Synthesis method of trioctyl phosphate

A technology of trioctyl phosphate and crude ester, which is applied in the chemical industry, can solve problems such as corrosion of production equipment, many reaction steps, and environmental pollution, and achieve the effects of energy saving, short reaction cycle, and increased economic benefits

Pending Publication Date: 2013-07-31
天津市联瑞阻燃材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are also many preparation methods of trioctyl phosphate in the prior art. These methods have their advantages respectively, but there are also many reaction steps in the preparation method, long routes, low efficiency, high energy consumption, corrosion of production equipment, cause environmental pollution

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  • Synthesis method of trioctyl phosphate
  • Synthesis method of trioctyl phosphate

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preparation example Construction

[0031] A kind of preparation method of trioctyl phosphate, general idea is as follows:

[0032] Step 1: Add phosphorus oxychloride dropwise to isooctyl alcohol to generate crude ester for synthesis reaction.

[0033] The second step: neutralize and balance the crude ester in the first step of transfer with alkaline solution.

[0034] The third step: wash the wet crude ester separated in the second step with hot water.

[0035] The fourth step: the final product trioctyl phosphate (TOP) is obtained by distilling and dehydrating the wet crude ester qualified in the third step.

[0036] To sum up, the production of trioctyl phosphate is to add phosphorus oxychloride dropwise to the raw material isooctyl alcohol at low temperature to react at a specified temperature (58-65°C); and pay attention to the discharge of hydrogen chloride to make the reaction go to the end, and then pass through alkali Neutralize and balance, wash with water until neutral, and distill under reduced pre...

Embodiment 1

[0045] A preparation method of trioctyl phosphate, the steps are as follows:

[0046] 1. Synthesis process:

[0047] According to the ratio of raw materials, put 280 kg of isooctyl alcohol into the synthesis tank, pump 115 kg of phosphorus oxychloride into the high-level tank; start the stirring of the synthesis tank, and raise the temperature to 47~53 °C through the jacket, Start to add phosphorus oxychloride dropwise to the synthesis kettle, control the temperature at 65±2°C, finish the addition within 4~6 hours, and continue to react for 4~6 hours to balance the acid produced by the reaction, use the acid absorber and collection tank The crude ester can be obtained by circulating the pump or absorbing with dilute alkali.

[0048] 2. Neutralization and balance process

[0049] Transfer the crude ester to the neutralization tank of the added lye (mass concentration: 3-5%, mass ratio of crude ester: lye: 4:1) for stirring and neutralization, time 1-1.5 Hours, temperature 70...

Embodiment 2

[0055] A preparation method of trioctyl phosphate, the steps are as follows:

[0056] 1. Synthesis process:

[0057] According to the ratio of raw materials, put 720 kg of isooctyl alcohol into the synthesis tank, pump 400 kg of phosphorus oxychloride into the high-level tank; start the stirring of the synthesis tank, and raise the temperature to 47~53 °C through the jacket, Start to add phosphorus oxychloride dropwise to the synthesis kettle, control the temperature at 65±2°C, finish the addition within 4~6 hours, and continue to react for 4~6 hours to balance the acid produced by the reaction, use the acid absorber and collection tank The crude ester can be obtained by circulating the pump or absorbing with dilute alkali.

[0058] 2. Neutralization and balance process

[0059]Transfer the crude ester to a 400 kg neutralization tank with added lye (mass concentration 3~5%) for 1~1.5 hours, temperature 70±3°C, and neutralize to control pH The value is 8~9; after passing thr...

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Abstract

The present invention relates to a synthesis method of trioctyl phosphate, and the method comprises the following steps of heating isooctanol to 47-53 DEG C, and adding phosphorus oxychloride in 4 to 6 hours while stirring, and the temperature is controlled at 65 + / - 2 DEG C; balancing for 4 to 6 hours and removing acid generated from reaction to obtain a crude ester; adding the crude ester into an alkaline solution, mixing for neutralization, and balancing for 1 to 1.5 hours at the temperature of 70 + / - 3 DEG C and the pH value is controlled between 8 and 9; separating and transferring the sediments into hot water of 80 + / - 2 DEG C, rinsing for 2 to 3 times, controlling the pH value of between 6.5 and 7.5, removing impurities to obtain qualified wet crude ester; pressure-reducing, distilling and separating the wet crude ester to get thefraction, and then cooling to obtain trioctyl phosphate. According to the invention, the condition of the production process can be easily controlled, the method is simple, the operation is convenient, the raw materials can be easily got, the reaction condition is controllable, the transportation and storage are convenient and safe, and the reaction period is short. The yield of trioctyl phosphate obtained by the method is increased from 72% to 81-83%, therefore the yield is significantly raised, the consumption is reduced and the economic benefits of enterprise are improved.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to trioctyl phosphate, in particular to a preparation method of trioctyl phosphate. Background technique [0002] Trioctyl phosphate (TOP), molecular formula C 24 h 51 o 4 P, with a relative molecular mass of 434.62 and a theoretical phosphorus content of 7.13%, has a structural formula 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 with trityl phosphate; when used with DOP, self-extinguishing products can be obtained. It can also be used in polyvinyl chloride ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
Inventor 张云刚张传义赵春忠刘雪坤
Owner 天津市联瑞阻燃材料有限公司
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