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Normal-pressure synthesis method of SAPO-11 molecular sieve

A technology of SAPO-11 and atmospheric pressure synthesis, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of complex synthesis method and high synthetic composition, and achieve the improvement of isomerization reaction activity and synthesis The method is mild and accelerates the effect of nucleation

Active Publication Date: 2020-07-14
QINGDAO UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the technical problems of complicated synthetic method of SAPO-11 molecular sieve and relatively high synthetic components in the prior art, the invention provides a normal-pressure synthetic method of SAPO-11 molecular sieve

Method used

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  • Normal-pressure synthesis method of SAPO-11 molecular sieve
  • Normal-pressure synthesis method of SAPO-11 molecular sieve
  • Normal-pressure synthesis method of SAPO-11 molecular sieve

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Effect test

Embodiment 1

[0022] According to deionized water, boehmite (with Al 2 o 3 In terms of), phosphoric acid (in P 2 o 5 ), organic amine di-n-propylamine, silica sol, and biochar in a molar ratio of 90:1.0:1.0:1.1:0.4:0.10 were sequentially added into the beaker, stirred for 8 hours to obtain a crystallization precursor, and the resulting crystallization precursor was transferred to In the crystallization kettle, under the condition of microwave power of 600w, after crystallization at 100°C for 8h (operating pressure is 10100pa), the crystallized product is obtained; it is washed and washed with deionized water whose quality is 4 times that of the crystallized product Filter, then dry at 100°C for 6h, and roast at 650°C for 8h, perform X-ray diffraction on the SAPO-11 molecular sieve with AEL structure, and analyze its diffraction pattern XRD, see figure 1 ,From figure 1 It can be seen that the synthesized product has the characteristic diffraction peak of SAPO-11 molecular sieve.

Embodiment 2

[0024] According to deionized water, boehmite (with Al 2 o 3 In terms of), phosphoric acid (in P 2 o 5 According to the molar ratio of 90:1.0:1.0:1.1:0.4:0.03:0.20, the organic amine di-n-propylamine and diisopropylamine, silica sol, seed crystal SAPO-11 molecular sieve powder and biochar were sequentially added into the beaker, Wherein the organic amine is a mixture of di-n-propylamine and diisopropylamine, and the mass ratio of the two in the mixture is 50%:50%. After the above solution is fully stirred for 6 hours, the crystallization precursor is obtained, and the crystallization precursor is transferred to the crystallization kettle. , under the condition of microwave power of 400w, after crystallization at 90°C for 12h (operating pressure is 10000pa), the crystallization product was obtained; it was washed and filtered with deionized water whose quality was 4 times that of the crystallization product, and then at 90 ℃ for 8 hours, then roasted at 550 ℃ for 6 hours, X-...

Embodiment 3

[0027] Deionized water, aluminum isopropoxide (as Al 2 o 3 In terms of), phosphoric acid (in P 2 o 5According to the molar ratio of 60:1.0:1.0:1.1:0.2:0.03:0.01, the mixture of diisopropylamine, silica sol, seed crystal seed SAPO-11 molecular sieve former powder and acetylene black, activated carbon is added into the beaker in order, and the above The solution was fully stirred for 2 hours to obtain a crystallization precursor, which was transferred to a crystallization kettle, and crystallized at 80°C for 4 hours under the microwave power of 200w (operating pressure was 10000pa), to obtain a crystallization product; The crystallized product was washed with deionized water twice the mass, filtered, dried at 80°C for 6 hours, and calcined at 450°C for 4 hours to obtain the SAPO-11 molecular sieve.

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Abstract

The invention belongs to the technical field of SAPO-11 molecular sieves, and discloses a normal-pressure synthesis method of an SAPO-11 molecular sieve. The method comprises the following steps: sequentially adding water, an aluminum source, a phosphorus source, organic amine, a silicon source and a carbon material into a container according to a specific molar ratio, performing stirring to prepare sol, and heating and crystallizing the sol under a microwave condition to obtain a molecular sieve SAPO-11, wherein the molar ratio of the water to the aluminum source (in terms of Al2O3) to the phosphorus source (in terms of P2O5) to the organic amine to the silicon source (in terms of SiO2) to the carbon material is (60-120):1.0:1.0:(1.1-1.4):(0.2-1.0):(0.01-0.50). The method has the advantages of mild conditions, smooth synthesis of the molecular sieve SAPO-11, substantial shortening of the synthesis induction period of the molecular sieve, and effective inhibition of the aggregation phenomenon of small crystal grains.

Description

technical field [0001] The invention relates to a SAPO-11 molecular sieve, in particular to an atmospheric pressure synthesis method of the SAPO-11 molecular sieve. Background technique [0002] SAPO-11 molecular sieve has good isomerization catalytic activity, and has been widely studied in petrochemical fields such as gasoline upgrading and diesel dewaxing. SAPO-11 molecular sieve has a one-dimensional straight pore structure. Normal alkanes can undergo isomerization reaction at the pore position on the outer surface of the grain to generate isomeric hydrocarbons. Moreover, SAPO-11 molecular sieve is mild in acidity and is not easy to cause cracking reactions of isomeric hydrocarbons. It is possible to increase the yield of isomeric hydrocarbons. [0003] The common synthesis method of SAPO-11 molecular sieve is hydrothermal synthesis method. Under high temperature conditions (usually >180°C), the self-generation pressure of water vapor is high, which puts forward high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
CPCC01B39/54C01B37/08Y02P30/20
Inventor 刘毓翔郑德将逄锦慧李露刘仕伟于世涛
Owner QINGDAO UNIV OF SCI & TECH
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