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Method for fully crystallizing SAPO-34 molecular sieve balls by using phosphorus-aluminum molecular sieve mother liquor

A SAPO-34, phospho-aluminum molecular sieve technology, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silico-aluminophosphate and other directions, to achieve the effect of increasing relative content, increasing product yield, and reducing dosage

Pending Publication Date: 2021-10-29
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, developing efficient green routes to synthesize industrially important zeolite catalysts remains a great challenge

Method used

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  • Method for fully crystallizing SAPO-34 molecular sieve balls by using phosphorus-aluminum molecular sieve mother liquor
  • Method for fully crystallizing SAPO-34 molecular sieve balls by using phosphorus-aluminum molecular sieve mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0022] using Al 2 O 3 : SiO 2 :P 2 O 5 =1:0.4:1 and SAPO-34 mother liquor to spray balls, screen 40-100 micron microspheres, and grind and pulverize the rest of the microspheres before spraying them. Dry roasting was carried out at 300°C, and the drying roasting time was 4h. The weight ratio of the microspheres to the mother liquor is 1:10, the template agent is triethylamine, and the weight ratio of the template agent to the weight of the microspheres is 1:1. The temperature was raised to 190°C under stirring, and the temperature was kept for 20h. After the crystallization is completed, the temperature is lowered, washed and dried.

Embodiment 2

[0024] using Al 2 O 3 : SiO 2 :P 2 O 5 =1:0.6:1 and SAPO-18 mother liquor to spray balls, screen 40-100 micron microspheres, grind and pulverize the rest of the microspheres and then spray the balls. At 200°C, dry roasting was carried out, and the drying roasting time was 4h. The weight ratio of the microspheres to the mother liquor is 1:15, the template agent is tetraethyl ammonium hydroxide, and the weight ratio of the template agent to the weight of the microspheres is 1:1. The temperature was raised to 180°C under stirring, and the temperature was kept for 20h. After the crystallization is completed, the temperature is lowered, washed and dried.

Embodiment 3

[0026] using Al 2 O 3 : SiO 2 :P 2 O 5 =1:0.6:1 and SAPO-5 mother liquor to spray balls, screen 40-100 micron microspheres, grind and pulverize the rest of the microspheres and then spray the balls. Dry roasting was carried out at 250°C, and the drying roasting time was 4h. The weight ratio of the microspheres to the mother liquor is 1:10, the template agent is tetraethyl ammonium hydroxide, and the weight ratio of the template agent to the weight of the microspheres is 1:0.5. The temperature was raised to 200°C under stirring, and the temperature was maintained for 20h. After the crystallization is completed, the temperature is lowered, washed and dried. The XRD pattern of the sample is shown in figure 1 , see SEM image figure 2 .

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Abstract

The invention discloses a method for fully crystallizing SAPO-34 molecular sieve spheres by using a phosphorus-aluminum molecular sieve mother liquor, which comprises the following steps: mixing the phosphorus-aluminum molecular sieve mother liquor, a silicon source, an aluminum source and a phosphorus source, spraying the spheres, screening 40-100 microns of microspheres, drying and roasting at 200-400 DEG C for 1-10 hours, grinding and crushing the rest microspheres, and spraying the spheres; mixing the microspheres with a phosphorus-aluminum molecular sieve mother solution, adding a template agent, heating to 160-220 DEG C under a stirring condition, crystallizing for 10-30 hours, cooling, washing and drying after the crystallization is finished, so as to obtain the SAPO-34 molecular sieve spheres. The method provided by the invention provides important technical support for industrial application of the SAPO-34 molecular sieve and treatment of the waste silicon-aluminum molecular sieve. The method provided by the invention has the advantages of simple process steps, strong operability and low recovery cost, and can realize recycling of the molecular sieve mother liquor.

Description

technical field [0001] The invention belongs to the field of molecular sieve material preparation, and in particular relates to a method for fully crystallizing SAPO-34 molecular sieve balls with a phosphorus-aluminum molecular sieve mother liquor. Background technique [0002] Coal chemical industry is an important branch of chemical industry. Due to the characteristics of more coal and less oil in China's geological structure, the use of coal to produce methanol and methanol to produce ethylene and other organic raw materials has become more and more important in recent years. There are more and more large-scale coal chemical enterprises of this type in China. and production is increasing. In the entire coal chemical industry chain, coal is first used to produce synthesis gas, then synthesis gas is produced to methanol, and then methanol is dehydrogenated to produce olefins. Among them, the production of ethylene from methanol is a very important link, in which SAPO- 34 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2002/72C01P2004/03
Inventor 季超臧甲忠于海斌刘冠锋李滨洪鲁伟宋万仓洪美花石芳
Owner CNOOC TIANJIN CHEM RES & DESIGN INST