A kind of phosphonate hydrolysis device and method

A technology of phosphonic acid ester and dimethyl propyl phosphonate is applied in the field of methyl phosphonate hydrolysis device and phosphonate hydrolysis device, which can solve the problem of difficulty in the source of phosphonic acid, and achieves reduction of equipment investment, convenient operation, methanol high content

Active Publication Date: 2021-09-24
青岛长荣化工科技有限公司
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  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved by the present invention is to study and design a phosphonate hydrolysis device and determine a scientific and rational use method for the problem of difficult source of phosphonic acid which restricts the development of downstream flame retardants of phosphonic acid

Method used

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  • A kind of phosphonate hydrolysis device and method

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Experimental program
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Effect test

Embodiment 1

[0041] (1) Preparation: Check and confirm that the stirring motor 19, steam pressure gauge 11, kettle pressure gauge 20, kettle temperature thermometer 17, and top temperature thermometer 24 are in good condition, open the vent valve 23, fraction inlet valve 29, and check that other valves are in good condition. Closed state, open feeding valve 15, add 300kg methylphosphonic acid dimethyl ester and 75kg methylphosphonic acid catalyst (filling coefficient is 0.75, catalyst quantity is 20% of phosphonate mass) in hydrolysis kettle 1, close feeding valve 15. Open the water filling valve 22 to add 270L of process water to the head tank 2 (filling coefficient is 0.9), close the water filling valve 22, and check to confirm that the supply of steam and circulating water is normal;

[0042] (2) Hydrolysis: Open the circulating water inlet valve 26 and the circulating water outlet valve 25 of the condenser 4, feed the circulating water into the shell side of the condenser 4, close the v...

Embodiment 2

[0045] (1) Preparation: Check and confirm that the stirring motor 19, steam pressure gauge 11, kettle pressure gauge 20, kettle temperature thermometer 17, and top temperature thermometer 24 are in good condition, open the vent valve 23, fraction inlet valve 29, and check that other valves are in good condition. In the closed state, open the feeding valve 15 and add 280kg dimethyl propylphosphonate and 70kg propylphosphonic acid catalyst to the hydrolysis kettle 1 (the charging coefficient is 0.70, and the amount of catalyst is 25% of the mass of phosphonate), and close the feeding valve 15 , open the water filling valve 22 to add process water to the head tank 2 to 270L (filling coefficient 0.9), close the water filling valve 22, and check to confirm that the supply of steam and circulating water is normal;

[0046] (2) Hydrolysis: Open the circulating water inlet valve 26 and the circulating water outlet valve 25 of the condenser 4, feed the circulating water into the shell s...

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Abstract

A phosphonate hydrolysis device and method belong to the technical field of organic phosphorus flame retardant synthesis. The present invention solves the problem of difficult sources of phosphonic acid. The device of the present invention includes a hydrolysis tank, a head tank, a packed tower, a condenser and a receiving tank. The water in the head tank is continuously dripped into the hydrolysis tank, and the process parameters such as suitable temperature and catalyst are controlled in the hydrolysis tank to make the phosphonate Hydrolysis, the mixed vapor of methanol and excess water, a by-product of hydrolysis, enters the packed tower and condenser in turn, where mass transfer, separation and liquefaction occur, water returns to the hydrolysis tank, and the distilled methanol is collected in the receiving tank. The device of the invention is suitable for hydrolysis of various methyl phosphonates, semi-continuous operation, simple and flexible operation method, complete hydrolysis, high efficiency, can obtain high-purity methanol and high-concentration phosphonic acid aqueous solution at the same time, and is suitable for industrial production and use.

Description

technical field [0001] The invention relates to a phosphonate hydrolysis device and method, in particular to a methyl phosphonate hydrolysis device and method, and belongs to the technical field of organic phosphorus flame retardant synthesis. Background technique [0002] Phosphonic acid is phosphoric acid (HO) 3 One or two hydroxyl groups in the PO molecule are replaced by alkyl or aryl groups. According to the number of replaced alkyl groups, it can be divided into alkyl phosphonic acid RP(O)(OH) 2 and dialkylphosphonic acid R 2 P(O)OH, especially the former, and the latter is dialkylphosphinic acid. [0003] The molecular structure of phosphonic acid contains carbon-phosphorus bonds, which have very high thermal stability and can only be broken at very high temperatures. [0004] Phosphonic acid has the characteristics of a dibasic acid, can undergo neutralization reactions with basic compounds, and can undergo esterification reactions with alcohols, and has a wide r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/18B01D3/00B01D3/42
CPCB01D3/009B01D3/4216B01J19/0013B01J19/0053B01J19/18B01J2219/00094
Inventor 韩忠山韩明序杨松慧
Owner 青岛长荣化工科技有限公司
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