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Preparation method of SAPO-34 molecular sieve and application of SAPO-34 molecular sieve to preparation of olefin through methanol conversion

A technology of SAPO-34 and molecular sieve, applied in the direction of molecular sieve catalyst, molecular sieve and alkali-exchanged phosphate, chemical instruments and methods, etc., can solve the problems of crystallization product recovery and washing loss, low solid content of synthetic gel, low volume output, etc. , to achieve the effect of controllable grain shape, grain size and high selectivity

Inactive Publication Date: 2017-11-28
天津众智科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem in the prior art is that the synthesis yield is low, or the solid content of the synthesis gel is low, resulting in a low output per unit volume of the overall high-pressure synthesis kettle, and the subsequent recovery and washing loss of the crystallization product is serious

Method used

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  • Preparation method of SAPO-34 molecular sieve and application of SAPO-34 molecular sieve to preparation of olefin through methanol conversion
  • Preparation method of SAPO-34 molecular sieve and application of SAPO-34 molecular sieve to preparation of olefin through methanol conversion
  • Preparation method of SAPO-34 molecular sieve and application of SAPO-34 molecular sieve to preparation of olefin through methanol conversion

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] (1) Gel preparation: First, 1110 grams of distilled water was added to a 4L autoclave, the stirring speed was 100 rpm, and 511.3 grams of pseudo-boehmite with a solid content of 70wt.% was slowly added, and the gel was pre-prepared in a 40°C oil bath. Heat, then slowly add 879.3 grams of phosphoric acid with a concentration of 85wt.%, stir evenly, then slowly add 55.6 grams of silica sol with a concentration of 40wt.%, stir evenly, finally add 1557 grams of tetraethylammonium hydroxide with a concentration of 25wt.% Aqueous solution, then add 26.4 grams of isopropylamine template agent and 30.4 grams of triethylamine template agent, increase the stirring speed to 200 rpm, stir for 5 hours, make the system a uniform gel; Cut at 3000 rpm for 20 minutes. Aging at room temperature (25°C) for 13 hours.

[0061] (2) Crystallization: With a heating rate of 0.04°C / min, the temperature is raised to 204°C, the crystallization time is 45 hours, and the stirring speed is 300 rpm. ...

Embodiment 2

[0068] (1) Gel preparation: First, 209.52 kg of distilled water was added to a 1000L high-pressure reactor, the stirring speed was 100 rpm, and 101.25 kg of pseudo-boehmite with a solid content of 70wt.% was slowly added, and preheated at 40°C. Preheat the high-temperature oil and control the temperature, then slowly add 166.35 kg of phosphoric acid with a concentration of 85wt.%, stir evenly, then slowly add 10.52 kg of silica sol with a concentration of 40wt.%, stir evenly, and finally add 294.60 kg of phosphoric acid with a concentration of 25wt.%. Tetraethylammonium hydroxide aqueous solution, then add 21.3 kilograms of diethylamine templating agent, increase the stirring speed to 500 rev / min, stir for 8 hours, make the system become uniform gel; Cut at 5000 rpm for 40 minutes. Aging at room temperature (25°C) for 16 hours.

[0069] (2) Crystallization: Heat up to 178°C at a heating rate of 0.36°C / min, crystallize for 20 hours, and stir at a speed of 60 rpm. After the cry...

Embodiment 3

[0076] (1) Gel preparation: First, 254.42 kilograms of distilled water is added to a 1000L high-pressure reactor, the stirring speed is 100 rpm, and 122.94 kilograms of pseudo-boehmite with a solid content of 70wt.% is slowly added, and it is heat-resistant at 40 ° C. The oil is preheated and temperature controlled, then slowly add 201.99 kg of phosphoric acid with a concentration of 85wt.%, stir evenly, then slowly add 12.77 kg of silica sol with a concentration of 40wt.%, stir evenly, and finally add 357.72 kg of phosphoric acid with a concentration of 25wt.%. Tetraethylammonium hydroxide aqueous solution, then add 30.4 kilograms of triethylamine template agent and 21.3 kilograms of diethylamine template agent, increase stirring speed to 600 rev / min, stir 18 hours, make system become homogeneous gel; The homogeneous gel was sheared on a homogenizer at 6000 rpm for 60 minutes. Aging at room temperature (25°C) for 16 hours.

[0077] (2) Crystallization: at a heating rate of 0...

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Abstract

A preparation method of a SAPO-34 molecular sieve comprises the following steps: adding an aluminium source into deionized water in a room-temperature stirring state; then adding a phosphorus source, and performing uniform stirring; after that, slowly adding a silicon source, and continually performing uniform stirring; at last, adding a tetraethylammonium hydroxide solution; continually adding one or more of isopropylamine, diethylamine and triethylamine after uniform stirring; performing stirring to ensure a homogeneous system; and performing homogeneity, crystallization, press-filtration, washing and calcining to obtain the SAPO-34 molecular sieve. The preparation method has the advantages that the molecular sieve is high in synthetic yield, high in degree of crystallinity and high in diene selectivity.

Description

technical field [0001] The invention provides a preparation method of molecular sieves. Specifically, it is the preparation method of SAPO-34 molecular sieve and its application in the conversion of methanol to olefins. Background technique [0002] SAPO-34 is a new silicon aluminum phosphorus molecular sieve with chabazite structure (CHA) invented by Union Carbide Corporation (UCC) in 1984. SAPO-34 molecular sieve has the advantages of medium-strength acid center, unique small window channel structure (eight-membered ring, pore diameter about 3.6 angstroms), large supercage, abundant micropores, large specific surface area, etc. Methanol to olefins (MTO), conversion of low-carbon oxygenated compounds such as methyl chloride and ethanol to olefins, high-carbon alkanes or olefins cracking to low-carbon olefins and other catalytic fields, automotive exhaust purification fields, membrane separation fields and functional materials fields have won Wide range of applications. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54B01J29/85C07C1/20C07C11/04C07C11/06
CPCB01J29/85C01B39/54C01P2002/72C01P2004/03C01P2004/38C01P2004/61C01P2006/12C07C1/20C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 常云峰褚绮周杰
Owner 天津众智科技有限公司