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A kind of sapo-44 molecular sieve and synthetic method thereof

A SAPO-44, molecular sieve technology, used in molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, chemical instruments and methods, etc., can solve the problems of surface element composition and body differences, and achieve excellent catalytic performance and gas adsorption and separation performance. Effect

Active Publication Date: 2015-11-18
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

Generally speaking, SAPO molecular sieves generally show the characteristics of silicon-rich crystal grain surface, but it is worth pointing out that even for the same SAPO molecular sieve, its surface element composition and bulk phase composition will vary with the synthesis conditions and the template used. There is a big difference due to the change of

Method used

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  • A kind of sapo-44 molecular sieve and synthetic method thereof
  • A kind of sapo-44 molecular sieve and synthetic method thereof
  • A kind of sapo-44 molecular sieve and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The molar proportions and crystallization conditions of each raw material are shown in Table 1. Concrete batching process is as follows, with 16.4g phosphoric acid (H 3 PO 4 Mass percentage composition 85%) mixes with 30g deionized water, stirs evenly, then adds 5.7g silica sol (SiO 2 mass percent content 30%), vigorously stirred for 1h. 21.5 g of hexamethyleneimine HMI (99% by mass) was added to the previous mixture, sealed and stirred for 30 min to obtain a homogeneous mixture, which was marked as A. In addition, 10g of pseudoboehmite (Al 2 o 3 Mass percent content 72.5%), 1.29g cetyltrimethylammonium bromide (CTAB) and 20.9g deionized water are mixed and stirred evenly, join in the mixture A, after sealing and stirring for 30min to make it mix evenly, the condensed The glue is transferred to a stainless steel reaction kettle. The molar ratio of each component in the synthesis system is 3.0HMI:0.4SiO 2 : 1Al 2 o 3 : 1P 2 o 5 :0.05CTAB:50H 2 O.

[0041] Ra...

Embodiment 2-10

[0052] The specific batching ratio and crystallization conditions are shown in Table 1, and the specific batching process is the same as in Example 1.

[0053] The synthetic sample is analyzed by XRD, and the result shows that the product synthesized in Example 2-10 has the structural characteristics of SAPO-44, and the XRD data result is close to Table 2, that is, the peak position and shape are the same, and the relative peak intensity is within ± fluctuate within 10%.

[0054] The surface and bulk phase element compositions of the molecular sieve products were analyzed by XPS and XRF, and the ratio of the silicon content on the outer surface to the bulk phase silicon content is listed in Table 1. The bulk phase element of the sample of Example 10 is Al 0.50 P 0.42 Si 0.08 .

[0055] The CHN elemental analysis of the raw powder samples of Examples 2-10 showed that the C / N molar ratio fluctuated at 6.0±0.05. The CHN elemental analysis results were normalized with the ino...

Embodiment 11

[0058]Take 3g of the synthetic samples of Examples 1-10 respectively, put them into a plastic beaker, add 3ml of 40% hydrofluoric acid solution to dissolve the molecular sieve skeleton under ice-water bath conditions, and then add 15ml of carbon tetrachloride to dissolve the organic matter therein. The composition of the organic matter was analyzed by GC-MS to show that the organic matter contained therein was hexamethyleneimine.

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Abstract

The invention relates to an SAPO-44 (silicoaluminophosphate-44) molecular sieve and a synthetic method thereof. The SAPO-44 molecular sieve is characterized by containing a template agent namely hexamethylene imine, the crystal surface of the molecular sieve is slightly rich in silicon, and the ratio of the outer surface silicon content to the bulk phase silicon content of crystals is 1.50-1.01. After being roasted in 400-700 DEG C air, the molecular sieve can be used as a catalyst for an acid-catalyzed reaction and a reaction for preparing olefin through oxygen-contained compound conversion.

Description

technical field [0001] The invention belongs to the field of SAPO molecular sieves, in particular to a SAPO-44 molecular sieve and a synthesis method thereof. Background technique [0002] In 1984, United Carbide Corporation (UCC) developed the SAPO molecular sieve series of silicoaluminophosphate (USP4440871). The molecular sieve is a kind of crystalline silicoaluminophosphate, and its three-dimensional framework structure is composed of PO 2 + , A1O 2 - and SiO 2 tetrahedron composition. Among them, SAPO-34 is a chabazite-like structure, the main channel is composed of eight rings, and the orifice is 0.38nm×0.38nm. Due to its suitable acidity and pore structure, SAPO-34 molecular sieve has attracted much attention because of its excellent catalytic performance in the reaction of methanol to light olefins (MTO). [0003] SAPO-34 molecular sieves are generally synthesized by hydrothermal method, using water as solvent, in a closed autoclave. Synthesis components incl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54B01J29/85C07C1/24C07C11/04C07C1/20C07C11/02B01J20/18B01J20/30
CPCY02P30/42Y02P20/52Y02P30/20Y02P30/40
Inventor 田鹏樊栋刘中民苏雄张莹杨越
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI