SU576763A1 - Method of preparing self-extinguishing polyurethans - Google Patents

Description

PRI mme R 2. Synthesis of polyurethane on the basis of polyoxyphopylamine, dafeyushmethandiocyanate and bis- (hydroxymethyl) phosphinic acid.

6.7 g polyoxyprotecheglycol with mol. 1000 and 3.35 g of 4,4-diphenylmethanedine ethoxyanate, under conditions analogous to example 1, are heated at 80 ° C for 90 minutes with constant stirring. The resulting prepolymer (mol. Weight 1500; the content of the cocoa palate groups 5.6%) is dissolved in 24.5 ml of dimethylformamide. A solution of 0.54 g of 5wc- (hydroxymethyl phosphinic acid in 1.3 ml of dimethylformamide) is added to the resulting solution at room temperature. After adding the entire solution, the reaction mixture is stirred for an additional 3 hours, after which the polymer solution is degassed under vacuum, poured onto Glass and dried at 50 ° C for 6-8 h

PRI me R 3. Polyurethane polyester based on polyoxytetramethylene glycol, toluishi diisocyanate and & is- (hydroxymethyl) phosphonate 1. ,

12.4 g of polyoxy tetramethylene glycol with a mol. Weight of 1000 and 14.3 g of toluyouhene diisuptate (mixture of 2.4 and 2,6 isomers in the ratio 80:20) are heated at 60 ° C for 60 MS with constant stirring. The obtained prepollmer (mol. Weight 1348; content of terminal isocyanate groups 6.2%) was dissolved in 39 ml of dimethylformamide. A solution of 0.8 g of 5hys (hydroxymethyl) phosphinic acid in 2 ml of dimethylformamide is added to the solution at room temperature, after which the reaction mixture is stirred for an additional 3 hours and 30 minutes. Then the polymer solution is degassed under vacuum, poured onto glass and dried at 50 ° C for 6-8 hours.

PRI me R 4. Synthesis of polyurethane based on prlioxypropylene glycol, toluylene diisocyanate and (hydroxymethyl) phosphinic acid.

12.4 g of polyoxypropylene glycol with mol. 1000 and 4.3 g of toluene diisocyanate are heated at 85-90 ° C for 90 minutes with constant stirring. The resulting prepolymer (mol. Weight 1348; content of terminal isocyanate rpjTin 6.2%) was dissolved in 39 ml of dimethylformamnd. A solution of 0.8 g (5ms- (oxymethyl) s | yusphinic acid in 2 ml of dimethylformamide) is added dropwise to the solution at room temperature. After adding the entire solution, the reaction mixture is stirred for another 3 h 30 min, then the polymer solution is degassed under vacuum, poured onto glass and dried

PRI me R 5. Synthesis of polyurethane based on polyoxytetramethylene glycol, 4,4-dniphenyl methane diuo-anocyanate and the diethylshmyuyu salt of bis (oxymethyl) phosphinic acid.

In a two-neck reactor equipped with a stirrer and a dropping funnel, 0.8 g (0.0063 gx hmol) b “c- (oxymethyl) fospsyuic acid will prevent. While stirring, 0.4 g (0.0063 g-mol) diethylamine is added dropwise to the acid. After the addition of the whole solution of diethylamine, the reaction mixture is stirred for 1 hour. Then benzene is distilled off under vacuum, the resulting salt is washed twice with ether and the mixture is evacuated. A solution of 10 g of a prepolymer (mol. Wt. 1500; content of cosmic isocyanate groups 5.6%) in 28 ml of dimethylformamide, obtained by the interaction of 6.7 g of polyoxytetramethylene glycol with a mol. Weight. 1000 and 3.35 g of 4,4-dipshme methane diisocyanate according to the procedure of Example 1. After adding the solution, the reaction mixture is stirred for another 4 hours at room temperature.The resulting polymer solution is degassed, poured onto glass and dried at 50 ° C for 8-9 hours.

PRI me R 6. Synthesis of polyurethane on the basis of polyoxytetramethylene glycol, 4,4-diphenylmethane zosh1anat and triethylamine with n- (oxymethyl) phosphonic acid.

To 1.5 g of the trapethylamine salt (hydroxymethyl) with {Biofluoric acid, obtained on the basis of 0.85 g of b / (c- (hydroxymethyl) phosphonic acid and 0.6 g of triethylamine), the solution 11 is added g nredpolymer (mol. weight 1500; content of terminal isodanate groups of 5.6%) in 29 ml of dimethylformamide obtained from 7.4 g of polyoxynpropylene glycol and 3.7 g of 4,4-diphenylmethane diisocyanate by the method of example 1. The reaction mixture is stirred for 3 h , then degassed, poured onto glass and dried.

On the basis of polyurethanes developed according to the invention, self-discharging films with high physicomechanical indicators are obtained: discontinuous (6) 130628 kg / cm, elongation (e) 2201020%, 1} adhesion to rubber and fabrics capable of reinforcement with fiberglass and other materials.

The study of thermo-oxidative resistance of polymers by the method of thermogravometry shows that weight loss (5%) is observed at 230-240 ° C.

A study of the flammability of polymers using the methods of spreading luiaMemi, a fire tube and a gravimetric method shows that the phosphorus containing polyurethanes synthesized can be attributed to self-extinguishing materials. The length of the burnt part is limited by the area of contact between the sample and the needle. Films - when squeezed over a period of 30 s, they lose 1-15% of their weight, while films produced by a known method lose 98% of their weight when they are melted. for 20-30 seconds

nojHiypeTaHbi can be used in folk farms as a film- and fiber-forming fabric, as well as decorative and finishing materials with lower combustibility.

Claims (1)

In the table npHBCj eabi, some properties of self-extinguishing polyurethanes based on hydroxyl-containing compounds, D1shzoshatov, bis- (oxymethyl) phosphonic acid and its salts. 7. The claims of the method for producing self-extinguishing polyurethanes by reacting a urethane prepolymer with NCO end groups with a phosphorus containing chain expander, characterized in that, in order to improve the fire resistance of the final product, bis (oxymethyl) phosphinic acid or its JR is used as an extension of the chain. and triethylamine ole and rukyution are carried out in a solution of cimethylformamide for 3-4 hours at 18-25 ° C. Sources of information taken into account during the examination: 1. USSR Author's Certificate No. 360354, cl. C 08 G 18/83, 1971.