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Hierarchically pored SAPO-11 molecular sieve and solid-phase synthesis method

A SAPO-11, solid-phase synthesis technology, applied in the field of material chemistry, can solve the problems of waste water and low yield, and achieve the effects of reducing waste water, increasing yield, and high crystallinity

Active Publication Date: 2017-03-22
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of multi-stage porous SAPO-11 molecular sieve and solid-phase synthesis method, be used to solve a large amount of waste water, The problem of low yield

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  • Hierarchically pored SAPO-11 molecular sieve and solid-phase synthesis method
  • Hierarchically pored SAPO-11 molecular sieve and solid-phase synthesis method
  • Hierarchically pored SAPO-11 molecular sieve and solid-phase synthesis method

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Embodiment 1

[0032] This embodiment provides a solid-phase synthesis method of multi-stage pore SAPO-11 molecular sieve. The solid-phase synthesis method includes: mixing and grinding a silicon source, an aluminum source, a mesoporous template, a microporous template, and a phosphorus source. The crystallization reaction is carried out at 140-220°C, and the product is centrifuged and dried, and then roasted to remove the template agent to obtain a hierarchical pore SAPO-11 molecular sieve.

[0033] As an example, the reaction time of the crystallization reaction is 12-72h. Preferably, the crystallization time of the crystallization reaction is 16-48h.

[0034] As an example, the reaction temperature range of the crystallization reaction is 160-200°C.

[0035] As an example, the silicon source is one or a mixture of white carbon black and sodium silicate. The aluminum source is one or a mixture of two or more of pseudo-boehmite, aluminum sulfate, and aluminum isopropoxide. The microporous templ...

Embodiment 2

[0041] This embodiment provides a solid-phase synthesis method of multi-porous SAPO-11 molecular sieve, which specifically includes: weighing 0.14 g white carbon black, 1.46 g pseudo-boehmite, 3.60 g di-n-propylamine phosphate, and 0.36 g sixteen Alkyl trimethyl ammonium bromide (CTAB), after mixing, grind for 10 minutes, put the obtained powder into a reactor, crystallize at 200 ℃ for 24 h, centrifuge the obtained product, and wash it at 80 ℃ Dry and roast at 600℃ for 6h to obtain the final product.

Embodiment 3

[0043] This embodiment provides a solid-phase synthesis method of multi-porous SAPO-11 molecular sieve, which specifically includes: weighing 0.14 g white carbon black, 1.46 g pseudo-boehmite, 3.14 g di-n-propylamine phosphate, and 0.36 g sixteen Alkyl trimethyl ammonium bromide (CTAB), mix and grind for 10 minutes, put the obtained powder into the reaction kettle, crystallize at 200℃ for 24h, centrifuge and wash the obtained product, dry it at 80℃ The final product was calcined at 600°C for 6 hours.

[0044] Figure 4 The XRD characterization results of the hierarchical pore SAPO-11 molecular sieve synthesized in this example are shown, and it can be seen that the product has a typical AEL structure with good crystallinity. Figure 5 It shows the scanning electron micrograph of the multi-porous SAPO-11 molecular sieve synthesized in this embodiment. It can be seen that the product is composed of balls and needle-like substances. Image 6 Shown is the nitrogen adsorption isotherm ...

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Abstract

The invention provides a hierarchically pored SAPO-11 molecular sieve and a solid-phase synthesis method. The solid-phase synthesis method comprises the steps that a solid silicon source, an aluminium source, a mesoporous template and a phosphorus source are mixed, ground and subjected to a crystallization reaction at 140-220 DEG C for 12-72 h, a product is dried centrifugally and roasted, and the hierarchically pored SAPO-11 molecular sieve is obtained after the template is removed. The conversion rate of a hydroisomerization reaction of n-hexadecane by the prepared hierarchically pored SAPO-11 molecular sieve is 83.5%, and the stereoselectivity is 82.1% (under reaction conditions of 290 DEG C, 6MPa, WHSV being 1<-1> and nH2:nC16 being 15. Compared with the prior art, the obtained product not only has a complete AEL structure of the SAPO-11 molecular sieve and higher crystallinity, but also has a mesoporous structure, besides, water is not used in a synthesis process of the molecular sieve, so that produced wastewater is reduced in a production process, and the yield and single-reactor yield are increased to a greater extent.

Description

Technical field [0001] The invention belongs to the field of material chemistry, and specifically relates to a multi-stage porous SAPO-11 molecular sieve and a solid phase synthesis method, and an application method for the hydroisomerization of long-chain alkanes. Background technique [0002] SAPO-11 molecular sieve is a non-zeolite mesoporous molecular sieve with AEL structure, which belongs to the orthorhombic crystal system and has a one-dimensional ten-membered ring pore structure with elliptical pores (0.64×0.39nm). Due to its suitable acid center and pore structure, SAPO-11 molecular sieve has been widely used in petrochemical fields such as normal hydrocarbon isomerization, alkylation, gasoline isomerization recovery octane number and lubricant isomerization dewaxing. [0003] The main component of wax in lubricating oil base oil is high melting point long-chain normal alkanes, which have high pour point and poor low-temperature flow properties. These properties can be im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01J29/85B01J35/10C07C5/27C07C9/22
CPCC01B37/08C01B39/54C07C5/2708B01J29/85C01P2004/61C01P2006/12C01P2006/14C01P2002/72C01P2004/32C01P2004/03C07C2529/85B01J35/60C07C9/22
Inventor 杜燕燕李久盛姜标张力张春风
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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