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Submicron SAPO-5/SAPO-18 composite molecular sieve and preparation method thereof

A SAPO-18, SAPO-5 technology, applied in the field of sub-micron SAPO-5/SAPO-18 composite molecular sieve and its preparation, can solve the problems of total olefin yield and service life that need to be improved

Active Publication Date: 2014-04-09
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] CN101935049B discloses a silicoaluminophosphate molecular sieve, which is actually a kind of AEI and CHA intergrowth silicoaluminophosphate molecular sieve, such as SAPO-18 and / or ALPO-18 molecular sieve, or SAPO-34 and / or ALPO-34 Molecular sieves are prepared by mixing aluminum sources, phosphorus sources, silicon sources, water, and templates in order to form a gel, and then performing aging and hydrothermal synthesis crystallization in sequence. In the above process, no molecular sieve seeds are used.
[0018] The particle diameters of ALPO-18 and / or SAPO-18 molecular sieves, ALPO-34 and / or SAPO-34 molecular sieves and low-silicon ALPO-5 / ALPO-18 molecular sieves disclosed in the above-mentioned patent documents are all in micron order, that is, their average The particle size is above 1 micron. Therefore, they still need to be improved in terms of total olefin yield and service life as active components of organic oxygen-containing compounds to produce low-carbon olefins.

Method used

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  • Submicron SAPO-5/SAPO-18 composite molecular sieve and preparation method thereof

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preparation example Construction

[0042] Preferably, the preparation method of the submicron composite molecular sieve chemically compounded by SAPO-5 molecular sieve and SAPO-18 molecular sieve of the present invention comprises the following steps in sequence:

[0043] (1) Mix the aluminum source, phosphorus source, silicon source, templating agent and water uniformly in proportion at a suitable temperature, for example, at a temperature of 20°C-90°C, to obtain an aluminum source, phosphorus source, silicon source, template agent and The mixed solution of water, in above-mentioned mixed solution, templating agent: SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 The molar ratio of O is (0.2-5.0): (0.1-0.6): 1: (0.7-1.3): 30-200;

[0044] (2) Aging the above mixed solution until a mixed gel is formed;

[0045] (3) Add SAPO-5 / SAPO-18 composite molecular sieve seed crystals to the above mixed gel in proportion to obtain aluminum source, phosphorus source, silicon source, template agent, water and SAPO-5 / SAPO-18 composite mo...

Embodiment 1

[0058] Embodiment 1: Preparation of submicron SAPO-5 / SAPO-18 chemical composite molecular sieve

[0059] 17.6 grams of pseudo-boehmite and 20.0 grams of deionized water are mixed and stirred to form an aluminum source solution, and 20.0 grams of phosphoric acid with a concentration of 85% by weight are mixed and stirred with 10.0 grams of deionized water to form a phosphorus source solution. The concentration of 2.9 grams is 40% by weight of silica sol and 4.5 grams of deionized water were mixed and stirred to form a silicon source solution.

[0060]Then, the phosphorus source solution is slowly added dropwise to the aluminum source solution to form a mixed solution of the aluminum source and the phosphorus source, and then the silicon source solution is added to the mixed solution of the aluminum source and the phosphorus source. Stir evenly for 1 hour to form a mixed solution of aluminum source, phosphorus source and silicon source, then add 18.8 grams of N,N-diisopropylethy...

Embodiment 2

[0066] Embodiment 2: Preparation of submicron SAPO-5 / SAPO-18 chemical composite molecular sieve

[0067] Except adding 0.5 gram in the mixed solution, instead of the mol ratio of 0.2 gram SAPO-5 molecular sieve / SAPO-18 molecular sieve being the SAPO-5 / SAPO-18 composite molecular sieve seed crystal of 0.3, repeat the process of implementing Lee 1, obtain sub Micron SAPO-5 / SAPO-18 composite molecular sieve, this composite molecular sieve is labeled as molecular sieve B.

[0068] In the above-mentioned preparation process, in the above-mentioned mixed solution, template agent: SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 The mol ratio of O is 1.6:0.2:1:0.95:50; In the above-mentioned mixed gel, take the weight of effective solid content in the mixed gel as a basis, the add-on of SAPO-5 / SAPO-18 compound molecular sieve crystal seed is 2.8%.

[0069] The SAPO-5 / SAPO-18 composite molecular sieve seed crystal whose molar ratio of SAPO-5 molecular sieve / SAPO-18 molecular sieve is 0.3 is SAPO-...

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Abstract

The invention discloses a submicron composite molecular sieve for preparing a catalyst for producing low-carbon olefin through organic oxygen compound and a preparation method of the submicron composite molecular sieve. The composite molecular sieve is formed by compounding an SAPO-5 molecular sieve and an SAPO-18 molecular sieve. Raw materials for preparing the composite molecular sieve satisfy the following condition: the molar ratio of SiO2: Al2O3: P2O5 is (0.1-0.6): 1: (0.7-1.3); the addition quantity of the SAPO-5 / SAPO-18 composite sieve screen crystal seed is 1.0 to 5.5 percent by adopting the weight of effective solid content in mixed gel as a benchmark. The SAPO-5 / SAPO-18 composite molecular sieve has submicron-meter granularity and is good in catalytic activity, long in service life and high in qualification molecular sieve yield.

Description

technical field [0001] The invention relates to a submicron SAPO-5 / SAPO-18 composite molecular sieve and a preparation method thereof. Background technique [0002] The catalytic materials used in the reaction of methanol to olefins are mainly acidic zeolites with small and medium pores. In 1982, UCC scientists Wilson S T and Flanigen E M first synthesized a new type of aluminophosphate (ALPO-n) molecular sieve in a hydrothermal system using organic amines as templates. AlPO-n series microporous molecular sieves with large pores and large pores have appeared one after another. [0003] In 1984, Lok et al. first introduced Si into AlPO-n series molecular sieves, and synthesized a new class of silicoaluminophosphate (SAPO-n) molecular sieves. This type of molecular sieves includes 13 three-dimensional framework structures composed of tetrahedrons. Channel structures ranging from six-membered rings to twelve-membered rings. Silicoaluminophosphate molecular sieve (SAPO-n) is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/85C07C1/20C07C11/04C07C11/06C07C11/08
CPCY02P20/52Y02P30/20Y02P30/40
Inventor 邢爱华张新锋王理石玉林金环年
Owner CHNA ENERGY INVESTMENT CORP LTD
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