Catalyst prepared by loading zinc trifluoromethanesulfonate on macroporous-mesoporous material, and preparation method and use thereof

A technology of zinc trifluoromethanesulfonate and mesoporous materials, which is applied in the direction of physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, carboxylate preparation, etc., and can solve the practical application of limited mesoporous materials value, chemical reactivity is not high, and macromolecules are difficult to enter the pores, etc., to achieve good acid conversion rate, reduce side reactions, and improve product purity.

Active Publication Date: 2013-06-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are only silicon hydroxyl groups on the surface of the pore walls of mesoporous materials, resulting in low chemical reactivity, which limits the practical application value of mesoporous materials.
In addition, the currently commonly used mesoporous materials have small pore diameters, with an average pore diameter of 6-9nm. If macromolecular catalytic reactions are carried out, it is difficult for macromolecules to enter the pores, which affects the catalytic effect.

Method used

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  • Catalyst prepared by loading zinc trifluoromethanesulfonate on macroporous-mesoporous material, and preparation method and use thereof
  • Catalyst prepared by loading zinc trifluoromethanesulfonate on macroporous-mesoporous material, and preparation method and use thereof
  • Catalyst prepared by loading zinc trifluoromethanesulfonate on macroporous-mesoporous material, and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Preparation of macroporous mesoporous material loaded with zinc trifluoromethanesulfonate

[0031] (1) 4.0 grams of P123 (the registration number in the American Chemical Abstracts is the substance of 9003-11-6, its average molecular weight Mn=5800) is added in the solution of 37% 16.4ml hydrochloric acid and 128ml water, stirred at 40 ℃ Until P123 is completely dissolved;

[0032] (2) Add 8.86 grams of ethyl orthosilicate to the above solution, and stir at 40° C. for 24 hours;

[0033] (3) Transfer the obtained solution to a polytetrafluoroethylene-lined reactor, and crystallize at 150° C. for 24 hours;

[0034] (4) Obtain the former powder mesoporous material after filtering, washing and drying;

[0035] (5) Washing the raw powder mesoporous material with ethanol under reflux conditions for 24 hours to remove the template agent to obtain a macroporous mesoporous material;

[0036] (6) Vacuum dry 1g of the above-mentioned macroporous mesoporous material at 1...

Embodiment 2

[0039] Embodiment 2 prepares methyl oleate

[0040] Weigh 1 gram of macroporous mesoporous material catalyst SBA-Zn(OTf) 2 , and then weighed 7.05 grams of oleic acid and 5.6 grams of methanol and put them into a 100ml three-necked flask together with a condenser, stirred for 4 hours under the condition of heating and reflux at 60°C, cooled to room temperature, centrifuged, and used gas chromatography Analysis of the liquid components of the reaction product showed that the content of methyl oleate was 50.5%, and the content of oleic acid was 40.8%. Macroporous Mesoporous Material Catalyst SBA-Zn(OTf) 2 Vacuum-dried at 150°C for 6 hours, cooled to room temperature, and recovered for reuse.

Embodiment 3

[0041] Embodiment 3 prepares methyl oleate with the catalyst that reclaims

[0042] 1 gram of macroporous mesoporous material catalyst SBA-Zn(OTf) that embodiment 2 recycles 2 , and then weighed 7.05 grams of oleic acid and 5.6 grams of methanol and put them into a 100ml three-necked flask together, and then added a condenser, stirred for 4 hours under the condition of heating and reflux at 60°C, cooled to room temperature, centrifuged, and used gas chromatography Analysis of the liquid components of the reaction product showed that the content of methyl oleate was 18.2%, and the content of oleic acid was 81.8%. Macroporous Mesoporous Material Catalyst SBA-Zn(OTf) 2 Vacuum-dried at 150°C for 6 hours, cooled to room temperature, and recovered for reuse.

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Abstract

The invention relates to a macroporous-mesoporous material SBA-15 loaded with zinc trifluoromethanesulfonate and a preparation method and use thereof. A novel catalyst is synthesized by loading zinc trifluoromethanesulfonate onto the mesoporous material SBA-15 with aperture between 10 and 14 nanometers. In the invention, macroporous-mesoporous material SBA-15 supported zinc trifluoromethanesulfonate is used as a catalyst for use in the methyl oleate synthesis reaction of oleic acid and methanol, the macropores in the catalyst allow macromolecular oleic acid and methanol to enter mesoporous porous channels to promote a catalytic reaction, side reactions in the catalysts reaction are reduced, product purity is improved, the catalyst can be recycled with high acid conversion rate and little pollution to the environment. The invention also provides a process for preparing a methyl oleate important chemical raw material by using the macroporous-mesoporous material to catalyze the reaction of oleic acid and methanol.

Description

technical field [0001] The invention relates to the technical field of catalytic synthesis, in particular to a macroporous mesoporous material loaded with zinc trifluoromethanesulfonate and an application thereof. Background technique [0002] Methyl oleate is an important chemical raw material. At present, oleic acid and methanol are synthesized by esterification under the action of sulfuric acid (Esterification of oleic acid by methanol catalyzed by p-toluenesulfoicacid and the cation-ex-change resins K241 and K1481 in supercritical carbondioxide [J]. Vieville C, Mouloungui Z, Gaset A. Ind Eng Chem Res, 1993, 32(9): 2065-2068.). Since sulfuric acid and the product are in the same liquid phase, it is difficult to completely separate them, and sulfuric acid corrodes instruments and also pollutes the environment. Therefore, many scientific researches are currently developing new catalysts to replace sulfuric acid. [0003] In 1998, Zhao Dongyuan and others synthesized a new ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J35/10C07C69/58C07C67/08
CPCY02P20/584
Inventor 谢伦嘉王彦强亢宇赵思源田宇孙竹芳冯再兴
Owner CHINA PETROLEUM & CHEM CORP
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