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Method for preparing oxidation catalyst of cyclopropene

A catalyst and epoxidation technology, applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problem of reducing catalyst activity, reducing the relative content of titanium-containing active components, and reducing the effective utilization rate of peroxy compounds and other problems to achieve the effect of high conversion rate, high selectivity and good technical effect

Active Publication Date: 2007-12-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is that in the preparation of propylene epoxidation catalysts in the prior art, it is easy to generate extra-skeleton titanium species, reduce the effective utilization rate of peroxygen compounds, and the binder added during molding reduces the titanium-containing active group in the catalyst. The relative content of parts, covering the titanium active center, and reducing the activity of the catalyst provide a new preparation method for propylene epoxidation catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 70 grams of macroporous silica gel (pore volume greater than 0.8 ml / g, specific surface area of ​​350 m 2 / gram), 15 grams of polyethylene glycol 4000 and 75 grams of 40% silica sol are fully mixed and kneaded, and extruded. The molded product was dried at 120°C for 24 hours and calcined at 550°C for 3 hours. Afterwards, 400 ml of toluene, 20 g of triethylamine, and 40 g of tetrabutyl titanate were added, and the mixture was stirred and reacted at 95° C. for 12 hours. After the reaction, wash with 500 milliliters of ethanol. Then, roast at 600°C for 5 hours, and pass water vapor for 1 hour under the condition of 250°C; hours, catalyst A was obtained.

Embodiment 2

[0025] 70 grams of macroporous silica gel (pore volume greater than 0.8 ml / g, specific surface area of ​​510 m 2 / gram), 20 grams of cellulose methyl ether and 110 grams of 30% silica sol are fully mixed and kneaded, and extruded. The molded product was dried at 140°C for 24 hours and calcined at 550°C for 3 hours. Afterwards, 500 ml of cumene, 20 g of diethylamine, and 40 g of tetrabutyl titanate were added, and the mixture was stirred and reacted at 70° C. for 6 hours. After the reaction, wash with 500 milliliters of ethanol. Then, roast at 550°C for 5 hours; at 400°C, pass water steam for 3 hours; after roasting at 600°C for 4 hours, cool down to 200°C, use high-purity nitrogen as a carrier gas, and pass 15 grams of trimethyl chloride The silane was reacted for 4 hours to obtain catalyst B.

Embodiment 3

[0027] Add a mixed solution of 38 grams of cetyltrimethylammonium chloride (CTMACl), 47 grams of tetramethylammonium hydroxide (TEAOH) and 200 grams of water into a container with a stirring device, stir and dissolve at room temperature Finally, 200 g of 40% silica sol was added, and the mixture was stirred and aged for at least 1 hour at room temperature. It was then crystallized at 120°C for 48 hours. Afterwards, the solid product was isolated, dried at 80°C, treated twice with 100 ml of ethanol at 70°C with stirring, and finally dried at 120°C. XRD analysis showed that the dried product had the characteristics of mesoporous MCM-41 with a surface area of ​​970 m 2 / gram.

[0028] Get all the above-mentioned dried samples and fully mix and knead with 15 grams of scallop powder, 100 grams of 25% silica sol and appropriate amount of water, and extrude into strips. The molded product was dried at 150°C for 12 hours and calcined at 530°C for 6 hours. Then, 300 ml of toluene, 18 ...

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Abstract

The invention relates to a preparation method for propylene epoxidation catalyst, which solves the questions that the propylene epoxidation catalyst is easy to produce other titanium outside the skeleton in the former technology, reducing the use rate of ultra-oxygen compound, reducing the relatively content of component with active titanium in the activator in the molding process, covering titanium active center, and reducing effect of activator. The invention uses molding oxidation silicon as carrier then putting titanium into the organic solvent; lastly adopting the scheme about water vapour and organic silicon to solve the problem, which can be used in epoxypropane propane industrial production.

Description

technical field [0001] The invention relates to a preparation method of a propylene epoxidation catalyst. Background technique [0002] Propylene oxide is an important basic chemical raw material, and it is the third largest organic chemical product in the output of propylene derivatives after polypropylene and acrylonitrile. Chlorohydrin method and co-oxidation method (Halcon method) are the main methods for industrial production of PO at present. These two methods account for more than 99% of the world's total production capacity, of which the co-oxidation method exceeds about 60%. [0003] The chlorohydrin method uses propylene and chlorine gas as raw materials. The process is relatively short, the process is mature, the operating load is flexible, the product selectivity is good, the yield is high, the production is relatively safe, the requirement for the purity of raw material propylene is not high, and the investment is small. The biggest disadvantage is the corrosi...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D301/19C07D303/04
CPCY02P20/52
Inventor 高焕新杨洪云金国杰
Owner CHINA PETROLEUM & CHEM CORP
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