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Toluene oxidation catalyst and preparation method thereof

An oxidation catalyst, toluene technology, applied in catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of uneconomical industrial production, high reaction temperature and difficult product separation and other problems, to achieve the effects of easy separation and purification, enhanced interaction, and high toluene conversion.

Inactive Publication Date: 2017-12-22
YANTAI ZHIBEN INTPROP OPERATIONS MANAGEMENT CO LTD
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  • Description
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Problems solved by technology

[0005] The direct oxidation of toluene to generate benzaldehyde under gas phase or liquid phase conditions is a relatively economical and environmentally friendly method. Chinese patent CN1068755 discloses a method for preparing benzaldehyde by gas phase oxidation of toluene. The selectivity of benzaldehyde prepared by this method reaches 60%, and the one-way yield of benzaldehyde can reach 16%. The method of direct oxidation of toluene through the gas phase method mainly has the defects of high reaction temperature and easy over-oxidation of toluene, and the selectivity of benzaldehyde decreases especially when the conversion rate is increased.
There are many reports about the direct oxidation of benzaldehyde under liquid phase conditions. As early as 2004, the Chinese patent No. CN1528726 disclosed a method of preparing benzene by liquid phase oxidation of toluene in an acidic or neutral ionic liquid and acetic acid mixed solvent. The method of formaldehyde is to oxidize toluene under the condition of 115~120 ℃. When the conversion rate of toluene is 42%, the selectivity of benzaldehyde is only 48%. This method uses a large number of expensive ionic liquid and acetic acid solvent, which greatly improves the production cost, and product separation is difficult, and industrial production is uneconomical. The patent CN02143361.5 of Dalian Institute of Chemical Physics discloses a preparation method for a catalyst for the oxidation of toluene to benzaldehyde. The active components of the catalyst are zirconium and other transition metals and alkali metals Or alkaline earth metal etc., use this catalyzer, at temperature 180-195 ℃, feed oxygen, react under the condition of pressure 0.8-1.2MPa, when toluene conversion rate is 13%, the selectivity of benzaldehyde is 86.6%, this method catalyst The preparation process is relatively complicated, and the oxidation is not easy to control in the aldehyde stage, and it is easier to generate benzoic acid
[0006] In summary, there is not yet a method for the production of benzaldehyde with simple reaction, energy saving and environmental protection, easy separation and recovery of product and solvent, high toluene conversion rate and benzaldehyde selectivity in the reaction

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  • Toluene oxidation catalyst and preparation method thereof
  • Toluene oxidation catalyst and preparation method thereof
  • Toluene oxidation catalyst and preparation method thereof

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Embodiment 1

[0025] A catalyst for direct oxidation of toluene to produce benzaldehyde, comprising the following components: 85wt% zinc oxide-alumina composite oxide carrier, wherein the molar ratio of zinc oxide to aluminum oxide is 1, 10wt% cerium, 2wt% vanadium, and 2wt% tin , Copper 1wt%.

[0026] The preparation method of above-mentioned catalyst comprises the steps:

[0027] 1) Weigh 150gAl(NO 3 ) 3 9H 2 O and 59.4gZn(NO 3 ) 2 ·6H 2 O was dissolved in 1200 mL of deionized water to make a total concentration of 0.5 mol L -1 Mixed salt solution, weigh 80g NaOH and dissolve in 400ml deionized water to prepare 5mol L -1 Add the NaOH solution drop by drop to the mixed salt solution under stirring conditions, keep the pH value of the system at 9-10 during the dropwise addition, continue stirring and aging for 3 hours after the NaOH solution is added dropwise, and the obtained product Filter, wash with deionized water repeatedly 3 times, place in a constant temperature drying oven a...

Embodiment 2

[0031] A catalyst for the direct oxidation of toluene to produce benzaldehyde, comprising the following components: 90wt% zinc oxide-alumina composite oxide carrier, wherein the molar ratio of zinc oxide to aluminum oxide is 1, cerium 5wt%, vanadium 2wt%, tin 0.1wt% %, copper 2.9wt%.

[0032] The preparation method of above-mentioned catalyst comprises the steps:

[0033] 1) Weigh 150gAl(NO 3 ) 3 9H 2 O and 59.4gZn(NO 3 ) 2 ·6H 2 O was dissolved in 1200 mL of deionized water to make a total concentration of 0.5 mol L -1 Mixed salt solution, weigh 80g NaOH and dissolve in 400ml deionized water to prepare 5mol L -1 Add the NaOH solution drop by drop to the mixed salt solution under stirring conditions, keep the pH value of the system at 9-10 during the dropwise addition, continue stirring and aging for 3 hours after the NaOH solution is added dropwise, and the obtained product Filter, wash with deionized water repeatedly 3 times, place in a constant temperature drying ov...

Embodiment 3

[0037] A catalyst for the direct oxidation of toluene to produce benzaldehyde, comprising the following components: 85wt% zinc oxide-alumina composite oxide carrier, wherein the molar ratio of magnesium oxide to aluminum oxide is 2, 0.5wt% cerium, 6wt% vanadium, and 5wt% tin %, copper 3.5wt%.

[0038] The preparation method of above-mentioned catalyst comprises the steps:

[0039] 1) Weigh 39.9gAlCl 3 and 40.8gZnCl 2 Dissolve in 1200mL deionized water to make a total concentration of 0.5mol L -1 Mixed salt solution, weigh 80g NaOH and dissolve in 400ml deionized water to prepare 5mol L -1 Add the NaOH solution drop by drop to the mixed salt solution under stirring conditions, keep the pH value of the system at 9-10 during the dropwise addition, continue stirring and aging for 3 hours after the NaOH solution is added dropwise, and the obtained product Filter, wash with deionized water repeatedly 3 times, place in a constant temperature drying oven at 100°C and dry, after dr...

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Abstract

The invention relates to a toluene oxidation catalyst and a preparation method thereof. The toluene oxidation catalyst comprises the following components: 85-90wt% of zinc oxide and aluminum oxide compounded oxide carrier, 0.5-10wt% of cerium, 2-6wt% of vanadium, 0.1-5wt% of tin and 1-3.5wt% of copper, wherein the mole ratio of zinc oxide to aluminum oxide is 1-2. The toluene oxidation catalyst provided by the invention takes the mixture of zinc oxide and aluminum oxide as a carrier; the catalyst has high methylbenzene conversion rate, benzaldehyde selectivity and reaction stability, excellent performance and mild reaction condition; the catalyst exits in the two phases of reactant and product and can be easily separated and purified.

Description

technical field [0001] This application is a divisional application for an invention patent application with the application number 201510465739.4, the application date is July 31, 2015, and the title is "a catalyst for direct oxidation of toluene and its preparation method". [0002] The invention relates to a catalyst, in particular to a catalyst for directly oxidizing toluene to produce benzaldehyde and a preparation method thereof, belonging to the technical field of industrial catalysis. Background technique [0003] Benzaldehyde is an important fine chemical product, which is widely used in industrial fields such as medicine, dyestuff, fragrance, pesticide and materials. The present disclosed production method of preparing benzaldehyde mainly contains following three kinds: toluene chlorination hydrolysis method, benzoic acid (ester) reduction method and toluene direct oxidation method. [0004] Chlorine is inevitably contained in the benzaldehyde produced by chlorina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/847C07C45/36C07C47/54
CPCB01J23/002B01J23/8472B01J37/0201B01J37/08B01J2523/00C07C45/36B01J2523/17B01J2523/43B01J2523/55B01J2523/3712B01J2523/27B01J2523/31C07C47/54
Inventor 姚康治薛静毕新忠
Owner YANTAI ZHIBEN INTPROP OPERATIONS MANAGEMENT CO LTD
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