Method for preparing oligomerization phosphoric acid ester or oligomerization phosphorous acid ester

Abstract

The invention discloses a preparation method of phosphate oligomer or phosphite ester oligomer. The method comprises the following steps that: a. in the condition of catalyst and heating, (formula 1) reacts with phosphorus oxychloride to produce triaryl phosphate or (formula 2) is employed to react with the phosphorus oxychloride to produce triaryl phosphite ester in the condition of catalyzer and heating; b. the triaryl phosphate is subject to ester exchange reaction with HO-R-OH in the condition of catalyst, antioxidant, heating and decompression to obtain phosphate oligomer; or triaryl phosphite ester is subject to ester exchange reaction with HO-R-OH in the condition of catalyst, antioxidant, heating and decompression to obtain phosphite ester oligomer; wherein, X is C1-4 alkyl; R is (formula 3); Hydroxyl in HO-R-OH is contrapuntal. The method has simple technique, short reaction time, good-quality products and high production yield and is convenient for industrialization.

Description

technical field The present invention relates to the preparation method of oligomeric phosphate or oligomeric phosphite. Background technique Oligomeric phosphate is a kind of flame retardant, and the synthesis method reported in the literature mainly contains 3 kinds at present: 1. phosphorus oxychloride reacts with bisphenol to obtain bisphenol tetrachlorobisphosphate, then carries out capping with phenol, obtains Target product; 2. After phosphorus oxychloride reacts with phenol to obtain diaryl phosphorus oxychloride, then reacts with bisphenol to obtain target product; 3. Replacing phenol with sodium phenate as raw material, that is, using sodium phenate to treat bisphenol tetrachlorobisphosphoric acid The ester is subjected to a capping reaction to obtain the product. Method 1. First of all, the first step to generate bisphenol tetrachlorobisphosphate is easy to generate polymers (the polymerization is too high, the product viscosity increases, and even becomes solid...

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Problems solved by technology

Third, the obtained crude product has a darker color and higher viscosity, and needs to be washed several times to remove impurities, causing serious pollution to the environment

Method two, the pure substance of diaryl phosphorus oxychloride is difficult to synthesize, it is easy to generate the mixture of one aryl phosphorus oxychloride, diaryl phosphorus oxychloride and triaryl phosphoric acid ester, if need diaryl phosphorus oxychloride then need to reduce the mixture Pressure distillation, the yield of the product obtained is not high

Method three, this method reduces energy consumption relative to method one, but the first step reaction is the same as the first step in method one, and there is the same problem, and the preparation of sodium phenate is more difficult because phenol is easily oxidized

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