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Preparation method of small-grain SAPO-34 molecular sieve

A SAPO-34 and molecular sieve technology, applied in the chemical field, can solve the problems of high cost and difficult industrial scale-up of the preparation process, and achieve the effects of easy operation, regular crystal form and simple steps

Inactive Publication Date: 2015-04-29
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is to provide a preparation method of small-grain SAPO-34 molecular sieve, which overcomes the problems of high cost of the existing small-grain SAPO-34 preparation method and difficult industrial scale-up of the preparation process.

Method used

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  • Preparation method of small-grain SAPO-34 molecular sieve
  • Preparation method of small-grain SAPO-34 molecular sieve
  • Preparation method of small-grain SAPO-34 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Under stirring at room temperature, 231.3g of aluminum isopropoxide (Al 2 o 3 Content is 26.3%) drop into 682g deionized water, slowly add 137.4g orthophosphoric acid (H 3 PO 4 Content is 85%), after stirring for 2h, add 71.4g silica sol (SiO 2 content is 30%), 266.4g triethylamine, 81.6gTMAmOH solution (TMAmOH content is 25%) and 51.3g n-hexane, after stirring for 3h, a uniform gel is formed; subsequently the gel is transferred to a 2L crystallization kettle, at 120rpm Crystallize at 180°C for 48 hours while stirring. After the crystallization is completed, the mixed solution is obtained, and the mixed solution is filtered to obtain a filter cake. While filtering, the filter cake is washed with deionized water until the pH value of the filtrate is less than 8, dried at 80-120°C for 3-8 hours, 550-600 Roasting at ℃ for 5-6 hours, the target product was obtained, which was named as A. After XRD and SEM characterization tests, it is found that product A has character...

Embodiment 2

[0036] Under stirring at room temperature, 105.8g of pseudo-boehmite (Al 2 o 3 Content is 76.5%) drop into 884.8g deionized water, add 183.0g orthophosphoric acid (H 3 PO 4 Content is 85%), after stirring for 2h, add 95.2g silica sol (SiO 2 content is 30%), 355.2g triethylamine and 54.5gTMAmOH solution (TMAmOH content is 25%), after stirring for 3h, a uniform gel is formed; then the gel is transferred to a 2L crystallization tank, and stirred at 120rpm at 190°C Heat preservation and crystallization for 48h. After the crystallization is completed, filter the mixed solution to obtain a filter cake. While filtering, wash the filter cake with deionized water until the pH value of the filtrate is less than 8. Dry at 80-120°C for 3-8 hours, 550-600 Roasting at ℃ for 5-6 hours, the target product was obtained, which was named as B. After XRD and SEM characterization tests, it is found that product B has the characteristic diffraction peaks of CHA, such as image 3 As shown, the...

Embodiment 3

[0038] Under stirring at room temperature, 96.8g of pseudo-boehmite (Al 2 o 3 Content is 76.5%) drop into 813g deionized water, add 168.3g orthophosphoric acid (H 3 PO 4 Content is 85%), after stirring for 2h, add 86.9g silica sol (SiO 2 Content is 30%), 216.7g triethylamine, 49.9gTMAmOH solution (TMAmOH content is 25%) and 67.1g toluene, after stirring for 3h, a homogeneous gel is formed; then the gel is transferred to a 2L crystallization kettle, stirred at 120rpm Under the condition of 200 ℃ heat preservation and crystallization for 48h. After the crystallization is completed, the mixed solution is obtained, and the mixed solution is filtered to obtain a filter cake. While filtering, the filter cake is washed with deionized water until the pH value of the filtrate is less than 8, dried at 80-120°C for 3-8 hours, 550-600 Roasting at ℃ for 5-6 hours, the target product was obtained, which was named as C. After XRD and SEM characterization tests, it was found that product...

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Abstract

The invention relates to a preparation method of a small-grain SAPO-34 molecular sieve. The preparation method comprises the following steps: mixing an aluminum source and a phosphorus source with deionized water, stirring for 1-5 h, then adding a silicon source, an organic amine template agent R, an auxiliary template agent R' and an organic solvent A, continuously stirring for 1-5 h to obtain a gel, transferring the gel into a crystallization kettle, crystallizing for 12-108 h at the temperature of 160-220 DEG C to obtain a mixed liquor, filtering the mixed liquor to obtain a filter cake, washing the filter cake with deionized water, drying, and roasting to obtain an SAPO-34 molecular sieve. On the basis of using a conventional organic amine template agent, a small amount of auxiliary template agent R' and organic solvent A are added, and the cube-shaped SAPO-34 molecular sieve which is high in degree of crystallinity, regular in crystal form and 0.2 microns in grain size is successfully prepared through a hydrothermal crystallization method; moreover, the method is simple in procedures and easy to operate, the SAPO-34 molecular sieve has a great industrialization development prospect, and is expected to be used as a catalyst for preparing low-carbon olefinethrough methanol conversio and a catalyst for treating automobile exhaust.

Description

technical field [0001] The invention relates to a preparation method of small-grain SAPO-34 molecular sieve, which belongs to the field of chemistry. Background technique [0002] SAPO-34 is made of SiO 2 , AlO 2- 、PO 2+ , a microporous crystal composed of three tetrahedral units, belongs to the CHA structure according to the regulations of the International Zeolite and Molecular Sieve Association (IZA). Although SAPO-34 has not appeared for a long time, due to its suitable pore structure, suitable acidity and high hydrothermal stability, it has better catalytic performance than ZSM-5 in the methanol-to-olefins reaction (MTO) And low carbon olefin selectivity, so it is considered as an ideal MTO catalyst. With the deepening of research, many scientific literatures have shown that SAPO-34 is effective in the selective catalytic reduction (SCR) of NO x It can also play an important catalytic role, and it is a new type of exhaust gas treatment catalyst with great potential...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
CPCC01B39/54C01B37/08C01P2002/72C01P2004/03C01P2004/62
Inventor 于成龙张文周振垒时立辉陈士辉矫志
Owner VALIANT CO LTD
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