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Method for catalytic reduction of bromo-sartan biphenyl waste residue by halogen-modified Pd/C catalyst

A technology of bromosartan biphenyl and catalyst, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry and other directions, can solve the problems of high toxicity of lead acetate, poor catalyst stability and the like

Pending Publication Date: 2022-05-13
山东艾孚特科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] CN104876836B discloses a method for preparing bromosartan biphenyl by using bromosartan biphenyl waste residue, the bromosartan biphenyl waste residue with lead acetate as inhibitor is directly converted into 2-cyano-4'-bromomethyl Biphenyl, but the lead acetate used is highly toxic and has poor catalyst stability
[0004] CN102659626B discloses a method for reducing bromosartan biphenyl waste residue. Under the action of Raney nickel catalyst, hydrogenation reaction is carried out to bromosartan biphenyl waste residue to obtain sartan biphenyl, although the price of the catalyst is relatively low , but requires further bromination to obtain bromosartan biphenyl

Method used

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  • Method for catalytic reduction of bromo-sartan biphenyl waste residue by halogen-modified Pd/C catalyst
  • Method for catalytic reduction of bromo-sartan biphenyl waste residue by halogen-modified Pd/C catalyst

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Effect test

Embodiment 1

[0023] The method for catalytic reduction of brominated sartan biphenyl waste residue by the Pd / C catalyst modified by bromine comprises the following steps:

[0024] (1) Preparation of bromine-modified Pd / C catalyst: Add 5gPd to a 200ml reaction flask with a loading capacity of 10% Pd / C catalyst, 50ml of an aqueous solution containing 0.01mol / L sodium bromide, stir at 30°C for 1h, and then Filter, wash the filter cake with water, and dry in a vacuum oven at 80°C for 12 hours to obtain a bromine-modified Pd / C catalyst, characterized by ICP, the content of Br based on Pd is 0.3mol%;

[0025] (2) Add 50g of bromosartan biphenyl waste residue (the percentage of 2-cyano-4'-dibromomethylbiphenyl is 94%), 100g of 1,2-dichloroethane to the 500ml reactor , water 50g, sodium hydroxide 6g, and bromine-modified Pd / C catalyst 0.5g; Replace the air in the reactor with nitrogen for three times, and then charge the hydrogen of 01MPa;

[0026] (3) Raise the temperature of the reactor to 80°C...

Embodiment 2

[0029] The method for catalytic reduction of brominated sartan biphenyl waste residue by the Pd / C catalyst modified by bromine comprises the following steps:

[0030] (1) Prepare bromine-modified Pd / C catalyst: add 5gPd to a 200ml reaction flask with a loading capacity of 10% Pd / C catalyst, 50ml of an aqueous solution containing 0.05mol / L sodium bromide, stir at 30°C for 1h, and then Filter, wash the filter cake with water, and dry in a vacuum oven at 80° C. for 12 hours to obtain a bromine-modified Pd / C catalyst, characterized by ICP, with a Br content of 0.5 mol% based on Pd;

[0031] (2) Add 50g of bromosartan biphenyl waste residue (the percentage of 2-cyano-4'-dibromomethylbiphenyl is 87%) and 100g of 1,2-dichloroethane to the 500ml reactor , water 50g, sodium hydroxide 6g, and bromine-modified Pd / C catalyst 0.5g; Replace the air in the reactor with nitrogen for three times, and then charge the hydrogen of 01MPa;

[0032] (3) Raise the temperature of the reactor to 80°C,...

Embodiment 3

[0035] The method for catalytic reduction of bromosartan biphenyl waste residue by the Pd / C catalyst modified by described iodine may further comprise the steps:

[0036] (1) Preparation of iodine-modified Pd / C catalyst: Add 5gPd to a 200ml reaction flask with a loading capacity of 10% Pd / C catalyst, 50ml of an aqueous solution containing 0.01mol / L sodium iodide, stir at 30°C for 1h, and then Filter, wash the filter cake with water, and dry at 80° C. for 12 h in a vacuum oven to obtain an iodine-modified Pd / C catalyst, which is characterized by ICP, and the content of I based on Pd is 0.5 mol%;

[0037] (2) Add 50g of bromosartan biphenyl waste residue (the percentage of 2-cyano-4'-dibromomethylbiphenyl is 82%), 100g of 1,2-dichloroethane to the 500ml reactor , water 50g, sodium hydroxide 6g, and iodine-modified Pd / C catalyst 0.5g; Replace the air in the reactor with nitrogen for three times, and then charge the hydrogen of 0.1MPa;

[0038] (3) Raise the temperature of the re...

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Abstract

The invention belongs to the technical field of catalytic reduction of bromo-sartan biphenyl waste residues, and particularly relates to a method for catalytic reduction of bromo-sartan biphenyl waste residues through a halogen-modified Pd / C catalyst. The method for reducing the bromo-sartan biphenyl waste residues comprises the steps that firstly, a halogen-modified Pd / C catalyst is prepared, then alkali, the halogen-modified Pd / C catalyst, an organic solvent and water are added into the bromo-sartan biphenyl waste residues, hydrogen is introduced, a heating reaction is conducted, reaction liquid is filtered, the solid halogen-modified Pd / C catalyst is filtered out, and the solid halogen-modified Pd / C catalyst is directly used for the next round of reaction after being washed with water; and carrying out rotary evaporation on the reaction liquid to remove the organic solvent to obtain a mixture of 2-cyano-4 '-bromomethyl biphenyl and sartan biphenyl, and carrying out recrystallization separation to obtain 2-cyano-4'-bromomethyl biphenyl. According to the method for catalytically reducing the bromo-sartan biphenyl waste residues by using the halogen-modified Pd / C catalyst, the yield of the recycled 2-cyano-4 '-bromomethyl biphenyl is high, and the utilization rate of the catalyst is high.

Description

technical field [0001] The invention belongs to the technical field of catalytic reduction of bromosartan biphenyl waste residue, and in particular relates to a method for catalytic reduction of bromosartan biphenyl waste residue by a halogen-modified Pd / C catalyst. Background technique [0002] Bromosartan biphenyl, that is, 2-cyano-4'-bromomethyl biphenyl, bromination of sartan biphenyl is an important method for preparing bromosartan biphenyl, but dibromobiphenyl will be generated during the reaction process Sartan biphenyl forms waste residue, which puts a lot of pressure on environmental protection. In the conversion and utilization of waste residue, people have made a lot of efforts. Among them, the process of using metal as catalyst and hydrogen as reducing agent is quite popular. This is because hydrogen is a green reducing agent and will not introduce new by-products. In the process of reductive debromination of waste slag, halogen salts will be generated. Since h...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C253/34C07C255/50B01J27/13
CPCC07C253/30C07C253/34B01J27/13C07C255/50Y02P20/584
Inventor 周倜王立芹张晓谦刘继凯岳峰相浩龙董翠翠张新一李继宾唐凯周兴波王海波夏明莹宋浩张丹丹周红财卞伟丽步长江焦研秦瑞昌刘正顺马海瑞吴士峰
Owner 山东艾孚特科技有限公司