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Recycling method of mother liquor for SAPO-34 molecular sieve synthesis

A SAPO-34, a technology for synthesizing mother liquor, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems such as the influence of catalyst performance, and achieve the effect of reducing production cost and high crystallinity

Active Publication Date: 2013-03-27
陕西煤化工技术工程中心有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

However, if the synthetic slurry is directly molded, it is easy to form accumulation and coverage of unreacted materials on the surface of the molecular sieve, which will affect the performance of the obtained catalyst.

Method used

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  • Recycling method of mother liquor for SAPO-34 molecular sieve synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 1.07kg of pseudo-boehmite, 0.41kg of phosphoric acid, 0.22kg of roasted kaolin, 11.9kg of water in proportion to the 12kg mother liquor obtained by crystallization and separation after hydrothermal synthesis of SAPO-34. After stirring for 2 hours, add 4.5 kg of kaolin, 3.2kg of silica sol, 0.5kg of graphite powder and 1.3kg of water were mixed and then sheared and sprayed to form solid microspheres. Add 33.75g of solid microspheres, 33g of triethylamine and 35.35g of water into a stainless steel reaction kettle, place the kettle in a homogeneous reactor at 200°C for crystallization for 24 hours, cool, centrifuge, and dry to obtain catalyst microspheres.

Embodiment 2

[0035] The preparation process of this example is the same as that of Example 1, except that the spray-formed microspheres are calcined at 300° C. for 2 hours and then subjected to hydrothermal crystallization treatment.

Embodiment 3

[0037]The preparation process of this example is the same as that of Example 1, and the difference is that 1.07kg of alumina, 0.61kg of phosphoric acid, 0.4kg of silicon oxide, and 13.5kg of water are sequentially added to 13kg of mother liquor, and after stirring for 10 hours, 5.7kg of kaolin is added , 2.6kg of silica sol, 0.2kg of starch, after mixing and shearing spray molding, the spray-molded microspheres were roasted at 400°C for 6h to obtain solid microspheres. 30g of solid microspheres, 68g of diethylamine and 60g of water were added to a stainless steel reaction kettle, and the kettle was placed in a homogeneous reactor at 200°C for 48 hours of stirring and crystallization, and spherical catalyst particles were obtained after separation.

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Abstract

The invention discloses a recycling method of mother liquor for SAPO-34 molecular sieve hydro-thermal synthesis, and relates to the technical field of molecular sieve synthesis. The method comprises the following steps: recovering mother liquor obtained by SAPO-34 molecular sieve hydro-thermal synthesis crystallization and separation, additionally adding a silicon source, an aluminium source, and a phosphorus source into the mother liquor used as a raw material, mixing, adding a substrate material, a binder, and a pore forming agent, preparing microsphere raw powder by spraying molding, putting the roasted microspheres and an aqueous solution of an organic template together into a stainless steel reaction vessel, performing in-situ crystallization to prepare a spherical SAPO-34 molecular sieve catalyst which can be used directly in a fluidized bed device.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and relates to a method for recycling a synthetic mother liquor, in particular to a method for recycling a mother liquor for synthesizing a SAPO-34 molecular sieve. Background technique [0002] SAPO-34 molecular sieve has chemical and physical properties such as suitable acidity, suitable pore structure, small pore size, large specific surface area, good adsorption performance, good thermal stability and hydrothermal stability. It exhibits excellent catalytic performance in the methanol-to-olefins (MTO) reaction. At present, the synthesis of SAPO-34 is mainly based on the hydrothermal synthesis method, but in the current hydrothermal synthesis method, the utilization rate of raw materials is low, and the synthetic mother liquor formed after the molecular sieve is separated contains more unreacted raw materials and a large amount of Water with organic templating agent. The dir...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 汪彩彩张军民刘建斌张世刚张随平罗熙张小虎张亚秦陈亚妮
Owner 陕西煤化工技术工程中心有限公司
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