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Molybdenum catalyst preparation method and application thereof

A catalyst and application technology, applied in the field of fine chemicals, can solve the problems of high cost, restriction of industrialization process, difficult separation and purification of products, etc., and achieve the effects of easy recovery, improved intrinsic safety level, and excellent catalytic activity

Active Publication Date: 2021-07-16
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using organic peroxides as oxygen sources has high cost, and the products after reaction are difficult to separate and purify, which restricts its industrialization process

Method used

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  • Molybdenum catalyst preparation method and application thereof
  • Molybdenum catalyst preparation method and application thereof
  • Molybdenum catalyst preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation method of molybdenum catalyst is as follows:

[0038] First, add 208 g of suberic acid, 34 g of ammonium dimolybdate, and 208 g of toluene into the reaction kettle. After nitrogen replacement, heat to 100° C. and react for 90 hours to remove the water and ammonia generated by the reaction to obtain a catalyst precursor.

[0039] Take the catalyst precursor obtained above and add it to another reaction kettle, add 81.6g of ammonia water (25wt%) dropwise to it within 1h at 10°C, then continue the reaction for 5h, cool down to room temperature after the reaction, filter and dry , to obtain a molybdenum catalyst, numbered Mo-1.

[0040] The preparation of other catalysts is the same as the above method, and the specific feeding amount and conditions are controlled in Table 1 and Table 2 below.

[0041] Table 1 Catalyst precursor synthesis conditions

[0042]

[0043] Table 2 Catalyst precursor treatment process

[0044] Numbering Ammonia / g ...

Embodiment 2-6

[0046] For five catalysts prepared in embodiment 1, carry out epoxidation reaction evaluation respectively:

[0047] Take the evaluation of catalyst Mo-1 as an example (embodiment 2) to introduce the evaluation method:

[0048] Add 500g of styrene, 5g of phenothiazine, and 0.05g of catalyst Mo-1 in the epoxidation reactor, then after the nitrogen replacement is complete, heat up to a reaction temperature of 70°C, and add 181g of hydrogen peroxide (concentration is 30wt% ), the reaction was continued for 20 h after the addition was completed. After the reaction was completed, the temperature was not lowered, and the phases were separated to obtain an oil phase and an aqueous phase, and then the temperature was lowered to 10°C.

[0049] After analysis, the conversion rate of hydrogen peroxide was 99.8%, and the selectivity of styrene oxide was 99.0%.

[0050] After the temperature of the water phase is lowered, the molybdenum catalyst is precipitated, and the catalyst is obtain...

Embodiment 7-11

[0058]After the water phase of Examples 2-6 was cooled, solids were precipitated, and solid substances could be obtained by simple settling and decanting. After uniform and simple drying treatment (drying at 100°C for 4h), 0.0482g of solid substances were obtained in Examples 2-6, respectively. 0.1051g, 0.1509g, 0.2580g, 0.5258g. The five solids are numbered Mo-1', Mo-2', Mo-3', Mo-4', Mo-5' respectively.

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Abstract

The invention discloses a molybdenum catalyst preparation method and application thereof, and the method comprises the following steps: preparing a molybdenum catalyst precursor from dicarboxylic acid and ammonium dimolybdate in the presence of a solvent, and treating the obtained solution with ammonia water to obtain the final catalyst. The molybdenum catalyst can be applied to an epoxidation reaction of styrene and hydrogen peroxide, after the reaction is finished, oil-water phase separation is performed, an oil phase is separated to obtain a styrene oxide product, and a water phase is simply separated to obtain the catalyst. According to the method, the conversion rate of styrene and hydrogen peroxide can be effectively increased, the content of byproducts is effectively reduced, the selectivity of the product styrene oxide is improved, the product is easy to separate, the catalyst is easy to recover, the molybdenum catalyst is recycled, and the method is a green synthesis process.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation process of a molybdenum catalyst and its application in epoxidation. [0002] technical background [0003] Styrene oxide is an important organic intermediate, mainly used in the synthesis of medicine, synthesis of spices, and the production of high polymers. [0004] At present, the industrial production of styrene oxide is mainly produced by catalytic oxidation of styrene. The traditional methods for producing styrene oxide include: halogen oxidation method and Haakon method. Although these methods are simple and convenient, they have serious environmental pollution and high material consumption and energy consumption. With the development of green chemistry, economical, rational and environmentally friendly synthetic methods pose new challenges to both industry and academia. The research and use of non-polluting oxidants (such as oxygen and hydrogen peroxide) and e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D301/12C07D303/04
CPCB01J31/2226C07D301/12C07D303/04B01J2531/64B01J2531/0213B01J2231/72Y02P20/584
Inventor 赵晶王漭初晓东牟通李俊平黎源
Owner WANHUA CHEM GRP CO LTD
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