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Synthesis method of tris(tribomoneopentyl) phosphate easy to produce industrially

A technique for the synthesis of tribromoneopentyl alcohol, which is applied in the field of synthesis of tris(tribromoneopentyl) phosphate, can solve the problems of product quality reduction, cumbersome water, and inability to completely remove it, so as to reduce the complexity of production , the effect of high product purity

Active Publication Date: 2016-06-08
WEIFANG TIANFU CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still continues the process of removing water from the raw materials of the reaction system in advance, which is cumbersome and cannot completely remove the water, resulting in a greatly reduced product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of synthetic method of tris (tribromoneopentyl) phosphate that is easy to industrialized production comprises the steps:

[0021] (1) Put dichloroethane as a solvent into the reaction kettle. The weight of the solvent is twice that of tribromoneopentyl alcohol. Add tribromoneopentyl alcohol into the reaction kettle to control the temperature at 20°C and stir for 0.5 hours to confirm the material dissolve;

[0022] (2) Add a dewatering agent of 1wt% tribromoneopentyl alcohol into the reactor, stir for 0.4 hours, and then add the catalyst into the reactor, wherein the dehydrating agent is phosphorus pentoxide, and the catalyst is Lewis acid three Aluminum chloride, the consumption of catalyzer is the 1wt% of tribromoneopentyl alcohol;

[0023] (3) Turn on the pressure absorption system of the reactor, keep the temperature in the reactor at 35°C, add phosphorus oxychloride dropwise, and control the dropwise addition within 4 hours. 80°C, the time used to raise the...

Embodiment 2

[0027] A kind of synthetic method of tris (tribromoneopentyl) phosphate that is easy to industrialized production comprises the steps:

[0028] (1) Put tetrachloroethane as a solvent into the reaction kettle. The weight of the solvent is 2.2 times that of tribromoneopentyl alcohol. Add tribromoneopentyl alcohol into the reaction kettle to control the temperature at 30°C and stir for 1 hour to confirm the material dissolve;

[0029] (2) Add a dewatering agent of 2wt% tribromoneopentyl alcohol into the reactor, stir for 0.5 hours, and then add the catalyst into the reactor, wherein the dewatering agent adopts molecular sieve, the catalyst adopts ferric chloride, and the catalyst The consumption is the 3wt% of tribromoneopentyl alcohol;

[0030] (3) Turn on the pressure absorption system of the reactor, keep the temperature in the reactor at 37°C, add phosphorus oxychloride dropwise, and control the drop to complete within 4.5 hours. After the dropwise addition, keep the tempera...

Embodiment 3

[0034] A kind of synthetic method of tris (tribromoneopentyl) phosphate that is easy to industrialized production comprises the steps:

[0035] (1) Put chlorobenzene as a solvent into the reaction kettle. The weight of the solvent is 2.4 times that of tribromoneopentyl alcohol. Add tribromoneopentyl alcohol into the reaction kettle to control the temperature at 40°C and stir for 1.5 hours to confirm the dissolution of the material;

[0036] (2) Add a dehydrating agent of 3wt% tribromoneopentyl alcohol to the reactor, stir for 0.6 hours, then add the catalyst into the reactor, wherein the dehydrating agent is phosphorus pentoxide, molecular sieve, anhydrous chlorine Calcium chloride, catalyzer adopts tin tetrachloride, antimony trichloride, and the consumption of catalyzer is the 5wt% of tribromoneopentyl alcohol;

[0037] (3) Turn on the pressure absorption system of the reactor, keep the temperature in the reactor at 40°C, add phosphorus oxychloride dropwise, and control the ...

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Abstract

A synthesis method of tris(tribomoneopentyl) phosphate easy to produce industrially includes the following steps that firstly, tribromoneopentyl alcohol is added into a reaction kettle, temperature is controlled to be 20-40 DEG C, and stirring is performed for 0.5-1.5 hours till it is confirmed that materials are dissolved; secondly, moisture scavenger is added, stirring is performed for 0.4-0.6 hour, and then a catalyst is added into the reaction kettle; thirdly, temperature is kept at 35-40 DEG C, phosphorus oxychloride is added dropwise, dropwise adding is controlled to be completed in 4-5 hours, heat preservation is performed for 0.5 hour at 40-50 DEG C after dropwise adding ends, then temperature is slowly raised to 80-140 DEG C, temperature raising time is 3 hours, the temperature is controlled, and a backflow reaction is performed for 10-15 hours; fourthly, solvents are evaporated out by means of temperature raising, the time during which the solvents are evaporated out is controlled to be 6-8 hours, cooling is performed after distillation of the solvents is completed, and the product is subjected to suction filtration and washing till the product becomes neutral. A mild reaction condition is adopted for the method, the purity of the obtained product is high, and the synthesis method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for synthesizing tris(tribromoneopentyl)phosphate which is easy for industrial production. Background technique [0002] Polyurethane is a typical thermosetting resin. Due to its relatively low cost and excellent performance such as good castability, it is used in the manufacture of various daily products including auto parts. However, polyurethane foam is flammable and, if ignited, tends to produce an uncontrollable burn. The industry has expended various efforts to develop flame retardant polyurethanes. At present, in some areas of polyurethane application such as automotive interior decoration, flame retardancy is required by law. Tris(tribromoneopentyl) phosphate is a flame retardant containing both phosphorus and bromine in the molecule. The bromine content is 70%, and the phosphorus content is 3%. It can meet the UL94V-2 flame retardancy of the polymer,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
CPCC07F9/091
Inventor 徐金伟任伟民丁加中潘光辉李君鹏马超
Owner WEIFANG TIANFU CHEM TECH
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