Novel method for rapidly preparing mesoporous SAPO-34 molecular sieve with small particle size

A technology of SAPO-34 and molecular sieve, which is applied in the direction of molecular sieve catalysts, including molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, can solve the problems of industrial application and cost, achieve long catalyst life, improve olefin yield, and high ratio Surface and Pore Volume Effects

Active Publication Date: 2019-01-11
岳阳慧璟新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method produces a large amount of COD sewage, which requires a lot of expensive treatment and cannot be applied industrially.

Method used

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  • Novel method for rapidly preparing mesoporous SAPO-34 molecular sieve with small particle size
  • Novel method for rapidly preparing mesoporous SAPO-34 molecular sieve with small particle size
  • Novel method for rapidly preparing mesoporous SAPO-34 molecular sieve with small particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0041] Example 1: Mix 0.8 mol of 85% phosphoric acid and 50 mol of water evenly to form a transparent solution. Slowly add 1 mol of alumina powder to the above solution to form a translucent slurry, add 0.1 mol of silica gel to the slurry at one time, add 1.0 mol of template agent under stirring, after adding, mix well at room temperature , transfer and seal the above slurry to a high-pressure reaction tank, heat up to 80 degrees and continue stirring for 24 hours. Then add 3.0 mol of mesoporous agent ethylene glycol amine (substituent R=H), mix evenly, heat up to 200 degrees at 25 degrees per hour, and crystallize for 3 hours under autogenous pressure of 200 degrees. After crystallization, The valve is opened to allow the water vapor to evaporate and the condensate is collected for reuse. The residue was cooled, the solid crystals were separated by filtration, washed with deionized water until neutral, and the solid was dried at 100°C under normal pressure. The obtained prod...

Embodiment example 2

[0046] Example 2: N-methyl substituted ethylene glycol amine as a pore-forming agent (substituent R=CH3). Mix 0.8 mol of 85% phosphoric acid and 50 mol of water to form a transparent solution. Slowly add 1 mol of alumina powder to the above solution to form a translucent slurry, add 0.1 mol of silica gel to the slurry at one time, add 1.0 mol of template agent under stirring, after adding, mix well at room temperature , transfer and seal the above slurry to a high-pressure reaction tank, and continue to stir for 24 hours. Then add 3.0 mol of mesoporous agent: N-methyl substituted ethylene glycol amine, raise the temperature to 200 degrees, and crystallize for 3 hours under the autogenous pressure of 200 degrees. After crystallization, open the valve to allow the water vapor to evaporate, and condense to collect Reuse. The residue was cooled, the solid crystals were separated by filtration, washed with deionized water until neutral, and the solid was dried at 100°C under norm...

Embodiment example 3

[0047] Example 3: N-ethyl substituted ethylene glycol amine as a pore forming agent (substituent R=CH2CH3). Mix 0.8 mol of 85% phosphoric acid and 50 mol of water to form a transparent solution. Slowly add 1 mol of alumina powder to the above solution to form a translucent slurry, add 0.1 mol of silica gel to the slurry at one time, add 1.0 mol of template agent under stirring, after adding, mix well at room temperature , transfer and seal the above slurry to a high-pressure reaction tank, and continue to stir for 24 hours. Then add 3.0 mol of mesoporous agent: N-ethyl substituted ethylene glycol amine, raise the temperature to 200 degrees, and crystallize for 3 hours under the autogenous pressure of 200 degrees. After crystallization, open the valve to allow the water vapor to evaporate, and condense to collect Reuse. The residue was cooled, the solid crystals were separated by filtration, washed with deionized water until neutral, and the solid was dried at 100°C under nor...

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Abstract

The invention provides a production method of a mesoporous SAPO-34 suitable for commercial applications. A hydrothermal synthesis method commonly used for industries is adopted, wherein a cheap organic pore-forming medium for commercial supply is introduced, the cheap organic pore-forming medium is not only capable of forming pores, but also capable of accelerating a crystallization process. Diethanolamine and N-substituted derivatives thereof form a large-pore structure once in a crystallization process, and the pore diameter of the large-pore structure can be regulated according to the sizeof a substituted organic group of the large-pore structure; and the formation time of a crystal nucleus is shortened by the N-substituted derivatives and a templating agent tetraethylammonium hydroxide (TEAOH), so that the crystallization process is accelerated. Crystallization can be finished within 3h, diethanolamine and the N-substituted derivatives thereof are removed by washing, and the generated SAPO-34 is high in crystallinity and high in olefin selectivity.

Description

technical field [0001] The invention relates to a new production process of SAPO-34 molecular sieve, specifically relates to the synthesis of silicoaluminophosphate molecular sieve with mesoporous structure, and is mainly used in coal-to-olefin CTO and methanol-to-olefin MTO catalyst products. Background technique [0002] In 1984, United Carbide Chemical Corporation (UCC) first discovered a new type of aluminum silicon phosphate molecular sieve with adjustable pore size, referred to as SAPO-n (US4440871 and US4499327). It is similar to chabazite, the crystal is an eight-membered ring, and oxygen atoms connect P, Al and silicon to form three-dimensional intersecting channels. SAPO-34 is one of them. It has a unique pore size of 0.43 to 0.5nm, which is just suitable for the entry and exit of methanol molecules. At the same time, Si (+4 valence) replaces P (+5 valence) and Al (+3 valence) in the molecular sieve. Acidic, so that it has a unique catalytic activity, so that coal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85C07C1/20C07C11/02
CPCB01J29/85C01B37/08C01B39/54C01P2002/72C01P2004/01C01P2006/80C07C1/20C07C2529/85C07C11/02
Inventor 赵玉亮邹新国张卫东
Owner 岳阳慧璟新材料科技有限公司
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