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Recycling process of sodium tetrachloroaluminate in phosphinothricin production

A technology of sodium tetrachloroaluminate and glufosinate, applied in aluminum chloride, aluminum halide, flocculation/sedimentation water/sewage treatment, etc., to reduce pollution, improve atom economy, and widely used

Active Publication Date: 2016-01-06
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the defects of the prior art, the purpose of the present invention is to provide a sodium tetrachloroaluminate recycling process in the production of glufosinate, solve the problem of sodium tetrachloroaluminate solid waste treatment, reduce environmental pollution, and realize No waste discharge

Method used

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  • Recycling process of sodium tetrachloroaluminate in phosphinothricin production
  • Recycling process of sodium tetrachloroaluminate in phosphinothricin production
  • Recycling process of sodium tetrachloroaluminate in phosphinothricin production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Decomposition of sodium tetrachloroaluminate and recovery of aluminum trichloride

[0031] Add 300ml of methanol and 300ml of methyl tert-butyl ether to 200g of sodium tetrachloroaluminate, heat to 80°C, filter while hot, the filter cake is sodium chloride, and the filtrate is methanol solution of aluminum trichloride, slowly cool down , stirred overnight, a large amount of white aluminum trichloride solids were separated out, filtered and dried to obtain 133.2 g of aluminum trichloride with a yield of 95%;

[0032] 2) Recycling of aluminum trichloride

[0033] In a 1L autoclave, add 100.0g (0.75mol) of aluminum trichloride prepared in 1), 134.0g (0.97mol) of phosphorus trichloride, 500ml of 1,1,2,2-tetrachloroethane, and pass chlorine Methane to 1Mpa, heat up to 80°C, react for 4 hours, cool down, filter, and dry to obtain 228.3g of white sandy solid with a yield of 95%;

[0034] Cycles

1

2

3

4

Ligand Yield (%)

95

90

85...

Embodiment 2

[0038] 1) Decomposition of sodium tetrachloroaluminate and recovery of aluminum trichloride

[0039] Add 300ml of ethanol and 300ml of tert-butyl ether to 200g of solid waste, heat to 85°C, and filter under heat. The filter cake is sodium chloride, and the filtrate is methanol solution of aluminum trichloride. Slowly cool down, stir overnight, and precipitate A large amount of white aluminum trichloride solids were filtered and dried to obtain 126.9 g of aluminum trichloride with a yield of 90%;

[0040] 2) Recycling of aluminum trichloride

[0041] In a 1L autoclave, add 100.0g (0.75mol) of aluminum trichloride prepared in 1), 134.0g (0.97mol) of phosphorus trichloride, 500ml of 1,1,2,2-tetrachloroethane, and pass chlorine Methane to 1Mpa, heat up to 80°C, react for 4 hours, cool down, filter, and dry to obtain 216.3g of white sandy solid with a yield of 90%;

[0042] 3) Preparation of polyaluminum chloride

[0043] Slowly add saturated sodium hydroxide solution dropwise t...

Embodiment 3

[0045] 1) Decomposition of sodium tetrachloroaluminate and recovery of aluminum trichloride

[0046] Add 300ml of isopropanol and 300ml of tert-butyl ether to 200g of solid waste, heat to 90°C, filter under heat, and the filter cake is sodium chloride. The filtrate is the methanol solution of aluminum trichloride. Slowly lower the temperature and stir overnight, a large amount of white aluminum trichloride solids are precipitated, filtered and dried to obtain 119.9 g of aluminum trichloride with a yield of 86%.

[0047] 2) Recycling of aluminum trichloride

[0048] In a 1L autoclave, add 100.0g (0.75mol) of aluminum trichloride prepared in 1), 134.0g (0.97mol) of phosphorus trichloride, 500ml of 1,1,2,2-tetrachloroethane, and pass chlorine Methane was raised to 1Mpa, and the temperature was raised to 80°C. After reacting for 4 hours, the temperature was lowered, filtered, and dried to obtain 230.3g of white sandy solid, with a yield of 96%.

[0049] 3) Preparation of polyalu...

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Abstract

The invention discloses a recycling process of sodium tetrachloroaluminate in phosphinothricin production. The process comprises the following steps that 1, mismatching and precipitation are carried out; 2, solids are filtered; 3, cooling precipitation is carried out; 4, reutilization is carried out; 5, cyclic utilization is carried out; 6, aluminum polychlorid is prepared. Sodium tetrachloroaluminate solid waste is changed into treasure, alchlor obtained after mismatching is recycled, the problem of treatment of sodium tetrachloroaluminate solid waste is solved, pollution to environment is reduced, no three waste is discharged, the atom economy of a reaction is improved, and large-scale production of phosphinothricin is facilitated. A mismatching agent and a poor solvent adopted in the process are low in price and easy to obtain, the whole process is easy and convenient to operate, and especially suitable for industrial production. Further prepared polymerization alchlor can be adopted as a water purifying agent, and is wide in application range and especially suitable for sewage treatment of chemical plants.

Description

technical field [0001] The invention relates to a solid waste treatment technology, in particular to a solid waste treatment process in glufosinate production. Background technique [0002] Glufosinate (Glufosinafe) is a highly efficient, low toxicity, non-selective herbicide first developed by Hoechest company, the trade name is Basta, and its molecular formula is: C 5 h 12 NO 4 P, whose structure is: [0003] [0004] Wherein diethyl methyl phosphite (formula II) is the key intermediate for the production of glufosinate. At present, there are two main routes for the industrial preparation of diethyl methyl phosphite: route 1, Hoechest’s original research patent EP0391329 discloses the reaction of phosphorus trichloride and triethyl phosphite to prepare diethyl chlorophosphite, chlorinated Diethyl phosphite reacts with Grignard reagent Class A magnesium bromide to produce diethyl methyl phosphite, and the process route is as follows: [0005] [0006] Route 2, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/56C02F1/52
Inventor 刘善和曾辉杨红兵夏向荣李凯杨桂宝
Owner ANHUI COSTAR BIOCHEM CO LTD
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