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Preparation method of dihydric phenol di(dialkyl phenyl organic phosphate)

A technology of phenyl phosphate and dihydric phenol is applied in the field of preparation of dihydric phenol bis[bis(2,6-dimethyl)phenyl phosphate], which can solve the problem of increasing the difficulty of product purification, many side reactions, etc. problems, to achieve the effect of reducing environmental protection treatment costs, good environmental protection, and reducing production costs

Active Publication Date: 2013-06-12
雅克(上海)化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process not only still needs two steps, each step also produces a large amount of HCl gas, the above defects still exist, and there are many side reactions, which will increase the difficulty of product purification

Method used

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  • Preparation method of dihydric phenol di(dialkyl phenyl organic phosphate)
  • Preparation method of dihydric phenol di(dialkyl phenyl organic phosphate)

Examples

Experimental program
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Effect test

Embodiment 1

[0024]Example 1: Add 328g of TXP into the reactor, slowly add 44g of resorcinol, raise the temperature to 80°C, add 4g of sodium diphenylborate catalyst, raise the temperature to about 100°C, start stirring, and turn on the vacuum, the extracted 2,6 —Xylenol is recovered by the condenser, the reaction temperature is slowly raised to 250°C, and the reaction is kept for 3 hours. Cool to 100°C, add 300g of ethanol solution, continue cooling to below 50°C, the product begins to recrystallize, the precipitate is filtered and washed with deionized water, and the precipitate is dried at 60°C to obtain 233g of white powder which is resorcinol Bis[bis(2,6-dimethyl)phenyl phosphate]XDP, yield: 85%, melting point: 103°C, main content: 98.1%. The liquid chromatogram is shown in the accompanying drawing, and the data of each product peak are shown in Table 1.

Embodiment 2

[0025] Example 2: Add 328g of TXP into the reactor, slowly put in 44g of hydroquinone, raise the temperature to 80°C, add 4g of sodium diphenylborate, repeat the above process, and obtain 240g of white powder which is hydroquinone bis[bis(2, 6-Dimethyl)phenyl phosphate], the yield is 87.6%, the melting point is 105°C, and the main content is 97.7%.

Embodiment 3

[0026] Example 3: Add 260g of TPP (triphenyl phosphate) into the reactor, slowly add 44g of resorcinol, repeat the above reaction process, add 60g of deionized water after the reaction is completed, stir at 70°C for one hour, separate layers, and The remaining water was removed by vacuum distillation in the oil layer to obtain 188g RDP with a yield of 81.7% and a main content of 97%.

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Abstract

The invention relates to an improvement on a preparation method of dihydric phenol di(dialkyl phenyl organic phosphate), which is characterized in that an ester exchange reaction is carried out on dihydric phenol and trialkyphosphate phenylester under the catalysis of a catalyst with a molar ratio of 1:2 to 1:3; and the synthesis is finished in one step. The preparation process is simple; a product is easily obtained and has high purity; compared with the prior art, the preparation method enhances the purity by 2% to 3%; in the preparation process, the environmental protection property is good; no pollutant or waste water is produced; the subsequent environmental protection treatment cost is largely reduced; the total preparation cost is also reduced; no HCl is produced; requirements (need of corrosion prevention due to no acidity) for equipment are also reduced; a device for collecting and treating HCl does not need to be added; and the environmental protection property is good in the preparation process.

Description

technical field [0001] The present invention is an improvement to the preparation method of dihydric phenol bis(dialkylphenyl phosphate), especially relates to a one-step synthesis method with simple method and good environmental protection of dihydric phenol bis(dialkylphenyl phosphate). Phosphate) preparation method is a further supplement to the preparation method of the applicant's previous patent application 200910033993.1 dihydric phenol (aryl polyphosphate) flame retardant. Background technique [0002] The decomposition temperature of engineering plastics is usually 300-550°C. In order to achieve the flame retardant effect, the flame retardant must be decomposed synchronously when the engineering plastics are ignited to achieve the flame retardant effect. If the decomposition is later than the engineering plastics, it will not be effective. Flame retardant, so it is required that the decomposition temperature range of the flame retardant should be in the range of 300...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/12
Inventor 沈琦周乐群仇国才吴仁铭周荣孙
Owner 雅克(上海)化工新材料有限公司
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