/1045 3. The method according to any one of the preceding claims, characterized in that the acids, from which the alkarylsulfonates originate, in the "/ ice can be produced by using a lienzol-containing hydrocarbon with 8 carbon atoms per molecule, with an olefin averaging 11-13 carbon atoms per molecule, alkylated and the resulting alkylate sulfonated " 4. The method according to any one of the preceding claims, characterized in that the Alkaryl sulfonate in an alkylbenzene with an average of 17-19 carbon atoms per molecule. 5ο method according to one of the preceding claims characterized in that the carboxylic acid, from which the product B originates, a "naphthenic acid" derived from petroleum, the liquid acid by-products, referred to as "tall oils", oleic acid, the dimer of oleic acid or an aliphatic acid uit a branched, saturated chain is. β ο Method according to one of the preceding claims, characterized in that the amino alcohol used in product B is monoethanolamine, diethanolamine and / or triethanolamine. 209830/1 045 7. The method according to any one of the preceding claims, characterized in that in the concrete or cement mortar per 1000 parts by weight of cement 0.03-0.1 parts by weight of a solution of 30-70% by weight ITodium alkylbenzenesulfonate in "detergent alkylate" 'and between T / 20 and 1/4 of the weight of the sulfonate solution monoethanolamine oleate and 0.0005-0.002 parts by weight of anti-foaming agent. ■ 8. Preparation for improving the properties of cement mortar or cement, into which an additive is incorporated, characterized by the content of at least one product A and one product B according to one of the preceding claims in concentrations of a ¹ or » \ b ¹ , whereby these correspond to the following ratio » ) 0.05 a · C b '^. 0.25a « 90 preparation according to claim 8 characterized ge -) indicates that the products A and B in a mixture of water and a solvent, namely, methyl, ethyl, isopropyl and / or isobutyl alcohols, Monomethyl-v monoethyl and / or monobutyl ethers of ethylene glycol or diethylene glycol, ethylene glycol, propylene glycol, Diethylene glycol and / or technically equivalent solution " are dissolved or dispersed o ■ ■ '-26- 209830/10 45 10. Preparation according to one of the preceding claims characterized in that they are next to products A and B in a ratio of 0.05 to 0.25 parts of product B per part of product A each part of product A from 0.01-0.05 parts antifoam agent, from 0.2-1 part solvent, namely methyl, ethyl, Isopropyl or isobutyl alcohol, monomethyl, monoethyl or monobutyl ethers of ethylene glycol or diethylene glycol, Ethylene glycol, propylene glycol, diethylene glycol and / or technically equivalent solvents up to 200 parts of water contains " 209830/1045