Oligomeric organic phosphate preparation method

A technology of organic phosphonates and dimethyl methylphosphonates is applied in the field of preparation of oligomeric organic phosphonates, and can solve the problems of slowness, unfavorable mass production, long reaction time and the like, so as to shorten the reaction time and save production. The effect of time and production cost saving

Active Publication Date: 2013-07-17
DYMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It can be seen that there is an obvious shortcoming in the above-mentioned preparation method: after the organic phosphine compound reacts with phosphorus pentoxide, in the reaction process with ethylene oxide, the reaction is carried out relatively slowly, the reaction time is very long, and a catalyst (octanoic acid suboxide) needs to be added. tin), which is not conducive to industrial mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In this embodiment, the preparation method of oligomeric organic phosphonate is as follows:

[0032] (1) Add 1 kg of dimethyl methylphosphonate into a three-necked flask, and add 1 kg of phosphorus pentoxide into the flask in batches under rapid stirring; Stir for 1 hour;

[0033] (2) Cool the reaction solution obtained in step (1) to 45°C, add 42g of distilled water dropwise, and stir at a constant temperature for 1 hour under the condition that the reaction temperature is 50-60°C;

[0034] (3) Add 15 g of trimethyl phosphite to the reaction solution obtained in step (2) to obtain a white translucent viscous liquid;

[0035] (4) Transfer the viscous liquid obtained in step (3) to an autoclave, and seal the reactor; heat to 80-90°C, replace with nitrogen, and slowly feed ethylene oxide into the reactor, while controlling the pressure to rise slowly, Keep the final pressure in the kettle at 1.0MPa, ventilate for 2 hours, meter 1315g of ethylene oxide, and stop the pass...

Embodiment 2

[0038] In this embodiment, the preparation method of oligomeric organic phosphonate is as follows:

[0039] (1) Add 1 kg of dimethyl methylphosphonate into a three-necked flask, and add 1 kg of phosphorus pentoxide into the flask in batches under rapid stirring; Stir for 1 hour;

[0040] (2) Cool the reaction solution obtained in step (1) to 45°C, add 42g of distilled water dropwise, and stir at a constant temperature for 30 minutes at a reaction temperature of 50-60°C;

[0041] (3) Add 15 g of trimethyl phosphite to the reaction solution obtained in step (2) to obtain a white translucent viscous liquid;

[0042] (4) Transfer the viscous liquid obtained in step (3) to an autoclave, and seal the reactor; heat to 90-95°C, replace with nitrogen, and slowly feed ethylene oxide into the reactor, while controlling the pressure to rise slowly, Keep the final pressure in the kettle at 0.8MPa, ventilate for 2 hours, meter 1285g of ethylene oxide, and stop the passage of ethylene oxid...

Embodiment 3

[0045] In this embodiment, the preparation method of oligomeric organic phosphonate is as follows:

[0046] (1) Add 1 kg of dimethyl methylphosphonate into a three-necked flask, and add 1 kg of phosphorus pentoxide into the flask in batches under rapid stirring; Stir for 1 hour;

[0047] (2) Cool the reaction solution obtained in step (1) to 45°C, add 42g of distilled water dropwise, and stir at a constant temperature for 30 minutes at a reaction temperature of 50-60°C;

[0048] (3) Add 15 g of trimethyl phosphite to the reaction solution obtained in step (2) to obtain a white translucent viscous liquid;

[0049] (4) Transfer the viscous liquid obtained in step (3) to the autoclave, seal the reactor; heat to 90-100°C, replace with nitrogen, and then slowly feed ethylene oxide into the reactor, while controlling the pressure to rise slowly, Keep the final pressure in the kettle at 0.6MPa, ventilate for 2.5 hours, meter and feed 1273g of ethylene oxide, and stop feeding ethyle...

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PUM

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Abstract

The invention provides an oligomeric organic phosphate preparation method. The preparation method comprises the following steps: 1, weighing dimethyl methylphosphonate and phosphorus pentoxide according to a mole ratio of 1.0:1.0-1.3:1.0, and reacting at 85-90DEG C; 2, cooling a reaction solution obtained in step 1 to 40-50DEG C, and adding a hydroxyl-containing compound; 3, adding trialkylphosphite to a reaction solution obtained in step 2; 4, heating a reaction solution obtained in step 3 to 40-120DEG C in a closed environment, and letting in oxirane for 2-3h while controlling the pressure to reach the slow rising of the pressure until the final pressure in a kettle is maintained in a range of 0.1-1.0MPa; and 5, stopping reacting when the hydroxyl value of a product is between 130 and 150 and the acid value of the product is 5-25mgKOH/g to obtain the product. The preparation method greatly shortens the time of the reaction with oxirane after the reaction of the organic phosphorus compound and phosphorus pentoxide and saves the production time and the production cost through reaction conditions comprising a high temperature and a high pressure without a catalyst, and is suitable for the industrialized production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing an oligomeric organic phosphonate. Background technique [0002] Oligomeric organic phosphonates, because of their good physical and chemical properties, are widely used in flame retardants for flammable substances such as plastics, textiles, paper, wood products, coatings (Edward D. Weil, Ralph B. Fearing and Fred Jaffe, Journal of FIRE RETARDANT CHEMISTRY, V9, (February 1982) p, 39). . [0003] At present, the commonly used preparation method is: through the reaction of organic phosphine compounds (such as dimethyl methylphosphonate) with phosphorus pentoxide, and then react with epoxy hydrocarbons (such as ethylene oxide) under normal pressure conditions (Ralph B. Fearing US 4199534, 1980). Adding hydroxyl-containing compounds (such as water, ethylene glycol, ethanol) in the reaction can adjust the molecular weight of the product and increas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C08G79/04
Inventor 石月朱泉郭玉良黄尚东
Owner DYMATIC CHEM
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