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Modified compound oxide catalyst, preparing method and use thereof

A technology of composite oxides and catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of insufficient stability of reaction induction period, catalytic activity and selectivity Low-level problems, to achieve the effect of shortening the reaction induction period, improving the effective utilization rate, and shortening the induction period

Inactive Publication Date: 2006-02-01
中国石油化工股份有限公司北京燕山分公司研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN 1 085 115 A proposes a composite oxide catalyst for phenol hydroxylation, especially a loaded composite oxide catalyst. The disadvantages are that the reaction induction period is not stable enough and relatively long, and the catalytic activity and selectivity are low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Prepared with 0.5mol / L Fe(NO 3 ) 3 , 0.25mol / L Cu(NO 3 )2 , 0.02moL / LSnCl 2 and 0.03mol / L Zn(NO 3 ) 2 A total of 5000ml of the mixed metal salt solution is ready for use.

[0047] Take 42.8ml of the above-mentioned mixed metal salt aqueous solution, add 171.2ml of deionized water, add 4g of pseudo-boehmite, stir evenly, drop in a 1mol / L NaOH aqueous solution until the precipitation is complete, stir and age for 120 minutes, filter, and wash with water 4 times, dried at 105°C for 2 hours, then roasted at 550°C for 6 hours, then exchanged twice with 100ml of ammonium sulfate aqueous solution with a concentration of 0.1mol / L, the exchange time was 4 hours, the exchange temperature was 80°C, and then heated at 105 ℃ drying for 2 hours, and 550 ℃ calcining for 6 hours to obtain the modified composite oxide catalyst A.

Embodiment 2

[0049] Prepared with 0.4mol / L Fe(NO 3 ) 3 , 0.1mol / L Mg(NO 3 ) 2 , 0.1mol / LCu(NO 3 ) 2 , 0.08mol / L SnCl 2 and 0.04mol / L Zn(NO 3 ) 2 A total of 2000ml of the mixed metal salt solution is ready for use.

[0050] Take 42.8ml of the above-mentioned mixed metal salt aqueous solution, add 171.2ml of deionized water, add 4g of carrier aluminum hydroxide, stir evenly, drop in a NaOH aqueous solution with a concentration of 1mol / L until the precipitation is complete, stir and age for 120 minutes, filter and wash Dry at 105°C for 2 hours, then roast at 550°C for 6 hours, then exchange with 100ml of 0.1mol / L ammonium chloride aqueous solution for 3 times, the exchange time is 4 hours, the exchange temperature is 80°C, and then dry at 105°C Calcined at 550°C for 2 hours for 6 hours to obtain Modified Composite Oxide Catalyst B.

Embodiment 3

[0052] Take 42.8ml of the aqueous solution of the mixed metal salt prepared in Example 1, add 171.2ml of deionized water, add 4g of γ-alumina, stir evenly, drop in a NaOH aqueous solution with a concentration of 1mol / L until the precipitation is complete, stir and age for 120 minutes, After filtering and washing, dry at 105°C for 2 hours, then roast at 550°C for 6 hours, then exchange twice with 100ml 0.1mol / L ammonium dihydrogen phosphate aqueous solution, the exchange time is 6 hours, the exchange temperature is 70°C, and then at 105 ℃ for 2 hours, and 550 ℃ for 6 hours to obtain the modified composite oxide catalyst C.

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Abstract

A modified composite oxide catalyst for hydroxylating the phenol to obtain phenyldiol, its preparing process and its usage are disclosed. Its preparing process features that the composite oxide catalyst is washed and exchanged by the solution of modifying anion chosen from halogen anion, SO4 anion and PO4 anion. Its advantages are high selectivity and short and stable inducing period.

Description

technical field [0001] The invention relates to a modified composite oxide catalyst for phenol hydroxylation to synthesize catechol and hydroquinone, its preparation method and its application. Background technique [0002] Phenol hydroxylation is the main method for preparing catechol and hydroquinone. US 4 410 501 and GB 2 116 974 use a titanium-containing heteroatom molecular sieve catalyst, use water or acetone as a solvent, and use an aqueous hydrogen peroxide solution with a mass concentration of 30% as an oxidant, phenol / hydrogen peroxide (molar ratio)=3, phenol conversion The efficiency is 25%, the diphenol selectivity is 90%, and the hydrogen peroxide utilization rate is 75%, but the reaction pore diameter of the catalyst is small (<0.7nm), the reactants and products are not easy to diffuse, the reaction speed is slow, and the catalyst synthesis The process is complicated, expensive, and the production cost is high. [0003] Yu Jianfeng et al. (Chemical Journal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/70B01J27/053B01J27/08B01J27/16C07C39/08C07C37/62
Inventor 张信芳张敬畅杨晓嫒
Owner 中国石油化工股份有限公司北京燕山分公司研究院
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