Method for regulating ZSM-5 molecular sieve morphology

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problems affecting the quality and yield of ZSM-5 molecular sieve, and the operable range of the amount of electrolyte added. Small, multi-waste, etc.

Active Publication Date: 2017-05-31
大连凯信科技研发有限公司
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Problems solved by technology

But these methods still have some problems
First of all, these adjustment methods are mainly based on the traditional hydrothermal synthesis of ZSM-5 molecular sieves, which have the problems of large amount of template agent, high crystallization temperature, low utilization rate of single kettle, and more waste liquid discharge; secondly, increasing The amount of template agent or adding seeds to prolong the crystallization time will greatly increase the synthesis cost of ZSM-5 molecular sieves, and will also generate more waste; the method of adding electrolytes, the operable range of the amount of electrolytes is relatively small Small, too large or too small will not have the corresponding effect; to adjust the degree of polymerization of the silicon source and aluminum source in the reaction raw materials, usually add water or acid during the synthesis, which reduces the basicity of ZSM-5 molecular sieve synthesis, Thereby it will affect the quality and yield of ZSM-5 molecular sieve

Method used

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  • Method for regulating ZSM-5 molecular sieve morphology
  • Method for regulating ZSM-5 molecular sieve morphology
  • Method for regulating ZSM-5 molecular sieve morphology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Dissolve 1.5g of sodium metaaluminate in 93g of water, then add 2.15g of disodium hydrogen phosphate dodecahydrate to a transparent and clear solution, and finally add 60g of silica sol, mix and stir for 20min to obtain a uniform solution, the molar ratio of each component is SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 O=1:0.02:0.01:25.24. Then an aerosol is formed by an aerosol generator, dried at 200°C to obtain silicon-aluminum-phosphorus oxide, 1g of silicon-aluminum-phosphorus oxide is placed in a 10ml stainless steel synthesis kettle lined with polytetrafluoroethylene, and then 0.6428g of tetrapropyl Ammonium hydroxide aqueous solution (tetrapropyl ammonium hydroxide mass fraction 25%), SiO in silicon aluminum phosphorus oxide 2 The molar ratio to tetrapropylammonium hydroxide and water is 1:0.05:1.7, sealed at 170°C for crystallization reaction for 48 hours, and the resulting solid product is dried at 100°C, then roasted at 540°C for 10h to remove Template agent to obtai...

Embodiment 2

[0036] Dissolve 1.5g of sodium metaaluminate in 147g of water, then add 4.3g of disodium hydrogen phosphate dodecahydrate to a transparent and clear solution, and finally add 60g of silica sol, mix and stir for 20min to obtain a uniform solution, the molar ratio of each component is SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 O=1:0.02:0.02:35.48. Then an aerosol is formed by an aerosol generator, dried at 200°C to obtain silicon-aluminum-phosphorus oxide, 1g of silicon-aluminum-phosphorus oxide is placed in a 10ml stainless steel synthesis kettle lined with polytetrafluoroethylene, and then 0.6428g of tetrapropyl Ammonium hydroxide aqueous solution (tetrapropyl ammonium hydroxide mass fraction 25%), SiO in silicon aluminum phosphorus oxide 2 The molar ratio to tetrapropylammonium hydroxide and water is 1:0.05:1.7, sealed at 170°C for crystallization reaction for 48 hours, and the resulting solid product is dried at 100°C, then roasted at 540°C for 10h to remove Template agent to obtai...

Embodiment 3

[0038] Dissolve 1.5g of sodium metaaluminate in 256g of water, then add 8.6g of disodium hydrogen phosphate dodecahydrate to a transparent and clear solution, and finally add 60g of silica sol, mix and stir for 20min to obtain a uniform solution, the molar ratio of each component is SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 O=1:0.02:0.04:55.96. Then an aerosol is formed by an aerosol generator, dried at 200°C to obtain silicon-aluminum-phosphorus oxide, 1g of silicon-aluminum-phosphorus oxide is placed in a 10ml stainless steel synthesis kettle lined with polytetrafluoroethylene, and then 0.6428g of tetrapropyl Ammonium hydroxide aqueous solution (tetrapropyl ammonium hydroxide mass fraction 25%), SiO in silicon aluminum phosphorus oxide 2 The molar ratio to tetrapropylammonium hydroxide and water is 1:0.05:1.7, sealed at 170°C for crystallization reaction for 48 hours, and the resulting solid product is dried at 100°C, then roasted at 540°C for 10h to remove Template agent to obtai...

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Abstract

The invention provides a method for regulating a ZSM-5 molecular sieve by using phosphorus species through aerosol auxiliary synthesis. According to the method, an aluminum source, a silicon source, water and a phosphorus source are mixed; an obtained mixture is uniformly stirred to form mixed liquid; aerosol is formed through an aerosol device; drying is performed to obtain amorphous form silicon aluminum phosphorus oxide; the silicon aluminum phosphorus oxide and a tetrapropylammonium hydroxide water solution are mixed; sealing is performed; crystallization is performed at 100 to 200 DEG C, wherein the crystallization time is 3h to 240h; obtained solid products are washed and dried or are directly dried to be roasted; the ZSM-5 molecular sieve is obtained. By the method, the precise regulation on the ZSM-5 molecular sieve morphology can be realized. The method has the advantages that the regulation process is simple; the template agent consumption is low; the pollution is small; the yield is high; good industrial application prospects are realized.

Description

technical field [0001] The invention relates to the technical field of ZSM-5 molecular sieves, in particular to aerosol-assisted synthesis and a method for adjusting the morphology of ZSM-5 molecular sieves by using phosphorus species. Background technique [0002] ZSM-5 molecular sieve is a high-silica zeolite with a three-dimensional cross-channel system invented by Mobil Corporation of the United States. It has good thermal stability, hydrothermal stability and acid resistance. It is mainly used in catalytic cracking, toluene disproportionation, benzene and toluene Alkylation, alkylation of low-carbon aromatics and other important traditional petrochemical fields. At the same time, ZSM-5 molecular sieve is also an important catalyst in coal chemical industry such as methanol to olefins, methanol to gasoline, methanol to aromatics, etc., and can also be used in automobile exhaust treatment (SCR technology) in the field of environmental protection. [0003] At present, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/50C01P2006/12C01P2006/14
Inventor 熊光尹金鹏
Owner 大连凯信科技研发有限公司
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