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Catalyst for synthesizing 3, 5-dichloroaniline, and preparation method and application of catalyst

A dichloroaniline and catalyst technology, applied in the field of catalysts for the synthesis of 3,5-dichloroaniline and its preparation, can solve the problems of serious environmental pollution, reduced reaction rate, and difficult handling, and achieve high catalytic reaction selectivity and adsorption Strong ability and high catalytic activity

Active Publication Date: 2019-12-31
XIAN CATALYST NEW MATERIALS CO LTD
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  • Description
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Problems solved by technology

[0003] (1) Electrolytic reduction method The electrolytic reduction method has been stuck in the research stage due to the constraints of electrode materials, equipment, cost and other factors, and the process route has not been able to achieve industrial production
[0004] (2) Chemical reduction method The chemical reduction method of iron powder will produce more wastewater, which is very difficult to deal with and causes serious environmental pollution. The alkali sulfide reduction method has a high cost and cannot obtain an ideal yield.
[0005] (3) The publication date of 1,3,5-trichlorobenzene ammonia solution method is May 31, 2017, and the Chinese patent document with application number 201611235021.7 discloses a method using 1,3,5-trichlorobenzene in transition metal A synthetic method for obtaining 3,5-dichloroaniline by ammonolysis under catalysis, which is simple in operation and short in reaction steps, but has the problem of low yield (<93%)
[0006] (4) Polychlorinated nitrobenzene hydrogenation route In order to avoid environmental pollution, people focus on the research of environmentally friendly catalytic hydrogenation reduction method, but this process also has the problem of dechlorination while hydrogenation
The date of publication is June 23, 2004, and the Chinese patent application document with application number 02148509.7 discloses that Pd, Pt / CNT (carbon nanotubes) are used as catalysts for catalytic hydrogenation, and the dehalogenation rate is reduced to 0.1%, but due to The cost of carbon nanotubes is too high to achieve industrial production
In addition, other literatures use chemical reagents such as ethanolamine and morpholine to add dechlorination inhibitors to the reaction system, which can also achieve low dechlorination rates. Difficulties

Method used

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  • Catalyst for synthesizing 3, 5-dichloroaniline, and preparation method and application of catalyst

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Experimental program
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Embodiment 1

[0030] The catalyst for the synthesis of 3,5-dichloroaniline in this embodiment includes a barium sulfate carrier, Pd and promoter metals loaded on the barium sulfate carrier, and in the catalyst, the mass percentage of Pd is 2.0%. The mass percentage of the auxiliary metal is 1.0%, and the auxiliary metal is Mn.

[0031] The preparation method of the catalyst for the synthesis of 3,5-dichloroaniline of the present embodiment comprises the following steps:

[0032] Step 1. Add 50g of barium sulfate carrier to 500mL of boric acid solution with a mass percentage of 2%, stir and reflux in a water bath at 80°C for 3h, filter, wash the retentate, and place the retentate after washing in an oven at 100°C for vacuum drying After 24 hours, add it to 250 mL of 5% sodium phosphite solution by mass, stir at room temperature for 24 hours, filter, wash, and vacuum-dry in an oven at 100°C for 24 hours to obtain pretreated barium sulfate;

[0033] Step 2, mixing the pretreated barium sulfat...

Embodiment 2

[0036]The catalyst for the synthesis of 3,5-dichloroaniline in this embodiment includes a barium sulfate carrier, Pd and promoter metals loaded on the barium sulfate carrier, and in the catalyst, the mass percentage of Pd is 1.0%. The mass percentage of the auxiliary metal is 0.5%, and the auxiliary metal is Co.

[0037] The preparation method of the catalyst for the synthesis of 3,5-dichloroaniline of the present embodiment comprises the following steps:

[0038] Step 1. Add 50g of barium sulfate carrier to 500mL of boric acid solution with a mass percentage of 15%, stir and reflux in a water bath at 100°C for 5h, filter, wash the retentate, and place the retentate after washing in an oven at 100°C for vacuum drying After 24 hours, add it to 250 mL of 10% sodium phosphite solution by mass, stir at room temperature for 20 hours, filter, wash, and vacuum-dry in an oven at 100°C for 24 hours to obtain pretreated barium sulfate;

[0039] Step 2, mixing the pretreated barium sulf...

Embodiment 3

[0042] The catalyst for the synthesis of 3,5-dichloroaniline in this embodiment includes a barium sulfate carrier, Pd and promoter metals loaded on the barium sulfate carrier, and in the catalyst, the mass percentage of Pd is 1.5%. The mass percentage of the auxiliary metal is 0.2%, and the auxiliary metal is Cu.

[0043] The preparation method of the catalyst for the synthesis of 3,5-dichloroaniline of the present embodiment comprises the following steps:

[0044] Step 1. Add 50g of barium sulfate carrier to 500mL of boric acid solution with a mass percentage of 25%, stir and reflux in a water bath at 100°C for 5h, filter, wash the retentate, and place the retentate after washing in an oven at 100°C for vacuum drying After 24 hours, add it to 250 mL of 20% sodium phosphite solution by mass, stir at room temperature for 20 hours, filter, wash, and vacuum-dry in an oven at 100°C for 24 hours to obtain pretreated barium sulfate;

[0045] Step 2, mixing the pretreated barium sul...

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Abstract

The invention discloses a catalyst for synthesizing 3, 5-dichloroaniline. The catalyst comprises a barium sulfate carrier, Pd, and an auxiliary agent metal, and the auxiliary agent metal is Mn, Fe, Co, Cu or Zn. In addition, the invention also provides a preparation method of the catalyst and a method for catalyzing hydrogenation of 3, 5-dichloronitrobenzene to synthesize 3, 5-dichloroaniline by using the catalyst. The catalyst is low in raw material cost, high in catalytic activity and good in selectivity,; when the catalyst is used for catalytic synthesis of 3, 5-dichloroaniline, no dechlorinating agent is needed, the raw material conversion rate reaches 100%, and the dechlorinating rate is 0.04% or lower. According to the catalyst prepared by adopting the method disclosed by the invention, active metal particles and a carrier are combined more firmly, are more highly dispersed and more uniform, the catalyst has good selectivity in reaction of catalyzing hydrogenation of 3, 5-dichloronitrobenzene to synthesize 3, 5-dichloroaniline, and the dechlorination rate is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of noble metal catalysts, and in particular relates to a catalyst for synthesizing 3,5-dichloroaniline, a preparation method and application thereof. Background technique [0002] 3,5-Dichloroaniline is an important intermediate of pesticides, medicines, dyes and pigments, and is widely used in the synthesis of medicines, dyes and plant growth promoters. Among them, the increase in the output of cyclic phthalimide agricultural fungicides has made 3,5-dichloroaniline become a trend that the supply exceeds the demand. At present, the synthetic methods of 3,5-dichloroaniline mainly include: [0003] (1) Electrolytic reduction method The electrolytic reduction method has been stuck in the research stage due to the constraints of electrode materials, equipment, cost and other factors, and the process route has not been able to realize industrial production. [0004] (2) Chemical reduction method The chemical re...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J37/02B01J37/16C07C209/36C07C211/52
CPCB01J27/053B01J37/16B01J37/0217C07C209/365B01J35/391B01J35/399C07C211/52Y02P20/584
Inventor 颜攀敦陈丹张洁兰张宇李小安高武李岳锋万克柔曾永康
Owner XIAN CATALYST NEW MATERIALS CO LTD
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