Method for synthesizing dimethyl methylphosphonate

A technology for dimethyl methyl phosphate and trimethyl phosphite, which is applied in the field of industrial production of dimethyl methyl phosphate, can solve the problems of unsuitability for industrial production, long reaction time and high production cost, and achieves improved performance. The effect of equipment utilization, shortening reaction time and improving synthesis yield

Active Publication Date: 2013-03-13
HUBEI XINGFA CHEM GRP CO LTD +1
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AI Technical Summary

Problems solved by technology

[0005] 2. Using dimethyl phosphite or dimethyl hypophosphite as a raw material synthesis method, dimethyl phosphite or dimethyl hypophosphite and methyl iodide undergo Michaelis-Becker reaction to obtain dimethyl methyl phosphate (Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 37:1744,1988; Phosphorus, Sulfur and Silicon and the Related Elements, 185(9):1845-1849, 2010; Phosphorus Sulfur and Silicon and the Related Elements, 181(3):511-518, 2006; Physical Chemistry Chemical Physics, 4(11): 2200-2205, 2002; Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 39 (5): 1076,1990); Using diazomethane as a methylating reagent can also convert dimethyl phosphite or dimethyl hypophosphite into dimethyl phosphate (Phosphorus, Sulfur and Silicon and the Related Elements , 73(1-4): 153 – 160, 1992) , and it was also reported that the target compound ...

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Under the protection of inert Ar gas, mix 0.48g (0.0025mol) of p-toluenesulfonic acid monohydrate and 6.20g (0.05mol) of trimethyl phosphite at room temperature, then raise the temperature to 140-150℃ for reaction, and control the pressure at 1.9- 3. Between 3 atmospheres, GC detected and tracked the reaction, and the raw materials basically disappeared after 4 hours. After vacuum distillation, 85-88°C / 15mmHg fractions were collected to obtain 5.18g of the target compound, with a yield of 84%.

Embodiment 2

[0033] Under the protection of inert nitrogen gas, mix 0.086g (0.0005mol) of anhydrous p-toluenesulfonic acid and 6.20g (0.05mol) of trimethyl phosphite at room temperature, then raise the temperature to 130-140°C for reaction, and control the pressure at 2.3- Between 3.8 atmospheres, after reacting for 6 hours, GC detection and tracking raw material conversion rate was greater than 98.5%, vacuum distillation, collected 90-92 ° C fraction (0.095Mpa, vacuum pressure gauge was not corrected), and the target product was 5.77g, the yield 93%, GC detection purity greater than 99%.

Embodiment 3

[0035] Under the protection of inert Ar gas, mix 0.086g (0.0005mol) of anhydrous p-toluenesulfonic acid and 6.20g (0.05mol) of trimethyl phosphite at room temperature, then raise the temperature to 150-160°C for reaction, and control the pressure at 9- Between 10 atmospheres, GC detected and tracked the reaction. After 6 hours, the raw material disappeared completely. After distillation under reduced pressure, the fraction at 92-94°C was collected (0.093Mpa, the vacuum pressure gauge was not corrected), and 5.72g of the target product was obtained, with a yield of 92%.

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Abstract

A method for synthesizing dimethyl methylphosphonate. Under protection of inert gas, A raw material trimethyl phosphite and a proper amount of benzene sulfonic acid catalyst are mixed and stirred; and a the mixture is subjected to a rearrangement reaction through a pressurized heating way, so as to synthesize a target product dimethyl methylphosphonate with yield up to 93% and purity higher than 99%. The invention has advantages of easily available raw materials, short synthesis time, simple production control, cheap and recyclable catalyst and little pollutant emission.

Description

technical field [0001] The invention belongs to the synthesis technology of alkyl phosphate ester compounds, and in particular relates to a preparation method capable of industrially producing dimethyl methyl phosphate. Background technique [0002] Plastic products have been widely used in construction, transportation, aviation, electrical appliances, household furniture and other fields, and these plastic products often need to be flame retardant. DMMP has high phosphorus content, excellent flame retardant performance, good solubility, miscible with water and various organic solvents or polymers; low viscosity, can also be used as a viscosity inhibitor; colorless and transparent, can be made into transparent or brightly colored Flame retardant products; small acid value of moisture, does not affect other properties of flame retardant products; small amount of addition, can greatly reduce product cost, low toxicity, non-corrosive, wide application range, suitable for variou...

Claims

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Application Information

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IPC IPC(8): C07F9/40
CPCY02P20/584
Inventor 李焰李国璋杨梅魏文彬刘畅杨玲陈祖兴
Owner HUBEI XINGFA CHEM GRP CO LTD
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