A kind of preparation method of molybdenum catalyst and its application

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: 2022-08-05
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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  • A kind of preparation method of molybdenum catalyst and its application
  • A kind of preparation method of molybdenum catalyst and its application
  • A kind of preparation method of molybdenum catalyst and its application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of molybdenum catalyst is as follows:

[0037] First, 208 g of suberic acid, 34 g of ammonium dimolybdate, and 208 g of toluene were added to the reaction kettle. After nitrogen replacement, the reaction was heated to 100 °C for 90 h, and the water and ammonia generated by the reaction were removed to obtain a catalyst precursor.

[0038] The catalyst precursor obtained above was added to another reaction kettle, and 81.6 g of ammonia water (25 wt %) was added dropwise to it within 1 h at 10 °C, and then the reaction was continued for 5 h. After the reaction was completed, the temperature was lowered to room temperature, filtered and dried. , to obtain a molybdenum catalyst, numbered Mo-1.

[0039] The preparations of other catalysts are the same as the above-mentioned methods, and the specific feeding amounts and conditions are controlled in the following Tables 1 and 2.

[0040] Table 1 Catalyst precursor synthesis conditions

[0041]

[00...

Embodiment 2-6

[0045] For the five catalysts prepared in Example 1, the epoxidation reactions were evaluated respectively:

[0046] Take the evaluation of catalyst Mo-1 as an example (Example 2) to introduce the evaluation method:

[0047] Add 500 g of styrene, 5 g of phenothiazine, and 0.05 g of catalyst Mo-1 to the epoxidation reaction kettle, then after nitrogen replacement is completed, the temperature is raised to a reaction temperature of 70 ° C, and 181 g of hydrogen peroxide (with a concentration of 30 wt%) is added to the system for 1 h. ), the reaction was continued for 20 hours after the addition, and after the reaction was completed, without cooling, the phases were separated by standing to obtain an oil phase and a water phase, and then the temperature was lowered to 10°C.

[0048] After analysis, the conversion rate of hydrogen peroxide was 99.8%, and the selectivity of ethylene oxide was 99.0%.

[0049] After the water phase is cooled, the molybdenum catalyst is precipitated,...

Embodiment 7-11

[0057]After the water phase of Example 2-6 was cooled down, solids were all precipitated, and solid substances were obtained by simple sedimentation and decanting. After unified and simple drying treatment (100 ° C drying for 4 h), 0.0482 g of solid substances were obtained in Examples 2-6, respectively. 0.1051g, 0.1509g, 0.2580g, 0.5258g. The five solids were numbered Mo-1', Mo-2', Mo-3', Mo-4', Mo-5' respectively.

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Abstract

The invention discloses a method for preparing a molybdenum catalyst and its application. The method firstly prepares a molybdenum catalyst precursor from dicarboxylic acid and ammonium dimolybdate in the presence of a solvent, and then treats the obtained solution with ammonia water to obtain the final catalyst. The molybdenum catalyst can be used in the epoxidation reaction of styrene and hydrogen peroxide. After the reaction, the oil-water phase and the oil phase are separated to obtain ethylene oxide product, and the water phase is simply separated to obtain the catalyst. The method can effectively improve the conversion rate of styrene and hydrogen peroxide, effectively reduce the content of by-products, improve the selectivity of the product ethylene oxide, the product is easy to separate, the catalyst is easy to recover, and the molybdenum catalyst can be recycled. 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 an epoxidation reaction. technical background [0002] Ethylene oxide is an important organic intermediate, which is mainly used in the synthesis of medicine, the synthesis of fragrances, and the production of high polymers. [0003] At present, the industrial production of ethylene oxide is mainly made by catalytic oxidation of styrene. The traditional methods of producing ethylene oxide are: halogen oxidation method and Haakon method. Although these methods are simple and convenient, they have serious environmental pollution and high material and energy consumption. With the development of green chemistry, economical, rational and environmentally friendly synthetic methods have presented new challenges to both industry and academia. The research and use of non-polluting oxidants (such as oxygen, hydrogen perox...

Claims

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Application Information

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Patent Type & Authority Patents(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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