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Zirconium silicate-modified mesoporous silicon oxide catalyst as well as preparation method and application thereof

A mesoporous silica and catalyst technology, which is applied in catalyst activation/preparation, physical/chemical process catalyst, carboxylate preparation, etc., can solve the problems of non-compliance with green environmental protection, waste acid waste water pollution, large catalyst consumption, etc. Less catalyst dosage, less by-products, and the effect of improving the conversion rate

Active Publication Date: 2018-11-13
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the mass ratio of 3-chloro-2 methacrylic acid to paraformaldehyde is 2.94:1, stannous chloride dihydrate is 8 times of the quality of paraformaldehyde, the quality of adding water is 6 times of paraformaldehyde, and the stirring speed is 30r / min, under normal temperature and pressure, after stirring for 4.5h, the obtained mixed solution is extracted with ethyl acetate, and after washing with NaCl aqueous solution, the reaction yield is above 98%. Although the above process route has a high yield, the amount of catalyst is too high Large, and HCl by-products will be generated at the same time, using water as a solvent is more likely to cause pollution of waste acid wastewater, so this route does not conform to the concept of green environmental protection

Method used

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  • Zirconium silicate-modified mesoporous silicon oxide catalyst as well as preparation method and application thereof
  • Zirconium silicate-modified mesoporous silicon oxide catalyst as well as preparation method and application thereof
  • Zirconium silicate-modified mesoporous silicon oxide catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 4g of P123, 140mL of 0.4mol / L hydrochloric acid solution into the three-necked flask in turn, stir at 40°C to dissolve P123 completely, then add 4g of n-butanol, stir at 40°C for 1h, then add 2.60g of oxychloride octahydrate Zirconium ZrOCl 2 ·8H 2 O, 8.50g tetraethyl orthosilicate (TEOS), uniformly stirred at 40°C for 20h, put the mixed liquid into a stainless steel hydrothermal synthesis kettle with a polytetrafluoroethylene liner, at 130°C After crystallization for 1 day, cool down to room temperature, take out the crystallization solution, filter, put the filter cake after filtration in an oven to dry at 60°C, and place the dried item in a muffle furnace at 550°C for 6 hours. Prepared zirconium silicate modified mesoporous silica catalyst, denoted as 0.2ZrSiO 4 - MS-T130 (wherein MS refers to mesoporous silica, 0.2 refers to the molar ratio of Zr to Si, and T130 refers to a crystallization temperature of 130° C.). From the XRD pattern of the catalyst (see fi...

Embodiment 2

[0032] Add 4g of P123, 140mL of 0.8mol / L hydrochloric acid solution into the three-necked flask in turn, stir at 40°C to completely dissolve P123, then add 4g of n-butanol, stir at 40°C for 1h, then add 5.2g of octahydrate oxychloride Zirconium ZrOCl 2 ·8H 2 O, 8.50g tetraethyl orthosilicate (TEOS), uniformly stirred at 40°C for 20h, put the mixed liquid into a stainless steel hydrothermal synthesis kettle with a polytetrafluoroethylene liner, at 130°C After crystallization for 1 day, cool down to room temperature, take out the crystallization solution, filter, put the filter cake after filtration in an oven to dry at 60°C, and place the dried item in a muffle furnace at 550°C for 6 hours. Prepared zirconium silicate modified mesoporous silica catalyst, denoted as 0.4ZrSiO 4 - MS-T130 (wherein MS refers to mesoporous silica, 0.4 refers to the molar ratio of Zr to Si, and T130 refers to a crystallization temperature of 130° C.). From the XRD pattern of the catalyst (see fig...

Embodiment 3

[0034] Add 6.3g of F127 and 140mL of 0.9mol / L hydrochloric acid solution into the three-necked flask in turn, stir at 40°C to dissolve F127 completely, then add 6.18g of n-butanol, stir at 40°C for 1 hour, then add 4.7g of zirconium chloride ZrCl 2 , 14.20g of sodium silicate, stirred evenly at 40°C for 20h, put the mixed liquid into a stainless steel hydrothermal synthesis kettle with polytetrafluoroethylene lining, crystallized at 110°C for 1 day, cooled To room temperature, take out the crystallization solution, filter, put the filtered filter cake in an oven to dry at 60°C, place the dried article in a muffle furnace and roast at 550°C for 6h to prepare the catalyst 0.4ZrSiO 4 - MS-T110 (wherein MS refers to mesoporous silica, 0.4 refers to the molar ratio of Zr to Si, and T110 refers to a crystallization temperature of 110° C.).

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Abstract

The invention discloses a zirconium silicate-modified mesoporous silicon oxide catalyst as well as a preparation method and application thereof. The catalyst is prepared by one-step hydrothermal condensation after a template agent, a structure directing agent, a silicon source and a zirconium source are added. The invention further discloses a method for synthesizing 3-methyl-butene-1-alcohol carboxylate by adopting the zirconium silicate-modified mesoporous silicon oxide catalyst. The method is that the 3-methyl-butene-1-alcohol carboxylate is generated by the condensation and the esterification of carboxylic acid, isobutene and formaldehyde. The zirconium silicate-modified mesoporous silicon oxide catalyst disclosed by the invention is mild in preparation condition, simple in preparationprocess and high in catalytic activity, is used for the catalytic synthesis of the 3-methyl-butene-1-alcohol carboxylate and has the advantages of being good in reaction activity, high in product yield, green, environmentally-friendly and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a zirconium silicate modified mesoporous silicon oxide catalyst and a preparation method and application thereof. Background technique [0002] In the past two decades, mesoporous materials have attracted extensive attention from researchers because of their high specific surface area, uniform tunable pore size, and narrow pore size distribution. These characteristics are conducive to better contact between reactants and active sites, faster diffusion, and can effectively promote the reaction. Among them, the introduction of Fe, Ti, Sn, Al, Zr and other heteroatoms on the silica can make it have catalytic activity. [0003] Literature [Journal of Colloid & Interface Science, 2011, 361 (1): 25] introduces a method for synthesizing zirconium silicate containing mesoporous structure without using template, and powder Zr[OSi(Ot-BuO) 3 ] 4 Added to the hydrochloric acid so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/08B01J35/04B01J37/10C07C67/00C07C69/145
CPCC07C67/00B01J21/08B01J37/10B01J35/56C07C69/145
Inventor 汤吉海乔旭梅秋敏张竹修李克崔咪芬费兆阳陈献刘清
Owner NANJING UNIV OF TECH
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