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Preparation method of high-activity anti-sulfur-poisoning palladium carbon catalyst

A palladium-carbon catalyst and sulfur poisoning technology, which is applied in the preparation of organic compounds, preparation of amino compounds, chemical instruments and methods, etc., can solve the problems that the reaction performance cannot be fully exerted, and achieve good practical value, strong sulfur poisoning ability, high The effect of catalytic performance

Inactive Publication Date: 2019-02-12
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still many defects in the current palladium carbon catalysts, which are usually affected by physical parameters such as the surface chemical properties, specific surface area, and pore structure of the product, so that the reaction performance cannot be fully exerted.

Method used

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  • Preparation method of high-activity anti-sulfur-poisoning palladium carbon catalyst
  • Preparation method of high-activity anti-sulfur-poisoning palladium carbon catalyst
  • Preparation method of high-activity anti-sulfur-poisoning palladium carbon catalyst

Examples

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Effect test

Embodiment 1

[0030] A kind of preparation method of highly active anti-sulfur poisoning palladium carbon catalyst, comprises the following steps:

[0031] Step 1, adding activated carbon to a hydrochloric acid solution with a mass concentration of 2% for cooking for 1 hour, the temperature of the cooking treatment is 80°C, filtering, adding the filtered activated carbon to a nitric acid solution with a mass concentration of 4% for cooking for 1 hour, and cooking The temperature of the solution is 80°C, filtered, washed with pure water until the pH is 6, and acid-treated activated carbon is obtained; the quality of the hydrochloric acid solution is 6 times that of the added activated carbon; the quality of the nitric acid solution is 6 times that of the activated carbon added to the hydrochloric acid solution 6 times the mass;

[0032] Step 2, the acid-treated activated carbon described in step 1 is added in the modifier solution, stirred for 10min to obtain slurry; 1%, the modifier is sod...

Embodiment 2

[0038] A kind of preparation method of highly active anti-sulfur poisoning palladium carbon catalyst, comprises the following steps:

[0039]Step 1, adding the activated carbon to the hydrochloric acid solution with a mass concentration of 2% and cooking for 0.5h, the temperature of the cooking treatment is 90°C, filtering, adding the filtered activated carbon to the nitric acid solution with a mass concentration of 4% and cooking for 0.5h, The temperature of the cooking treatment is 90°C, filtered, washed with pure water until the pH is 7, and acid-treated activated carbon is obtained; the quality of the hydrochloric acid solution is 8 times that of the added activated carbon; the quality of the nitric acid solution is 8 times that of the added hydrochloric acid solution. 8 times the mass of activated carbon;

[0040] Step 2, the acid-treated gac described in step 1 is added in the modifier solution, stirred for 20min to obtain a slurry; 5%, the modifier is dodecylbenzenesul...

Embodiment 3

[0045] A kind of preparation method of highly active anti-sulfur poisoning palladium carbon catalyst, comprises the following steps:

[0046] Step 1, adding the activated carbon to the hydrochloric acid solution with a mass concentration of 2% and cooking for 0.25h, the temperature of the cooking treatment is 100°C, filtering, adding the filtered activated carbon to the nitric acid solution with a mass concentration of 4% and cooking for 0.25h, The temperature of the cooking treatment is 100°C, filtered, washed with pure water until the pH is 8, and acid-treated activated carbon is obtained; the quality of the hydrochloric acid solution is 10 times that of the added activated carbon; the quality of the nitric acid solution is 10 times that of the added hydrochloric acid solution. 10 times the mass of activated carbon;

[0047] Step 2, the acid-treated activated carbon described in step 1 is added in the modifier solution, stirred for 30min to obtain a slurry; the modifier solu...

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Abstract

The invention discloses a preparation method of a high-activity anti-sulfur-poisoning palladium carbon catalyst. The preparation method includes the following steps: step 1, adding activated carbon into hydrochloric acid for cooking, performing filtering, adding solids obtained by filtration into nitric acid for cooking, and performing filtering and washing to obtain the acid-treated activated carbon; step 2, adding the acid-treated activated carbon into a modifier solution, and stirring the solution to obtain paste; step 3, adding the paste into an assistant metal salt solution, and stirringthe solution to obtain an activated carbon solution loaded with assistants; step 4, adding the activated carbon solution loaded with the assistants into a palladium chloride solution, adjusting the pH, stirring the solution to obtain a palladium suspension; step 5, reducing and filtering the palladium suspension, washing solids obtained by filtration, and centrifuging and spin-drying the solids toobtain the high-activity anti-sulfur-poisoning palladium carbon catalyst. The preparation method has the advantages that metal on the carrier surface of the obtained palladium carbon catalyst is highly dispersed, and high catalytic activity and anti-sulfur stability in hydrogenation of nitrobenzyl aniline and ortho-nitrotoluene are achieved.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, and in particular relates to a preparation method of a highly active sulfur-poisoning-resistant palladium-carbon catalyst. Background technique [0002] Palladium carbon catalyst is a new type of material prepared by loading metal palladium on activated carbon. It has the characteristics of small feeding amount, high activity, good selectivity, stable performance, green environmental protection and easy recycling. It is widely used in petrochemical, Pharmaceutical industry, electronics industry, dyes and fragrances industry and other fine chemical hydrogenation reduction process. [0003] Palladium carbon catalyst belongs to supported catalyst, wherein the more commonly used loading method is impregnation method or spray method, and its preparation method includes: carrier activated carbon pretreatment (acid-base treatment, oxidation treatment, etc.), preparation of c...

Claims

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Application Information

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IPC IPC(8): B01J23/63B01J23/89B01J35/10C07C209/00C07C209/36C07C211/46C07C211/47
CPCC07C209/00C07C209/36B01J23/63B01J23/8906B01J23/8913B01J23/892B01J23/894B01J35/61C07C211/46C07C211/47
Inventor 翟康张磊王昭文颜攀敦李岳锋李小虎张涵唐良张力万克柔曾永康
Owner XIAN CATALYST NEW MATERIALS CO LTD
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