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A method for reducing the hydrolysis rate of cyclododecanone oxime in sulfuric acid extraction process

A cyclododecanone oxime and extraction technology, which is applied in the field of reducing the hydrolysis of cyclododecanone oxime in the sulfuric acid extraction process, can solve the problems of reducing the heat transfer coefficient of the reactor, increasing the difficulty of separation, and affecting product quality.

Active Publication Date: 2021-04-20
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because cyclododecanone oxime has a certain polarity, the alkane solution of cyclododecanone oxime usually contains 0.1-0.2wt% water, and cyclododecanone oxime undergoes hydrolysis reaction under acidic conditions to generate cyclododecanone during the extraction process. The equation is shown below. Cyclododecanone generated by hydrolysis can be further reacted with sulfuric acid to generate carbonization. Carbonization will reduce the heat transfer coefficient of the reactor, block the pipeline, increase the difficulty of subsequent separation, and affect product quality.

Method used

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  • A method for reducing the hydrolysis rate of cyclododecanone oxime in sulfuric acid extraction process
  • A method for reducing the hydrolysis rate of cyclododecanone oxime in sulfuric acid extraction process
  • A method for reducing the hydrolysis rate of cyclododecanone oxime in sulfuric acid extraction process

Examples

Experimental program
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Effect test

Embodiment 1

[0060] Preparation of the modified organosilicon defoamer (that is, the sulfur-containing carboxyl fluorine-containing silicone oil of formula (V):

[0061] 60°C, under normal pressure, 39.2g of fluoromethyl silicone oil (x=1, y=1, compound of formula (I)) and 24g of tetramethylcyclotetrasiloxane (compound of formula (II)) were stirred and mixed for reaction 4h, to obtain fluorine-containing hydrogen-containing silicone oil (compound of formula (III));

[0062] Add 52g hexenyl thiocarboxylic acid (formula (IV) compound, n=2) and 0.0115g 98% concentrated sulfuric acid (0.01wt%) in the reaction solution, continue to react 2.5h at 90 ℃, after the reaction finishes, obtain modified Sexual organosilicon defoamer (x=1, y=1, z=4, n=2, formula (V) compound);

[0063] Add 5.76g of white carbon black and 3.63g of dodecanedioic acid to the reaction solution, and stir at 130°C for 2h to obtain a strong acid-resistant defoamer that can be used in concentrated sulfuric acid systems, wherei...

Embodiment 2

[0070] Preparation of the modified organosilicon defoamer (that is, the sulfur-containing carboxyl fluorine-containing silicone oil of formula (V):

[0071] 80°C, under normal pressure, 78.02g of fluoromethyl silicone oil (x=30, y=40, compound of formula (I)) and 12g of tetramethylcyclotetrasiloxane (compound of formula (II)) were stirred and mixed for reaction 5h, to obtain fluorine-containing hydrogen-containing silicone oil (compound of formula (III));

[0072] Add 42.8g dodecenylthiocarboxylic acid (formula (IV) compound, n=8) and 0.0266g 98% concentrated sulfuric acid (0.02wt%) in reaction liquid, continue reaction 3h at 100 ℃, after reaction finishes, obtain Modified silicone defoamer (x=30, y=40, z=20, n=8, compound of formula (V));

[0073] Add 13.28g of white carbon black and 7.31g of dodecyl carboxylic acid to the reaction solution, and stir at 180°C for 3 hours to obtain a modified strong acid-resistant defoamer that can be used in concentrated sulfuric acid system...

Embodiment 3

[0080] Preparation of the modified organosilicon defoamer (that is, the sulfur-containing carboxyl fluorine-containing silicone oil of formula (V):

[0081] 70°C, under normal pressure, stir and mix 24.62g of fluoromethyl silicone oil (x=10, y=10, compound of formula (I)) and 7.2g of tetramethylcyclotetrasiloxane (compound of formula (II)) React for 8h to obtain fluorine-containing hydrogen-containing silicone oil (compound of formula (III));

[0082] Add 15.6g hexenylthiocarboxylic acid (formula (IV) compound, n=2) and 0.0071g 98% concentrated sulfuric acid (0.015wt%) in the reaction solution, continue to react 4h at 95 ℃, after the reaction finishes, obtains modified Sexual organosilicon defoamer (x=10, y=10, z=12, n=2, formula (V) compound);

[0083] Add 3.79g of white carbon black and 1.9g of dodecanedioic acid to the reaction solution, and stir at 150°C for 2.5h to obtain a strong acid-resistant defoamer that can be used in concentrated sulfuric acid systems, wherein the...

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Abstract

The invention provides a method for reducing the hydrolysis rate of cyclododecanone oxime in the sulfuric acid extraction process, said method comprising the following steps: a) adding the alkane solution of cyclododecanone oxime into the extraction reaction kettle, controlling the extraction reaction The temperature and pressure in the kettle are continuously stirred, and a strong acid-resistant defoamer is added to the extraction system to evaporate the alkane solvent in the extraction system and the water entrained in the reaction system; b) add pretreated concentrated sulfuric acid for extraction, and the mass fraction of sulfuric acid in the pretreated concentrated sulfuric acid is 99-100%. The method provided by the invention can effectively reduce the hydrolysis rate of cyclododecanone oxime in the extraction process.

Description

technical field [0001] The invention relates to the technical field of extraction of dodecanone oxime, in particular to a method for reducing the hydrolysis of cyclododecanone oxime in a sulfuric acid extraction process. Background technique [0002] As a special nylon product, compared with general nylon (such as nylon 6), nylon 12 has the advantages of low water absorption, high toughness, wear resistance and swelling resistance. Globally, Nylon 12 (and Nylon 11) have replaced metal materials as indispensable and hard-to-replace non-metallic materials such as automotive fuel pipes and air brake hoses. In addition, in the fields of submarine cables, solar energy, medical treatment, 3D printing, etc., nylon 12 has demonstrated superior performance advantages. [0003] Cyclododecanone is obtained by oximation, extraction, rearrangement, and polymerization to obtain nylon 12. It is a traditional synthesis method for nylon 12, wherein the alkane solution usually extracted from...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/04
CPCB01D11/0484B01D11/0492
Inventor 边新建李俊平张彦雨张少伟孟熙王伟丛振霞吴训锟陈海波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD