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Production method of trioctyl phosphate

A technology of trioctyl phosphate and a production method, applied in the field of chemical material production, can solve problems such as unrefined products, unfavorable production efficiency, air pollution, etc., and achieve the effects of shortening esterification time, improving production efficiency, and saving usage

Active Publication Date: 2013-12-11
HANGZHOU QIANYANG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the reaction time of the esterification process is too long, requiring more than 8 hours, which is not conducive to the improvement of production efficiency; in addition, the product obtained is not refined and has a low purity; the hydrogen chloride gas produced by the reaction is not processed in time, cause air pollution

Method used

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  • Production method of trioctyl phosphate

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Experimental program
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Effect test

Embodiment 1

[0044] First add measured isooctyl alcohol into the mixing tank, cool it down to below -15°C with frozen brine, then add measured phosphorus oxychloride in batches under vacuum conditions, the material ratio is phosphorus oxychloride to octanol moles The ratio is 1:3.10. Then add metered catalyst, the catalyst consumption is 0.5% of the mass of phosphorus oxychloride. Control the adding speed of phosphorus oxychloride, so as to control the mixing temperature not higher than 20°C, and reduce the occurrence of side reactions.

[0045] Under the vacuum condition of -0.097MPa, the above-mentioned mixed materials are slowly heated up. In the early stage, the temperature rise rate is controlled at about 15-20°C / h, so that the hydrogen chloride gas generated by the reaction can be discharged in time to reduce the occurrence of side reactions. After 3 hours of reaction, when the material in the reactor reaches 80°C, speed up the temperature rise rate and control it at 30°C. ℃ / h to s...

Embodiment 2

[0051] The material proportioning of embodiment 1 is phosphorus oxychloride and octanol molar ratio is 1: 3.15, and the mol ratio of lye and phosphorus oxychloride is 1: 15, under the vacuum condition of-0.097MPa, above-mentioned mixing Good materials slowly heat up. In the early stage, the heating rate is controlled at about 15-20°C / h, so that the hydrogen chloride gas produced by the reaction can be discharged in time to reduce the occurrence of side reactions. After 3 hours of reaction, when the material in the reactor reaches 90°C, speed up the heating rate and control it at 30°C. ℃ / h to speed up the reaction. Because the amount of octanol decreases in the later stage of the reaction, the reaction rate is relatively slow. In order to improve the product yield, when the reaction temperature reaches 110° C., add 10% of the above-mentioned octanol amount to the reaction system and react for 1 hour. When the temperature rises to 150° C., the reaction ends. The reaction time ...

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Abstract

The invention relates to a production method of trioctyl phosphate. The trioctyl phosphate is obtained by reacting phosphorus oxychloride and isooctyl alcohol under the action of titanium tetrachloride; the integral production process comprises the following process steps of: mixing; esterifying; neutralizing, and washing; dealcoholizing; carrying out refining treatment; carrying out dewatering pressure filtration, and the like. The synthetic method disclosed by the invention can be used for adding the phosphorus oxychloride in batches under a production process condition, controlling the temperature of a mixing process, greatly reducing the generation of side reaction and enhancing the purity of products; the synthetic method disclosed by the invention can be used for furthest improving the transformation ratio of the phosphorus oxychloride by utilizing the proportion, namely the mole ratio of the phosphorus oxychloride and octanol at 1:(3.10-3.15), saving the usage amount of the octanol and saving the cost, thereby being favorable to industrial large-scale production.

Description

technical field [0001] The invention belongs to the field of chemical material production, in particular to a production method of trioctyl phosphate. Background technique [0002] Trioctyl phosphate (TOP), molecular formula C 24 h 51 o 4 P, relative molecular mass is 434.62, theoretical phosphorus content is 7.13%, its structural formula is as follows: [0003] [0004] Trioctyl phosphate is one of the more practical flame-retardant and cold-resistant plasticizers, used in vinyl resins, cellulose resins, phenolic resins, polyurethanes, synthetic rubbers, solvents, defoamers, etc.; its low-temperature performance is excellent It is based on adipate, and has anti-mildew and flame-retardant effects. Although the thermal stability and plasticizing performance are slightly poor, it can be improved when used in combination with tricresyl phosphate; self-extinguishing products can be obtained in combination with DOP. It can also be used in polyvinyl chloride cable materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
Inventor 黄阳卫陈勤勇吴周华
Owner HANGZHOU QIANYANG TECH
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