SU203231A1 - Process for producing polyarylates - Google Patents

Description

(21) 835325/23-О5

(22) 09.05,63

(46) 07.15.83. Bü № 26 (72) M.S. Akutin, V.V. Korshak, L.A. Rocovilova, R. D. Zhilina and D. Islan l.

(53) 678.674 (088.8)

(54) (57) METHOD FOR OBTAINING POLYARILES Using interfacial polychromatics and hyalaria terephthalic (isophthalic) acids and cyan, this is due to the fact that, in order to increase the resistance to thermal-oxidative processes at elevated temperatures, it is reduced to a mixture of oxygen and cyan. taken in mixture with cichlorogicria of methylphosphonic and phenylphosphonic acids.

A known method for producing polyarylates by interfacial polycondensation of cyan and dichlorangiarites with ()) taqi and isophthalic acid However, these polyarilates, when processed under the influence of oxygen and high temperatures, can be made from high-quality materials,

The following method is possible. the production of IepMOCToftKHx polya-° latoWe recyclable without decomposition

The preparation of these polyarylags is carried out by mechanic {phase g oliconcentration of cyan (2.2 "dioxy-4,4-diphenylpropane) with terephthalic (respectively, i -ophthalic) and -methylphosphine or phenylphosphoric acid dichlorides.

Phosphorus-containing cyanogens are introduced into the reaction in the amount of Hgbweach. counting on dian

The rigidity of polyarylates is carried out as follows.

A round bottom flask equipped with a mech, a chemical mesheshasha, a reverse hopopole, a thermometer and a dropping boil, at 20–2–5 ° C, is charged with a alkaline dian solution, and an organic phase of the mixture was added to KOTOipoMy (with a constant stirrer) from the dropping funnel. terephthalic and methylphosphonic acids in an organic solvent (tt-xylene, benzene, etc.,) that are immiscible with Wocoio. The reaction mixture is stirred at 20-25 C for 15 minutes, after which they will dissolve for 15 minutes. The precipitated polymer o is filtered from an organic-water solution, followed by washing the precipitate on the filter with a hot water of a negative reaction in the presence of noHOJ3 chlorine (sample). The washed polymer is subjected to 60-80 ° C

constant TOita, Exit POLYMB

ra. The specific viscosity of a 0.5% polymer solution in a mixture of tetrachloro a with phenol 0, is 65. The softening temperature of polymers 340-360 C.

The physicochemical properties of the effervescent phosphorus-containing polyarylates are preastated.

Example 1. To 200 ml of a water-alkaline solution of 2.2 aioxy 4,4 difanilpropane, containing 4.61 g of 2,2-aioxy 4,4 1-phenylpropane and 2j49 g KOH, 200 ml of org are added

The niobium phase containing 4.07 g of tert-phthalic acid cichlorogicride and 0.027 g of methylphosphonic acid dichloride dissolved in G-xylene. 5 The reaction is carried out with vigorous stirring and a temperature of 2O-25 ° C. 1 “15 minutes, after which the reaction mixture is kept at this temperature for 15 minutes. Formed polmer

10 is filtered off, washed on the filter with hot water until a negative reaction. the presence of chlorine ions {sample with. and dried at a constant weight. The yield of the polymer is 91%, the temperature of disintegration is 360 ° C, the specific viscosity is 0, the solution of the polymer in a mixture of tetrachloroethane with phenol (bO4O) is 0.65.

Example 2. To 20O ml of an aqueous alkaline solution 2, α-cyoxy 4.4 -

20 cificiline containing 4.61 g of 2.2 dioxy-4,4-diphenylpropane and 2.49 g of KOHfv are added 200 ml of the organic phase containing 4.04 g of terephthalic acid cichloride, O, O53 g of methylphosphine acid dichlorogaride, dissolved in D) -xylene. The reaction is carried out according to the mode described in Example 1. The polymer yield is 87.5%, the softening temperature is 360 ° C,

Q is the specific viscosity of polymer solution in a mixture of phenol with tetrachloroethane 0.63,

Example Z. To 200 ml of an aqueous, alkaline solution of 2,2-aioxI 4.4 of ciphenylpropane containing 4.91 g of 2,2-aioxy-4,4-diphenylpropane and 2.61 g of KOH, 200 ml of the organic phase containing 4.16 g of terephthalic acid chloride chloride and 0.1417 g of methylphosphinic acid dichloride dissolved in P-xylene. The reaction is carried out according to the regime described in example 1. A polymer yield of 85.5%, 5 a specific viscosity of 0.5% of a polymer solution in a mixture of phenol O tetrachlo | ethane, 0.27; softening temperature 350 ° C. g

Example 4. To 200 ml of an aqueous alkaline solution of 2.2 dioxy-, 4 diphenylpropane, containing 4.90 g of 2,2-dioxy-4,4-cyphenylpropane and 2.61 g of KOH, 20 O ml of organic phase containing 3.94 g dichloro terephthalic anhydride and

In Example 1. The polymer yield is 80.5%, the specific viscosity is 0.23, and the softening temperature.

Example 5. To 20O ml of water-j alkaline solution of 2,2 - dioxy-4,4 - tsienilpropana containing 4.64 g of 2,2-dioxy-4,4-cyphenylpropane and 2.42 g of KOH, 200 are poured ml of the organic phase containing dichlorangits tOrits of isophthalic acid and 0, O53 g Methylphosphinic acid, dissolved in and-xylene. The reaction is carried out according to the mode of example 1. The polymer yield is 67.5%,

specific viscosity, 0.20, softening temperature ZrO С,

Example 6. To 200 ml of a water-alkaline solution of 2,2-aioxy-4,4-diphenylpropane containing 4.39 g of 2,2-cyoxy-4,4-diphenylpropane and 2.49 g of KOH, 200 ml of the organic phase are added, containing 3.91 g of aihlbrn anhydride of isophthalic acid and 0.133 g of methylphosphinic acid dichlorohydrin dissolved in P-xylene. The reaction is carried out according to the mode of example 1, the polymer yield is 65.9%, the specific viscosity is 0.16, and the softening temperature.

Softening temperature

370

360 Waela viscosity 0.5% solution & blend () in chloroethane and phenol 0.72 O, 5 0.65 Flammability Burns On Not th-Not burns Metope redistribution- Casting Casting P-burns & press processing in a reusable note

300

340

350

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Claims (1)

METHOD FOR PRODUCING POLYARYL TOV by the method of interfacial polycondensation of terephthalic (isophthalic) acid and cyanide cychlohydrides, characterized in that, in order to increase resistance to thermo-oxidative processes at elevated temperatures, terephthalic (isophthalic) acid dichlorofluorophosphoric acid and hydrogen phosphorides have been taken up.