Sn-Zr/SBA-15 mesoporous molecular sieve catalyst, and preparation method and application thereof

A mesoporous molecular sieve and catalyst technology, applied in the field of catalytic material preparation, can solve the problems of specific surface, pore volume and pore diameter reduction, and achieve the effects of low preparation cost, easy availability of preparation raw materials, good water resistance and thermal stability

Inactive Publication Date: 2017-04-26
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Liu Huiqing et al. (Chemical Industry and Engineering, 2016, 33(1): 29-34) reported that SBA-15 and SnCl 4 ·5H 2 O with ethanol as solvent, stirred at room temperature for 24h, then added 1mol / L H 2 SO 4 Immersed for 5h to prepare SBA-15 mesoporous molecular sieve catalyst loaded with metal Sn, but there is a considerable part of SnO 2 Agglomerates are deposited on the surface and channels of mesoporous molecular sieves, resulting in a decrease in specific surface area, pore volume, and pore size.

Method used

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  • Sn-Zr/SBA-15 mesoporous molecular sieve catalyst, and preparation method and application thereof
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  • Sn-Zr/SBA-15 mesoporous molecular sieve catalyst, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0028] (1) Preparation of Sn-Zr / SBA-15 mesoporous molecular sieve

[0029] 10 grams of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is added to dissolve in the dilute hydrochloric acid aqueous solution of 500ml0.0319mol / l, add 1.1g zirconium oxychloride octahydrate again, at 38 Stir well at ℃ until the solution is clear and form mixture 1; add 1.9g of tin tetrachloride pentahydrate to 50ml of 0.0319mol / l dilute hydrochloric acid aqueous solution to dissolve, then add 22.5g of ethyl orthosilicate, and stir at 25℃ until clear, forming mixture 2; at 38°C, slowly add mixture 1 to mixture 2, in H 2 O and H + In a slightly acidic aqueous solution with a mass molar ratio of 1011:1, mix and stir for 24 hours to form a mixture 3; then transfer the mixture 3 to a polytetrafluoroethylene reactor, stand for crystallization at 100°C for 24 hours, filter, and The filter cake was washed with deionized water, dried at 60°C for 8 hours, then transferred to a m...

Embodiment 2

[0037] Embodiment 2: experimental procedure is the same as embodiment 1, and its difference is: when preparing mesoporous molecular sieve, zirconium oxychloride octahydrate is not added in the mixture 1, and the tin tetrachloride pentahydrate quality that dissolves with dilute hydrochloric acid aqueous solution is 3.8g, And it is not mixed with ethyl orthosilicate to form mixture 2, but it is directly added to mixture 1 with orthosilicate ethyl, at 40 ° C, H 2 O and H + Under the condition of slightly acidic aqueous solution with a mass molar ratio of 922:1, mixed and stirred for 24 hours, a Sn-SBA-15 catalyst without mesopore structure with a mass molar ratio of Sn and Si elements of 0.051:1 was prepared, which was used to catalyze phenol Formaldehyde alkylation reaction synthesizes bisphenol F product, and its mass yield is only 36.71%.

Embodiment 3

[0038] Embodiment 3: experimental procedure is the same as embodiment 1, and its difference is: when preparing mesoporous molecular sieve, be to use 125ml of 20 grams of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer Dissolve in distilled water, stir and clarify, then add 375ml of 0.29mol / l hydrochloric acid aqueous solution without adding zirconium oxychloride octahydrate to form mixture 1, stir mixture 3 for 24h and crystallize at H 2 O and H + Under the condition of slightly acidic aqueous solution with a mass molar ratio of 280:1, the Sn-SBA-15 mesoporous molecular sieve catalyst with a mass molar ratio of Sn and Si elements of 0.039:1 is prepared, which is used to catalyze the alkylation reaction of phenol-formaldehyde Synthetic bisphenol F product, its mass yield is only 55.74%.

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Abstract

The invention discloses a Sn-Zr/SBA-15 mesoporous molecular sieve catalyst, and a preparation method and application thereof. The Sn-Zr/SBA-15 mesoporous molecular sieve catalyst is prepared from a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, stannic chloride pentahydrate, zirconium oxychloride octahydrate and ethyl orthosilicate through hydrothermal crystallization consisting of successive step-by-step hydrolysis and mixing under a weakly acidic condition. The prepared Sn-Zr/SBA-15 mesoporous molecular sieve catalyst is used for catalyzing alkylation of phenol and formaldehyde for synthesis of bisphenol F and has high catalytic activity. Sn is effectively doped into SBA-15 without destroying the mesoporous structure of the SBA-15; SnO2 aggregate is prevented from formation and blocking of the channels of the molecular sieve; a weakly acidic aqueous solution solvent is used for synthesis, so the method is green, environment-friendly and low in preparation cost; and the catalyst is easy to separate, recover and reuse.

Description

[0001] Technical field: [0002] The invention relates to a Sn-Zr / SBA-15 mesoporous molecular sieve catalyst and a preparation method and application thereof, belonging to the technical field of preparation of catalytic materials. Background technique [0003] SBA-15 mesoporous molecular sieve has been used as a catalytic carrier material due to its highly ordered and regular pore structure, large specific surface area, good hydrothermal stability and abundant surface silanol, especially in the preparation of solid acid catalysts. On the one hand, SBA-15 mesoporous molecular sieve doped with Sn is easy to form Lewis acidic sites and solid acid with stable performance, low cost, and less corrosion to equipment, which has attracted attention. [0004] Hao Jiao et al. (Industrial Catalysis, 2014, 22(1): 29-34) mentioned that anhydrous SnCl 4 As the tin source and toluene as the solvent, the Sn-modified SBA-15 mesoporous molecular sieve, that is, SnCl 4 / SBA-15, which has high c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035C07C37/20C07C39/16
CPCB01J29/035B01J2229/18C07C37/20C07C39/16Y02P20/50Y02P20/52
Inventor 刘跃进秦晓东李勇飞
Owner XIANGTAN UNIV
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