Method for compositing alkyl phosphonic acid dialkyl ester

The technology of a dialkyl alkylphosphonate and a synthesis method, which is applied in the chemical industry, can solve problems such as high requirements for industrial equipment, unsuitability for industrial production, and impact on industrial production safety, so as to achieve cost saving of raw materials, easy acquisition, and high production efficiency. high rate effect

Active Publication Date: 2013-05-01
HUBEI XINGFA CHEM GRP CO LTD
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AI Technical Summary

Problems solved by technology

SiF is produced during the reaction 4 and HF, so the requirements for industrial equipment are higher, thus increasing the production cost
In addition, difluoroalkylphosphine oxides are not easy to synthesize
[0009] Dunach et al. can synthesize dimethyl alkyl phosphonate by reacting dialkyl alkyl phosphite with tertiary peroxyalcohol at room temperature for 10 min. Because peroxide is used, the cost is too high and it will also affect Industrial production safety, not suitable for industrial production

Method used

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  • Method for compositing alkyl phosphonic acid dialkyl ester
  • Method for compositing alkyl phosphonic acid dialkyl ester

Examples

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Effect test

example 1

[0024] Under the protection of nitrogen, 5 mmol of trimethyl phosphite, 10 mg of potassium carbonate, and 20 mg of benzonitrile were successively added to a 25 mL round bottom flask, heated to reflux for reaction, and the pressure was maintained at 1.2-1.4 MPa. Distilled under high pressure to collect fractions, namely the product, the yield was 88.9%.

example 2

[0026] Under the protection of inert nitrogen gas, add 5mmol of triethyl phosphite, 10 mg of sodium carbonate, and 15 mg of o-chlorobenzonitrile in a 25mL round-bottomed flask, and heat to reflux for reaction. After the reaction was over, vacuum distillation was performed to collect fractions, namely the product of 92.6% in yield.

example 3

[0028] Under the protection of inert nitrogen gas, add 5 mmol of tripropyl phosphite, 10 mg of sodium hydroxide, and 15 mg of o-chlorobenzonitrile to a 25 mL round-bottomed flask successively, heat to reflux for reaction, and maintain the pressure at 1.2-1.4 MPa, GC After the end of the follow-up reaction, distillation under reduced pressure was carried out to collect fractions, namely the product of 91.5% in yield.

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Abstract

A method for compositing alkyl phosphonic acid dialkyl ester is characterized in that phosphorous acid trialkyl ester is taken as a raw material and alkyl phosphonic acid dialkyl ester is composited under alkali conditions through catalyst. The specific compositing steps are as follows: phosphorous acid trialkyl ester, alkali, catalyst are added in a container in sequence, a reflux reaction is performed, and the pressure is controlled to be within 1.2 to 1.4 MPa; and when the reaction is over, underpressure distillation is performed, distillate is collected, and then alkyl phosphonic acid dialkyl ester is obtained. Phosphorous acid trialkyl ester used in the method, which is taken as the raw material, is low in cost and easy to get; and the method has the advantages of high productivity and simplicity in operation and is more suitable for mass production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for synthesizing dialkyl alkyl phosphonate. Background technique [0002] Dialkyl alkyl phosphonates are widely used in flame retardant of polyurethane foam, unsaturated polyester resin, epoxy resin and furan resin. For example, dimethyl methyl phosphate can be used as the main intermediate in the synthesis of organophosphorus pesticides such as glufosinium ammonium. Traditional dialkyl alkyl phosphonates are mainly synthesized from trialkyl phosphite through Michaelis-Arbuzov rearrangement under the catalysis of alkylating reagents. [0003] Slaton et al. used trialkyl phosphite as a raw material to obtain dialkyl methyl phosphonate by Michaelis-Arbuzov rearrangement reaction with a methyl iodide catalyst under conditions such as heating to reflux and microwave irradiation. The yield is 75%, but methyl iodide is very expensive, has a low boiling point, is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40
Inventor 熊涛魏文彬陈松何西平林萌
Owner HUBEI XINGFA CHEM GRP CO LTD
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