Halogen-containing diphosphate or preparation method of halogen-containing diphosphorous acid ester

A technology of halogen-containing diphosphite and halogen-containing diphosphate, which is applied in the field of preparation of halogen-containing diphosphate or halogen-containing diphosphite, and can solve problems such as difficult product quality assurance, serious environmental pollution, and difficult control of conditions , to achieve the effect of low production cost, good color and short reaction time

Inactive Publication Date: 2008-07-09
ZHENJIANG SANWA FLAME RETARDANT ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Method 1 and method 3 have cumbersome steps, high energy consumption, serious environmental pollution, many side reactions and difficult conditions to control
The first step of method 2 is to control the first substitution is difficult, the reaction has by-product acid, the post-processing is difficult, and the quality of the product is difficult to guarantee

Method used

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  • Halogen-containing diphosphate or preparation method of halogen-containing diphosphorous acid ester
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  • Halogen-containing diphosphate or preparation method of halogen-containing diphosphorous acid ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add POCl 3 153.3g, catalyst aluminum isopropoxide 1.6g. Turn on the condensed water, stir, heat up to 40°C and start to pass Through 145g, passed through in 6-7 hours, and the temperature was controlled at 50-60°C. After passing through, keep it warm at about 60°C for 2 hours, and remove unreacted After filtration, 273.9 g of a colorless and transparent product tris(β-chloroethyl)phosphate (TCEP) was obtained, with a yield of 96.0%. The catalyst aluminum isopropoxide is recovered and reused.

[0036] Take the above TCEP 80.0g, anhydrous Na 2 CO 3 0.8g was added to a 150ml three-necked flask equipped with a magnetic stirrer and a thermometer, heated and stirred, heated to 185°C, 13.5g of dihaloalkane was distilled off, and 63.3g of colorless and transparent product diphosphate was obtained by filtration, with a yield of 95.6 %.

Embodiment 2

[0038] Add POCl 3 153.3g, catalyst solid superacid SO 4 2- / TiO 2 / La 3+ 2.1g. Turn on the condensed water, stir, heat up to 40°C and start to pass Through 145g, passed through in 6-7 hours, and the temperature was controlled at 50-60°C. After passing through, keep it warm at about 60°C for 2 hours, and remove unreacted After filtration, 273.9 g of a colorless and transparent product TCEP was obtained, with a yield of 96.0%. Catalyst solid superacid SO 4 2- / TiO 2 / La 3+ Recycle and reuse.

[0039] Take 80.0g of TCEP and 0.8g of KOH, put them into a 150ml three-necked flask equipped with a magnetic stirrer and a thermometer, heat and stir, heat to 185°C, distill 13.3g of dihaloalkanes, and filter to obtain the colorless and transparent product diphosphate 62.2 g, yield 93.9%.

Embodiment 3

[0041] Add POCl 3 153.3g, catalyst anhydrous AlCl 3 2.0g. Turn on the condensed water, stir, heat up to 40°C and start to pass Through 145g, passed through in 6-7 hours, and the temperature was controlled at 50-60°C. After passing through, keep it warm at about 60°C for 2 hours, and remove unreacted After filtration, 270.5 g of a colorless and transparent product TCEP was obtained, with a yield of 94.8%. Catalyst anhydrous AlCl 3 Recycle and reuse.

[0042] Take TCEP 80.0g, anhydrous K 2 CO 3 0.8g was added to a 150ml three-necked flask equipped with a magnetic stirrer and a thermometer, heated and stirred, heated to 185°C, 13.5g of dihaloalkanes were distilled off, filtered to obtain 62.8g of colorless and transparent product diphosphate ester, yield 94.8 %.

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Abstract

The invention relates to a process for preparation which contains halogen two-phosphate or halogen diphosphate, which is divided into the procedures that firstly, ethylene oxide and propylene oxide or epichlorohydrin and phosphorus oxychloride or tribromide oxygen phosphorus are reacted under the conditions of catalyst and heating and generate trialkyl phosphate with halogen, or ethylene oxide and propylene oxide or epichlorohydrin and phosphorus trichloride or phosphorus tribromide are reacted under the conditions of catalyst and heating and generate phosphorous acid, secondly, the trialkyl phosphate with halogen conducts transesterification under the conditions of catalyst and heating to gain diphosphate with halogen and halogenated hydrocarbons, or phosphate-containing brine conducts transesterification under the same condition to gain diphosphite with halogen and halogenated hydrocarbons. The catalyst of the first procedure adopts acid catalyst, and the catalyst of the second procedure adopts alkaline catalyst, and the dosage of catalyst of each procedure is respectively 0.05-2.5 of the total amount of reagent raw material of the procedure. The total yield of the product of the invention is 90-97%, and the product has the advantages of good color, low acid value, excellent viscosity, and does not need additional decolor process.

Description

technical field [0001] The invention relates to a preparation method of halogen-containing diphosphate or halogen-containing diphosphite. Background technique [0002] Halogen-containing diphosphate or halogen-containing diphosphite is a kind of flame retardant, which contains two elements of halogen (mainly chlorine and bromine) and phosphorus in its molecule, which has a good synergistic effect, and because of its large molecular weight and space Large steric hindrance has the characteristics of non-volatility, hydrolysis resistance, and good thermal stability. It can be widely used in the flame retardancy of polyolefins, polyesters, artificial fibers, and polyurethanes, and has a good development prospect. [0003] There are mainly three synthetic methods reported in the literature: [0004] 1. Cold synthesis: Phosphorus trichloride, chlorine, and halogenated alcohols are used to synthesize phosphite triesters under the action of pyridine, and then transesterified with d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C07F9/141
Inventor 杨锦飞章庚柱于春红黄东平杨智中
Owner ZHENJIANG SANWA FLAME RETARDANT ENG TECH CO LTD
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