System and method for continuously producing diethyl methylphosphonite

Patent metadata

Field	Value
Publication number	US-12509478-B2
Application number	US-202017924373-A
Country	US
Kind code	B2
Filing date	Nov 18, 2020
Priority date	Oct 10, 2020
Publication date	Dec 30, 2025
Grant date	Dec 30, 2025

Abstract

The present invention provides a system for continuously producing diethyl methylphosphonite, comprising a rapid mixing reactor and a material circulation subsystem. An inlet of the rapid mixing reactor is provided with a rapid mixing component; the rapid mixing component comprises a first liquid inlet and a second liquid inlet; the second liquid inlet is used for feeding a material containing methylphosphonous dichloride; the material circulation subsystem comprises a filter, a material distribution unit, an acid binding agent premixer, and a heat exchanger, which are connected in sequence; the filter is also provided with a solid waste outlet; the material distribution unit is also provided with a diethyl methylphosphonite outlet; the acid binding agent premixer is also provided with a reaction raw material inlet and an acid binding agent inlet; an inlet of the filter is connected to an outlet of the rapid mixing reactor; and an outlet of the heat exchanger is connected to the first liquid inlet. A method for continuously producing the diethyl methylphosphonite by using the system can achieve large-scale continuous production of the diethyl methylphosphonite, and has the advantages of high product yield, stable production, and high production benefit.

First claim

The invention claimed is:

1 . A system for continuously producing diethyl methylphosphonite, comprising:
a mixing reactor and a material circulation subsystem; wherein an inlet of the mixing reactor is provided with a mixing member comprising a first liquid inlet and a second liquid inlet, wherein the second liquid inlet is configured to feed a methylphosphonous dichloride-containing material; wherein the material circulation subsystem comprises a filter, a unit for distributing materials, an acid-binding agent premixer and a heat exchanger that are sequentially connected, wherein the filter is further provided with a solid waste outlet, the unit for distributing materials is further provided with an diethyl methylphosphonite outlet, the acid-binding agent premixer is further provided with an reaction raw material inlet and an acid-binding agent inlet; wherein the reaction raw material inlet is configured to feed ethanol; wherein an inlet of the filter is connected with an outlet of the mixing reactor, and an outlet of the heat exchanger is connected with the first liquid inlet; wherein the mixing member is selected from a venturi nozzle, a jet nozzle or a hedging flow nozzle.

2 . The system for continuously producing diethyl methylphosphonite according to claim 1 , wherein the mixing reactor is further provided with a vacuumization unit.

3 . The system for continuously producing diethyl methylphosphonite according to claim 1 , wherein the filter is selected from the group consisting of a plate and frame filter, a leaf filter, a rotary drum filter, a centrifugal filter and combinations thereof.

4 . The system for continuously producing diethyl methylphosphonite according to claim 1 , wherein the acid-binding agent premixer is selected from the group consisting of an absorption tower, a bubbling bed, an airlift loop reactor, a jet reactor, a mechanically stirring tank and combinations thereof.

5 . A method for continuously producing diethyl methylphosphonite using the system according to claim 1 , comprising:
step a), mixing an ethanol-containing reaction raw material, an acid-binding agent and a material circulating in the unit for distributing materials in the acid-binding agent premixer uniformly, to obtain a mixed material; step b), cooling the mixed material obtained in step a) by the heat exchanger and then introducing the mixed material into the mixing reactor via the first liquid inlet; and at the same time introducing a methylphosphonous dichloride-containing material into the mixing reactor via the second liquid inlet, and mixing the mixed material and the methylphosphonous dichloride-containing material under the action of the mixing member to carry out a reaction, to obtain a reaction mixture; and step c), passing the reaction mixture obtained in step b) through a filter to remove solid waste generated from the reaction, and then introducing the reaction mixture into the unit for distributing materials, to obtain diethyl methylphosphonite and the material circulating in the unit for distributing materials separately, wherein the material circulating in the unit for distributing materials is used in step a).

6 . The method for continuously producing diethyl methylphosphonite according to claim 5 , wherein the acid-binding agent in step a) is an organic amine having a structural formula of NR 1 R 2 R 3 ;
wherein R 1 , R 2 , and R 3 are independently selected from H, methyl, ethyl, propyl, butyl or phenyl.

7 . The method for continuously producing diethyl methylphosphonite according to claim 5 , wherein in step b), the methylphosphonous dichloride in the methylphosphonous dichloride-containing material and the ethanol and the acid-binding agent in the mixed material have a molar ratio of 1:(0.5-50):(1-15).

8 . The method for continuously producing diethyl methylphosphonite according to claim 5 , wherein in step b), the reaction is performed at a temperature from −40° C. to 100° C.

9 . The method for continuously producing diethyl methylphosphonite according to claim 5 , wherein in step c), the diethyl methylphosphonite and the material circulating in the unit for distributing materials obtained from the unit for distributing materials have a mass ratio of 1:(0.1-100).

Assignees

• Zhejiang Wynca Chemical Industry Group Co Ltd
• Univ Tsinghua

Inventors

• Wang Tiefeng
• Zhou Shuguang
• Lan Xiaocheng
• Qin Long
• Li Banghao
• Yu Shenluan
• Zhang Huahai
• Jiang Shengbao
• Tu Minhai
• Zhu Xiaohong

Classifications

• C07F9/50 Primary

  Organo-phosphines · CPC title

• C07F9/4816 Primary

  Acyclic saturated acids or derivatices which can have further substituents on alkyl · CPC title