Preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate

A technology of p-aminophenyl and hydroxyethyl sulfone, which is used in the synthesis of reactive dye intermediates, can solve the problems of palladium-carbon catalysts, such as easy sulfur poisoning price, low production efficiency, and low catalytic selectivity.

Inactive Publication Date: 2018-05-08
广东众和高新科技股份公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to overcome the defects in the above-mentioned existing production process, technicians have developed a preparation method for p-aminophenyl-β-hydroxyethyl sulfone sulfate. Although the production method disclosed in CN103626684A has improved the yield to a certain extent, its yield It is about 92%. Adopting this method to produce p-aminophenyl-beta-hydroxyethyl sulfone sulfate uses less hydrogen peroxide and palladium-carbon catalyst consumption, and also reduces the output of three wastes, but the palladium-carbon catalyst used in this method is easy to sulfur Poisoning and expensive, more importa

Method used

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  • Preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate
  • Preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate
  • Preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate

Examples

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Effect test

Embodiment 1

[0070] A preparation method of p-aminophenyl-β-hydroxyethyl sulfone, the steps are as follows:

[0071] The solid oxidizing material p-nitrophenyl-β-hydroxyethyl sulfone, methyl alcohol and modified framework nickel are added in the hydrogenation autoclave, and the mass ratio of solid oxidizing material, methanol and modified framework nickel is 1:4: 0.05, the purity of methanol is 99.99wt%, and then carry out hydrogenation reaction at 70°C and hydrogen pressure of 1.5MPa for 4h; Hydrogen product p-aminophenyl-β-hydroxyethyl sulfone;

[0072] The modified skeleton nickel uses nickel as the skeleton, including: 85 parts by mass of Ni, 15 parts by mass of Al, and 4 parts by mass of metal additive; the metal additive is Mo; it is prepared by the following method:

[0073] (1) Melt down in an inert atmosphere after metal additive is mixed with the nickel-aluminum alloy powder that contains nickel 85wt%, obtain alloy, continue roasting 3h in melting furnace, with 0.5 * 10 6 After...

Embodiment 2

[0076] A preparation method of p-aminophenyl-β-hydroxyethyl sulfone, the steps are as follows:

[0077] The solid oxidizing material p-nitrophenyl-β-hydroxyethyl sulfone, methyl alcohol and modified framework nickel are added in the hydrogenation autoclave, and the mass ratio of solid oxidizing material, methanol and modified framework nickel is 1:4: 0.03, the purity of methanol is 99.99wt%, and then the hydrogenation reaction is carried out at 85°C and the hydrogen pressure is 2.0MPa for 3.5h; Hydrogenation product p-aminophenyl-β-hydroxyethyl sulfone;

[0078] Wherein the modified skeleton nickel uses nickel as the skeleton, including: 90 parts by mass of Ni, 10 parts by mass of Al, and 8 parts by mass of metal additives; the metal additive is Cu; prepared by the following method:

[0079] (1) Melt down in an inert atmosphere after metal additive is mixed with the nickel-aluminum alloy powder that contains nickel 90wt%, obtain alloy, continue roasting 4h in melting furnace,...

Embodiment 3

[0082] A preparation method of p-aminophenyl-β-hydroxyethyl sulfone, the steps are as follows:

[0083] The solid oxidizing material p-nitrophenyl-β-hydroxyethyl sulfone, methyl alcohol and modified framework nickel are added in the hydrogenation autoclave, and the mass ratio of solid oxidizing material, methanol and modified framework nickel is 1:4: 0.02, the purity of methanol is 99.99wt%, and then hydrogenation reaction is carried out at 100°C and hydrogen pressure of 2.5MPa for 3h; Hydrogen product p-aminophenyl-β-hydroxyethyl sulfone;

[0084] Wherein the modified skeleton nickel uses nickel as the skeleton, including: 80 parts by mass of Ni, 20 parts by mass of Al, and 5 parts by mass of metal additive; the metal additive is Cr; prepared by the following method:

[0085] (1) Melt down in an inert atmosphere after metal additive is mixed with the nickel-aluminum alloy powder that contains nickel 80wt%, obtain alloy, continue roasting 3h in melting furnace, with 0.8 * 10 ...

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Abstract

The invention relates to preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate. The preparing methods both comprise the steps that p-aminophenyl-beta-hydroxyethylsulfonyl and hydrogen are used as raw materials, modified framework nickel is used as a hydrogen-adding catalyst, a catalytic hydrogenation reaction is conducted in a solvent toobtain reduction liquid, and modified framework nickel and the solvent in the reduction liquid are separated and removed to obtain p-minophenyl-beta-hydroxyethylsulfonyl sulphonate; according to modified framework nickel, nickel is used as a framework, and modified framework nickel is prepared from, by mass, 75-95 parts of Ni, 3-15 parts of Al and 2-10 parts of metal adjuvant; the metal adjuvantcomprises the combination of any one or at least two of Mo, Cu and Cr. The yield can reach 94% or above; preparation of p-minophenyl-beta-hydroxyethylsulfonyl sulphonate is a continuous production technology, the technology is simplified, the production efficiency is high, the quality is stable, the production cost is low, and the economic benefit and social benefit are obvious.

Description

technical field [0001] The invention relates to the technical field of synthesis of reactive dye intermediates, in particular to a preparation method of aminophenyl-β-hydroxyethylsulfone and p-aminophenyl-β-hydroxyethylsulfone sulfonate. Background technique [0002] At present, the production method of p-aminophenyl-beta-hydroxyethyl sulfone sulfonate is to adopt raw materials such as p-acetanilide, chlorosulfonic acid, sodium pyrosulfite, sodium hydroxide, oxirane, sulfonic acid to synthesize, and Synthesis includes the following steps: [0003] A, sulfonation process: first add metered chlorosulfonic acid (excessive) in the sulfonation kettle, then put the measured antipyretic ice into the sulfonation kettle for reaction, the sulfonation reaction is an exothermic reaction, use The ice brine below -10°C is cooled and controlled through the jacketed reactor to make the reaction go smoothly. A large amount of hydrogen chloride gas is generated during the reaction, and the ...

Claims

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Application Information

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IPC IPC(8): C07C315/04C07C317/36B01J23/883B01J23/755B01J23/86B01J23/887
CPCC07C315/02C07C315/04C07C319/14C07C317/36C07C323/12C07C317/18
Inventor 冯懿张宏秋
Owner 广东众和高新科技股份公司
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