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Toluene liquid-phase selective oxidation catalyst and preparation method thereof

A selective oxidation and catalyst technology, which is applied in catalyst activation/preparation, physical/chemical process catalysts, hydrocarbon oxidation to prepare oxygenated compounds, etc., can solve the problems of low toluene conversion, decomposition at elevated reaction temperature, and low toluene concentration, etc. To achieve the effect of rational utilization of resources and high conversion rate

Inactive Publication Date: 2011-02-16
NORTHWEST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main defect of this method is: the conversion rate of toluene is low, and the concentration of toluene in the reaction tail gas is relatively low, thus makes the recycling of toluene difficult; Benzoic acid is main product and the yield of benzaldehyde and benzyl alcohol is very low, and produces considerable deep oxidation product
When the amount of vanadium acetate was 0.1 mmol, the conversion of toluene was the highest (19.8%); when the amount of vanadium acetate was 0.03 mmol, the selectivity of benzaldehyde was the highest (72.8%); with the increase of reaction temperature, the conversion of toluene and The selectivity of benzaldehyde increases; at 363 K, the conversion rate of toluene is the highest (15.4%), and at the same time, the selectivity of benzaldehyde is also the highest (63%). Continue to increase the reaction temperature to decompose hydrogen peroxide, resulting in the yield of benzaldehyde reduce

Method used

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  • Toluene liquid-phase selective oxidation catalyst and preparation method thereof
  • Toluene liquid-phase selective oxidation catalyst and preparation method thereof
  • Toluene liquid-phase selective oxidation catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1-6

[0049] Embodiment 1-6 illustrates, selects different transition metal element Me, adopts co-precipitation method, the transition metal vanadate catalyst (Me) prepared under different conditions x V y O) and its catalytic performance for liquid-phase selective oxidation of toluene. The preparation method of each catalyst is as follows: (1) determine Me x V y The molar ratio of Me / V in the O catalyst is 1 / 1; accordingly, the corresponding soluble metal salt is weighed; and it is just dissolved with an appropriate amount of deionized water to obtain a clear solution. (2) Under the condition of rapid stirring, mix the above-mentioned aqueous solutions of Me and V, and use nitric acid solution (concentration: 1 mol / liter) to adjust the pH value of the mixed solution to keep the mixed solution in a clear state. (3) Slowly add 25% (mass) ammonia solution dropwise to the rapidly stirred above mixture, and stir while adding until the precipitation is complete. Then, under the condi...

Embodiment 7-9

[0054] Examples 7-9 illustrate the preparation of Ni-V-O catalysts under different conditions by co-precipitation method and their catalytic performance when used in the liquid-phase selective oxidation of toluene. The preparation method of each catalyst is as follows: (1) determine Me x V y The molar ratio of Me / V in the O catalyst is 1 / 2, 1 / 1 and 2 / 1; accordingly, the corresponding soluble metal salt is weighed; and it is just dissolved with an appropriate amount of deionized water to obtain a clear solution. (2) Under the condition of rapid stirring, mix the above-mentioned aqueous solutions of Me and V, and use nitric acid solution (concentration: 1 mol / liter) to adjust the pH value of the mixed solution to keep the mixed solution in a clear state. (3) Slowly add 25% (mass) ammonia solution dropwise to the rapidly stirred above mixture, and stir while adding until the precipitation is complete. Then, under the conditions of pH value of 11 and room temperature, static agi...

Embodiment 10-12

[0059] Examples 10-12 illustrate the Co-V-O catalysts prepared under different conditions by using the sol-gel method and their catalytic performance when used in the liquid-phase selective oxidation of toluene. The preparation method of the catalyst is as follows: under the condition of rapid stirring, according to the distribution ratio of the catalyst components, a certain amount of soluble vanadium salt aqueous solution and soluble Me metal salt aqueous solution are mixed, and the pH value is adjusted so that the mixed solution remains in a solution state. Next, under the condition of rapid stirring, an appropriate amount of surfactant or organic high polymer is added to the above mixed liquid, and stirred while adding, until a viscous colloid is formed. Then, the colloid is statically aged for 4-12 hours. Finally, the colloid was filtered and washed to obtain a solid product. Solid product at 110-150 o C dry for 4-8 hours at 550-850 o C is calcined for 4-8 hours to obt...

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Abstract

The invention discloses a toluene liquid-phase selective oxidation catalyst and a preparation method thereof. The catalyst is transition metal or rare earth vanadate which has the composition shown by MexVyO, wherein Me is one of transition metals of VIB, VIIB or VIIIB group; V is vanadium; and the molar ratio x / y of Me to V is 0.1 to 10. The catalyst provided by the invention can be used for toluene liquid-phase oxidation reaction, the conversion rate of the toluene is high and the main product is benzaldehyde; by changing the composition and modulating reaction conditions of the catalyst, the proportion of the benzaldehyde to benzoic acid in the product can be changed; the catalyst does not pollute equipment and environment; and a solved used in the reaction can be recovered and rational resource utilization is basically realized.

Description

technical field [0001] The invention relates to a catalyst for producing benzaldehyde, benzyl alcohol and benzoic acid by liquid-phase selective oxidation of toluene, a preparation method and application thereof, and belongs to the technical field of catalyst preparation and application. Background technique [0002] Benzyl alcohol, benzaldehyde and benzoic acid are all important fine chemical raw materials and products, with very considerable market prospects and economic benefits. Taking benzaldehyde as an example, it is predicted that in the next few years, the demand for benzaldehyde in my country will increase at an annual rate of about 7%; by 2015, the market demand for benzaldehyde in my country will reach about 30,000 tons per year. "Benzaldehyde demand accounts for about 46% of the total benzaldehyde demand. Although my country's benzaldehyde production capacity has been able to meet the total market demand for benzaldehyde, "chlorine-free" benzaldehyde still needs ...

Claims

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Application Information

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IPC IPC(8): C07C33/22C07C47/54C07C63/06B01J37/03B01J23/847B01J23/34B01J23/22C07C27/12
Inventor 张昕张贵泉林涛龚婷祁敏
Owner NORTHWEST UNIV
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