The way to obtain a latex of a copolymer of vinylidenechloride

 

(57) Abstract:

Usage: in the field of polymer technology, namely how to obtain latexes of copolymers of vinylidenechloride used in the manufacture of latex paints, polymer compositions. The inventive process copolymerization VDH with vinyl chloride and unsaturated carboxylic acid is carried out in the presence of a mixture of emulsifiers, one of which is alkylphosphonate sodium with the number of carbon atoms in the alkyl 12-18, and as another emulsifier used ammonium salt of sulfonated 15-20 wt. % alkylperoxo ether of polyethylene glycol with a number of carbon atoms in the alkyl 8-12 and the number of hydroxyethyl groups 10-12 in number in a mixture of emulsifiers 65-75 wt. % when the content of the emulsifier mixture of 3,5-5,0 by weight of comonomers. table 1.

The invention relates to the field of polymer technology, namely a process for the production of latexes of copolymers of vinylidenechloride (VDH), used in the manufacture of latex paints (VDK), polymer compositions may be used to produce frost-resistant latex copolymers VDH with vinyl chloride (I) unsaturated carboxylic acid (maleic, f is lastnosti, due to the unique combination of several of their properties: high water, acid and alkali, non-combustible, odorless, resistant to organic solvents, mineral oils.

Increasing the frost resistance of latex used for these purposes is the actual problem, the solution of which can significantly reduce the cost of transporting and storing them in the winter.

For aqueous dispersions of copolymers produced as a commercial product, an important property is also aggregate stability, because many consumers have high requirements for the retention of latex, which must be not less than three months. In addition, aggregate stability required for transportation of latex over long distances.

It is known that the incorporation in the copolymer VDH RIN unsaturated carboxylic acids such as methacrylic, acrylic or maleic increases the frost resistance of latex. However, the resistance of these latexes does not meet the requirements of use, for example, VDK (at least 5 cycles of freezing at minus 40oC for 6 hours and thawing at 20-25oC for 18 h) and accounted for the receipt of high-concentration aleksov copolymers VDH with I [2] by copolymerization VDH with I in aqueous emulsion in the presence of a water-soluble initiator and an emulsifying system, consisting of alcohol and ionic emulsifier, and as an alcohol, a mixture of fatty alcohols with an unbranched chain WITH14-C16or17-C180,5-0,8 wt.h. and as an emulsifier alkylphosphonate sodium12-C18in the alkyl, at a ratio of components of the emulsifying system 1:3-1:5, respectively, in a process carried out at a dosage VDH and a mixture of fatty alcohols WITH14-C16or17-C18during copolymerization. Get the latex with the following mechanical properties: stability during storage is more than 6 months, the dry matter content of more than 60 wt. the surface tension of 35 to 40 mn/m, pH 7.0 to 8.0, but latex does not have frost (see table, example N 16). Introduction in the polymerization recipe of 1.5 wt.h. unsaturated carboxylic acids (maleic, fumaric or takenaway) only slightly improves the frost resistance of latex of a copolymer based on VDH (1-2 cycles).

The technical result of the invention is to increase the frost resistance of latex copolymer VDH with I and unsaturated carboxylic acid.

The result is achieved that the method of obtaining LVII water-soluble initiator and a mixture of emulsifiers, containing alkylphosphonate sodium with the number of carbon atoms in the alkyl radical of 12-18, with dosage VDH and mixtures of emulsifiers in the course of polymerization, the mixture of emulsifiers contains 65-75 wt. ammonium salts of sulfonated 15-20 wt. alkylphenolates ether of polyethylene glycol with a number of carbon atoms in the alkyl radical 8-12 and the number of hydroxyethyl groups of 10-12 when the concentration of the mixture of emulsifiers is 3.5 to 5.0% by weight of comonomers.

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

Example 1 (invention).

In a reactor with a volume of 4 l and load (wt.h.) 92 demineralized water, 1,5 maleic acid, 0,6 alkylphosphonate sodium 1,4 ammonium salts of sulfonated 15 wt. alkylperoxo ether of polyethylene glycol with a number of carbon atoms in the alkyl 8-12 and the number of hydroxyethyl groups 10-12 (emulsifier S-10, THE 6-02-09-13-87), 0.6 ammonium persulfate, 19 VDH and 34 I, with stirring, the reaction mixture is heated to 50oC and carry out the copolymerization at a constant temperature. Through 1 h after reaching the set temperature start to dose in the reactor 45,5 VDH and the mixture (solution) of 0.6 alkylphosphonate sodium, 1.4 emulsifier With 10 and 8 of demineralized water. With the ATM. After stavki monomers latex Tegaserod vacuum when the vacuum 700-720 mm RT.article and temperature 55oC for 1 h If the concentration of residual monomers not reduced below 0.03 wt. I and 0.01 wt. VDH, the operation of the degassing continued for 0.5-1 hours After degassing the reactor through latex miss gaseous ammonia to pH 7.0, then gradually add 2.0 to 2.5 wt. including crystalline NH4HCO3, after which the pH of the latex is raised to 8.0. Get a latex of a copolymer with the content, wt. VDH 64-66, I 32-35, unsaturated carboxylic acid 1-2.

Frost latex define in the chamber with a temperature of minus 40oC. the Latex in the amount of 100-125 ml is placed in a jar of tinplate volume of 250 ml (diameter 70-75 mm, height 65 mm) and incubated in a chamber at minus 40oC for 6 hours defrosting the latex occurs at 20-25oC for 18 h After thawing few ml of latex was poured on a glass plate (or Petri dish), and then tilt it at 45ofor draining excess latex. Latex believe stands the test, if the latex film on the glass is homogeneous.

Stability in storage is determined by observation of the sample latexes) and visually the presence of coagulum in the form of sediment at the bottom of the flask.

The dry residue is determined by drying in a heating Cabinet at a temperature of 755oC to constant weight; the surface tension according to the method of Du-Nui, pH at pH meters type LPU or monomer EV-74.

The process conditions copolymerization VDH with I and unsaturated carboxylic acid and the properties of the obtained latex of the copolymer are shown in table.

Examples 2-15 (invention), examples 17-23 (for comparison) carried out as in example 1. Conditions of the copolymerization process and properties of the obtained latexes of copolymers are shown in table.

The way to obtain a latex of a copolymer of vinylidenechloride by copolymerization of vinylidenechloride, vinyl chloride and an unsaturated carboxylic acid in an aqueous medium in the presence of a water-soluble initiator and a mixture of emulsifiers containing alkylphosphonate sodium with the number of carbon atoms in the alkyl radical of 12 to 18, with a dosage of vinylidenechloride and mixtures of emulsifiers in the course of polymerization, characterized in that the mixture of emulsifiers contains 65-75 wt. ammonium salts of sulfonated 15 -20 wt. alkylperoxo ether of polyethylene glycol with a number of carbon atoms in the alkyl radical of 8 to 12 and the number of hydroxyethyl groups 10 12 when the concentration of the

 

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