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Mesoporous materials containing zinc arene sulfonate and its preparation and application

A mesoporous material, zinc hydrocarbon sulfonate technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, molecular sieve catalysts, etc., can solve the problem of limited scope of catalytic applications

Active Publication Date: 2011-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the modification of mesoporous materials reported in the literature is mostly one-time modification, and the modified mesoporous materials only have a single functional group, and the range of catalytic applications is limited.

Method used

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  • Mesoporous materials containing zinc arene sulfonate and its preparation and application
  • Mesoporous materials containing zinc arene sulfonate and its preparation and application
  • Mesoporous materials containing zinc arene sulfonate and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1 Preparation of mesoporous material containing zinc ethylbenzene sulfonate

[0047] In the first step, 4.0 grams of P123 (the substance with the registration number of 9003-11-6 in the American Chemical Abstracts, its average molecular weight Mn = 5800) was added to a solution of 2 equivalents (2N) of 120 ml of hydrochloric acid and 6 ml of water. Stir at 40°C until P123 is completely dissolved;

[0048] In the second step, 8.2 ml of ethyl orthosilicate was added to the above solution, stirred at 40°C for 45 minutes, and then 1.3 g of 2-(4-chlorosulfonylphenyl)ethyltrimethoxysilane was added, and at 40 °C stirring for 24 hours;

[0049] The 3rd step, the obtained solution is transferred to the reaction kettle lined with polytetrafluoroethylene, and crystallized at 100 ° C for 24 hours;

[0050] Step 4: After filtering, washing and drying, the original powder mesoporous material is obtained;

[0051] Step 5, washing the original powder mesoporous material wit...

Embodiment 2

[0055] Example 2: Preparation of cyclohexanone-1,2-propanediol ketal 0.5 g of mesoporous material was weighed Then weigh 10 grams of cyclohexanone, 12 grams of 1,2-propanediol, and 20 grams of toluene and put them into a 100ml three-necked flask, add a water separator and a condenser, and stir for 50 minutes under the condition of heating and refluxing water separation. After cooling to room temperature, centrifugation and analysis of the reaction product liquid components by gas chromatography, except for toluene (content 83.20%) and cyclohexanone-1,2-propanediol ketal (content 16.80%), no cyclohexanone etc. were detected Other components (that is, the conversion rate of cyclohexanone is close to 100%, and the selectivity of cyclohexanone-1,2-propanediol ketal is close to 100%), solid catalyst mesoporous material It was vacuum-dried at 150° C. for 6 hours, cooled to room temperature, and recovered for reuse.

Embodiment 3

[0056] Example 3: Preparation of cyclohexanone-1,2-propanediol ketal with recovered catalyst 0.5 g of mesoporous material recovered from Example 2 Put 10 grams of cyclohexanone, 12 grams of 1,2-propanediol, and 20 grams of toluene into a 100-ml three-necked flask, add a water separator and a condenser, and stir for 30 minutes under the condition of heating and refluxing water and cooling to After room temperature, centrifugation was performed, and the composition of the reaction product liquid was analyzed by gas chromatography. The conversion rate of cyclohexanone was close to 100%, and the selectivity of cyclohexanone-1,2-propanediol ketal was close to 100%.

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Abstract

The invention relates to the technical field of catalyst synthesis, in particular to a mesoporous material containing zinc sulfonate of aromatic hydrocarbons and its preparation method and application. The mesoporous material is used as a catalyst to prepare cyclohexanone- The reaction process of 1,2-propanediol ketal has the advantages of high conversion rate, high selectivity, reduced side reactions, improved product purity, high conversion rate and high selectivity after repeated use, and less environmental pollution .

Description

technical field [0001] The invention relates to the technical field of catalytic synthesis, in particular to a mesoporous material containing zinc aromatic sulfonate. Background technique [0002] Cyclohexanone 1,2-propanediol ketal is a carbonyl ketal compound. It has the characteristics of a carbonyl ketal compound, and its chemical properties are stable. The aroma is better than that of the parent ketone. It can play the role of coordinator in floral fragrances (He Jian, Sun Baoguo. Fragrance Chemistry and Technology - Natural, Synthetic, and Harmonious Fragrances [M]. Beijing: Chemical Industry Press, 1995: 259-260). Studies have shown that some solid acids (such as H3PW12O40, TiSiW12O40 / TiO2, H3PW12O40 / PAn, etc.) have a good catalytic effect on the synthesis of acetal (ketone) reaction (Luo Yumei, Yang Shuijin. Catalytic synthesis of ketal by phosphotungstic acid catalyst [J]. Rare Metal, 2004, 28(4):787-789). Although solid acid as a catalyst has the advantages of ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J29/00C07D317/72
Inventor 谢伦嘉亢宇王伟赵思源田宇冯华升孙竹芳冯再兴
Owner CHINA PETROLEUM & CHEM CORP