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A method for catalytically preparing tris-(2-chloroethyl) phosphite

A technology for catalytic preparation of phosphite, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc. High rate, high purity, good atom economy effect

Active Publication Date: 2015-12-02
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are various defects in the above methods
For example, the method reported in GB1048070A needs to add a solvent, the aftertreatment is loaded down with trivial details, and the catalyst 2-chloroethanol used is more toxic
The method reported in US3888953A needs to add an excessive amount of ethylene oxide, but the price of ethylene oxide is more expensive, the cost is high, and it is not conducive to environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In the dry reaction bottle, install mechanical stirring, thermometer, gas distributor and reflux condenser, place the reaction device in a low-temperature water bath, and use N 2 Replace the air in the bottle for 2 times, add 2500.0 g (18.2 mol) of newly distilled phosphorus trichloride under nitrogen protection, 1.3 g of ferric chloride and stannous oxalate (weight ratio 3: 7) combined catalyst, and treat that the internal temperature drops to Below 10°C, start stirring, feed ethylene oxide gas through the gas distributor, quantitatively feed 2444.8g (55.5mol, feed time 16.5h) of ethylene oxide, maintain the reaction temperature at 5-30°C, feed After the end, the temperature was kept at 30-40° C., and the reaction was continued for 0.5 h. After the end of the reaction, 4841.0 g of the target product was obtained by distillation under reduced pressure, with a GC purity of 97.00% and a yield of 98.70%.

Embodiment 2

[0021] In the dry reaction bottle, install mechanical stirring, thermometer, gas distributor and reflux condenser, place the reaction device in a low-temperature water bath, and use N 2 Replace the air in the bottle for 2 times, add newly distilled phosphorus trichloride 2500.0g (18.2mol) under nitrogen protection, ferric chloride and stannous oxalate (weight ratio 3: 5) combined catalyst 2.0g, treat that the internal temperature drops to Below 10°C, start stirring, feed ethylene oxide gas through the gas distributor, quantitatively feed 2444.8g (55.5mol, feed time 16.5h) of ethylene oxide, maintain the reaction temperature at 5-30°C, feed After the end, the temperature was kept at 30-40°C, and the reaction was continued for 0.5h. After the end of the reaction, 4855.7g of the target product was obtained by distillation under reduced pressure, with a GC purity of 97.50% and a yield of 99.00%.

Embodiment 3

[0023] In the dry reaction bottle, install mechanical stirring, thermometer, gas distributor and reflux condenser, place the reaction device in a low-temperature water bath, and use N 2 Replace the air in the bottle for 2 times, add 2500.0 g (18.2 mol) of newly distilled phosphorus trichloride under nitrogen protection, 2.0 g of ferric chloride and stannous oxalate (weight ratio 3: 6) combination catalyst, and treat that the internal temperature drops to Below 10°C, start stirring, feed ethylene oxide gas through the gas distributor, quantitatively feed 2427.2g (55.1mol, feed time 16.5h) of ethylene oxide, maintain the reaction temperature at 5-30°C, feed After the end, the temperature was kept at 30-40° C., and the reaction was continued for 0.5 h. After the end of the reaction, 4850.8 g of the target product was obtained by distillation under reduced pressure, with a GC purity of 97.33% and a yield of 98.90%.

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Abstract

The invention discloses a process for catalyzing preparation of tricresyl phosphite-(2-chloroethyl) ester. Phosphorus trichloride serves as a raw material, a catalyst is added, then ethylene oxide is added, a reaction is conducted at the temperature in the range of 0-60 DEG C for 10-20 hours, and reduced pressure distillation is conducted, so that a target product of the tricresyl phosphite-(2-chloroethyl) ester is obtained, the gas chromatography (GC) purity is no less than 96%, and the yield is no less than 98.5%. Compared with the prior art, the process has the advantages that the usage amount of the ethylene oxide is low, the product purity is high, the quality is stable, and the process has good industrial application prospects.

Description

technical field [0001] The invention relates to a method for catalytically preparing tris-(2-chloroethyl)phosphite. Background technique [0002] Tris(2-chloroethyl)phosphite, also known as 2-chloroethanol phosphite (3:1), is an important intermediate for the preparation of the plant growth regulator ethephon, and can also be used to prepare the flame retardant tris(2- Chloroethyl) phosphate and other phosphorus-based flame retardants can also be used as functional additives for lubricating esters, plasticizers, and washable antistatic agents. They have been widely used in pesticides, chemicals, and materials industries. . [0003] In the prior art, GB1048070A (1965) discloses a freshly distilled phosphorus trichloride as a raw material, petroleum ether, benzene, toluene, cyclohexane, diisopropyl ether, etc. as a solvent, adding a weight ratio of 0.05 -5% 2-chloroethanol is used as a catalyst solvent, ethylene oxide is added for reaction, and the method for preparing tris(...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/141
Inventor 刘斌杨伟领兰红丽廖本仁揭元萍张春雷
Owner SHANGHAI HUAYI GRP CO
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