Solid catalyst for preparing epoxy phenylethane by epoxidation of styrene and preparation method

A technology of styrene oxide and solid catalyst, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of serious pollution, immaturity, and difficult recovery of catalysts

Inactive Publication Date: 2004-12-29
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To sum up, although oxygen and air are ideal as oxygen sources to oxidize styrene to styrene oxide, this method is not mature at this stage, and most of them use complex catalysts, which are operated in a homogeneous reaction mode, and the catalysts are difficult to obtain. Recycling, serious pollution, so it is necessary to find a new solid-phase catalyst and reaction system that is easy to separate from the product and can be used repeatedly, and ensure high styrene conversion rate and selectivity of styrene oxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Weigh Co(NO 3 ) 2 ·6H 2 0.34g of O was dissolved in 160g of deionized water, and then 8.0g of MCM-41 without removing the template was added. After stirring for 1 hour at room temperature, it was placed in a water bath at 80°C for 20 hours. Filter the above mixture, wash with a large amount of deionized water to wash away the unexchanged cobalt ions; dry the filter cake in vacuum at 40°C for 1 day; roast the dried solid at 550°C for 6 hours, and control the heating rate at 1 ℃ / min; Grind the calcined solid into powder to obtain 0.78wt% CoO x / MCM-41 catalyst. The MCM-41 molecular sieve without removing the template is prepared by hydrothermal synthesis, and the specific steps are as follows: Weigh Na 2 SiO 3 ·9H 2 33.8g of O and 22.3g of hexadecyltrimethylammonium bromide were dissolved in deionized water and mixed. Adjust the pH of the above mixture to about 11 with hydrochloric acid with a concentration of about 4N. Stir while adding, and then stir. Keep it for...

Embodiment 2

[0025] Example 2: Weigh Co(NO 3 ) 2 ·6H 2 O 2.4g was dissolved in 160g deionized water, and then 8.0g of MCM-41 without removing the template was added. After stirring for 1 hour at room temperature, it was placed in a water bath at 80°C for 20 hours. Filter the above mixture, wash with a large amount of deionized water to wash away the unexchanged cobalt ions; dry the filter cake in vacuum at 40°C for 1 day; roast the dried solid at 550°C for 6 hours, and control the heating rate at 1 ℃ / min; Grind the calcined solid into powder to obtain 6.1wt% CoO x / MCM-41 catalyst. The MCM-41 molecular sieve without removing the template was prepared by the hydrothermal synthesis method as in Example 1.

[0026]The catalytic reaction is carried out in an atmospheric pressure bath reactor. Pipette 1.146ml styrene and 20ml DMF solvent into a 100ml glass flask, 6.1wt% CoO x / MCM-41 catalyst 0.2g was put into the above mixed liquid. The reaction conditions and product analysis were the same as in ...

Embodiment 3

[0028] Example 3: Weigh Co(NO 3 ) 2 ·6H 2 O 1.2g was dissolved in 160g of deionized water, and then 8.0g of MCM-41 without removing the template was added. After stirring for 1 hour at room temperature, it was placed in a water bath at 80°C for 20 hours. Filter the above mixture and wash with a large amount of deionized water to wash away the unexchanged cobalt ions; the filter cake is vacuum dried at 40°C for 1 day; the dried solid is roasted at 550°C for 6 hours, and the heating rate is controlled at 1 ℃ / min; Grind the calcined solid into powder to obtain 2.1wt% CoO x / MCM-41 catalyst. The MCM-41 molecular sieve without removing the template was prepared by the hydrothermal synthesis method as in Example 1.

[0029] The catalytic reaction is carried out in an atmospheric pressure bath reactor. Pipette 1.146ml styrene and 20ml DMF solvent into a 100ml glass flask, 2.1wt% CoO x / MCM-41 catalyst 0.2g was put into the above mixed liquid. The reaction conditions and product analysis ...

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Abstract

The catalyst is VIII metal oxide or VIII metal oxide loaded on silica carrier, and has the composition of MOx or nMOx/SiO2, where SiO2 is mesoporous silica of pore size 1.5-30 nm, MOx is the oxide of VIII metal Fe or Co, and n=0.5 %-8 % is the weight percentage of metal oxide in the catalyst. The catalyst is prepared through ion exchange process or soaking process. Under proper reaction condition, the styrene converting rate within 4 hr may reach 40 %, epoxide selectivity may reach 60 %, and the side product is benzaldehyde mainly except small amount of phenylacetaldehyde and benzoic acid. The catalyst has no obviously lowered styrene converting rate and epoxide selectivity after repeated use.

Description

Technical field [0001] The invention relates to a solid catalyst for preparing styrene oxide by epoxidation of styrene with oxygen as an oxygen source. Background technique [0002] Styrene oxide can be used as a diluent, UV-absorber, and flavoring agent for epoxy resins. It is also an important intermediate in organic synthesis, pharmaceutical and perfume industries, such as β-benzene produced by hydrogenation of styrene oxide. Ethanol is the main component of rose oil, clove oil, and neroli oil, and is widely used in the preparation of food, tobacco, soap and cosmetic flavors. In recent years, the domestic and foreign demand for β-phenylethanol and medical levamisole has increased sharply, and the supply of styrene oxide is in short supply, which has brought broad development prospects to the research of preparing styrene oxide. [0003] Industrially, styrene oxide is prepared by the halohydrin method or hydrogen peroxide catalyzed epoxidized styrene synthesis method. The haloh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/064C07D301/04
Inventor 张庆红汤清虎梁军王野
Owner XIAMEN UNIV
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