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
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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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