SAPO (silicoaluminophosphate) molecular sieve as well as preparation method and application thereof

A silicoaluminophosphate and molecular sieve technology, applied in the field of molecular sieves, can solve the problems of identification, weak characteristic diffraction peak width, and few synthetic reports.

Active Publication Date: 2017-08-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In silicoaluminophosphate molecular sieves, due to the highly disordered intergrowth of eutectic molecular sieves, the respective characteristic diffraction peaks are broadened and ver...

Method used

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  • SAPO (silicoaluminophosphate) molecular sieve as well as preparation method and application thereof
  • SAPO (silicoaluminophosphate) molecular sieve as well as preparation method and application thereof
  • SAPO (silicoaluminophosphate) molecular sieve as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] The molar ratios and crystallization conditions of each raw material are shown in Table 2. The specific batching process is as follows: the diisopropanolamine solid is dissolved into a liquid solvent in a 60°C water bath, and the pseudo-boehmite (Al 2 o 3 mass percentage content 72.5%) and diisopropanolamine (mass percentage content 99%) mixing and stirring, then add silica sol (SiO 2 Mass percent composition 30.04%), stir well, then phosphoric acid (H 3 PO 4 mass percentage 85%) was added dropwise, stirred evenly, then water and trimethylamine solution were added, stirred evenly to form a gel, and the gel was transferred to a stainless steel reaction kettle. After putting the reaction kettle into the oven, the temperature was programmed to 200°C for dynamic crystallization for 18 hours. After the crystallization, the solid product was centrifuged, washed, and dried in air at 100° C. to obtain the molecular sieve raw powder sample. The XRD spectrum of the sample sh...

Embodiment 2-18

[0077] The specific batching ratio and crystallization conditions are shown in Table 2, and the specific batching process is the same as in Example 1.

[0078] Synthetic samples were analyzed by XRD, and the XRD data results were close to those in Table 3. According to different synthesis conditions, the 2θ value of diffraction peak A varies between 12.82°~13.2°, the 2θ value of diffraction peak B varies between 17.63°~18.15°, and the 2θ value of diffraction peak C varies between 21.80°~22.40° The 2θ value of the diffraction peak D varies between 25.92° and 26.38°. In the XRD diffraction data of all samples, the peak intensity of diffraction peak B is the largest, and the relative peak intensity is 1; According to the difference of synthetic conditions, the relative peak intensity of diffraction peak A (I A / I B ) varies between 0.1 and 0.5, the relative peak intensity of diffraction peak C (I C / I B ) varies between 0.1 and 0.7, the relative peak intensity of the diffract...

Embodiment 19

[0082] Carry out to the former powder sample of embodiment 1-10 13 C MAS NMR analysis by diisopropanolamine and trimethylamine 13 The C MAS NMR standard spectrum was compared, and it was found that the sample had resonance peaks of diisopropanolamine and trimethylamine at the same time. Quantitative analysis was carried out based on the unique non-overlapping NMR peaks of the two substances to determine the ratio of the two.

[0083] XRF was used to analyze the bulk phase element composition of the molecular sieve product, and CHN element analysis was performed on the raw powder samples of Examples 1-7. Integrated CHN elemental analysis, XRF and 13 As a result of C MAS NMR analysis, the composition of the obtained molecular sieve powder is shown in Table 4.

[0084] Table 4

[0085] Example Sample powder composition 1 0.04DIPA 0.09TMA (Si 0.162 Al 0.450 P 0.388 )O 2

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Abstract

The invention discloses a novel SAPO (silicoaluminophosphate) molecular sieve. An X-ray diffraction spectrum of the novel SAPO molecular sieve comprises following four diffraction peaks: a diffraction peak A, a diffraction peak B, a diffraction peak C and a diffraction peak D, wherein for the diffraction peak A, 2theta is in a range from 12.82 degrees to 13.2 degrees, and peak intensity is IA; for the diffraction peak B, 2theta is in a range from 17.63 degrees to 18.15 degrees, and peak intensity is IB; for the diffraction peak C, 2theta is in a range from 21.80 degrees to 22.40 degrees, and peak intensity is IC; for the diffraction peak D, 2theta is in a range from 25.92 degrees to 26.38 degrees, and peak intensity is ID; the peak intensity IB of the diffraction peak B is the maximum; a peak intensity ratio of each of other diffraction peaks except the diffraction peak A, the diffraction peak C and the diffraction peak D to the diffraction peak B does not exceed 0.07. The SAPO molecular sieve is taken as a catalyst to be applied to an acid catalyzed reaction and a reaction for preparing olefins from an oxygen-containing compound through conversion, and shows good catalysis performance; the SAPO molecular sieve is used for separation of CO2 from CH4 and/or N2 and shows good gas adsorptive separation performance.

Description

technical field [0001] The application relates to a novel SAPO molecular sieve, its synthesis method and application, and belongs to the field of molecular sieves. Background technique [0002] The silicoaluminophosphate molecular sieve (SAPO) series molecular sieves were developed by United Carbide Corporation (UCC) in 1984 (US4440871). 2 , AlO 2 - , PO 2 + A microporous crystal composed of three tetrahedral units. Because the skeleton is negatively charged, there are balance cations outside the skeleton, so it has cation exchange properties. When the cation outside the skeleton is H + When , the molecular sieve has an acidic center, so it will have acid-catalyzed reaction properties. Aluminosilicate molecular sieves have been used as active components of catalysts in the fields of oil refining and petrochemicals, such as catalytic cracking, hydrocracking, isomerization, alkylation of aromatics, conversion of oxygen-containing compounds, etc. [0003] Generally, the ...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54B01J29/85C07C1/20C07C11/04C07C11/06B01J20/18B01D53/02
CPCB01D53/02B01D2253/108B01J20/18B01J29/85B01J2229/40C01B37/08C01B39/54C01P2002/72C01P2004/03C01P2004/30C01P2004/61C01P2006/12C01P2006/14C07C1/20C07C11/04C07C11/06Y02C20/40Y02P20/151Y02P20/50Y02P20/52Y02P30/20Y02P30/40
Inventor 田鹏王德花刘中民向骁杨淼郜贝贝
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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