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Two-step dislocation method of cyclohexanone oxime with water

A cyclohexanone oxime and translocation technology is applied in the field of two-step translocation of cyclohexanone oxime with water, which can solve the problem of high concentration of oleum, and achieve the effects of simplifying production process, reducing requirements and satisfying pressure drop.

Inactive Publication Date: 2003-02-05
JUHUA GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This allows a higher concentration of oleum to be used in the reaction

Method used

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  • Two-step dislocation method of cyclohexanone oxime with water
  • Two-step dislocation method of cyclohexanone oxime with water

Examples

Experimental program
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Effect test

Embodiment 1

[0014] In a nylon factory, the raw material used is cyclohexanone oxime with a water content of 4-6%. The original one-step transposition technology was used for transposition reaction. In order to test the quality of the product caprolactam sulfonate, potassium permanganate solution was used for titration. The value is 0.7~0.8. In order to ensure the product quality, the ratio of oleum and cyclohexanone oxime is about 1.7. The two-step transposition technology of this patent is used to produce caprolactam sulfonate. The titer value is less than or equal to 0.6. The ratio of cyclohexanone oxime is reduced to below 1.45, so that the consumption of fuming sulfuric acid in the production process and the consumption of ammonia for the subsequent treatment of caprolactam sulfonate have been greatly reduced, and environmental pollution has been reduced simultaneously.

[0015] The specific design parameters are as follows:

[0016] 1) The process conditions of the two-step transposi...

Embodiment 2

[0019] Use cyclohexanone oxime with a water content of 7.2% as raw material, circulate with 138.66g of caprolactam sulfonate, add 6.36g of fuming sulfuric acid, add 4g of cyclohexanone oxime, and react at 75-85°C. The time is 55 minutes, and the titration value of the caprolactam sulfonate obtained is 0.61, and its SO# 3 The content is controlled at about 3.23%. Example 3 Use cyclohexanone oxime with a water content of 1.71% as a raw material, circulate with 430 g of caprolactam sulfonate, add 25.3 g of oleum, add 26.8 g of cyclohexanone oxime, and react between 80 and 100 ° C , the reaction time is 55 minutes, the titer value of the obtained caprolactam sulfonate is 0.66, and its SO# 3 The content is controlled at about 5.30%.

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Abstract

The present invention adopts aqueous cyclohexanone oxide and fuming sulfuric acid to make them produce reaction to prepare caprolactam sulfoacid ester, then uses ammonia to make treatment to obtain caprolactam. Said reaction is implemented by two steps: first step is strong exothermal reaction, and its reaction temp. is 60-120 deg.C, and its second step is that it uses free SO3 being in the system to make reaction, and the content (wt%) of free SO3 is 1-10%. Said invention possesses the following advantages: its production pross is simple, does not produce side product, and can reduce consumption of fuming sulfuric acid and formation of ammonium sulfate, etc.

Description

technical field [0001] The invention relates to a two-step water-carrying cyclohexanone oxime transposition method. Background technique [0002] At present, common patents generally use pure cyclohexanone oxime to react with excess oleum to prepare caprolactam sulfonate, and then neutralize it with ammonia to obtain caprolactam. In common patents, in order to achieve the purpose of purifying cyclohexanone oxime so that cyclohexanone oxime does not carry water, it is necessary to use toluene as a solvent for dehydration in the previous process reaction. When pure cyclohexanone oxime is used in the transposition reaction, the viscosity of the product is high, which requires high homogenization and mixing, and the reaction temperature is also high, reaching 120-125 ° C. Since cyclohexanone oxime is a heat-sensitive substance , which affects the quality of the reaction product. At the same time, due to the extremely high viscosity of the reaction pro...

Claims

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Application Information

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IPC IPC(8): C07C249/14C07C251/44C07D201/04
Inventor 刘建青徐有田吴素芳马炯戎建军谢方友王樟茂
Owner JUHUA GRP