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A kind of 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: 2015-08-05
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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  • A kind of submicron sapo-5/sapo-18 composite molecular sieve and preparation method thereof
  • A kind of submicron sapo-5/sapo-18 composite molecular sieve and preparation method thereof
  • A kind of 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 the SAPO-5 molecular sieve and the SAPO-18 molecular sieve of the present invention comprises the following steps in turn:

[0043] (1) Mix the aluminum source, phosphorus source, silicon source, template agent and water uniformly at a suitable temperature, for example, at a temperature of 20°C to 90°C in proportion to obtain an aluminum source, phosphorus source, silicon source, template agent and The mixed solution of water, in the above 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) Ageing the above mixed solution until a mixed gel is formed;

[0045] (3) Add SAPO-5 / SAPO-18 composite molecular sieve crystal seeds to the above mixed gel in proportion to obtain a composite molecular sieve crystal including aluminum source, phosphorus source, silicon source, template...

Embodiment 1

[0058] Example 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 were mixed and stirred to form an aluminum source solution, and 20.0 grams of phosphoric acid with a concentration of 85% by weight was mixed and stirred with 10.0 grams of deionized water to form a phosphorus source solution, and 2.9 grams of concentration was 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 uniformly for 1 hour to form a mixed solution of aluminum source, phosphorus source and silicon source, then add 18.8 grams of N,N-diisopropylet...

Embodiment 2

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

[0067] Except adding 0.5 g instead of 0.2 g of SAPO-5 / SAPO-18 composite molecular sieve seed crystals with a molar ratio of SAPO-5 / SAPO-18 molecular sieve to the mixed solution of 0.3, repeat the process of step 1 to obtain sub- Micron SAPO-5 / SAPO-18 composite molecular sieve, the composite molecular sieve is marked as molecular sieve B.

[0068] In above-mentioned preparation process, 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 1.6:0.2:1:0.95:50; in the above-mentioned mixed gel, based on the weight of the effective solid content in the mixed gel, the amount of SAPO-5 / SAPO-18 composite molecular sieve seeds added is 2.8%.

[0069] The SAPO-5 / SAPO-18 composite molecular sieve seeds with the above-mentioned SAPO-5 molecular sieve / SAPO-18 molecular sieve molar ratio of 0.3 are SAPO-5 / SAPO-18 composite molecular sieve...

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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 methanol-to-olefin reaction are mainly acidic zeolites with small pores and mesopores. In 1982, scientists Wilson ST and Flanigen EM of United Carbon Corporation (UCC) first synthesized a new type of aluminophosphate (ALPO-n) molecular sieve with organic amine as a template in a hydrothermal system. Pore ​​and macroporous AlPO-n series of microporous molecular sieves appeared one after another. [0003] In 1984, Lok et al. first introduced Si into the AlPO-n series of molecular sieves and synthesized a new class of silicoaluminophosphate (SAPO-n) molecular sieves. The pore structure from six-membered ring to twelve-membered ring. Silicoaluminophosphate molecular sieve (SAPO-n) is made of [SiO 4 ], [AlO 4 ] - and [PO 4 ] + Microporous crystals with small pores, mesopores...

Claims

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Application Information

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Patent Type & Authority Patents(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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