Modified molecular sieve catalyst, preparation method thereof and styrene oxide preparation method

A catalyst and molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of increased post-processing difficulties, unsatisfactory product selectivity, low utilization rate, etc., to avoid heavy metal pollution, The effect of improving the intrinsic safety of the system and reducing the degree of polymerization

Active Publication Date: 2020-06-23
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this invention is that the maximum conversion rate is only 75%
[0009] In summary, from the existing reports, in the homogeneous catalyst system, H 2 o 2 As an oxidant, the utilization rate is low, and the incompletely converted H in the system 2 o 2 Increased post-processing difficulties; non-homogeneous catalysts are based on peroxides or O 2 As an oxidizing agent, the product selectivity is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of catalyst: Gd content 1%, polymerization inhibition factor content 1%.

[0038] (1) Preparation of rare earth modified MCM-41

[0039] The synthetic method of rare earth metal modified all-silicon MCM-41:

[0040] Take a certain amount of anhydrous sodium metasilicate 610g, dissolve it in 3050mL deionized water, adjust the pH=8 with sulfuric acid (6mol / L) solution, stir the formed gel at room temperature for 1h, and then add 20% deionized 728 g of an aqueous solution of hexaalkyltrimethylammonium bromide (CTAB) was prepared as a mother liquor, and the mother liquor was stirred at 20° C. for 24 hours. Then add 8.6g of Gd(NO 3 ) 3 ·6H 2 O, in a PTFE-lined stainless steel autoclave, the hydrothermal synthesis reaction was carried out at 120 ° C. After 48 hours, the autoclave was taken out, and the solid product obtained was filtered, washed and dried, and the reaction was carried out under the protection of a nitrogen atmosphere. Calcined in an oven at 1...

Embodiment 2

[0046] Preparation of the catalyst: the content of Y is 2%, and the content of polymerization inhibition factor is 2%.

[0047] (1) Preparation of rare earth modified MCM-41

[0048] The synthetic method of rare earth metal modified all-silicon MCM-41:

[0049] Take a certain amount of anhydrous sodium metasilicate 610g, dissolve it in 3050mL deionized water, adjust the pH=8 with sulfuric acid (6mol / L) solution, stir the formed gel at room temperature for 1h, and then add 20% deionized 728 g of an aqueous solution of hexaalkyltrimethylammonium bromide (CTAB) was prepared as a mother liquor, and the mother liquor was stirred at 40° C. for 10 h. Then add 25.8g of Y (NO 3 ) 3 ·6H 2 O, in a PTFE-lined stainless steel autoclave, the hydrothermal synthesis reaction was carried out at 150 ° C. After 10 hours, the autoclave was taken out, and the obtained solid product was filtered, washed and dried, and then the reaction was carried out under the protection of a nitrogen atmosphe...

Embodiment 3

[0055] Preparation of catalyst: Eu content 5%, polymerization inhibitor content 10%.

[0056] (1) Preparation of rare earth modified MCM-41

[0057] The synthetic method of rare earth metal modified all-silicon MCM-41:

[0058] Take a certain amount of anhydrous sodium metasilicate 610g, dissolve it in 3050mL deionized water, adjust the pH=8 with sulfuric acid (6mol / L) solution, stir the formed gel at room temperature for 1h, and then add 20% deionized 728 g of an aqueous solution of hexaalkyltrimethylammonium bromide (CTAB) was prepared as a mother liquor, and the mother liquor was stirred at 50° C. for 14 hours. Then add 44.0g of Eu(NO 3 ) 3 ·6H 2 O, in a PTFE-lined stainless steel autoclave, the hydrothermal synthesis reaction was carried out at 200 ° C. After 4 hours, the autoclave was taken out, and the obtained solid product was filtered, washed and dried. Calcined in an oven at 150°C for 4h, and then fired in a muffle furnace at 900°C in an air atmosphere for 4h to...

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PUM

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Abstract

The invention discloses a modified molecular sieve catalyst and a preparation method thereof. The modified molecular sieve catalyst is MCM-41 / M-N, MCM-41 is a molecular sieve, M is a rare earth metal,N is a polymerization inhibition factor, based on the total mass of the catalyst, the content of M is 1-5%, and the content of N is 1-10%. The catalyst is obtained through multi-step modification such as rare earth metal modification, pore-enlarging modification, polymerization inhibition factor coordination modification, and the like. The invention mainly solves the defects of low catalyst stability, unsatisfactory product selectivity and yield and unsatisfactory process safety in the prior art. The catalyst is used for preparing styrene oxide, the reaction activity and selectivity are improved, the styrene polymerization degree is reduced, the intrinsic safety of the process is improved, the production cost is reduced, various defects in the prior art are overcome, and the catalyst canbe used for industrial production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a modified molecular sieve catalyst and a preparation method thereof, and a preparation method of styrene oxide. Background technique [0002] Styrene oxide, also known as styrene oxide, is an important intermediate in organic synthesis, which can be used to produce epoxy resins, UV absorbers, etc., and is also an important raw material in the pharmaceutical and perfume industries. β-phenylethyl alcohol and levamisole, etc. In recent years, the market demand for styrene oxide has been increasing, showing a situation of short supply. [0003] The synthesis methods of styrene oxide mainly include haloalcohol method, peroxyacid oxidation method, direct oxidation method and so on. [0004] At present, the main process of styrene oxide is the haloalcohol method, which can obtain a product yield of about 80%, but there are problems such as high raw material consumption, serious equipmen...

Claims

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Application Information

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IPC IPC(8): B01J29/03C07D301/19C07D303/04
CPCB01J29/0308C07D301/19B01J2229/18C07D303/04Y02P20/52
Inventor 赵晶王漭牟通李俊平黎源
Owner WANHUA CHEM GRP
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