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Silicoaluminophosphate molecular sieve with RHO framework structure and preparation method of silicoaluminophosphate molecular sieve

A technology of silicoaluminophosphate and skeleton structure, which is applied in the direction of molecular sieve catalysts, including molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, and can solve problems such as high silicon content and affecting catalytic effects

Pending Publication Date: 2019-10-22
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

[0005] The reported synthesis methods include hydrothermal method, dry glue method and amine thermal method, but diethylamine is mostly used as template in the synthesis process, and diethylamine has a strong guiding ability to SAPO-34 as template, so Competing phase of SAPO-34 often occurs during synthesis
Patent CN 106892440A uses N,N'-dimethylethylenediamine as a template to synthesize SAPO molecular sieve with RHO structure, but the molecular sieve has a high silicon content and a large number of silicon islands exist, which affects the catalytic effect

Method used

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  • Silicoaluminophosphate molecular sieve with RHO framework structure and preparation method of silicoaluminophosphate molecular sieve
  • Silicoaluminophosphate molecular sieve with RHO framework structure and preparation method of silicoaluminophosphate molecular sieve
  • Silicoaluminophosphate molecular sieve with RHO framework structure and preparation method of silicoaluminophosphate molecular sieve

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Embodiment 1

[0099] The preparation of embodiment 1 sample 1

[0100] Preparation of RHO-SAPO seed crystal SEED1:

[0101] Using the synthesis method in the document Chem. Mater. 2011, 23, 1406-1413, a RHO-SAPO molecular sieve of about 1 micron was synthesized. The obtained molecular sieve was calcined at 600° C. for 4 hours to remove the template agent. Then it was placed in a ball mill at a speed of 550 rpm for 2 hours to obtain RHO-SAPO seed crystals, which were named SEED1.

[0102] Preparation of RHO-SAPO molecular sieve sample 1:

[0103] Mix 4.040g aluminum isopropoxide (99%), 1.806g phosphoric acid (85%), and 3.449g N-methyl n-butylamine (99%) in 17.280g deionized water and stir evenly, then add 0.490g white Carbon black (96%), after dissolving 1.428g cetyltrimethylammonium bromide (99%), add it to the above-mentioned gel system, stir vigorously and mix uniformly to obtain mixture I; then, RHO-SAPO seed Add mixture I, the addition amount of RHO-SAPO seed crystal is Al in the mi...

Embodiment 2

[0104] The preparation of embodiment 2 sample 2

[0105] Preparation of RHO-SAPO seed crystal SEED2:

[0106] Using the synthesis method in the document CrystEngComm.2015, 17, 8555-8561, a RHO-SAPO molecular sieve with a diameter of about 200 nanometers was synthesized. The obtained molecular sieve was calcined at 600° C. for 4 hours to remove the templating agent to obtain the RHO-SAPO seed crystal, which was named SEED2.

[0107] Preparation of RHO-SAPO molecular sieve sample 2:

[0108] The specific operation is the same as in Example 1, the difference being that 0.490g white carbon black (96%) is changed into 0.830g tetraethyl orthosilicate (96%) in Example 1, and the crystallization condition is changed into 180 ℃ of crystallization 24h, the rest of the conditions remain unchanged. The obtained RHO-SAPO molecular sieve is designated as sample 2. The obtained sample 2 was subjected to XRD diffraction analysis, and its spectrum was similar to that of sample 1, indicatin...

Embodiment 3

[0109] The preparation of embodiment 3 sample 3

[0110] Preparation of RHO-SAPO seed crystal SEED3:

[0111] Using the synthesis method in the document Chem. Mater. 2011, 23, 1406-1413, a RHO-SAPO molecular sieve of about 1 micron was synthesized. The obtained molecular sieve was calcined at 600° C. for 4 hours to remove the templating agent to obtain the RHO-SAPO seed crystal, which was named SEED3.

[0112] Preparation of RHO-SAPO molecular sieve sample 3:

[0113] The specific operation is the same as that in Example 1, except that the crystallization process is aging at 120° C. for 2 hours and crystallization at 240° C. for 8 hours. The obtained RHO-SAPO molecular sieve is designated as sample 3. Part of the obtained sample was taken for XRD diffraction analysis, and its spectrum was similar to that of sample 1, indicating that the synthesized sample was a molecular sieve with a RHO structure. The scanning electron micrograph (SEM) of sample 3 is similar to that of sa...

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Abstract

The invention discloses a silicoaluminophosphate molecular sieve with an RHO framework structure. The anhydrous chemical composition of the molecular sieve is as shown in a formula I: mR.(Si<x>Al<y>P<z>)O2, wherein R represents a templating agent, and the structural formula of R is shown in a formula II and / or a formula III (please see the description for the formulas); R1, R2 and R3 are independently selected from hydrocarbon groups of C1-C6; at least one of R1 and R2 is an alkyl group of C1-C6; and the RHO-SAPO molecular sieve can be used for an acid catalytic reaction and has high olefin selectivity.

Description

technical field [0001] The application relates to a silicoaluminophosphate molecular sieve, in particular to a silicoaluminophosphate molecular sieve with an RHO skeleton structure and its preparation method and application, belonging to the field of chemical materials. Background technique [0002] In 1982, the United States Union Carbide Corporation (UCC) developed a series of PO 2 + and AlO 2 - Aluminum phosphate molecular sieve AlPO with regular channels or cage structure composed of tetrahedral shared vertices (J.Am.Chem.Soc.1982,4,1146-1147;). Then in 1984, Si atom isomorphically substituted for P and Al, and another series of silicoaluminophosphate molecular sieve SAPO was synthesized (J.Am.Chem.Soc.1982,4,1146-1147;). The AlPO molecular sieve framework is electrically neutral, while the SAPO molecular sieve is electronegative due to the introduction of silicon, so the SAPO molecular sieve after roasting has proton acid sites, so that the SAPO molecular sieve has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85C07C1/20C07C11/02C07C11/04C07C11/06
CPCB01J29/85C01B37/08C01B39/54C01P2002/72C01P2002/86C01P2004/03C01P2004/61C01P2004/62C07C1/20C07C2529/85C07C11/02C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 郭鹏闫娜娜田鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI