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Catalyst for synthesizing benzaldehyde by carrying out liquid-phase high-selectivity catalytic oxidation on methylbenzene

A catalytic oxidation, high selectivity technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, organic compound preparation, etc., can solve the problem of high reaction temperature, serious environmental pollution, catalyst, Solvent products are difficult to separate, and achieve the effects of high selectivity and yield, easy separation, and mild reaction conditions

Inactive Publication Date: 2013-09-11
NANJING INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although both catalytic systems show high catalytic activity, the high reaction temperature in the gas-phase catalytic oxidation process is prone to deep oxidation, resulting in generally low selectivity of target products.
In terms of liquid-phase catalytic oxidation, the MC catalytic system is relatively mature, but the selectivity of the target product still needs to be improved. At the same time, it is difficult to separate the catalyst, solvent and product, and the environmental pollution is serious, which is not suitable for the development of modern chemical industry; recently Kesavan et al. Science, 2011, 331(6014): 185-199 reported the liquid-phase catalytic oxidation of toluene by activated carbon-supported Au, Pd nano-alloy catalyst (Au-Pd / C) under solvent-free conditions, and found that when n(Au) in the catalyst : When n(Pd)=1:1.85, react 27h under 160 ℃, the conversion rate of toluene is 94.4%, the selectivity of benzyl benzoate can reach 85.5%, but the selectivity of benzaldehyde is only 1.0%, how to optimize the catalysis System to improve the selectivity of benzaldehyde is one of the problems to be solved urgently

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 7.2Kg Mg(NO 3 ) 2 ·6H 2 O, 3.1Kg Ba(NO 3 ) 2 and 7.5Kg Al(NO 3 ) 3 9H 2 O is made into 200L solution with deionized water; 2.1Kg Na 2 CO 3 Make a 200L solution with deionized water, mix the two solutions, stir vigorously at 60°C for 0.5 hours, and add NH 4 OH controls the pH value of the mixed solution to be 8.0. The obtained colloid is filtered or centrifugally dehydrated, washed with water until neutral, dried at 100°C, and placed at 300°C under N 2 Calcined in the atmosphere for 4 hours, the obtained sample was placed in 50L of ammonium fluoride aqueous solution with a percentage concentration of 1%, and 50L of 0.2mol / L CTAB was added thereto, the temperature was controlled at 60°C, and NH 4 OH controls the pH of the mixed solution to be 8.0. After 12 hours, 7.2Kg of Cu(NO 3 ) 2 ·3H 2 O, add 30% H at the same molar number as the ammonium fluoride 2 o 2 Aqueous solution, stirred for 24 hours, the obtained colloid was filtered or centrifugally dehydrated...

Embodiment 2

[0025] 6.1Kg Mg(NO 3 ) 2 ·6H 2 O, 1.4Kg Ca(NO 3 ) 2 4H 2 O and 2.3Kg Al(NO 3 ) 3 9H 2 O was made into 7.2L solution with deionized water; 0.6Kg Na 2 CO 3 Make 7.2L solution with deionized water, mix the two solutions, stir vigorously at 60°C for 0.5 hours, and add NH 4 OH controls the pH value of the mixed solution to be 11.5. The obtained colloid is filtered or centrifugally dehydrated, washed with water until neutral, dried at 100°C, and placed at 700°C under N 2 Calcined in the atmosphere for 4 hours, the obtained sample was placed in 50L of ammonium fluoride aqueous solution with a percentage concentration of 10%, and 50L of 0.2mol / L CTAB was added thereto, the temperature was controlled at 60°C, and NH 4 OH controls the pH value of the mixed solution to be 11.5. After 12 hours, add 0.87Kg of Cu(NO 3 ) 2 ·6H 2 O and 1.0Kg of Fe(NO 3 ) 2 ·6H 2 O, add 30% H at the same molar number as the ammonium fluoride 2 o 2 Aqueous solution, stirred for 24 hours, the ...

Embodiment 3

[0027] 6.1Kg Mg(NO 3 ) 2 ·6H 2 O, 1.6Kg Ba(NO 3 ) 2 and 3.8Kg Al(NO 3 ) 3 9H 2 O was made into 40L solution with deionized water; 1.1Kg Na 2 CO 3 Make a 40L solution with deionized water, mix the two solutions, stir vigorously at 60°C for 0.5 hours, and add NH 4 OH controls the pH of the mixed solution to be 10.0. The obtained colloid is filtered or centrifugally dehydrated, washed with water until neutral, dried at 100°C, and placed at 500°C under N 2 Calcined in the atmosphere for 4 hours, the obtained sample was placed in 50L of 3.0% ammonium bromide aqueous solution, and 50L of 0.2mol / L TritonX-10 was added therein, the temperature was controlled at 80°C, and NH 4 The OH control mixed solution pH value is 10.0. After 12 hours, add 1.4Kg of Cr (NO 3 ) 2 9H 2 O and 1.0Kg of V(NO 3 ) 2 ·6H 2 O, add 30% H at the same molarity as ammonium bromide 2 o 2 Aqueous solution, stirred for 12 hours, the obtained colloid was filtered or centrifugally dehydrated, dried ...

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Abstract

The invention discloses a novel catalyst for carrying out liquid-phase high-selectivity catalytic oxidation on methylbenzene. The catalyst mainly takes an alkaline-earth metal composite oxide with high temperature stability as a carrier and metals (V, Cr, Mn, Fe, Co, Ni, Cu, Au, Pd and Pt) with high activity as catalytic oxidation active centers. The prepared catalyst shows high selectivity and activity in liquid-phase oxidation of methylbenzene. Under the conditions that the reaction temperature is 90-160 DEG C, the reaction time is 2-48 hours and the pressure of air or oxygen is 0.5-2.0MPa, the highest selectivity of benzaldehyde can be 94.0% and the highest conversion rate of methylbenzene also reaches 45.0%. Compared with the reported results, the prepared catalyst has the advantages that the catalyst still has good mesoporous structure under high temperature; in the catalysis process, the conversion rate of methylbenzene and the yield of benzaldehyde are high; and meanwhile, any solvent or organic additive is not added to a reaction system and the catalyst has the advantages of high yield, low cost, no environmental pollution, easy separation, good repeatability and the like.

Description

technical field [0001] The invention relates to a novel catalyst for producing benzaldehyde by liquid-phase highly selective oxidation of toluene and a preparation method thereof. Background technique [0002] Volatile organic compounds (VOCs) are one of the common exhaust gases, mainly from petrochemical, paint production, metal coating, printing and varnish and other production fields. Volatilizing into the atmosphere will not only pollute the environment, but also endanger human health. If VOCs are converted into useful chemical products or chemical intermediates, it can not only reduce the discharge of waste, but also turn waste into treasure and improve economic benefits. Toluene, one of the most harmful and polluting VOCs members, can be oxidized to produce benzyl alcohol, benzaldehyde, benzoic acid, benzyl benzoate, etc. These products are widely used as general intermediates in dyes, solvents, fragrances, Plasticizers, dyes, preservatives, flame retardants and other...

Claims

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Application Information

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IPC IPC(8): B01J23/78B01J23/26B01J23/889B01J23/58B01J23/66C07C47/54C07C45/36
Inventor 王晓丽吴功德丁克强张方刘献锋孙雯郑鹏飞
Owner NANJING INST OF TECH
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