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Method for synthesizing diethyl hydroxylamine by using slurry reactor

A technology of diethylhydroxylamine and slurry bed, which is applied in the field of slurry bed synthesis of diethylhydroxylamine, can solve problems such as non-recyclability and post-processing difficulties, and achieve low incidence of side reactions, high effective utilization rate, and high product quality. The effect of high purity

Pending Publication Date: 2021-02-05
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent CN 109096143 A adopts heteropolyacid loaded as catalyst, and triethylamine, acetic acid and hydrogen peroxide as raw materials to synthesize diethylhydroxylamine. After the reaction is completed, inorganic salts will be produced, which is difficult for post-processing and cannot be reused.

Method used

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  • Method for synthesizing diethyl hydroxylamine by using slurry reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Catalyst pretreatment: Weigh 1.476g of copper nitrate and dissolve it in water, add 50g of TS-1 molecular sieve with a silicon-titanium ratio of 50%; load at 50°C for 2h, dry at 100°C, and bake at 550°C for 6h.

[0026] Weigh 36g of the above-mentioned pretreated catalyst, add it into the slurry bed reactor, mix diethylamine and tetrahydrofuran at a mass ratio of 1:1, and pump them into the slurry tank reactor with 27.5% hydrogen peroxide respectively with a metering pump Carry out the reaction, control the feed rate of hydrogen peroxide to be 36g / h, the mol ratio of diethylamine and hydrogen peroxide to be 2.5:1, control the reaction temperature to be 70°C, the reaction pressure to be 0.1mpa, and the control selectivity in the reaction chromatogram to be 99%, the product and hydrogen peroxide The effective utilization rate is 97.5%, and the reaction yield is 94%.

Embodiment 2

[0028] Catalyst pretreatment: Weigh 1.476g of copper nitrate and dissolve it in water, add 50g of TS-1 molecular sieve with a silicon-titanium ratio of 50%; load at 50°C for 2h, dry at 100°C, and bake at 550°C for 6h.

[0029] Weigh 36g of the above-mentioned pretreated catalyst, add it into the slurry bed reactor, mix diethylamine and tetrahydrofuran at a mass ratio of 1:1, and pump them into the slurry tank reactor with 27.5% hydrogen peroxide respectively with a metering pump Carry out the reaction, control the feed rate of hydrogen peroxide to be 30g / h, the mol ratio of diethylamine and hydrogen peroxide to be 2:1, control the reaction temperature to be 80°C, the reaction pressure to be 0.05mpa, and the control selectivity in the reaction chromatogram to be 99%. The effective utilization rate is 97%, and the reaction yield is 92.5%.

Embodiment 3

[0031] Catalyst pretreatment: Weigh 1.476g of copper nitrate and dissolve it in water, add 50g of TS-1 titanium-silicon molecular sieve with a silicon-to-titanium ratio of 50%; load at 50°C for 2h, dry at 100°C, and bake at 550°C for 6h.

[0032] Weigh 36g of the above-mentioned pretreated catalyst, add it into the slurry bed reactor, mix diethylamine and tetrahydrofuran at a mass ratio of 1:1, and pump them into the slurry tank reactor with 27.5% hydrogen peroxide respectively with a metering pump Carry out the reaction, control the feed rate of hydrogen peroxide to be 18g / h, the mol ratio of diethylamine and hydrogen peroxide to be 2.5:1, control the reaction temperature to be 60°C, the reaction pressure to be 0.05mpa, and the control selectivity in the reaction chromatogram to be 99%, the product and hydrogen peroxide The effective utilization rate is 97.3%, and the reaction yield is 93.5%.

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Abstract

The invention discloses a method for synthesizing diethyl hydroxylamine by using a slurry reactor, and belongs to the field of fine chemical synthesis. The preparation method comprises the following steps of: firstly, modifying a catalyst which takes a titanium silicalite molecular sieve as a carrier, and loading soluble copper salt on the titanium silicalite molecular sieve, with copper accounting for 0.1-5% of the mass of the titanium silicalite molecular sieve; putting the modified titanium silicalite molecular sieve as a catalyst into a slurry bed reactor, mixing diethylamine and a solventat a certain temperature and under a certain pressure, pumping the mixture and hydrogen peroxide into the slurry bed reactor according to a certain ratio, carrying out a reaction, collecting the reaction liquid, and carrying out post-treatment. By adopting the catalyst in the invention for reaction, the effective utilization rate of hydrogen peroxide is greater than 96%, and the selectivity of diethyl hydroxylamine is greater than 99%. The method can be used for continuous synthesis, a device does not need to be frequently disassembled, the operation is convenient, the catalyst can be supplemented under the condition that the catalyst is lost, and the method is energy-saving and environment-friendly.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis, and in particular relates to a method for synthesizing diethylhydroxylamine in a slurry bed. Background technique [0002] Diethylhydroxylamine (DEHA) belongs to disubstituted hydroxylamine derivatives. Because of its high efficiency, non-toxicity, and easy separation, it is often used as a polymerization inhibitor and terminal terminator for olefin monomers, as well as silicone rubber production aids and organic compounds. It is a chemical synthesis intermediate and can also be used as an oxygen scavenger in the steam boiler water system, not only for low temperature deoxygenation, but also for high temperature steam condensate water circulation system. Its oxygen removal function is better than hydrazine and carbohydrazide; when there is a catalyst, its oxygen removal function is higher. Diethylhydroxylamine is also used as a passivator for metals on the water side of equipment. In addi...

Claims

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Application Information

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IPC IPC(8): C07C239/10B01J29/89
CPCC07C239/10B01J29/89B01J2229/40B01J2229/186
Inventor 王蕊王庆吉李进王炳春王贤彬
Owner CHINA CATALYST HLDG CO LTD
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