SAPO (Si, Al, P, O)-44 molecular sieve as well as preparation method thereof

A technology of SAPO-44 and molecular sieve, applied in the field of preparation of SAPO-44 molecular sieve, can solve the problems of easy wall sticking, pollution, inability to completely separate the template agent mother liquor, etc., and achieve the effect of reducing the dosage and improving the technical effect.

Active Publication Date: 2014-01-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to overcome the problems in the prior art that the synthesis of SAPO-44 molecular sieve is easy to stick to the wall, agglomerate and the mother liquor of template agent cannot be completely separated, cannot be recycled and will cause environmental pollution, and provides a new The preparation method of SAPO-44

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Fully mix 10.5g of phosphoric acid (85% aqueous solution) with 30.0g of deionized water, add 6.9g of pseudo-boehmite powder into the mixed solution of phosphoric acid and water under vigorous stirring, and then add 5.5g of silica sol ( Contains SiO 2 30%), wherein the molar composition of each component added is: Al 2 o 3 :P 2 o 5 : SiO 2 =1.0:1.0:0.6. After continuing to stir at room temperature for two hours, gradually increase the reaction temperature to 80° C., and along with the evaporation of moisture in the reaction process, the viscosity of the system gradually increases until finally it becomes dry glue. Grind the obtained dry glue into powder, take the mixed solution of the dry glue and 4.5g of cyclohexylamine, 3.3g of diethylamine and 10.0g of water (volume ratio is 1:1:2) and fully mix them under stirring, and place in In a stainless steel autoclave, crystallize at 185° C. for 24 hours after the autoclave is sealed. After the crystallization reaction,...

Embodiment 2

[0019] Fully mix 13.8g of phosphoric acid (85% aqueous solution) with 50.0g of deionized water, add 7.1g of alumina powder into the mixed solution of phosphoric acid and water under vigorous stirring, and then add 9.7g of silica sol (containing SiO 2 30%), wherein the molar composition of each component added is: Al 2 o 3 :P 2 o 5 : SiO 2 =1.0:0.8:0.4. After continuing to stir at room temperature for two hours, gradually increase the reaction temperature to 80° C., and along with the evaporation of moisture in the reaction process, the viscosity of the system gradually increases until finally it becomes dry glue. Grind the obtained dry glue into powder, take the mixed solution of the dry glue and 5.3g cyclohexylamine, 8.4g triethylamine and 10.0g water (volume ratio is 1:2:1.6) and fully mix them under stirring, place in In a stainless steel autoclave, crystallize at 180° C. for 36 hours after the autoclave is sealed. After the crystallization reaction, the stainless ste...

Embodiment 3

[0022] Fully mix 10.5g of phosphoric acid (85% aqueous solution) with 30.0g of deionized water, add 6.9g of alumina powder into the mixed solution of phosphoric acid and water under vigorous stirring, and then add 1.8g of silica sol (containing SiO 2 30%), wherein the molar composition of each component added is: Al 2 o 3 :P 2 o 5 : SiO 2 =1.0:0.9:0.2. After continuing to stir at room temperature for two hours, gradually increase the reaction temperature to 80° C., and along with the evaporation of moisture in the reaction process, the viscosity of the system gradually increases until finally it becomes dry glue. Grind the obtained dry glue into powder, take the mixed solution of the dry glue and 9.0g cyclohexylamine and 10.0g water (volume ratio is 1:1) and fully mix them under stirring, put them in a stainless steel autoclave, and put the autoclave Crystallize at 180°C for 36 hours after sealing. After the crystallization reaction, the stainless steel autoclave was coo...

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Abstract

The invention relates to a preparation method of an SAPO (Si, Al, P, O)-44 molecular sieve, which mainly solves the problem that in the prior art, wall adhesion and agglomeration phenomena exist in an SAPO-44 molecular sieve synthetic process and a template agent cannot be recycled. Due to the adoption of the technical scheme which comprises the following steps: firstly, preparing molecular sieve precursor sol by an aluminum source, a silicon resource and a phosphorus source; then, drying the sol to a dry sol; and finally mixing dry sol fine powder and an aqueous liquor of the organic amine template agent and placing the mixture in a stainless steel high pressure kettle for crystallization for 16-72 hours at 150-210 DEG C, the problem is solved, wherein the template agent is a compound template agent selected from a single cyclohexylamine template agent or any one of diethylamine, triethylamine, tetraethyl ammonium hydroxide and di-n-propylamine templates and cyclohexylamine. The method can be used for technical preparation of the SAPO-44.

Description

technical field [0001] The invention relates to a preparation method of SAPO-44 molecular sieve. Background technique [0002] In 1982, United Carbide Corporation (UCC) introduced AlPO for the first time. 4 Molecular sieve. The framework of this type of molecular sieve is neutral, has no exchangeable cations, lacks the protonic acid required for the catalytic activity of carbon ions, and exhibits weak acid catalytic performance. In 1984, Lok et al introduced Si into AlPO 4 Among the series of molecular sieves, a series of silicoaluminophosphate (SAPO) molecular sieves were synthesized, the framework of which is electronegative, so has exchangeable cations, and has proton acidity. The crystal structure of SAPO-44 is similar to chabazite type (CHA), and its basic structural unit is a double six-membered ring. These double six-membered rings are connected by some four-membered rings to form a three-dimensional channel structure with the largest eight-membered ring. It belon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 赵昱刘红星王伟管洪波
Owner CHINA PETROLEUM & CHEM CORP
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