Method for preparing Pd/C catalyst for one-step-method synthesis of alkyl cyclohexyl anone liquid-crystal intermediates

A catalyst and alkyl ring technology, applied in the field of industrial catalyst preparation, can solve the problems of easy deactivation of the catalyst and low yield of the target product, and achieve the effects of good dispersibility, simplified operation and strong complexing ability

Active Publication Date: 2019-05-17
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the one-step synthesis of alkylcyclohexylcyclohexanone by Pd / C catalyzed alkylcyclohexylphenol still has problems such as low yield of target product and easy deactivation of the catalyst.

Method used

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  • Method for preparing Pd/C catalyst for one-step-method synthesis of alkyl cyclohexyl anone liquid-crystal intermediates
  • Method for preparing Pd/C catalyst for one-step-method synthesis of alkyl cyclohexyl anone liquid-crystal intermediates

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Embodiment 1

[0027] The catalyst of this embodiment comprises Ti-doped modified activated carbon, active component Pd and auxiliary agents, and the auxiliary agents are Zn and Sn; the mass percentage of Pd in ​​the catalyst is 5%, and the mass percentage of Zn is 1.0%, and the mass percentage of Sn is 0.5%.

[0028] The preparation method of catalyst comprises:

[0029] Step 1. Activated carbon pretreatment: Dissolve 35.55g of butyl titanate in a mixed solution of 365mL of absolute ethanol, 80mL of acetylacetone and 20mL of nitric acid, add 95g of activated carbon, stir for 30min, evaporate the solvent to dryness, and age at 25°C for 24h. N at 800°C 2 Protective treatment for 30 minutes to obtain Ti-doped modified activated carbon;

[0030]Step 2, Pd precursor preparation: measure the H2O with a Pd mass concentration of 0.05g / mL 2 PdCl 4 Solution 100mL, add 200mL disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution with a concentration of 0.2mol / L and a pH of 6, then...

Embodiment 2

[0034] The catalyst of this embodiment comprises Ti-doped modified activated carbon, active component Pd and auxiliary agents, and the auxiliary agents are Zn and Sn; the mass percentage of Pd in ​​the catalyst is 5%, and the mass percentage of Zn is 0.3%, and the mass percentage of Sn is 0.05%.

[0035] The preparation method of catalyst comprises:

[0036] Step 1. Activated carbon pretreatment: Dissolve 35.55g of butyl titanate in a mixed solution of 365mL of absolute ethanol, 80mL of acetylacetone and 20mL of nitric acid, add 95g of activated carbon, stir for 30min, evaporate the solvent to dryness, and age at 25°C for 12h. N at 500°C 2 Protective treatment for 2h to obtain Ti-doped modified activated carbon;

[0037] Step 2, Pd precursor preparation: measure the H2O with a Pd mass concentration of 0.05g / mL 2 PdCl 4 Solution 100mL, add 200mL of disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution with a concentration of 0.2mol / L and a pH of 6.4, then ...

Embodiment 3

[0041] The catalyst of this embodiment comprises Ti-doped modified activated carbon, active component Pd and auxiliary agents, and the auxiliary agents are Zn and Sn; the mass percentage of Pd in ​​the catalyst is 5%, and the mass percentage of Zn is 0.8%, and the mass percentage of Sn is 0.4%.

[0042] The preparation method of catalyst comprises:

[0043] Step 1. Activated carbon pretreatment: Dissolve 35.55g of butyl titanate in a mixed solution of 365mL of absolute ethanol, 80mL of acetylacetone and 20mL of nitric acid, add 95g of activated carbon, stir for 30min, evaporate the solvent to dryness, and age at 25°C for 20h. N at 700°C 2 Protective treatment for 30 minutes to obtain Ti-doped modified activated carbon;

[0044] Step 2, Pd precursor preparation: measure the H2O with a Pd mass concentration of 0.05g / mL 2 PdCl 4 Solution 100mL, add 200mL disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution with a concentration of 0.2mol / L and a pH of 6, the...

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Abstract

The invention discloses a method for preparing a Pd / C catalyst for one-step-method synthesis of alkyl cyclohexyl anone liquid-crystal intermediates. The catalyst comprises Ti doped modified activatedcharcoal, an active ingredient Pd and auxiliaries, wherein the auxiliaries comprise Zn and Sn. The preparation method comprises the steps: 1. preparing the Ti doped modified activated charcoal; 2. preparing a Pd active ingredient precursor; 3. adding a stabilizer, a precipitant and a reducer into the Ti doped modified activated charcoal, carrying out pulping with pure water, then, carrying out uniform stirring, dripping the Pd active ingredient precursor, and carrying out uniform stirring, so as to obtain mixed pulp; 4. heating up the mixed pulp, then, carrying out heat-preserving reduction, carrying out cooling, then, adding a ZnCl2 solution and a SnCl2 solution, carrying out stirring, and then, carrying out filtering, thereby obtaining the Pd / C catalyst for one-step-method synthesis of the alkyl cyclohexyl anone liquid-crystal intermediates. The catalyst prepared by the method has good selectivity to alkyl cyclohexyl anone, a reaction system can achieve very good yield without addingNa2CO3 and the like, the operation is simplified, and the cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of industrial catalyst preparation, and in particular relates to a preparation method of a Pd / C catalyst for synthesizing an alkylcyclohexylcyclohexanone liquid crystal intermediate in one step. Background technique [0002] The liquid crystal material synthesized with alkylcyclohexylcyclohexanone as an intermediate has excellent comprehensive properties such as low viscosity, moderate refractive index and wide liquid crystal phase temperature range, and has a very good market prospect. The traditional preparation method of this type of compound is to use Raney Ni as a catalyst to catalyze alkylcyclohexylphenol to generate alkylcyclohexylcyclohexanol, and then use chromium oxides as a catalyst to catalyze the oxidation of alkylcyclohexylcyclohexanol to generate alkyl Cyclohexyl cyclohexanone, a two-step reaction. The method needs to be carried out under harsh conditions of high temperature and high pressure...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/62
Inventor 张鹏闫江梅李岳锋唐良万克柔曾永康张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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