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A kind of catalyst for synthesizing 3,5-dichloroaniline and its preparation method and application

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

Active Publication Date: 2022-07-05
XIAN CATALYST NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of catalyst for synthesizing 3,5-dichloroaniline and its preparation method and application

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Experimental program
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Embodiment 1

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

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

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

[0033] Step 2, mixing and beatin...

Embodiment 2

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

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

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

[0039] Step 2, mixing...

Embodiment 3

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

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

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

[0045] Step 2, mixin...

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Abstract

The invention discloses a catalyst for synthesizing 3,5-dichloroaniline, comprising a barium sulfate carrier, Pd and an auxiliary metal, wherein the auxiliary metal is Mn, Fe, Co, Cu or Zn. In addition, the present invention also provides a preparation method of the catalyst and a method for catalyzing the hydrogenation of 3,5-dichloronitrobenzene to synthesize 3,5-dichloroaniline by using the catalyst. The catalyst of the invention has low raw material cost, high catalytic activity and good selectivity, and when used for catalyzing synthesis of 3,5-dichloroaniline, no dechlorination agent is required, the conversion rate of the raw material reaches 100%, and the dechlorination rate is below 0.04% . The catalyst prepared by the method of the present invention has stronger binding between the active metal particles and the carrier, and is more highly dispersed and uniform, and has good performance in catalyzing the hydrogenation of 3,5-dichloronitrobenzene to synthesize 3,5-dichloroaniline. selectivity, greatly reducing the dechlorination rate.

Description

technical field [0001] The invention belongs to the technical field of precious metal catalysts, and in particular relates to a catalyst for synthesizing 3,5-dichloroaniline and 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 production of cyclophthalimide agricultural fungicides has made 3,5-dichloroaniline become a trend in short supply. At present, the synthetic method of 3,5-dichloroaniline mainly includes: [0003] (1) Electrolytic reduction method Electrolytic reduction method has been in the research stage due to the constraints of electrode materials, equipment, cost and other factors, and this process route has not been able to achieve industrial production. [0004] (2) Chemical reduction method The chemical reduction method of ir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053B01J37/02B01J37/16C07C209/36C07C211/52
CPCB01J27/053B01J37/16B01J37/0217B01J35/0046B01J35/0093C07C209/365C07C211/52Y02P20/584
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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