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Solvent thermal synthesis method of SAPO (silicoaluminophosphate) molecular sieve and catalyst prepared by SAPO molecular sieve

A synthesis method and technology of SAPO-34, applied in the synthesis field of SAPO molecular sieve, can solve the problems of increased synthesis cost, low crystallinity of RHO-SAPO molecular sieve, difficult separation, etc., and achieves improved ethylene propylene selectivity and excellent catalytic performance. , the effect of low waste liquid generation

Inactive Publication Date: 2012-07-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the hydrothermal synthesis method with the participation of surfactants, on the one hand, since the synthesis process uses water as the continuous phase and main solvent of the synthesis system, a large amount of waste liquid that is difficult to use will be generated after synthesis, which increases the pressure of environmental protection treatment; On the other hand, relatively expensive surfactants are used in the synthesis process, which increases the synthesis cost
In the xerogel synthesis method without the participation of surfactants, the silicon-phosphorus-aluminum xerogel must first be configured, and the process is complicated; moreover, the crystallinity of the RHO-SAPO molecular sieve obtained by this synthesis method is not high, and the obtained RHO-SAPO molecular sieve It is often difficult to separate from the uncrystallized silicon-phosphorus-aluminum xerogel by washing and other methods

Method used

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  • Solvent thermal synthesis method of SAPO (silicoaluminophosphate) molecular sieve and catalyst prepared by SAPO molecular sieve
  • Solvent thermal synthesis method of SAPO (silicoaluminophosphate) molecular sieve and catalyst prepared by SAPO molecular sieve
  • Solvent thermal synthesis method of SAPO (silicoaluminophosphate) molecular sieve and catalyst prepared by SAPO molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 7.03g activated alumina (Al 2 o 3 Mass percentage composition 72.5%) mixes and stirs with 60ml triethylamine, and adds 10.30g orthophosphoric acid (H 3 PO 4 Mass percent composition 85%), 5.69g silica sol (SiO 2 Mass percentage content 28.2%), 0.50g ethanol and 0.3g deionized water, stir vigorously to make it evenly mixed, and after stirring at 40°C for 10h, transfer the gel to a stainless steel reaction kettle, at a crystallization temperature of 180°C Under dynamic synthesis for 60 hours. After the crystallization, the solid product was centrifuged, washed, and dried in air at 100° C. to obtain 14.1 g of raw powder (15% weight loss on calcination). The samples were analyzed by XRD. The XRD data are shown in Table 1, and the results show that the synthesized product is SAPO-34 molecular sieve.

Embodiment 2

[0041] 7.03g activated alumina (Al 2 o 3 Mass percentage composition 72.5%) mixes with the triethylamine of 50ml diethylamine and 15ml and stirs, and in stirring state, once adds 9.5g orthophosphoric acid (H 3 PO 4 Mass percent composition 85%), 4.55g silica sol (SiO 2 Mass percent content 28.2%), 0.38g methanol, vigorously stirred to make it evenly mixed, and after stirring at 55°C for 12h, the gel was transferred to a stainless steel reactor, and dynamically synthesized at a crystallization temperature of 180°C for 100 hours. After the crystallization, the solid product was centrifuged, washed, and dried in air at 100° C. to obtain 13.0 g of the original powder (14.1% weight loss on calcination). The samples were analyzed by XRD. The XRD data are shown in Table 2, and the results show that the synthesized product is SAPO-34 molecular sieve.

Embodiment 3

[0045] 7.03g activated alumina (Al 2 o 3 Mass percentage composition 72.5%) mixes and stirs with the morpholine of 23.13ml triethylamine and 60ml, and once adds 10.30g orthophosphoric acid (H 3 PO 4 Mass percent composition 85%), 4.55g silica sol (SiO 2 mass percent content 28.2%), 1.0g ethanol and 2.04g deionized water, stir vigorously to make it evenly mixed, and after stirring at 35°C for 12h, transfer the gel to a stainless steel reaction kettle, and crystallize at 210°C Dynamic synthesis at temperature for 24 hours. The solid product was centrifuged, washed with deionized water until neutral, and dried in the air at 100° C. to obtain 13.6 g of raw powder (calcination weight loss 14.5%). The samples were analyzed by XRD, and the data are shown in Table 3. The XRD data indicated that the synthesized product was SAPO-34 molecular sieve.

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Abstract

The invention relates to a solvent thermal synthesis method of an SAPO (silicoaluminophosphate) molecular sieve and a catalyst prepared by the SAPO molecular sieve. The solvent thermal synthesis method provided by the invention is characterized in that organic amine is directly used as a solvent and a template agent of a synthesis system, and the SAPO molecular sieve is prepared through solvent thermal synthesis.

Description

technical field [0001] The invention relates to a method for synthesizing SAPO molecular sieves. [0002] The present invention also relates to the catalytic application of the above-mentioned materials in the reaction of converting oxygen-containing compounds into light olefins. Background technique [0003] Since a series of aluminum phosphate molecular sieves and their derivatives were successfully synthesized in the patent US 4310440 applied by Union Carbide Corporation in 1982, aluminum phosphate molecular sieves and their heteroatom-substituted derivatives have been a research hotspot in the field of materials and catalysis. one. The technical feature of this kind of SAPO molecular sieve synthesis is to use silicon source, aluminum source, phosphorus source and different templates to synthesize, and the structural unit is composed of PO 2+ , AlO 2- and SiO 2 Composition of tetrahedrons. Among these molecular sieves, some molecular sieves with small pore structure ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85C07C1/20C07C11/04C07C11/06
CPCC01B39/54B01J29/85C01B37/08Y02P30/20Y02P30/40C07C1/20C07C2529/85
Inventor 田鹏刘中民张莹樊栋苏雄
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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