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Method for synthesis of monosodium 8-amino-1-naphthol-3,6-disulfonate through hydrogenation catalysis and catalyst

A technology of hydrogenation catalysis and monosulfuric acid, applied in the field of chemistry, can solve the problems of large catalyst recycling, low catalyst recycling times, unsuitable for industrial production, etc., and achieves the effects of low cost, stable reaction and easy control.

Inactive Publication Date: 2016-01-27
甘肃悦美达实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The catalyzer of the hydrogenation reduction process of the above 8-amino-1-naphthol-3,6-disulfonic acid monosodium salt is mainly Raney nickel, nickel alloy, palladium / carbon catalyst, etc., because a large amount of ammonium salts are contained in the reaction solution , sulfonic acid substances and other complex components, which makes the above-mentioned hydrogenation reduction process prone to catalyst poisoning, so that the catalyst is quickly deactivated, and there are big problems in the recycling of the above-mentioned catalysts, and the recycling times of the catalysts are low, resulting in High production cost, not suitable for industrial production

Method used

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  • Method for synthesis of monosodium 8-amino-1-naphthol-3,6-disulfonate through hydrogenation catalysis and catalyst

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Experimental program
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Effect test

Embodiment 1

[0021] Preparation of the catalyst used in the hydrogenation catalytic synthesis of 8-amino-1-naphthol-3,6-disulfonic acid monosodium salt: the catalyst is an activated carbon-supported three-way catalyst, which uses nickel nitrate, ammonium molybdate, nitric acid Prepare iron as a precursor to obtain a precursor solution containing nickel-molybdenum-iron active elements, and then soak activated carbon in the precursor solution for 6 to 48 hours. The element, molybdenum element, and iron element are added in a mass ratio of 1:0.2-0.5:0.1-0.2:0.01-0.2. After the nickel-molybdenum-iron active element is fully absorbed by the activated carbon, it is filtered and dried, and then placed in a high-temperature oven for curing. The high-temperature curing temperature is 200-320°C, and the high-temperature curing time is 3-12 hours. After curing, it is reduced by introducing hydrogen gas under high temperature conditions, the high temperature reduction temperature is 300-400°C, and the...

Embodiment 2

[0023] Take 1000g of the nitro-T ammonium salt reaction liquid after sulfonation, nitration, denitrification, and ammonia water neutralization as the reaction raw material, add 30% ammonia solution at room temperature, and adjust the pH of the reaction raw material to 7.5. The pretreated reaction solution is transferred into an autoclave, and an activated carbon-supported nickel-molybdenum-iron three-way catalyst is added. The catalyst is prepared by the method in Example 1, wherein the mass ratio of activated carbon, nickel element, molybdenum element, and iron element is 1:0.5:0.2:0.2, and the preparation conditions are prepared in Example 1. Activated carbon-loaded Optimal conditions for nickel-molybdenum-iron three-way catalysts. The amount of the catalyst used is 5% of the weight of the nitro T ammonium salt, the catalytic reaction temperature is 100° C., the hydrogen gas is introduced at a pressure of 1.0 MPa, and the catalytic reaction is carried out for 5 hours to obta...

Embodiment 3

[0025] Take 1000g of the nitro-T ammonium salt reaction liquid after sulfonation, nitration, denitrification, and ammonia water neutralization as the reaction raw material, add 30% ammonia solution at room temperature, and adjust the pH of the reaction raw material to 9.5. The pretreated reaction solution is transferred into an autoclave, and an activated carbon-supported nickel-molybdenum-iron three-way catalyst is added. The catalyst is prepared by the method in Example 1, wherein the mass ratio of activated carbon, nickel element, molybdenum element, and iron element is 1:0.5:0.2:0.2, and the preparation conditions are prepared in Example 1. Activated carbon-loaded Optimal conditions for nickel-molybdenum-iron three-way catalysts. The amount of the catalyst used is 20% of the weight of the nitro-T ammonium salt, the catalytic reaction temperature is 160° C., the hydrogen gas is introduced at a pressure of 5.0 MPa, and the catalytic reaction is carried out for 8 hours to obtai...

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Abstract

The invention discloses a method for synthesis of monosodium 8-amino-1-naphthol-3,6-disulfonate through hydrogenation catalysis and a catalyst. The catalyst is an active-carbon-loaded nickel molybdenum iron three-way catalyst. The method is as follows: a nitro T ammonium salt reaction liquid is employed as a reaction raw material, pH value adjustment pretreatment of the reaction raw material is carried out, then hydrogenation reduction is carried out by the active-carbon-loaded nickel molybdenum iron three-way catalyst, then alkali fusion and acidification are carried out, and monosodium 8-amino-1-naphthol-3,6-disulfonate is prepared. Preparation for the catalyst is simple, he nitro T ammonium salts can be reduced to amino T ammonium salts effectively, and the problems of catalyst poisoning, rapid inactivation and low recovery frequency and the like in the hydrogenation reduction process can be solved. The synthetic method raises the yield and the product purity of the hydrogenation catalysis technology greatly, generation of waste water and environment pollution are reduced, the technology steps are simple and safe, and the reaction is stable and easy to control.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a method for synthesizing 8-amino-1-naphthol-3,6-disulfonic acid monosodium salt by hydrogenation catalysis and a catalyst used therefor. Background technique [0002] Compound 8-amino-1-naphthol-3,6-disulfonic acid monosodium salt (English name: 8-Amino-1-naphthol-3,6-disulfonicacidmonosodium salt, CAS number: 5460-09-3, molecular formula: C 10 h 8 o 7 NS 2 Na, molecular weight: 341) is an important intermediate in the dye industry and an important intermediate in the production of water-soluble dyes. Its main purpose is to synthesize azo dyes, such as acid magenta 6B, acid scarlet G, acid black 10B, direct black, Reactive Brilliant Red K-2BP, Reactive Violet K-3R, Reactive Dark Blue K-R and more than 90 kinds of fuels, these dyes are used for dyeing woolen and cotton fabrics, and can also be used for the production of medicines. Since some dyes synthesized by benzidine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/883C07C309/50C07C303/32
Inventor 尚可心
Owner 甘肃悦美达实业有限公司
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