A kind of catalyst and its preparation method for dns hydrogenation reduction preparation das

A technology of catalysts and carbon catalysts, applied in catalyst protection, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problem of high selectivity that has not been reported in literature, catalyst life is impossible to talk about, Heavy metals pollute the reaction liquid and other problems, achieve the effects of improving life, ecology and environment friendliness, and solving low selectivity

Active Publication Date: 2019-05-03
上海合丽亚日化技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2011103425758 This application relates to a palladium-loaded mesoporous carbon catalyst to commercial TiO 2 As a carrier, prepared as Ni-Au-Pt / TiO 2 Nano multi-metal catalyst, although the preparation of the catalyst is simple, but precious metals such as gold and platinum are needed, so the cost of the catalyst is high
It has been verified by experiments that the selectivity cannot achieve satisfactory results, and the life of the catalyst is out of the question. Not only is the selectivity not up to standard, but it will also bring serious consequences of heavy metal pollution of the reaction solution.
[0006] At present, although many institutions in China are researching the preparation of DAS by catalytic hydrogenation of DNS, according to public reports, it is basically focused on how to improve the catalytic selectivity of hydrogenation, but the actual selectivity and the high Selectivity has not been reported in the literature

Method used

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  • A kind of catalyst and its preparation method for dns hydrogenation reduction preparation das
  • A kind of catalyst and its preparation method for dns hydrogenation reduction preparation das
  • A kind of catalyst and its preparation method for dns hydrogenation reduction preparation das

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Experimental program
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Effect test

Embodiment 1

[0042] Catalyst preparation:

[0043] 1. Weigh 10.0g (dried product) of Pd / C (Typ37 3% Pd) catalyst from Johnson Matthey Company, put it in a 250ml four-necked bottle, add 100ml pure water, and add 10% PVP (3000) aqueous solution under stirring 0.3g; heat up to 45°C, add 0.7ml of 0.2M lead acetate aqueous solution, 0.7ml of 0.2M bismuth trichloride hydrochloric acid solution, and 1.4ml of 0.2M potassium chromium sulfate aqueous solution.

[0044] 2. After the addition, slowly raise the temperature to 80°C, add 10ml of 10% sodium formate, then rapidly raise the temperature to reflux, and keep the first bulb at reflux. After refluxing for 3 hours, cool to 30°C and filter with suction. The filter cake was put into a vacuum drying oven at 105°C for vacuum drying, and after 3 hours, the power was turned off and cooled naturally. The next morning, the vacuum was lifted to take out the catalyst, and put it in a desiccator for later use.

[0045] The specific method of preparing DA...

Embodiment 2

[0048] The preparation method of self-made Pd / C: Weigh 35.0g of activated carbon (pre-activated) into a 1000ml four-necked flask, add 700ml of pure water at about 70°C, stir and heat up, add 7.0g of 10% PEG600 aqueous solution, and heat up to 80°C ℃, add 28.3ml of 0.4M palladium chloride hydrochloric acid solution, quickly add 15ml of formaldehyde solution under stirring, add 6.86% NaOH solution to adjust the pH value to 9.0. After adjustment, keep warm at 80°C for 0.5 hours. Filter and wash the filter cake repeatedly until the pH of the washing filtrate is neutral. After pumping, the filter cake was dried in the air at room temperature, and then dried in a desiccator filled with potassium hydroxide to obtain a dried catalyst, which was stored in a sealed bottle for future use.

[0049] Catalyst preparation:

[0050] 1. Weigh 34.9g of self-made Pd / C (3.44%Pd) catalyst, put it in a 1000ml four-necked flask, add 700ml of pure water, and add 0.7g of 10% PEG1500 aqueous solution...

Embodiment 3

[0055] Catalyst preparation:

[0056] 1. Weigh 34.9g of self-made Pd / C catalyst, put it in a 1000ml four-necked flask, add 700ml of pure water, and add 0.2g of 10% LAS aqueous solution under stirring. Heat up to 65°C, add 0.4ml of 0.2M lead acetate aqueous solution, 0.7ml of 0.2M potassium chromate solution, and 1.0ml of 0.2M sodium tungstate aqueous solution in sequence.

[0057] 2. After the addition, the temperature was raised to reflux, and 1.5ml of formic acid solution was carefully added. After reflux for 4.5 hours, cool to 30°C and filter with suction. After the filter cake is fully washed, it is placed in a vacuum drying oven for 2 hours at 65°C, 2 hours at 95°C, and 2 hours at 105°C.

[0058] The specific method of preparing DAS by DNS hydrogenation reduction is as follows:

[0059] Add 7.00g of hydrogenation catalyst, 600g of 18% DNS solution, a little flushing water to a 1L autoclave in sequence, seal the autoclave, first evacuate it, and when the vacuum degree r...

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Abstract

The invention relates to the catalyst field, and in particular relates to a catalyst for preparing DAS by from DNS by hydrogenation reduction and a preparation method thereof. The catalyst comprises a palladium / carbon catalyst, a surfactant and a passivating agent, wherein the weight ratio of the palladium / carbon catalyst to the surfactant is 100:0.1 to 5; a solvent of the catalyst is pure water, and the weight of the pure water is 3-20 times, preferably 5-10 times, of the weight of the palladium / carbon catalyst. The catalyst has the advantages of high yield, high content of high performance liquid chromatography, low impurity, fast reaction speed, short production period, light product color, low iron ion content, low production energy consumption and the like. The catalyst not only solves the problem that the catalyst selectivity of DNS catalytic hydrogenation is not high in previous reports, and meanwhile the service life of the catalyst is greatly improved.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a catalyst for preparing DAS by hydrogenation reduction of DNS and a preparation method thereof. Background technique [0002] DAS acid (4,4'-diaminostilbene-2,2'-disulfonic acid) is an important raw material for the production of stilbene bistriazine amino-type brighteners, and is also an important intermediate for the manufacture of direct dyes and reactive dyes It can also be used to synthesize insecticides. For a long time, industrial production has adopted the Bechamp reduction method of nitroaromatics, that is, iron powder reduction method. Its principle is to reduce nitroaromatics to corresponding aromatic amines with iron powder, ferrous chloride and dilute acid. This method is simple in operation, low in production cost, and easy to control, but it will produce a large amount of solid waste iron sludge. Although there are comprehensive utilizations to produce iron red, the cur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J33/00C07C309/46C07C303/22
Inventor 孙桥张贵民
Owner 上海合丽亚日化技术有限公司
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