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Preparation of hydroxylamine by one-step method using oxime hydrolysis reaction and infiltration gasification film separation coupling technique

A technology of pervaporation membrane and hydrolysis reaction is applied in the field of preparation of hydroxylamine salt, which can solve the problems such as the conversion rate of only 75%, and achieve the effects of less variety of raw materials, mild reaction conditions and easy operation.

Inactive Publication Date: 2008-01-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Under the conditions of 85°C and the molar ratio of ethanol and oleic acid as the reaction raw materials, the conversion rate of oleic acid exceeds 95% after the reaction is carried out for 3 hours; while under the same reaction conditions, the reaction without the pervaporation device takes 4 hours to basically reach Balanced, conversion rate is only 75%

Method used

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  • Preparation of hydroxylamine by one-step method using oxime hydrolysis reaction and infiltration gasification film separation coupling technique
  • Preparation of hydroxylamine by one-step method using oxime hydrolysis reaction and infiltration gasification film separation coupling technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A. According to the quantification that the molar ratio of hydrochloric acid to cyclohexanone oxime in the reaction solution is 2, measure 200ml of 2.1mol / L hydrochloric acid solution, weigh 23.73g of cyclohexanone oxime with a purity of 95%, and mix it to prepare into a reaction solution.

[0036]B. Add the reaction liquid to the feed liquid tank of the reaction device coupled with the pervaporation membrane separation process shown in Figure 1 . The membrane module used is a flat-plate pervaporation membrane module as shown in Figure 2, wherein the pervaporation membrane is a flat-plate composite membrane as shown in Figure 3, the material of the separation layer is polydimethylsiloxane, and the membrane area is 150.72 cm 2 , with a thickness of 20 μm; the support layer is a microporous polytetrafluoroethylene membrane with a thickness of 40 μm and a micropore diameter of 0.2 μm. The reaction temperature was controlled at 50°C.

[0037] C. The reaction solution was ...

Embodiment 2

[0040] A. According to the quantification that the molar ratio of hydrochloric acid and butanone oxime in the reaction solution is 2, measure 200ml of 2.1mol / L hydrochloric acid solution, weigh 18.27g of butanone oxime with a purity of 99%, and mix it to prepare a reaction solution liquid.

[0041] B. Carry out according to step B among the embodiment 1.

[0042] C. After the reaction was carried out for 2.5 hours, the reaction liquid was collected, and 100 ml of toluene was added thereto according to the volume ratio of toluene to the reaction liquid of 0.5:1, and the oil and water phases were separated to obtain the mother liquor of hydroxylamine hydrochloride.

[0043] The concentration of hydroxylamine hydrochloride was analyzed by titration. Under the same conditions, the equilibrium conversion rate of butanone oxime hydrolysis reaction in hydrochloric acid solution is 23.2%, while using this technology, after the reaction is carried out for 2.5 hours, the reaction conve...

Embodiment 3

[0045] A. According to the quantification that the molar ratio of sulfuric acid and cyclohexanone oxime in the reaction solution is 0.5, measure 200ml of 0.5mol / L sulfuric acid solution, weigh 23.73g of cyclohexanone oxime with a purity of 95%, and mix it to prepare into a reaction solution.

[0046] B. Carry out according to step B among the embodiment 1.

[0047] C. Carry out according to step C among the embodiment 1.

[0048] The concentration of hydroxylamine hydrochloride was analyzed by titration. Under the same conditions, the equilibrium conversion of cyclohexanone oxime hydrolysis reaction in sulfuric acid solution is 4.2%. Using this technology, after the reaction is carried out for 4.5 hours, the conversion rate reaches 66.7%, and the concentration of hydroxylamine hydrochloride in the mother liquor reaches 39.29g / L.

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Abstract

In this invention, oxime is used as raw material being hydrolyzed in acid solution. Said hydrolytic process is coupled with osmotic vaporization membrane separation technique. The produced organic by-product ketone is removed by said membrane directionally and high efficiently. Thus recovers the limitation of the reaction chemical equilibrium of the hydrolysis, proceeding the reaction to the direction of production of hydroxylamine salts. This technique enhances the conversion rate greatly with high yield of hydroxylamine salts. This inventive method is better than prior art method with advantages of: simple process, less kinds of raw materials being needed, easy to operation, no side reaction, mild reaction condition and high yield of hydroxylamine salts being up to 80%.

Description

Technical field: [0001] The present invention relates to a preparation method of hydroxylamine salt, in particular to a method of using oxime as a raw material, using pervaporation membrane separation technology to efficiently and directionally remove organic by-products generated in the hydrolysis process of oxime, improve the reaction conversion rate and the yield of hydroxylamine salt, one-step Method for synthesizing hydroxylamine salt. Background technique: [0002] (1) Hydroxylamine salt and production method thereof [0003] Hydroxylamine salt is a chemical product with a wide range of uses. The main hydroxylamine salts include hydroxylamine sulfate, hydroxylamine hydrochloride, hydroxylamine nitrate, and hydroxylamine phosphate. Hydroxylamine hydrochloride is mainly used as a raw material for synthetic industries such as pharmaceuticals, spices, rubber chemicals, and dyes; hydroxylammonium sulfate and hydroxylamine phosphate are mainly used for the production of cap...

Claims

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Application Information

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IPC IPC(8): C01B21/14
Inventor 张卫东姜德强任钟旗杨婧杨龙
Owner BEIJING UNIV OF CHEM TECH
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