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Method for selectively synthesizing sapo-15 and sapo-34 molecular sieves

A technology of SAPO-15 and SAPO-34, which is applied in the field of preparation of inorganic porous materials, can solve the problems of long crystallization time, cumbersome process of active aluminum source, and large amount of template agent

Inactive Publication Date: 2021-06-15
SHANXI DATONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] In general, the current methods for synthesizing AlPO-15 or SAPO-15 molecular sieves have the following problems: no organic template is used, the crystallization time is long, and step-by-step crystallization is required; and the preparation of active aluminum source by ammonia water is cumbersome. , and the crystallization time is long; the use of organic templates to synthesize AlPO-15 or SAPO-15 molecular sieves has the problem of large amounts of templates
In addition, no selective synthesis of pure phase SAPO-15 and SAPO-34 molecular sieves has been reported so far

Method used

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  • Method for selectively synthesizing sapo-15 and sapo-34 molecular sieves
  • Method for selectively synthesizing sapo-15 and sapo-34 molecular sieves
  • Method for selectively synthesizing sapo-15 and sapo-34 molecular sieves

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Experimental program
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Effect test

Embodiment 1

[0040] The synthesis of embodiment 1 pure phase SAPO-34 molecular sieve

[0041] First, 9.2 ml of phosphoric acid was dissolved in 28.0 g of deionized water, then 9.2 g of pseudoboehmite, 4.1 g of gaseous silicon dioxide, 11.6 ml of morpholine and 39 ml of water were added in sequence, and stirred evenly. The molar ratio of each species is SiO 2 :Al 2 o 3 :R:P 2 o 5 :H 2 O=0.76:1.0:1.48:0.87:41.3, the above reaction sol was sealed in a 150 ml stainless steel autoclave with a polytetrafluoroethylene liner, crystallized at 200°C for 48 hours, and quickly dropped to At room temperature, the solid product was separated by filtration, washed with deionized water to neutrality, and dried overnight at 100°C to obtain the product, which was tested by X-ray diffraction (XRD). Diffraction (XRD) pattern see attached figure 1 .

Embodiment 2

[0042] The synthesis of embodiment 2 pure phase SAPO-15 molecular sieves

[0043] First, dissolve 9.2 ml of phosphoric acid in 28.0 g of deionized water, then add 9.2 g of pseudoboehmite, 4.1 g of gaseous silicon dioxide, 11.6 ml of morpholine and 15 ml of water in sequence, stir evenly, and then add 16.6 g of ammonium chloride and 24ml water. The molar ratio of each species is SiO 2 :Al 2 o 3 : R: P 2 o 5 :H 2 O: NH 4 + =0.76:1.0:1.48:0.87:41.3:3.3, seal the above reaction sol in a 150 ml stainless steel autoclave with polytetrafluoroethylene lining, crystallize at 200°C for 48 hours, drop rapidly after taking out the autoclave to room temperature, filter to separate the solid product, wash with deionized water to neutrality, and dry overnight at 100°C to obtain the product, which is the crystal phase structure of pure phase SAPO-15 molecular sieve by X-ray diffraction (XRD), and the X-ray of the sample The ray diffraction (XRD) pattern is shown in the appendix fi...

Embodiment 3

[0044] Example 3 Synthesis of SAPO-5, SAPO-15 and SAPO-34 mixed crystal molecular sieves

[0045] First, dissolve 4.6 ml of phosphoric acid in 14.0 g of deionized water, then add 4.6 g of pseudoboehmite, 2.1 g of gaseous silicon dioxide, 5.8 ml of morpholine and 7.5 ml of water in sequence, stir evenly, and then add 0.91 g ammonium chloride and 12ml water. The molar ratio of each species is SiO 2 :Al 2 o 3 :R:P 2 o 5 : H 2 O: NH 4 + =0.76:1.0:1.48:0.87:41.3:0.18, the above reaction sol was sealed in a 100 ml stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 200°C for 48 hours. to room temperature, filter to separate the solid product, wash with deionized water until neutral, and dry overnight at 100°C to obtain the product, which is SAPO-5, SAPO-15 and SAPO-34 mixed crystal molecular sieves by X-ray diffraction (XRD) The crystal phase structure of the sample, the X-ray diffraction (XRD) figure of the sample is shown in the attached im...

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Abstract

The invention relates to a method for selectively synthesizing pure-phase SAPO‑15 and SAPO‑34 molecular sieves. Phosphorus source, aluminum source, silicon source and template agent (R) are added into water in proportion, and stirred evenly at room temperature to obtain a mixed solution A, transfer the mixed solution A into a high-pressure reactor, hydrothermally crystallize at 180-220°C for 12-96 hours, wash and dry after cooling to obtain the product; on the basis of synthesizing SAPO-34 molecular sieve, only add one Additives and control the amount of additives can selectively synthesize pure phase SAPO-15 molecular sieves. In addition, only need to change the amount of additives to synthesize mixed crystal molecular sieves of SAPO-15 and SAPO-34, or SAPO-5, SAPO-15 and SAPO-34 mixed crystal molecular sieve, the reaction process is easy to control, and the amounts of silicon source, aluminum source, phosphorus source, template agent and water in the reaction system remain unchanged.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic porous materials, in particular to a method for selectively synthesizing SAPO-34 molecular sieves and SAPO-15 molecular sieves. Background technique [0002] Phosphate molecular sieves are an important family of microporous crystal materials. The design, synthesis, and development of phosphate microporous compounds with novel structures have always been a matter of concern. In 1982, Wilson S. T. and Flanigen E. M. of UCC (UCC) first disclosed (US4310440) a series of aluminum phosphorus molecular sieves AlPO 4 -n (n is number, n=5, 8, 11, 12, 14, 16, 17, 18, 20, 21, 22, 23, 25, 26, 28, 31) synthetic method. AlPO 4 -n molecular sieve is made of [AlO 2 ] - and [PO 2 ] + A porous inorganic material composed of two tetrahedral units, with a neutral skeleton, weak acidity and poor thermal stability. For this reason, in 1984, Lok B.M. et al. (US 4440871) of UCC first introduced S...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2002/72
Inventor 张海荣潘启亮刘红艳韩生华沈腊珍王蕊宋卫红邵云雪郭瑶池蒋煜郭永
Owner SHANXI DATONG UNIV
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