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Preparation method of high-purity SAPO-44 microporous molecular sieve

A SAPO-44, microporous molecular sieve technology, applied in the field of molecular sieve preparation, can solve the problems of cumbersome preparation process, increase preparation steps, etc., achieve the effect of short cycle, improve crystallinity, and facilitate industrial application

Active Publication Date: 2015-07-01
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the purity of SAPO-44, patents CN201210363833.5 and CN201310499121.0 use composite templates to synthesize SAPO-44 through two crystallization processes at different temperatures, but these methods increase the preparation steps and make the preparation process cumbersome

Method used

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  • Preparation method of high-purity SAPO-44 microporous molecular sieve

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preparation example Construction

[0028] The molecular sieve preparation method of the present invention specifically comprises the following steps:

[0029] (1) Mix the composite template agent, phosphorus source, aluminum source, silicon source, and water evenly to obtain a mixture gel.

[0030] (2) Transfer the gel mixture to a reaction kettle, heat it up to 150-250°C in an airtight manner, and crystallize at a constant temperature under autogenous pressure for a period of time. After the crystallization is complete, cool it down to room temperature naturally.

[0031] (3) The crystallized product is centrifuged, washed until neutral, and dried, and the dried solid product is roasted in the air at 450-650°C to completely remove the composite template agent to obtain SAPO-44 microporous molecular sieve.

Embodiment 1

[0034] Prepare SAPO-44 with tetraethylenepentamine (TEPA) and TMHD double templating agent, the steps are as follows:

[0035] 1. According to the molar ratio of SiO 2 :Al 2 o 3 :P 2 o 5 :TEPA:TMHD:H 2 O=0.75:1:1.25:0.54:2.5:50 Weigh silica sol, pseudoboehmite, phosphoric acid, TEPA, TMHD and water.

[0036] 2. Dissolve 0.8280g TEPA in 7.2g deionized water, add 2.3058g phosphoric acid, 1.0461g pseudoboehmite, 1.2267g silica sol and 3.4746g TMHD in sequence, and continue stirring for 12 hours. The reactant was transferred to a stainless steel reaction kettle, sealed and heated to 200°C, and then cooled to room temperature naturally after constant temperature crystallization under autogenous pressure for 96 hours. The crystallized product was separated by centrifugation and washed with deionized water several times to neutralize the precipitate. The product was dried in a drying oven at 100°C for 12 hours and calcined in a tube furnace at 550°C for 6 hours to obtain a soli...

Embodiment 2

[0038] 1. According to the molar ratio of SiO 2 :Al 2 o 3 :P 2 o 5 :DETA:TMHD:H 2 O=0.8:1:1.2:0.6:2.5:50 Weigh tetraethyl orthosilicate, aluminum oxyhydroxide, phosphorous acid, DETA, TMHD and water.

[0039] 2. Dissolve 0.4952g DETA in 7.2g deionized water. 1.8522g of phosphorous acid, 1.2307g of aluminum oxyhydroxide, 4.5357g of ethyl orthosilicate and 3.4746g of TMHD were added in sequence, and stirring was continued for 12 hours. The reactant was transferred to a stainless steel autoclave, heated to 210°C in a closed manner, and crystallized at a constant temperature under its own pressure for 96 hours, and then naturally cooled to room temperature. The precipitate was washed with deionized water several times until the filtrate was neutral, the product was dried in a drying oven at 100°C for 12 hours, and calcined in a tube furnace at 550°C for 6 hours to obtain a solid powder. The obtained product is analyzed by XRD diffraction to be pure SAPO-44 microporous molec...

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Abstract

The invention discloses a preparation method of a high-purity SAPO-44 microporous molecular sieve. The method comprises the following steps: preparing mixture gel by taking a phosphorus source, an aluminum source, a silicon source, a composite template agent and water as raw materials, performing closed crystallization on the mixture gel, washing, drying and roasting the obtained crystalized product to remove the composite template agent, to obtain an SAPO-44 microporous sieve, wherein the composite template agent is R1 and R2, the R1 is ethanediamine (EDA), diethylenetriamine (DETA), triethylene tetramine (TETA), tetraethylenepentamine (TEPA) or pentaethylenehexamine (PEHA), and R2 is N,N,N',N'-tetramethyl-1,6-hexamethylenediamine (TMHD). The formation of the SAPO-44 is promoted by using an organic composite template agent, the high-purity SAPO-44 molecular sieve can be obtained only by once crystallization through adjustment of the usage amount, the preparation process is easy to operate, the period is short, and the industrial application is facilitated.

Description

technical field [0001] The invention relates to a preparation method of SAPO-44 microporous molecular sieve, in particular to a preparation method of high-purity SAPO-44 microporous molecular sieve, which belongs to the technical field of molecular sieve preparation. Background technique [0002] Silicoaluminophosphate molecular sieve (SAPO-n) is developed by Union Carbide Corporation of the United States and is composed of SiO 2 、PO 2 + and AlO 2 - Microporous crystals composed of three tetrahedrons, where n represents different crystal structures. There are many types of SAPO series structures, which can be divided into large-pore molecular sieves larger than 50 nm (such as SAPO-5), medium-pore molecular sieves between 2-50 nm (such as SAPO-11) and smaller than 2 nm. Small pore molecular sieves (such as SAPO-34, SAPO-44), etc. The good pore structure makes SAPO-n molecular sieves have excellent shape selectivity, and can be used as catalysts in many hydrocarbon conv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 张昭良周钰浩辛颖李倩于明强
Owner UNIV OF JINAN
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