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Green oxidation bifunctional catalyst, preparation method and applications thereof

A dual-function catalyst and catalyst technology, which is applied in the field of catalysis, can solve problems such as the inability to solve the problem of engineering implementation of raw materials and prices of supported gold catalysts in the whole process of dark operation, and achieve the effects of green preparation, oxidation inhibition, and high-efficiency preparation

Active Publication Date: 2017-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN104549413A discloses a noble metal Au catalyst with TS-1 as the carrier to form a coupling CO / H 2 O / O 2 Direct H 2 o 2 It is a dual-functional catalyst for the reaction and the reaction of benzene hydroxylation to phenol, and has achieved good experimental results, but it still cannot solve the problems that affect industrial applications such as the necessary full-process dark operation and high raw material prices in the preparation process of supported gold catalysts. implementation issues

Method used

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  • Green oxidation bifunctional catalyst, preparation method and applications thereof
  • Green oxidation bifunctional catalyst, preparation method and applications thereof
  • Green oxidation bifunctional catalyst, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 0.755g Cu(NO 3 ) 2· 9H 2 O with 0.315g AgNO 3 Dissolve in 30ml of deionized water to prepare a solution I with a metal ion concentration of 0.170mol / L; weigh 0.612g of NaBH in an ice-water bath 4 Dissolve 0.064g NaOH in 16ml deionized water, add 4g TS-1 molecular sieve carrier with a silicon-titanium molar ratio of 50, and continue stirring for 0.5h to obtain 1.0mol / L NaBH 4 Solution II of the reducing agent.

[0024] Keep the ice-water bath and stirring conditions, use a peristaltic pump to slowly add solution I to solution II, continue stirring for 0.5h after the addition is completed, and slowly add 0.5mol / L HCl aqueous solution to the excess NaBH 4 Completely decompose, showing that there are no more bubbles; after continuing to stir for 0.5h, high-speed centrifugation, and washing with deionized water until no chlorine ions are detected in the clear solution on the upper layer of the centrifuge tube, the solid is moved to a vacuum drying oven, and it is re...

Embodiment 2

[0026] Take 0.755g Cu(NO 3 ) 2· 9H 2 O with 0.315g AgNO 3 and 0.334g PdCl 2 Dissolve in 30ml of deionized water to prepare a solution I with a metal ion concentration of 0.220mol / L; weigh 0.871g of NaBH in an ice-water bath 4 Dissolve 0.092g NaOH in 23ml of deionized water, add 4g of TS-1 molecular sieve carrier with a silicon-titanium molar ratio of 50, and continue stirring for 0.5h to obtain 1.0mol / L NaBH 4 Solution II of the reducing agent.

[0027] Keep the ice-water bath and stirring conditions, use a peristaltic pump to slowly add solution I to solution II, continue stirring for 0.5h after the addition is completed, and slowly add 0.5mol / L HCl aqueous solution to the excess NaBH 4 Completely decompose, showing that there are no more bubbles; after continuing to stir for 0.5h, high-speed centrifugation, and washing with deionized water until no chlorine ions are detected in the clear solution on the upper layer of the centrifuge tube, the solid is moved to a vacuum ...

Embodiment 3

[0029] Take 0.755g Cu(NO 3 ) 2· 9H 2 O with .315g AgNO 3 and 0.506g RuCl 3· 3H 2 O was dissolved in 30ml deionized water to prepare a solution I with a metal ion concentration of 0.220mol / L; under ice-water bath conditions, weigh 1.003g NaBH 4 Dissolve 0.108g of NaOH in 27ml of deionized water, add 4g of TS-1 molecular sieve carrier with a silicon-titanium molar ratio of 50, and continue stirring for 0.5h to obtain 1.0mol / L NaBH 4 Solution II of the reducing agent.

[0030] Keep the ice-water bath and stirring conditions, use a peristaltic pump to slowly add solution I to solution II, continue stirring for 0.5h after the addition is completed, and slowly add 0.5mol / L HCl aqueous solution to the excess NaBH 4 Completely decompose, showing that there are no more bubbles; after continuing to stir for 0.5h, high-speed centrifugation, and washing with deionized water until no chlorine ions are detected in the clear solution on the upper layer of the centrifuge tube, the solid...

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Abstract

The present invention relates to a green oxidation bifunctional catalyst, a preparation method and applications thereof, and belongs to the technical field of catalysis. In the prior art, the green catalytic oxidation process generally uses H2O2 as the oxidant, or uses the mixed use of the supported Au catalyst, the metal oxide catalyst, the heteroatom molecular sieve and other different types of catalysts, such that the storage and transportation security is low, the catalyst preparation process is cumbersome, the price is high, the non-phenol aromatic hydrocarbon by-product selectivity is high, and the industrial application is difficult. A purpose of the present invention is mainly to solve the problems in the prior art. The technical scheme of the present invention comprises that a green oxidation bifunctional catalyst supported on a TS-1 molecular sieve carrier and containing Cu and at least a second metal selected from Ag, Pd and Ru is prepared by using an in-situ reduction co-precipitation method. With the technical scheme, the problems in the prior art are well solved. The catalyst of the present invention can be used for the coupling process of the in-situ synthesis of H2O2 with CO / H2O / O2 and the benzene hydroxylation reaction so as to achieve the green and efficient preparation of phenol.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a green oxidation dual-function catalyst and its preparation method and application. Background technique [0002] As we all know, phenol is an important bulk organic chemical raw material, and has broad applications in the fields of pharmaceutical intermediates, pesticides, spices, dyes, auxiliaries, and resins. Facing the ever-increasing demand for phenol, the development of a green phenol production process to replace the complicated process, high energy consumption, strong corrosion, and a large amount of low-value acetone by-product or as an important supplement has become an urgent development of scientific research and industry. direction. Among them, H 2 o 2 The reaction of phenol to phenol by hydroxylation of benzene as an oxidant is considered to be a green production process of phenol. Chinese patent CN129961C discloses that acid-treated activated car...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07C39/04C07C37/60C01B15/027
CPCY02P20/52
Inventor 金中豪董静宣东刘苏王仰东
Owner CHINA PETROLEUM & CHEM CORP
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