A method for resource utilization of diethyl methylphosphonite high boilers

A technology of diethyl methyl phosphite and alkyl methyl phosphinate, which is applied in the field of resource utilization of diethyl methyl phosphite rectified high boilers, can solve the problem of harsh reaction conditions and safety problems. hidden dangers

Active Publication Date: 2021-09-14
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

US6770779 and US4549995 respectively disclose the method of carrying out catalyst alkylation reaction with element phosphorus to obtain monoalkyl phosphinate and reacting alkyl phosphine dichloride with alcohol to

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] This embodiment provides a method for resource utilization of diethyl methylphosphonite distillation high boilers, said method comprising the following steps:

[0034] (1) Heat 100g of diethyl methylphosphonite rectified high boiler to 40°C, add 26.5g of 2% hydrochloric acid solution (0.015mol) dropwise to the high boiler, after the addition, hydrolyze for 3h, distill Reclaim ethanol to obtain feed liquid A;

[0035] (2) Mix the material liquid A obtained in step (1) with 100g of n-butanol (1.35mol), heat to reflux temperature, and react at 100-110°C. During the reaction, the water produced by the reaction is separated until anhydrous is formed to obtain Feed liquid B;

[0036] (3) Rectify the liquid B obtained in step (2) at -0.098MPa, collect fractions with a fraction temperature of 65-70°C, recover excess n-butanol added during the rectification process, and obtain methylphosphonous acid Mono-n-butyl ester, purity 97.5%, yield 93.0% (based on the sum of diethyl met...

Embodiment 2

[0038] This embodiment provides a method for resource utilization of diethyl methylphosphonite distillation high boilers, said method comprising the following steps:

[0039] (1) Heat 150g of diethyl methylphosphonite rectified high boiler to 80°C, add 40.0g of 3% hydrochloric acid solution (0.033mol) dropwise to the high boiler, after the addition, hydrolyze for 2h, distill Reclaim ethanol to obtain feed liquid A;

[0040] (2) Mix the material liquid A obtained in step (1) with 150g of n-butanol (2.03mol), heat to reflux temperature, and react at 110-120°C. During the reaction, the water produced by the reaction is separated until anhydrous is formed to obtain Feed liquid B;

[0041] (3) Rectify the feed liquid B obtained in step (2) at -0.095MPa, collect fractions with a fraction temperature of 70-75°C, recover excess n-butanol added during the rectification process, and obtain methylphosphonous acid Mono-n-butyl ester with a purity of 98.5% and a yield of 94.5% (based on th...

Embodiment 3

[0043] This embodiment provides a method for resource utilization of diethyl methylphosphonite distillation high boilers, said method comprising the following steps:

[0044] (1) Heat 100 g of diethyl methylphosphonite rectified high boiler to 60° C., 88.3 g of 2% hydrochloric acid solution (0.05 mol) is added dropwise to the high boiler, after the dropwise addition, the hydrolysis reaction is carried out for 0.5 h, Ethanol is reclaimed by distillation to obtain feed liquid A;

[0045] (2) The feed liquid A obtained in step (1) is mixed with 54g n-butanol (0.73mol) and 70g n-butanol (0.95mol) recovered in Example 2, heated to reflux temperature, and reacted at 110~120°C, Separating the water produced by the reaction during the reaction until anhydrous is generated to obtain the feed liquid B;

[0046] (3) Rectify the feed liquid B obtained in step (2) at -0.08MPa, collect the fraction with a fraction temperature of 80-85°C, recover the excessively added n-butanol during the r...

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Abstract

The invention provides a method for resource utilization of diethyl methylphosphonite rectification high boilers. The method comprises mixing the high boilers of diethyl methylphosphonite rectification with hydrochloric acid, and performing a hydrolysis reaction. Finally, the ethanol is recovered by distillation to obtain the feed liquid A; the obtained feed liquid A is mixed with an alkyl alcohol, and reacted under heating and reflux conditions until anhydrous is generated to obtain the feed liquid B; the obtained feed liquid B is rectified to obtain methyl sulfide Alkyl phosphonates. The method can reduce waste discharge in the production process of diethyl methylphosphinate, protect the environment, has mild reaction conditions, does not need to add a catalyst, has low treatment cost, hardly generates waste liquid in the process, and is economical and environment-friendly.

Description

technical field [0001] The invention belongs to the field of diethyl methylphosphonite production, and relates to a method for resource utilization of diethyl methylphosphonite rectification high boilers. Background technique [0002] Diethyl methylphosphonite is a very important organic intermediate, mainly used in the synthesis of herbicide glufosinate-ammonium. Traditional synthetic methods generally include two types: 1) Phosphorus trichloride reacts with triethyl phosphite to obtain chlorophosphite, and then reacts with methylmagnesium chloride to obtain diethyl methylphosphonite; 2) methyl dichloride Phosphine reacts with absolute ethanol to obtain diethyl methylphosphonite. The above two routes obtain the crude product of diethyl methylphosphonite. While the pure product is obtained through rectification and purification, a certain amount of high boilers from distillation will remain at the bottom of the kettle. The main components include monoethyl methylphosphonite...

Claims

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Application Information

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IPC IPC(8): C07F9/48
CPCC07F9/4816C07F9/4866
Inventor 周曙光秦龙余神銮王萍闫涛涛姜胜宝祝小红付萍
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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