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Methoxylamine preparation method and methoxylamine hydrochloride preparation method

A technology of methoxyamine hydrochloride and methoxyamine, which is applied in the field of coal chemical industry, can solve the problems of high energy consumption for dehydration and separation and consumption of large oil resources, and achieve the effects of reducing equipment requirements, improving production efficiency, and being easy to operate

Active Publication Date: 2020-12-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, ethylene glycol is mainly produced by the petrochemical technology route: ethylene oxide is used as raw material to prepare ethylene oxide through epoxidation, and then hydration is used to prepare ethylene glycol; this technology needs to consume a lot of petroleum resources, and dehydration and separation consume a lot of energy

Method used

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  • Methoxylamine preparation method and methoxylamine hydrochloride preparation method
  • Methoxylamine preparation method and methoxylamine hydrochloride preparation method
  • Methoxylamine preparation method and methoxylamine hydrochloride preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Embodiment 1 Different nickel-based catalysts catalyze the reaction of hydrogen reduction methyl nitrite to produce methoxyamine

[0057] The nickel-based catalysts of different carriers were tabletted, pulverized, and passed through a 10-mesh sieve, and 5g of nickel-based catalysts (1wt%) with a particle size of less than 10 meshes were packed into a glass tube reactor with a diameter of 15mm. The reaction gas composition was 23.4vol %H 2 , 33.0vol% methyl nitrite, 3.4vol% Ar (internal standard), 40.2vol% N 2 , the reaction temperature is 70°C, and the total WHSV of the reaction gas is 1.0h -1 , the reduction reaction was carried out under normal pressure.

[0058] The results obtained on different supported catalysts are shown in Table 1.

[0059] Table 1 Catalytic hydrogen reduction of methyl nitrite to methoxyamine by different nickel-based catalysts

[0060]

[0061] As can be seen from the results in Table 1, different nickel-based catalysts catalyze the hy...

Embodiment 2

[0062] Embodiment 2 Catalyst particle diameter influence

[0063] 1wt%Ni / ɑ-Al 2 o 3 The nickel-based catalyst was tabletted, crushed, and passed through sieves with different meshes, and 5g of 1wt%Ni / ɑ-Al with a particle size smaller than the corresponding meshes was taken. 2 o 3 Put it into a glass tube reactor with a diameter of 15mm, and the reaction gas composition is 23.4vol%H 2 , 33.0vol% methyl nitrite, 3.4vol% Ar (internal standard), 40.2vol% N 2 , the reaction temperature is 70°C, and the WHSV is 1.0h -1 , the reduction reaction was carried out under normal pressure.

[0064] The results obtained from the reaction results of catalysts with different particle sizes are shown in Table 2.

[0065] Table 2 Catalytic hydrogen reduction of methyl nitrite to methoxyamine by nickel-based catalysts with different particle sizes

[0066]

[0067] It can be seen from the results in Table 2 that the particle size of the catalyst has a significant impact on the conversio...

Embodiment 3

[0068] Embodiment 3 nickel loading influence

[0069] The particle diameter is that 20 mesh 5g nickel-based catalysts are packed into a glass tube reactor with a diameter of 15mm, and the reaction gas composition is 23.4vol%H 2 , 33.0vol% methyl nitrite, 3.4vol% Ar (internal standard), 40.2vol% N 2 , the reaction temperature is 70°C, and the WHSV is 1.0h -1 , the reduction reaction was carried out under normal pressure.

[0070] The reaction results on different catalysts are shown in Table 3.

[0071] Table 3 Ni-based catalysts with different nickel loadings catalyzed hydrogen reduction of methyl nitrite to methoxyamine

[0072]

[0073] It can be seen from the results in Table 3 that the nickel loading has a significant impact on the conversion rate of methyl nitrite. As the nickel loading increases, the conversion rate of methyl nitrite gradually increases and then remains the same. The trend of methoxyamine yield is the same as the conversion rate of methyl nitrite....

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Abstract

The invention discloses a methoxylamine preparation method which at least comprises the following steps of enabling feed gas containing methyl nitrite and a reducing agent to be in contact with a reduction reaction catalyst in a reactor, and performing reduction reaction to obtain methoxylamine. According to the method, the important intermediate methyl nitrite in the technical process of preparing ethylene glycol from coal can be fully utilized, and the conversion rate of methyl nitrite is high. The invention also provides a method for preparing methoxylamine hydrochloride by taking methoxylamine obtained by the method as a raw material.

Description

technical field [0001] The application relates to a method for preparing methoxyamine and a method for preparing methoxyamine hydrochloride, belonging to the field of coal chemical industry. Background technique [0002] Methoxyamine hydrochloride is an important pesticide and pharmaceutical intermediate. In pesticide synthesis, it can be used to produce pesticides such as phenylacetone oxime, clethodim, sethoxydim and other herbicides; in pharmaceutical synthesis, it can be used to produce cephalosporin antibiotics, such as cefuroxime, sulfamethoxazole, norethindr Ming, hydroxyurea, etc. In recent years, the demand for cephalosporin antibiotics such as cefuroxime has continued to increase, and the market demand for methoxyamine hydrochloride has also continued to increase. [0003] At present, the production technology of methoxyamine hydrochloride in my country is backward, the three wastes are serious, and the production cost is high. Therefore, it is of great signific...

Claims

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Application Information

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IPC IPC(8): C07C239/20
CPCC07C239/20
Inventor 高进马继平徐杰孙志强孙颖
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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