The method of obtaining water-soluble lacquer binders

 

(57) Abstract:

We propose an improved method of obtaining water-soluble lacquer binders and their use for the preparation of water-soluble fillers for coating vehicles. Binders include water-soluble after neutralization of the carboxyl groups of the reaction product of a carboxyl group and having at least one end of the locking isocyanate group of the polyurethane resin (polycarboxylic component) having a hydroxyl group complex polyester ( polyhydroxy component) and component matching. By special selection of components binders and using a special process operations for the combination of these components binders can be achieved further improvement in the storage stability of varnishes. 2 s and 5 C. p. F.-ly, 4 PL.

The invention concerns a method of obtaining water-soluble lacquer binders and their use to create a hot drying varnishes, in particular, water-soluble fillers for coating cars.

Binders include water-soluble after neutralization of the carboxyl groups of the reaction product from the maul (polycarboxylic component) having hydroxyl group of the polyester (polyhydroxy component) and component matching.

The combination of binders from polycarboxylic component, polyhydroxylated component and the component cross-linking are described, for example, in patents Austria NN 328587, 388738, 388382 and laid out in the European application N A2-0330139.

Using such a combination of binders is achieved preferred for applying coloring rheological properties of varnishes and very good strength of adhesion of paint films hot drying on the metal substrate or the primer, and also with respect to subsequent layers, thus ensuring the production of high quality, water-soluble fillers, which are used in the automotive industry.

Requirements in industrial practice on the part of consumers to water-soluble fillers, are constantly changing and requires a large effort to provide universally applicable products.

Unexpectedly, it was found that due to the special choice of components binders and using a special process operations for combining these components binders can be further uluchsheniya water-soluble lacquer binders, which contain the reaction product of polycarboxylic component polyhydroxyethyl component, and component matching, which differs in that

(A) from 10 to 80 weight percent, preferably from 15 to 40 weight percent, polyurethane resin which has a carboxyl group in accordance with the acid number of from 70 to 160 mgKOH/g in the molecule at least one end-blocked isocyanate group, however, does not contain any free hydroxyl groups or residues of fatty acid number of more than 12 carbon atoms, and the boundary number of viscosity is from 6.5 to 12.0 ml/g, preferably from 8.0 to 11.0 ml/g, measured in N,N-dimethylformamide (DMF) at a temperature of 20oC, reacts with

(B) 20 to 90 weight percent, preferably 60 to 85 weight percent, optionally arithmeticians polyester resin with a hydroxyl number from 50 to 500 mgKOH/g, an acid number of less than 20 mgKOH/g and the boundary number viscosity of from 8.0 to 13.0 ml/g, preferably from 9.5 to 12.0 ml/g, measured in N,N-dimethylformamide (DMF) at a temperature of 20oC, at a temperature of from 90 to 170oC, preferably at a temperature of 10 - 20oC higher than the temperature of removal of blocking Stalino from 14.5 to 16.5 ml/g, measured in N, N-dimethylformamide at a temperature of 20oC, without exceeding the boundary of solubility in water, and then

(I) from 60 to 90 weight percent of the reaction product, before or after partial or complete neutralization of the carboxyl groups with inorganic or organic bases, however, before adding the essential parts of water, mixed with

(II) 10 to 40 weight percent water-insoluble component crosslinking at a temperature of from 40 to 100oC and diluted with water until ready for further processing of the content of solids, and the amount of interest for the composition of a combination of A and B or I and II, based on the solid, respectively 100.

The invention relates in addition to the methods according to the invention water-soluble lacquer binders tools and their application to the formulation of water-soluble varnishes hot drying, in particular for the preparation of water-soluble fillers (primed surface for painting cars.

Thanks to additional relatively resistant to hydrolysis connection polycarboxylic component (A) with polyhydroxyethyl component (B) using a urethane group, b is KTA (I) in the reaction with the component joining (II) and due to adulteration of the component stitching to add significant parts of water significantly increases the stability of the formulated using obtained in accordance with the invention, combinations of binders, what, in particular, has implications for use in industrial painting plants with an annular linear systems.

In addition, combinations of binders in comparison with the products of the prior art can be shared by large proportions of the components of the stitching. When storing lacquers impossible to determine the stratification of lacquer components. Thanks to the ability to influence the reactivity of varnishes in the extended range if necessary, you can also improve the adhesion of the intermediate layer film hot drying.

Used as polycarboxylic component (A) polyurethane resin contains as a specific raw material digidrokhinopimarovoi acid and is in accordance with the claims carboxyl group in accordance with the acid number of from 70 to 160 mgKOH/g and per molecule at least one end-blocked isocyanate groups. In accordance with the definition polycarboxylic component (A) contains in addition no hydroxyl groups, no residues of fatty acid number of more than 12 carbon atoms. The blocking means is cleaved at elevated temperatures, i.e. at the temperature of the reaction link is (I) from (A) and (B), after partial or complete neutralization of the carboxyl groups using a base, preferably with a secondary or tertiary alkylamine or alkanolamine, is soluble in water.

Polyurethane resin get in a known manner by reacting a mixture of MDI and partially blocked with monohydroxylic compounds and/or butanonoxime MDI using dihydroxypentanoic acid and, if necessary, by using the polyol, and quantitative ratios are selected so that the molecule is free from hydroxyl groups polycarboxylic component (A) has in average at least one end-blocked isocyanate group.

As polyisocyanate compounds are primarily used standard diisocyanates, such as, for example, toluylenediisocyanate, isophorondiisocyanate or hexamethylenediisocyanate, and if necessary also the isocyanate prepolymers.

For blocking the free NCO-groups use monohydroxyl connection, in particular, monoparty, as, for example, 2-ethyl-hexanol, simple monoether glycols and polyoxyalkylene or butanonoxime, and choose takiego component (A), i.e., the temperature of the separation should be between 80 and up to a maximum of 160oC. Polycarboxylic component (A) has a boundary number viscosity of from 6.5 to 12.0 ml/g, preferably from 8.0 to 11.0 ml/g, measured in N,N-dimethylformamide (DMF) at a temperature of 20oC.

As polyhydroxylated component (B) use of film-forming polyester resin, which differ a hydroxyl number from 50 to 500 mgKOH/g, an acid number of less than 20 mgKOH/g and the boundary number viscosity of from 8.0 to 13.0 ml/g, preferably from 9.5 to 12.0 ml/g, measured in N,N-dimethylformamide at a temperature of 20oC. Obtained from polyolene and polycarboxylic acid polyester resin can be optionally polyurethane groups and can be modified using monocarboxylic acids which contain from 5 to 20 carbon atoms. However, the proportion of fatty acid number should not exceed 15 weight percent.

Components (A) and (B) react at a temperature of from 90 to 170oC, preferably at a temperature which is higher by 10 - 20oC temperature removal of the blocking means to the end isocyanate groups in polycarboxyl component (A), to the boundary viscosity number from 13.5 to 18.0 ml/g, etc is IMO to consider the reaction product (I) after neutralization of the carboxyl groups should be perfectly soluble in water. Quantitative ratios are in the range from 10 to 80 weight percent, preferably from 15 to 40 weight percent of component (A) and from 20 to 90 weight percent, preferably from 60 to 85 weight% for the component (B), referred to the solid substance, and the amount of interest is respectively 100, and they are selected so that the reaction product (I) has an acid number of at least 25 mgKOH/g, preferably from 30 to 50 mgKOH/g

Then the reaction product (I) before or after partial or complete neutralization of the carboxyl groups with inorganic or organic bases, however, to add significant parts of water, is mixed with the water-insoluble component stitching (II), and diluted with water to suitable for further processing of the solids content.

As a component of knitting (II) are preferably used standard blocked diisocyanates or blocked polyisocyanates, which should have a minor fraction of the organic solvents.

To control tverdolistvennyh diisocyanates or polyisocyanates, preferably combinations of "soft" and "hard" types in the ratio of from 10 to 35 weight percent to 90 to 65 weight percent. Under "soft" types should, in particular, to understand the products that are obtained from diisocyanates or polyisocyanates by education biureta or oligomerization, for example of hexamethylenediisocyanate. In the case of "hard" types was used as the source of products of the diisocyanates or polyisocyanates containing cycloaliphatic or aromatic hydrocarbon residues. As such diisocyanates should be called: toluylenediisocyanate, tetramethylcyclopentadienyl, diphenylmethanediisocyanate, dicyclohexylmethane, isophorondiisocyanate.

In addition, as an integral component parts of crosslinking (II) can also be used water-soluble blocked polyisocyanates. Preferably such blocked polyisocyanates admixed after the above-mentioned dilution with water.

As bases for neutralizing the carboxyl groups of the reaction product (I) is preferably used secondary or tertiary alkylamines followed or alkanolamine.

The quantitative ratio of the reaction product (I) and component ssnow respectively is 100.

Further processing is obtained in accordance with the invention lacquer binders is carried out in a known manner. The products are preferably used as binders for water-soluble fillers, in particular for coating automobiles.

The following examples explain the invention without limiting its scope. All data in parts or percentages are, if not otherwise noted, the weight units.

In the examples the following abbreviations are used:

DGM - diethylethylenediamine simple ether

MIBK - methylisobutylketone

TDI - toluylenediisocyanate (standard isomeric mixture containing about 80% 2,4-TDI and about 20% 2,6-TDI)

EEW epoxy equivalent weight.

Getting polycarboxylic components

Component (A1). In an appropriate reaction vessel was placed a solution of 810 parts (6 moles) dimethylpropionic acid 946 parts dietilaminoetilovogo ether and 526 parts of isobutyl ketone. Within 4 hours to this solution at a temperature of 100oC at the same time add a mixture of 870 parts (5 mole) of the diisocyanate and 528 parts (2 mol) is half blocked by using etilenglikolevye of dietilaminoetilovogo ether and mixture (2:1) until the solids content of 60%. Component (A1) has an acid number of 140 mgKOH/g and the boundary viscosity number, measured in N,N-dimethylformamide (DMF) at a temperature of 20oC, of 9.3 ml/year

Half blocked toluylenediisocyanate obtained by adding 90 parts (1 mol) etilenpropilendienovogo ether 174 (1 mol) of toluylene diisocyanate for 2 hours at a temperature of 30oC and through subsequent reactions to NCO-value of 16 to 17%.

Component (A2). In the same way as in the case of component (A1), 945 parts (7 moles) dimethylolpropionic acid 1079 parts dietilaminoetilovogo ether and 599 parts of isobutyl ketone react with 1044 parts (6 mol) of toluylene diisocyanate and 528 parts (2 mol) is half blocked by using etilenpropilendienovogo ester diisocyanate. Component (A2) has a solids content of 60%, an acid number of 140 mgKOH/g and the boundary viscosity number, measured in N,N-dimethylformamide (DMF) at a temperature of 20oC, of 10.2 ml/year

Component (A3). In the same way as in the case of component (A1), the solution of 270 parts (2 mol) dimethylolpropionic acid and 118 parts (1 mol) of hexanediol in 361 part dietilaminoetilovogo ether and 181 parts methylisobutyl is 22 parts (2 mol) is half blocked by using butanonoxime toluylene diisocyanate and the reaction is continued until the conversion of all NCO groups. Then, using DGM/MIBK (2:1) is the solids content of 60%. Component (A3) has an acid number 89 mgKOH/g and the boundary viscosity number, measured in N,N-dimethylformamide (DMF) at a temperature of 20oC, 9.7 ml/year

Half blocked toluylenediisocyanate obtained using the additive 174 parts (2 mol) butanonoxime to 696 parts (4 mol) of toluylene diisocyanate for 2 hours at a temperature of 30oC and subsequent reactions to CO-values from 28 to 29%.

Getting polyhydroxylated components

Component (B1). In a suitable reaction vessel atrificial 130 parts (1.1 mol) of hexanediol-1,6, 82 parts (0.6 mol) of monopentaerythritol, 8 parts (0.05 mol) of isononanoic acid, 28 parts (0.1 mol) ricinulei fatty acid series (digitalisierung castor oil fatty acid) and 50 parts of isophthalic acid at a temperature of 210oC until an acid number of less than 4 mgKOH/g, the Viscosity of a 50% solution in etilenglikolevye air in accordance with DIN 53211 at 20oC is 125 seconds, the boundary viscosity number, measured in N,N-dimethylformamide at a temperature of 20oC, is 9.8 ml/year Component*B1 does not belong to the invention.

Component (B2 is stilletos, 28 parts (0.1 mol) of linoleic acid, 83 parts (0.5 mol) of isophthalic acid and 68 parts (0.3 mol) of anhydride trimellitic acid at a temperature of 230oC until an acid number of less than 4 mgKOH/g, the Viscosity of a 50% solution in etilenglikolevye air in accordance with DIN 53211 at a temperature of 20oC is 165 seconds. The boundary viscosity number, measured in N,N-dimethylformamide at a temperature of 20oC, 10.5 ml/year

Component (B3). 259 parts (1.35 mol) of tripropyleneglycol, 8 parts (0.05 mol) of isononanoic acid, 42 parts (0.15 mol) isoperational linoleic acid, 68.5 parts (0.5 mol) of monopentaerythritol and 175 parts (1.05 mol) of isophthalic acid etherification in the presence of 0.5 parts of dibutyltindilaurate at a temperature of 220oC until an acid number of 4 mgKOH/g Viscosity according to DIN 53211 at 20oC 70% solution in etilenglikolevye the air is 120 seconds. After dilution with 260 parts of methyl ethyl ketone at a temperature of 70oC for 3 hours add 70 parts (0.4 mol) of toluylene diisocyanate. The temperature is maintained until, until you have converted all of NCO-groups. Methyl ethyl ketone is removed in vacuum and then the initial mixture resultsresolution air in accordance with DIN 53211 at a temperature of 20oC is 58 seconds. The boundary viscosity number, measured in N,N-dimethylformamide at a temperature of 20oC, is 12.1 ml/year

The Component (B4). 259 parts (1.35 mol) of tripropyleneglycol, 25 parts (0.15 mol) of isophthalic acid and 97 parts (0.5 mol) of anhydride trimellitic acid etherification in the presence of 0.2 part of dibutyltindilaurate at a temperature of 220oC until an acid number of 15 mgKOH/g, the Viscosity of a 50% solution in etilenglikolevye air in accordance with DIN 53211 at a temperature of 20oC is 60 seconds. Boundary value viscosity, measured in N,N-dimethylformamide at a temperature of 20oC, is 11.4 ml/year

Next, we present the values of hydroxyl numbers for the above components B1, B2, B3, B4:

Component*B1 - 94 mgKOH/g

Component B2 - 185 mgKOH/g

Component B3 - 97 mgKOH/g

Component B4 - 220 mgKOH/g

Obtaining the component (I) binders

In accordance with those specified in the table. 1 quantitative ratios are mixed with each other polycarboxylic component (A) and polyhydroxy component (B) and the solvent is removed in vacuum to a significant extent during the heating to the reaction temperature. This Tampere, moreover, the sample after neutralization with dimethylethanolamine is perfectly soluble in water. Components directly processed further in accordance with examples 1 - 4.

Examples 1 to 4

In accordance with the data table. 2 the reaction product (I) at a temperature of from 40 to 100oC is mixed with forming a cross connection component (II) and using dimethylethanolamine set the specified degree of neutralization. You can also neutralize the reaction product (I) to add forming a cross connection component (II). The mixture is then diluted with deionized water. As forming a cross connection component (II) were used:

IC 1 - commercial (trade) blocked using butanonoxime the polyisocyanate (triple hexamethylenediisocyanate with isocyanurate structure), for example, Desmo N 3390, Bayer.

IC 2 - commercial (trade) blocked using butanonoxime the polyisocyanate (triple hexamethylenediisocyanate with burynai structure), for example, Desmodur N 100, Bayer.

The stability testing and storage of light lacquer-based binders in accordance with example 4

Stability was tested on a light water spray. D

Composition and digital indicators light varnish are shown in table. 5.

Bright varnishes are stored in sealed glass bottles at a temperature of 40oC. the test Results storage are summarized in table. 3.

Check binders in accordance with the invention as automotive fillers

Binders in accordance with examples 1 to 4 and example 3 of European published application N A2-0330139 serves as automotive fillers.

286 parts of a 35 percent binder

50 parts of titanium dioxide (rutile)

40 parts of barium sulphate

10 parts of micro-talc

0.2 parts of a particulate pigment

13.8 parts of water.

Varnishes have a solids content of about 50%, a pH value of about 8.0 a (installed using dimethylethanolamine) and a viscosity of about 1.2 P at a temperature of 20oC.

Fillers are using sprinklers on coated by immersion in an electrolytic bath cathode deposited primer, zinc phosphated steel sheet (thickness of the primer of about 20 μm).

The curing of the filler is carried out in a convection drying chamber for 20 minutes at a temperature of 140 innocase automotive coating varnish based on alkyd and melamine resins, which is cured for 30 minutes at a temperature of 135oC. (dry film Thickness 35 2 μm).

Strength properties of the film (resistance to solvents, resistance) and mechanical parameters in all layers meet the requirements of practice.

Strength relative to the shock of rubble tested using a device that simulates the impacts of gravel. "SPLITT" Single "Projectile" Launching Impact-Tester). The method is described in detail in the journal FARBE + LACK, room 8/1984. For this test, the contact angle is 5othe ball diameter is 3 mm with a weight of 0.5 was selected speed collision 100 km/h. Check the samples were tested at a temperature of +20oC and -20oC. In the table (rounded) specifies the damaged surface in mm2and naked in the damaged layer. (Sheet - B, primer - G, compound - F).

The test results are given in table. 4 and do not show characteristic differences.

1. The method of obtaining water-soluble lacquer binders containing product obtained by the interaction polycarboxylic component polyhydroxyether component and a crosslinking component, wherein as polycarboxylic component is isocyanate and MDI, partially blocked with monohydroxylic compounds and/or butanonoxime, with dihydroxypentanoic acid and, if necessary, a polyol, and containing carboxyl groups in accordance with the acid number of from 70 to 160 mg KOH/g, and also having in the molecule at least one terminal blocked isocyanate group, however, does not contain any free hydroxyl groups or fatty acid residues with more than 12 C-atoms and having a limit viscosity of from 6.5 to 12.0 ml/g, measured in N, N-dimethylformamide at 20oAnd as polyhydroxylated component, taken in an amount of 20 to 90 wt.%, use polyester resin, if necessary, modified urethane, with a hydroxyl number of 50 to 500 mg KOH/g, acid number less than 20 mg KOH/g and the limiting viscosity number ranging from 8.0 to 13.0 ml/g, measured in N, N-dimethylformamide at 20oWith, and the process is carried out at 90 - 170oTo obtain a product having a limit viscosity of from 13.5 to 18.0 ml/g, measured in N, N-dimethylformamide at 20oWith, and which is completely soluble in water, and then mixed for 60 to 90 wt.% the obtained product I, before or after partial or complete neutralization of the carboxyl groups near is from blocked diisocyanates, and/or blocked polyisocyanates, and/or mixtures thereof, at 40 - 100oWith, after that spend the dilution water until ready for further processing of the content of solids, and the amount of interest for the composition of a combination of And and or of I and II in terms of solid matter is respectively 100.

2. The method according to p. 1, characterized in that as dihydroxypentanoic acid is used dimethylolpropionic acid.

3. The method according to p. 1, characterized in that as component In use polyester resin containing up to 15 wt.% monocarboxylic acids with 5 to 20 C-atoms.

4. The method according to p. 1, characterized in that polycarboxylic component And having a limit viscosity 8,0 - 11,0 ml/g, measured in N, N-dimethylformamide at 20oWith the use of 15 to 40 wt.%, and polyhydroxy component In having a limit viscosity of 9.5 to 12.0 ml/g, are used in amounts of 60 to 85 wt.% and the process is carried out at a temperature of 10 - 20oWith higher temperature the removal of the blocking means for the terminal isocyanate groups of component A, with the product I having a limit viscosity of from 14.5 to 16.5 ml/g, measured in N, N-dimethylformamide the mi and pick up so, the product I has an acid number of at least 25 mg KOH/g

6. The method according to p. 4, characterized in that the product I has an acid number of from 30 to 50 mg KOH/g

7. Water-soluble lacquer binder based on the product of the interaction polycarboxylic component And polyhydroxyether component and a crosslinking component that is received pursuant to sub.1 to 5 and used in the formulations of water-soluble varnishes hot drying, in particular as water-soluble fillers for paint finishes on cars.

 

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FIELD: self-crossing dispersion for dressing of glass-fiber.

SUBSTANCE: the invention is pertaining to the field of the self-crossing dispersion for dressing of glass-fiber on the basis of polyurethane, polyurethane-polyurea or polyurea used for dressing glass-fiber. The invention is also dealt with a method of production of the indicated dispersion and with a sizing compound for glass-fiber. The indicated dispersion contains the blocked isocyanate groups bound with the polymer and in addition the reaction-capable hydroxyl or amino groups bound with the polymer. The dispersion is stable at storing up to 50 °C and is self-crossing at the temperature of 90°C up to 280°C. The dispersion represents a reaction product - a) at least one polyolic component; b) at least one di-, tri- and / or a polyisocyanate component, c) at least one hydrophilic nonionic or a (potentially) ionic component; d) at least one component, which is distinct from a)- or b)-, having molecular mass - 32-500 and at least one isocyanate-reaction capable group; and e) at least one monofunctional blocking component. The offered dispersions are suitable for use in the capacity of coatings for mineral emulsion carriers, textile and leather, lacquers and polishes for wood, and also may be applied as paint primers, bases, joint fillers or finishing coatings.

EFFECT: the invention allows to use the dispersions as coatings for mineral emulsion carriers, textile and leather, lacquers and polishes for wood and to applied them as paint primers, bases, joint fillers or finishing coatings.

21 cl, 4 ex

FIELD: chemistry of polymers, chemical technology.

SUBSTANCE: invention relates to mixtures consisting of blocked polyisocyanates designated as hardening agents in monocomponent lacquers of hot drying and comprising: (a) blocked polyisocyanate based on 1,6-diisocyanate hexane; (b) blocked polyisocyanate based on cycloaliphatic diisocyanates chosen from group comprising 1-isocyanato-3,3,5-trimethyl-5-ixocyanatomethylcyclohexane, bis-(4-isocyanatocyclohexyl)methane, 2,6-bis-isocyanatonorbornane, 2,5-bis-isocyanatonorbornane, 1,4-bis-isocyanatomethylcyclohexane and their mixtures, and (c) 3,5-dimethylpyrazole as a single blocking agent of agent of polyisocyanates named in (a) and (b). Blocked polyisocyanates are taken in the weight ratio (a) : (b) = 1:(1.8-2.2). Using mixtures of blocked polyisocyanates provides preparing clear lacquers with good acid resistance, stability against scratching and thermal yellowing.

EFFECT: improved and valuable properties of agents.

1 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: hydropyle blocked polyisocyanates are produced by the method wherein: A) one or the several organic polyisocyanates interact with B) one or several organic compounds, containing, at least, one isocyanate reactive group and comprising b1) non-ionic hydropyle groups based on simple poly-alkylenoxide-polyethers containing at least 30 wt % of ethylene-oxide links, and/or b2) ionic or potentially ionic hydropyle groups a forming dissociation equilibrium depending upon pH in interaction with water, and, depending upon pH not having a charge and being charged positively or negatively, or interact with C) one or several blocking means containing, at least, one cyclic ketone with CH-acidity of the general formula (2) where X is the electron-acceptor group, R1, R2 mean independently from each other the hydrogen atom, saturated or unsaturated aliphatic residual containing up to 12 carbon atoms, n is 1, and, if necessary, interacting with one or several (cyclic)aliphatic mono- or polyamines with the amount of amino groups in a molecule of 1 to 4 and molecular weight of up to 400 note that, if necessary, it interacts with one or several multinuclear spirits with the number of hydroxyl groups in a molecule from 1 to 4 and molecular weight of up to 400, and, if necessary, with amino spirits in the presence D) of one or several catalysts or, if necessary, with auxiliary substances and additives and, if necessary E), with solvents. Polyisocyanates can be used for manufacturing varnishes, coatings, sizes, glues and molded products.

EFFECT: improved method of producing hydropyle blocked polyisocyanates.

6 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to blocked polyisocyanates, applied for obtaining of bonding means for thermohardening lacquers, paints and such other subjected to thermo processing systems, as adhesive substances or elastomers, they serve as means for net-like structure formation for polyol components. Blocked polyisocyanates have general formula (I): Said polyisocyanates are obtained by interaction of polyisocyanates of general formula (II)

with secondary amines of general formula (III)

EFFECT: obtaining of polyisocyanates, which ensure lower temperature of net-like structure formation and, therefore thermoprocessing, they are also stable as to crystallisation in organic solutions, which favours appreciable reduction of viscosity of such solutions, because it allows to reduce solvent content.

14 cl, 2 tbl, 15 ex

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