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Zinc trifluoromethanesulfonate-loaded spherical mesoporous material, and preparation method and application thereof

A technology of zinc trifluoromethanesulfonate and mesoporous materials, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of low chemical reaction activity and limited practical application Value and other issues, to achieve the effect of high product purity, less side reactions, and high conversion rate

Active Publication Date: 2013-03-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the size of the mesoporous material SBA-16 spheres reported in the literature is at the millimeter level, and the surface of the pore wall of the mesoporous material SBA-16 has only silicon hydroxyl groups, resulting in low chemical reactivity, which greatly limits its practical application value.

Method used

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  • Zinc trifluoromethanesulfonate-loaded spherical mesoporous material, and preparation method and application thereof
  • Zinc trifluoromethanesulfonate-loaded spherical mesoporous material, and preparation method and application thereof
  • Zinc trifluoromethanesulfonate-loaded spherical mesoporous material, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Preparation of Spherical Mesoporous Materials Loaded with Zinc Trifluoromethanesulfonate

[0032] (1) 2.0 grams of F108 (Fuka company trade name Substance F108) with 5.24 g K 2 SO 4 Add to 60 grams of 2N hydrochloric acid solution, stir at 38°C until F108 is completely dissolved;

[0033] (2) Add 4.2 grams of ethyl orthosilicate to the above solution, stir at 38°C for 15 minutes, and then stand at 38°C for 24 hours;

[0034] (3) Transfer the obtained solution to a polytetrafluoroethylene-lined reaction kettle, and crystallize at 100° C. for 24 hours;

[0035] (4) adding 100 grams of deionized water to dilute, filter, wash and dry to obtain the former powder of spherical mesoporous material;

[0036] (5) Washing the raw powder mesoporous material with ethanol under reflux conditions for 24 hours, removing the template agent, and obtaining spherical mesoporous materials;

[0037] (6) 1g of spherical mesoporous material was vacuum-dried at 150°C for 6 hours...

Embodiment 2

[0040] Embodiment 2 prepares cyclohexanone-1,2-propanediol ketal

[0041] Weigh 0.5 g of spherical mesoporous material FDU-Zn(OTf) loaded with zinc trifluoromethanesulfonate 2 , then weigh 10 grams of cyclohexanone and 12 grams of 1,2-propanediol and put them into a 100ml three-neck flask together, add a condenser, stir for 60 minutes under the condition of heating and reflux, and after cooling to room temperature, centrifuge and use Gas chromatographic analysis of the product components in the liquid phase of the reaction showed that cyclohexanone was 5.3%, and cyclohexanone-1,2-propanediol ketal was 69.3%. Solid catalyst mesoporous material FDU-Zn(OTf) after centrifugation 2 Vacuum-dried at 150°C for 6 hours, cooled to room temperature, and recovered for reuse.

Embodiment 3

[0042] Embodiment 3 prepares cyclohexanone-1,2-propanediol ketal with the catalyst that reclaims

[0043] The 0.5 gram mesoporous material FDU-Zn(OTf) that embodiment 2 recycles 2 , put 10 grams of cyclohexanone and 12 grams of 1,2-propanediol into a 100ml three-neck flask, add a condenser, stir for 60 minutes under heating and reflux conditions, cool to room temperature, centrifuge, and use gas chromatography Analysis of the liquid components of the reaction product revealed that cyclohexanone was 4.0%, and cyclohexanone-1,2-propanediol ketal was 72.9%.

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Abstract

The invention relates to the technical field of catalyst synthesis, in particular to a zinc trifluoromethanesulfonate-loaded spherical mesoporous material, and a preparation method and application thereof. The mesoporous material serves as a catalyst which is used for a reaction process for preparing cyclohexanone-1,2-propylene glycol from cyclohexanone and 1,2-propylene glycol. The mesoporous material has the advantages of high conversion rate of a reactant after a catalytic reaction, a small number of side reactions, high product purity, high conversion rate after repeated use and environmental friendliness.

Description

technical field [0001] The invention relates to the technical field of catalytic synthesis, in particular to a mesoporous material containing zinc sulfonate of aromatic hydrocarbons and a preparation method and application thereof. Background technique [0002] Due to the high surface area and pore volume of mesoporous materials (Kresge, C.T.; Leonowicz, M.E.; Roth, W.J.; Vartuli, J.C.; Beck, J.S. Nature 1992, 359, 710.), easy-to-modulate regular nanopores, abundant and Easy-to-design surface groups, as well as tunable macroscopic morphologies (such as membranes, fibers, spheres, etc.), have shown unique development potential in the fields of protein separation, biosensors, catalysis, optical devices, adsorption, and microelectronics (Zhao , D.; Yang, P.; Huo, Q.; Chmelka, B.F.; Stucky, G.D. Curr. Opin. Solid State Mater. Sci. 1998, 3, 111.3 Mann, S.; Asefa, T.; MacLachan, M.J.; Coombs, N.; Ozin, G.A. Nature 1999, 402, 867. MacLachlan, M.J.; Ginzburg, M.; Coombs, N.; Raju, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J35/10B01J35/08C07D317/72
Inventor 亢宇谢伦嘉王彦强赵思源田宇孙竹芳冯再兴
Owner CHINA PETROLEUM & CHEM CORP
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