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Catalyst for liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid and preparation method thereof

A technology of nitrotoluene and sulfonic acid solution, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of low noble metal loading, good product purity, low product purity, etc., achieve low dechlorination, improve catalytic activity, environmental protection low pollution effect

Active Publication Date: 2014-10-08
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical purpose of the present invention is aimed at in the process of producing CLT acid with toluene sulfonation route, when adopting iron powder etc. as catalyst reduction 6-chloro-3 nitrotoluene-4-sulfonic acid, the reduction yield produced is low, the product In order to solve the problems of low purity and serious environmental pollution, a new catalyst for the liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid in the production process of CLT acid is provided. The catalyst has good hydrogenation activity , high selectivity, low dechlorination, and low loading of precious metals. When using this catalyst to reduce 6-chloro-3nitrotoluene-4-sulfonic acid, the reduction rate is high, the product purity is good, and the environmental pollution is less

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In this example, the catalyst used for the liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid is supported by Raschig ring type (that is, single-hole cylindrical) alumina, and on its surface The active component Pt is loaded, and the active component Pt is distributed in an eggshell shape on the surface of Raschig ring alumina. The specific preparation process of the catalyst is as follows.

[0031] (1) Take 0.098 moles of Raschig ring-type alumina and calcinate at 500°C for 2 hours, then cool to room temperature. The purity of Raschig ring-type alumina is 95.5%, and the specific surface area is 103 m 2 / g, the pore volume is 0.5 ml / g carrier;

[0032] (2) Mix the Raschig-ring-type alumina treated in step (1) with 2 ml of chloroplatinic acid solution, add water to dissolve, then add 10 ml of sodium hydroxide aqueous solution, and impregnate at a constant temperature of 80 ° C for 2 hours, then water Calcining at 500°C for 2 hours ...

Embodiment 2

[0039] In this example, the catalyst used for the liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid is supported by Raschig ring-type alumina, and the active component Pt is loaded on its surface, and The active component Pt is distributed in an eggshell shape on the surface of Raschig ring-type alumina, and the carrier is also loaded with additive Na 2 O. The specific preparation process of the catalyst is as follows.

[0040] (1) Exactly the same as step (1) in Example 1;

[0041] (2) Exactly the same as step (2) in Example 1;

[0042] (3) Add 0.5 milliliters of sodium carbonate to the reaction product obtained in step (2), then reduce it in 50 milliliters of hydrazine hydrate aqueous solution; finally wash and dry to obtain the finished catalyst, wherein the active component Pt mass accounts for 0.2% of the mass of ring alumina, Na 2 The mass of O accounts for 0.05% of the mass of Raschig ring alumina.

[0043] The catalyst prepar...

Embodiment 3

[0046] In this example, the catalyst used for the liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid is supported by Raschig ring-type alumina, and the active component Pt is loaded on its surface, and The active component Pt is distributed in an eggshell shape on the surface of Raschig ring-type alumina, and the carrier is also loaded with additive K 2 O. The specific preparation process of the catalyst is as follows.

[0047] (1) Take 0.098 moles of Raschig-ring alumina and calcinate at 600°C for 1.5 hours, then cool to room temperature. The purity of Raschig-ring alumina is 99.6%, and the specific surface area is 142 m 2 / g, the pore volume is 0.6 ml / g carrier;

[0048] (2) Mix the Raschig-ring-type alumina treated in step (1) with 2 ml of chloroplatinic acid solution, add water to dissolve, then add 10 ml of sodium hydroxide aqueous solution, and impregnate at a constant temperature of 80 ° C for 2 hours, then water washing and dryi...

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Abstract

The invention provides a catalyst for the liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid (CLT acid) and a method for preparing the catalyst. The alumina (Al2O3) in the columnar structure or spherical structure is used as the carrier, and the active component which is the platinum (Pt) is supported on the surface of the carrier so that the Pt / Al2O3 catalyst preferentially distributed like an eggshell is formed, wherein the mass of the platinum is 0.05-10% of that of the carrier. Compared with the prior art, the catalyst provided by the invention has good hydrogenation activity, high selectivity and low dechlorination. When the catalyst is used for the hydrogenation reduction and the production of the CLT acid, high reduction rate is achieved, the product has good purity, and less pollution is caused to the environment.

Description

technical field [0001] The invention relates to the technical field of CLT acid, in particular to a catalyst for liquid-phase hydrogenation reduction reaction of 6-chloro-3-nitrotoluene-4-sulfonic acid and a preparation method thereof. Background technique [0002] 6-chloro-3-aminotoluene-4-sulfonic acid, its English name is 6-chloro-3-nitrotoluene-4-sulfonic acid, referred to as CLT acid. CLT acid is an important red organic pigment intermediate, which can be used to synthesize lake organic pigments such as plastic scarlet, new treasure red 36b, golden light red c, etc. The pigment is widely used in paints, coatings, colored inks, rubber, plastic coloring, etc. At present, the total production capacity of CLT acid in the world has reached 23,600 tons per year, among which China is the country with the largest production capacity of CLT acid in the world, accounting for about 44.9% of the world's total production capacity. [0003] In the past 20 years, my country's CLT aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/42C07C309/48C07C303/22
Inventor 周生虎胡义波
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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