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Method for preparing cyclododecanone oxime

A technology of cyclododecanone oxime and cyclododecanone, which is applied in the field of preparation of cyclododecanone oxime, can solve the problems of low utilization rate of hydrogen peroxide and achieve the effects of increasing utilization rate, increasing reaction rate and reducing thermal decomposition rate

Active Publication Date: 2021-10-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even if this document and CN1421432A report use ammonium salt as an auxiliary agent, the utilization rate of hydrogen peroxide is still lower than 90%, and the reaction time required for the conversion rate of cyclododecanone to reach 99.5% is still more than 1h

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 100g cyclododecanone, 200g isopropanol, 0.5g TS-1, 0.5g Ti-MWW, 0.05g ZIF-8, 0.05g ZIF-67 and 0.5g dodecyldihydroxyethylamine oxide to 1L stainless steel In the reaction kettle, the stirring was turned on, and the temperature was heated to 90°C.

[0045] Maintaining the reaction temperature, 93g of 30wt% ammonia water and 68g of 30wt% hydrogen peroxide were evenly added to the reaction kettle, the feeding time was 30min, and after the feeding was completed, the aging was continued for 30min.

[0046] After the reaction, the reaction solution was analyzed, and the conversion rate of cyclododecanone was 99.54%, the selectivity of cyclododecanone oxime was 99.2%, and the utilization rate of hydrogen peroxide was 92.3%.

Embodiment 2

[0048]100g of cyclododecanone, 1000g of isopropanol, 1.67g of TS-1, 8.33g of Ti-MWW, 3.75g of ZIF-8, 1.25g of ZIF-67 and 15g of lauryl amidopropyl amine oxide were added to the 1L stainless steel reactor, opened With stirring, the temperature was raised to 80°C by heating.

[0049] Maintaining the reaction temperature, 93g of 20wt% ammonia water and 61g of 40wt% hydrogen peroxide were evenly added into the reaction kettle, the feeding time was 20min, and after the feeding was completed, the aging was continued for 40min.

[0050] After the reaction, the reaction solution was analyzed, and the conversion rate of cyclododecanone was 99.61%, the selectivity of cyclododecanone oxime was 99.6%, and the utilization rate of hydrogen peroxide was 94.1%.

Embodiment 3

[0052] 100g of cyclododecanone, 400g of isopropanol, 1.33g of TS-1, 2.67g of Ti-MWW, 1.67g of ZIF-8, 0.83g of ZIF-67 and 4g of N-dodecyloxymorphine were added to the 1L stainless steel reactor , start stirring, and heat up to 85 °C.

[0053] Maintaining this reaction temperature, 80g of 27wt% ammonia water and 66g of 34wt% hydrogen peroxide were evenly added to the reaction kettle, the feeding time was 24min, and after the feeding was completed, the aging was continued for 36min.

[0054] After the reaction, the reaction solution was analyzed, and the conversion rate of cyclododecanone was 99.80%, the selectivity of cyclododecanone oxime was 99.7%, and the utilization rate of hydrogen peroxide was 96.7%.

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Abstract

The invention discloses a method for preparing cyclododecanone oxime. The method comprises the following steps: 1) heating a mixture of cyclododecanone, a solvent, a catalyst, a hydroxylamine protective agent and an auxiliary agent to a preset temperature; and (2) adding ammonia water and hydrogen peroxide into the mixture in the step (1) for reaction, and continuously aging until the reaction is finished after the charging is finished. A metal organic framework compound (MOFs) is used as a hydroxylamine protective agent, so that the utilization rate of hydrogen peroxide is increased; and amine oxide or ammonium carboxylate is used as an auxiliary agent, so that the ammoximation reaction rate is increased, and meanwhile, the thermal decomposition rate of hydrogen peroxide is reduced. By adopting the method, the conversion rate of the cyclododecanone can reach 99.5% or above and the utilization rate of the hydrogen peroxide can be increased to 90% or above after the reaction is carried out for 1 hour.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for preparing cyclododecanone oxime. Background technique [0002] In the early 1980s, the Italian company Enichem developed a new catalytic material - titanium silicon molecular sieve TS-1. Under the catalysis of TS-1, cycloalkanone, ammonia and hydrogen peroxide can undergo ammoximation reaction, and the cycloalkanone can be directly prepared in one step. Alkanone oxime creates conditions for the birth of new cycloalkanone oxime production technology. In 1994, Enichem Company built a 12kt / a caprolactam industrial experimental unit in Porto Maraghera, Italy using the ammonia oxime process. After that, Baling Petrochemical, Shenma Group and Quzhou Juhua also adopted the ammonia oxime technology to build a 100,000-ton or more caprolactam plant. Caprolactam plant, the development of cyclohexanone ammoximation technology has matured. [0003] Compared with cyclohexanone a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/08C07C251/44
CPCC07C249/08C07C251/44Y02P20/584
Inventor 边新建李俊平黎源张永振袁帅
Owner WANHUA CHEM GRP CO LTD
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