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Synthesis method of silicoaluminophosphate molecular sieve SAPO-34

A technology of SAPO-34 and synthesis method, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of high template price, high cost, unfavorable industrial production and promotion, etc., and achieve high-efficiency recycling , avoid pollution, novel and efficient preparation method

Inactive Publication Date: 2015-03-25
天津神能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These templates are generally expensive and the cost of synthesis is too high, which is not conducive to large-scale industrial production and promotion.

Method used

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  • Synthesis method of silicoaluminophosphate molecular sieve SAPO-34
  • Synthesis method of silicoaluminophosphate molecular sieve SAPO-34

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 8. Add 301g of phosphoric acid with a mass percentage of 85% to 31g of the mother liquor synthesized by using triethylamine as a template agent. After mixing evenly, slowly add 5.505g of pseudo-boehmite (Al2O3 mass percentage is 66.7%), and then fully stir evenly for about 2h; then add 2.28g of silica sol (SiO2 mass percentage is 30%) and stir thoroughly, while stirring, use organic template triethylamine or other to adjust the pH of the colloid to 6.0-7.0, about 8.0ml of triethylamine is used. Stir well, then put it into a crystallization kettle for hydrothermal dynamic crystallization at 200°C for 24 hours, filter, wash and dry the product, and XRD phase analysis shows that it is a pure phase SAPO-34 molecular sieve (see figure 1 ) is 105% relative to the crystallinity synthesized without mother liquor.

Embodiment 2

[0017] 8.301g of phosphoric acid with a mass percentage of 85% was added to 31g of the mother liquor synthesized with tetraethylammonium hydroxide as a template, and after mixing evenly, 5.505g of pseudo-boehmite (Al2O3 with a mass percentage of 66.7%) was slowly added, and then fully Stir evenly for about 2 hours; then add 2.28g of silica sol (SiO2 mass percentage is 30%) and stir thoroughly, while stirring, use organic template tetraethylammonium hydroxide or other to adjust the pH value of the colloid to about 7.5, about 12ml TEAOH ( TEAOH mass percent is 35%). Stir well, then put it into a crystallization kettle for hydrothermal dynamic crystallization at 200°C for 24 hours, after the product is filtered, washed, and dried, XRD phase analysis shows that the crystallinity of SAPO-34 molecular sieve is pure phase compared to that synthesized without mother liquor is 110%.

Embodiment 3

[0019] 8. Add 301g of phosphoric acid with a mass percentage of 85% to 31g of the mother liquor synthesized with morpholine as a template agent, mix well and slowly add 5.505g of pseudo-boehmite (Al2O3 mass percentage is 66.7%), and then fully stir for about 2 hours ; Then add 2.28g of silica sol (SiO2 mass percentage is 30%) and stir well, while stirring, use organic template tetramorpholine or other to adjust the pH value of the colloid to about 7.5, and about 5ml of morpholine (TEAOH mass percentage is 35% ). Stir well, then put it into a crystallization kettle for hydrothermal dynamic crystallization at 200°C for 24 hours, after the product is filtered, washed, and dried, XRD phase analysis shows that the crystallinity of SAPO-34 molecular sieve is pure phase compared to that synthesized without mother liquor was 112%.

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Abstract

The invention provides a synthesis method of a silicoaluminophosphate molecular sieve SAPO-34, belonging to the field of catalyst preparation methods. The method comprises the following steps: by using a recovered mother solution of a previously synthesized sample as the volume consumption required by synthesis, adding a phosphorus precursor into the recovered mother solution, uniformly mixing, slowly adding an aluminum precursor, and sufficiently stirring uniformly; adding a silicon precursor, sufficiently stirring, and regulating the pH value of the colloid to 6.0-7.0 with an organic template while stirring; and sufficiently stirring uniformly, crystallizing in a crystallizing kettle at 160-220 DEG C for 0.5-100 hours, centrifuging, washing, and drying to obtain the SAPO-34 molecular sieve catalyst. The method is novel, has the advantages of high efficiency and favorable repetitiveness, greatly lowers the synthesis cost, effectively avoids the environmental pollution caused by mother solution discharge, and implements circular and efficient utilization of the raw material.

Description

technical field [0001] The invention belongs to the field of catalyst preparation methods, and in particular relates to a synthesis method of silicoaluminophosphate molecular sieve SAPO-34. Background technique [0002] In 1984, the United States Union Carbide Corporation (UCC) developed a series of silicoaluminophosphate molecular sieves (SAPO-n, n represents the structural model). One of the most eye-catching is SAPO-34 molecular sieve. SAPO-34 molecular sieve made of PO 4 , AlO 4 and SiO 4 The tetrahedrons are connected with each other; it has an elliptical cage and a three-dimensional pore structure composed of oxygen eight-membered rings. The shape of the oxygen eight-membered ring may be oval, circular or wrinkled, and the size of the pore varies with the shape of the oxygen eight-membered ring, but the effective diameter of the pore remains between 0.43 and 0.50 nm. The pore volume is 0.42cm3 / g, the space symmetry group is R3m, it belongs to the trigonal crystal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2002/72C01P2004/03
Inventor 袁忠勇王震宇李晓文王宝义
Owner 天津神能科技有限公司
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