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Ruthenium palladium/carbon catalyst of cyclohexanecarboxylic acid synthesized through benzoic acid hydrogenation and preparation method and application thereof

A cyclohexylformic acid, carbon catalyst technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc. Expensive and other problems, to achieve the effect of simple production and recycling process, lower recycling cost and lower production cost

Inactive Publication Date: 2016-01-20
HIGH TECH RES INST NANJING UNIV LIANYUNGANG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the molten benzoic acid has low reactivity, the process conditions are harsh, and the precious metal Pd is expensive
The disadvantage is that its reaction conversion rate and selectivity are not high. At the same time, supercritical carbon dioxide extraction requires a pressure of 10 MPa. The process is relatively complicated, and the investment and energy consumption are high. The active component of the catalyst, rhodium, is a rare metal and is expensive.
The disadvantage is that the reactivity of nickel is high, but the selectivity is poor, the by-products are many, the separation is difficult, and the active component Pd is expensive
[0006] Looking at the situation at home and abroad, the hydrogenation of benzoic acid to synthesize cyclohexanecarboxylic acid mostly uses noble metals as catalysts, and the metal element Pd is the majority. Although the product has good performance and wide application, it is expensive, so it has not been widely used.
At the same time, due to the high temperature of this type of reaction, the complex process, and the long contact time between the catalyst and the product, it is easy to cause a secondary reaction, resulting in a decrease in reaction selectivity, and the catalyst is prone to oxidation and poisoning, resulting in a decrease in reactivity and reducing the number of times the catalyst is used. Therefore, it is necessary to develop New Hydrogenation Catalyst and Synthetic Technology

Method used

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  • Ruthenium palladium/carbon catalyst of cyclohexanecarboxylic acid synthesized through benzoic acid hydrogenation and preparation method and application thereof
  • Ruthenium palladium/carbon catalyst of cyclohexanecarboxylic acid synthesized through benzoic acid hydrogenation and preparation method and application thereof

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Experimental program
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Effect test

preparation example Construction

[0027] Preparation of ruthenium palladium / carbon catalyst:

[0028] Step 1, preparation of carbon material, mix potato powder, resorcinol, zinc chloride and water evenly, heat, then hydrolyze and polymerize at 95-100°C for 24-36h, take out the mixture and dry at 200-250°C after the reaction is completed 2 -8h, then carbonize at 500-700°C for 10-15h, then wash the carbonized solid product until it is free of chloride ions and then dry it;

[0029] Step 2, prepare soluble ruthenium salt and palladium salt solution, and then impregnate the carbon material with ruthenium salt and palladium salt solution respectively by vacuum equivalent impregnation method, impregnate for 2-10 hours, and then dry at 80°C-150°C for 2-8h Obtain ruthenium palladium / carbon catalyst precursor;

[0030] Step 3, adding NaOH solution to the ruthenium palladium / carbon catalyst precursor obtained in step 2, adjusting the pH to 9-13, precipitating for 0.5-6h and standing for 0.5-3h;

[0031] In step 4, for...

Embodiment 1

[0037] Preparation of ruthenium palladium / carbon catalyst:

[0038] Step 1, the preparation of carbon materials, mix 20g of potato powder, 5g of resorcinol, 65g of zinc chloride and water evenly and put them in an oil bath at 96°C for hydrolysis polymerization. After reacting for 30h, take out the mixture and put it in an oven at 220°C Dry in medium temperature for 8 hours, then transfer to a carbonization furnace for 12 hours at a constant temperature of 650°C, and finally wash the obtained solid product until there is no chloride ion, dry it for use, and the specific surface area of ​​the prepared carbon carrier is 1460m 2 / g, the most probable pore diameter is 7.8nm;

[0039] Step 2, prepare 3 mol / L ruthenium chloride solution and 1.0 mol / L palladium chloride solution respectively according to 5.0% ruthenium load and 0.5% palladium load of active components;

[0040] Step 3, take 5g of carbon material, impregnate the prepared ruthenium and palladium solutions respectively ...

Embodiment 2

[0046] Preparation of ruthenium palladium / carbon catalyst:

[0047] Step 1, preparation of carbon material, mix 20g of potato flour, 5g of resorcinol, 65g of zinc chloride and water evenly, then place in an oil bath at 95°C for hydrolysis polymerization, and take out the mixture after reacting for 36h in an oven at 200°C Dry in medium temperature for 8 hours, then transfer to a carbonization furnace for 10 hours of constant temperature carbonization at 700°C, and finally wash the obtained solid product until there is no chloride ion, dry it for use, and the specific surface area of ​​the prepared carbon carrier is 1580m 2 / g, the most probable pore diameter is 7.2nm;

[0048] Step 2, configure 3mol / L ruthenium acetate solution and 1.0mol / L palladium acetate solution respectively according to active component ruthenium loading 5.0% and palladium loading 0.1%;

[0049] Step 3, take 5g of carbon material, impregnate the prepared ruthenium and palladium solutions respectively by ...

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Abstract

The invention discloses a ruthenium palladium / carbon catalyst of cyclohexanecarboxylic acid synthesized through benzoic acid hydrogenation. The catalyst comprises a carbon material carrier, an active component of metal element Ru nanoparticles and an auxiliary of metal element Pd nanoparticles. The loading capacity of the Ru nanoparticles is 0.5-0.8%, and the loading capacity of the Pd nanoparticles is 0.05-2.0%. The invention further discloses a preparation method of the ruthenium palladium / carbon catalyst. Firstly, the carbon material carrier is prepared, then the active component ruthenium and the auxiliary palladium are loaded, a catalyst precursor is obtained, and finally the catalyst precursor is dried and reduced. The catalyst avoids use of a large amount of palladium, has high reaction activity, selectivity and stability, can be used circularly and remarkably reduces production cost. The catalyst is used for synthesizing cyclohexanecarboxylic acid through benzoic acid catalytic hydrogenation. The raw material conversion rate is 100%, the purity of a target product can be higher than 99.5%, process conditions are moderate, equipment is simple, three wastes are not emitted, and industrialization is easily achieved.

Description

technical field [0001] The invention relates to a high-activity and high-stability ruthenium-palladium / carbon catalyst for synthesizing cyclohexyl formic acid by hydrogenation of benzoic acid and its preparation method and application, belonging to the technical field of catalytic hydrogenation. Background technique [0002] Cyclohexylcarboxylic acid is an important intermediate in organic synthesis. It is a good photocuring agent and can be used in the synthesis of anti-pregnancy 392 and the new drug praziquantel for the treatment of schistosomiasis. Its derivatives such as methyl cyclohexanoate, trans 1-4-Isopropylcyclohexanecarboxylic acid is an important intermediate in the synthesis of many chemical products and medicines. [0003] CN101092349A discloses a kind of hydrogenation method of benzoic acid, and its process is: under the existence of Pd / C catalyzer and Ru / C auxiliary agent, the benzoic acid of melting and hydrogen carry out hydrogenation reaction in reactor, t...

Claims

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Application Information

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IPC IPC(8): B01J23/46C07C61/08C07C51/36
Inventor 江笑宋金文臧涵朱小方陈林周华兰
Owner HIGH TECH RES INST NANJING UNIV LIANYUNGANG
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