Preparation method of catalyst for epoxidation of 1-butene to prepare 1,2-epoxybutane

A technology of butylene oxide and catalyst, which is applied in the field of catalyst preparation for epoxidation of 1-butene, can solve the problems of cumbersome and complicated catalyst preparation procedures, unsolved problems such as hydrolysis of organic titanium sources, and inability to improve catalytic activity, and achieve good catalytic performance. High activity, good catalytic effect, high titanium content

Active Publication Date: 2018-12-28
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although better catalytic activity is obtained by improving the mass transfer effect, the reactants are easy to self-polymerize during the reaction, and the conversion rate of the effective product is low. More importantly, this method has carried out silanization treatment in the post-treatment of the catalyst, resulting in The catalyst preparation process is cumbersome and complicated, and the repeatability is low
[0004] Patent CN1418876A achieved high reactivity and selectivity by loading titanium-silicon molecular sieve synthesized by hydrothermal method on alumina carrier, adding alkali metal and alkaline earth metal oxide components to the catalyst, but this method is only applicable to When hydrogen peroxide is used as the oxidant, the effect is not ideal when the commonly used CHP is selected as the oxidant; in addition, since this method only loads the active component on the alumina carrier, it inevitably causes the problem that the active component is easy to lose
Moreover, the problem of hydrolysis of the organic titanium source is still not solved in the catalyst preparation process of this method, and the catalytic activity cannot be improved to the best degree.

Method used

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  • Preparation method of catalyst for epoxidation of 1-butene to prepare 1,2-epoxybutane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 23.0g tetraethyl orthosilicate, 1.0g butyl titanate, and 20.3g lauryl polyoxyethylene ether; stir and dissolve 24.5g lauryl polyoxyethylene ether in 100ml absolute ethanol, heat Stir for 1 h; slowly add 23.0 g of ethyl orthosilicate dropwise to the three-neck flask under stirring; half an hour later slowly add 4.0 g of butyl titanate dropwise, and finally do not add absolute ethanol to 220 ml. The pH of the reaction system was measured to be 2.0 with a magnetic pH meter, and the temperature was controlled to stir at 75° C. for 24 hours. After cooling and standing for 3 hours, the crystalline product was separated; after drying at 110°C, it was calcined in a muffle furnace at 550°C for 6 hours to obtain the original titanium-silicon molecular sieve catalyst powder.

[0033] The raw titanium-silicon molecular sieve powder obtained above was pressed into tablets and sieved, and the 20-40 mesh particles were packed into a fixed-bed reactor in a catalyst evaluation dev...

Embodiment 2

[0036] The preparation method of titanium silicon molecular sieve is operated with embodiment 1. Take 1.4g of tetrabutyl titanate.

[0037] The relative molar content of the components is:

[0038] SiO 2 / TiO 2 =23 Template / SiO 2 =0.37

Embodiment 3

[0040] The preparation method of titanium silicon molecular sieve is operated with embodiment 1. Take 2g of tetrabutyl titanate.

[0041] The relative molar content of the components is:

[0042] SiO 2 / TiO 2 =16 Template / SiO 2 =0.37

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Abstract

The invention relates to a preparation method for a catalyst used for preparing 1,2-epoxybutane through epoxidation of 1-butene. The preparation method comprises adding a template into a solvent, stirring at 20-100 DEG C, and adding proper amount of an acid to adjust pH to 2-9; mixing a silicon source and a titanium source according to a prescribed ratio, adding into the above solution, and crystallizing the solution with stirring, so as to obtain a gel mixed solution; standing the gel mixed solution at 40-100 DEG C for 12 h-48 h; and separating the gel product to obtain a white solid precipitate, performing washing and drying to obtain a catalyst raw powder, then roasting in muffle furnace, so as to obtain the catalyst applied to epoxidation of 1-butene. The method solves the disadvantages that a conventional butene epoxidation catalyst is relatively low in activity, low in titanium-source utilization rate, low in selectivity and not high in epoxybutane product yield. The method avoids the disadvantage that active compositions in the formed silicon-titanium molecular sieve lose due to hydrolysis of the titanium source, and is effectively applied to prepare 1,2-epoxybutane through epoxidation of 1-butene.

Description

technical field [0001] The invention relates to a method for preparing a catalyst for epoxidizing 1-butene. Background technique [0002] my country's 1-butene is mainly obtained from ethylene plant and refinery catalytic cracking unit by-product C4 fraction and ethylene dimerization. With the development of MTBE (methyl tert-butyl ether) synthesis, 1-butene and MTBE are co-produced There are more and more devices. At present, the production capacity of 1-butene in my country is as high as 120,000 tons per year. Converting 1-butene into an important organic chemical intermediate butylene oxide is a bold idea to increase the added value of products and effectively utilize 1-butene. [0003] The relatively successful methods for industrial production of epoxides mainly include the chlorohydrin method and the co-oxidation method. The chlorohydrin method is more widely used, but a large amount of waste water is generated in the production process, which consumes a lot of energy ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C07D303/04C07D301/19
Inventor 赵耀吴美玲周灵杰陈玮娜马颖涛
Owner CHINA PETROLEUM & CHEM CORP
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