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Method for synthesizing small grain SAPO-18/SAPO-34 eutectic molecular sieve

A technology of SAPO-18 and SAPO-34, applied in the field of molecular sieves, can solve the problems of low catalytic activity and single pore size of molecular sieves

Active Publication Date: 2014-06-25
淄博齐创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

Chinese patent CN102372291A discloses a SAPO-18 / SAPO-34 eutectic composite molecular sieve and its preparation method, which solves the problems of single pore size and low catalytic activity of existing molecular sieves
But so far, the synthesis of small-grain SAPO-18 / SAPO-34 eutectic molecular sieves has not been reported

Method used

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  • Method for synthesizing small grain SAPO-18/SAPO-34 eutectic molecular sieve
  • Method for synthesizing small grain SAPO-18/SAPO-34 eutectic molecular sieve
  • Method for synthesizing small grain SAPO-18/SAPO-34 eutectic molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: 1) 12g pseudo-boehmite (Al 2 o 3 content is 65wt%) mixed with 12g water to form mixed solution A; 2) mixed 17.4g phosphoric acid with 4g water to form solution B; 3) mixed solution B and solution A evenly under stirring; 4) added 6.9 g triethylamine, 6 g tetraethylammonium hydroxide, and 0.4 g silica sol (41.1 wt%), and finally add 0.058 g polyethylene glycol, and stir evenly to obtain a molecular sieve synthetic liquid. 5) Transfer the prepared molecular sieve synthesis solution into a crystallization kettle, seal it and crystallize at 200°C for 2 days. After the crystallization is completed, the crystallization kettle is taken out, rapidly cooled, washed, and dried at 110°C to obtain a molecular sieve product. The XRD results show that the product is a SAPO-18 / SAPO-34 eutectic molecular sieve (such as figure 2 Shown by the middle line A), the AEI / CHA in the crystal is 67 / 33. SEM results show that the sample boundary is obvious, and the crystal size is ...

Embodiment 2

[0033] Example 2: 1) Mix 18g aluminum isopropoxide and 19.8g water to form mixed solution A; 2) Mix 5.22g phosphoric acid and 19.8g water to form solution B; 3) Mix B solution and A solution evenly under stirring 4) Add 2.28g of triethylamine, 1.8g of tetraethylammonium hydroxide and 4.86g of ethyl orthosilicate successively under stirring, add 0.055g of polyethylene glycol, and stir evenly to obtain a molecular sieve synthetic liquid. 5) Transfer the prepared molecular sieve synthesis solution into a crystallization kettle, seal it and crystallize at 200°C for 2 days. After the crystallization is completed, the crystallization kettle is taken out, rapidly cooled, washed, and dried at 110°C to obtain a molecular sieve product. The XRD results show that the product is a SAPO-18 / SAPO-34 eutectic molecular sieve (such as figure 2 Line B), the AEI / CHA in the crystal is 62 / 38. SEM results show that the sample boundary is obvious, and the crystal size is about 320-560nm (such as ...

Embodiment 3

[0034]Example 3: 1) 12g of pseudo-boehmite (Al2O3 content of 65wt%) was mixed with 18g of water to form a mixed solution A; 2) 8.8g of phosphoric acid was mixed with 18g of water to form a solution B; 3) under stirring, the B The solution was mixed evenly with liquid A; 4) 23g of triethylamine, 5g of diethylamine and 0.4g of silica sol (41.1wt%) were sequentially added under stirring, and 0.09g of polyethylene glycol was added, and stirred evenly to obtain a molecular sieve synthetic liquid. 5) Transfer the prepared molecular sieve synthesis solution into a crystallization kettle, seal it and crystallize at 200°C for 3 days. After the crystallization is completed, the crystallization kettle is taken out, rapidly cooled, washed, and dried at 110°C to obtain a molecular sieve product. The XRD results show that the product is a SAPO-18 / SAPO-34 eutectic molecular sieve (such as figure 2 Line C), the AEI / CHA in the crystal is 65 / 35. SEM results show that the sample boundary is o...

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Abstract

The invention discloses a method for synthesizing a small grain SAPO-18 / SAPO-34 eutectic molecular sieve. The method is mainly characterized in that a single-template agent or a double-template agent is adopted, a crystal growth inhibitor is added in the synthetic process, and the synthesis parameters are adjusted to carry out crystallization under high-speed stirring. The specific method comprises the following steps: forming a mixed solution A through an aluminum source and water; forming a mixed solution B through a phosphorus source and water; uniformly mixing the solution B with the solution A in a stirring state; sequentially adding the template agent and a silicon source in the stirring state; adding the crystal growth inhibitor, performing hydrothermal crystallization under high-temperature stirring, separating, washing and drying to obtain the molecular sieve. The obtained molecular sieve is characterized by using a powder X-ray diffractometer, and a ratio of AEI / CHA in the eutectic molecular sieve is calculated to be about 50 / 50-70 / 30 through DIFFaX. The obtained molecular sieve is small in grain and large in specific surface area and has high activity, selectivity and stability in an olefin preparation reaction through a catalyst methanol.

Description

technical field [0001] The invention belongs to molecular sieves, in particular to a method for synthesizing small-grain SAPO-18 / SAPO-34 eutectic molecular sieves. Background technique [0002] The silicoaluminophosphate series (SAPO) molecular sieve is a new type of molecular sieve developed by the United Carbide Corporation (UCC) in 1982. It is a microporous crystal composed of three tetrahedral units: SiO2, AlO2-, and PO2+. Catalysts containing SAPO or AlPO show excellent performance in the conversion of methanol or dimethyl ether to light olefins (US4499327). With the increasing depletion of petroleum resources, the process of preparing low-carbon olefins through coal chemical industry has attracted more and more attention from scientists. It is of great practical significance to develop a catalyst with excellent performance for the conversion of methanol or dimethyl ether to produce low-carbon olefins. [0003] Studies have shown that SAPO-34 and SAPO-18 molecular siev...

Claims

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Application Information

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IPC IPC(8): B01J29/85C07C11/04C07C11/06C07C1/20
CPCY02P20/52Y02P30/20Y02P30/40
Inventor 吉向飞赵娇娇李竞
Owner 淄博齐创新材料科技有限公司
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