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Preparation method of SAPO-34 molecular sieve

A technology of SAPO-34 and molecular sieve, which is applied in the field of preparation of SAPO-34 molecular sieve, can solve the problems of low single-pot yield and poor repeatability, and achieve the effect of shortening the induction period

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of hydrothermal synthesis of SAPO-34 molecular sieve has disadvantages such as poor reproducibility after scale-up and low single-pot yield.

Method used

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preparation example Construction

[0020] The preparation method of SAPO-34 molecular sieve provided by the invention is characterized in that comprising the steps:

[0021] (1) The phosphorus source and the aluminum source are adjusted according to (0.6~1.2)P 2 o 5 :Al 2 o 3 :(20~60)H 2 The molar ratio of O is mixed evenly, and dried to obtain phosphor-aluminum dry glue A with a solid content of not less than 60%;

[0022] (2) Contact and mix the aluminum phosphate dry glue A with the template agent and the silicon source to obtain the mixture B, in which, 1 mole of Al in the aluminum phosphate dry glue A 2 o 3 Calculated, the added amount of the template agent is (1-2.5) moles, and the added amount of the silicon source is expressed as SiO 2 Calculated as 0.1 to 1 mole;

[0023] (3) Put the mixture B in a closed reaction kettle to crystallize under autogenous pressure and recover the product, wherein, the crystallization is carried out in three stages in sequence from low to high temperature range, and...

Embodiment 1

[0046] Weigh 7g of dry rubber powder and dissolve it in 10g of deionized water, stir evenly, mix with the solution obtained by adding 11g of 85% analytical pure orthophosphoric acid into 10g of deionized water and stir evenly, and dry at 80°C to obtain phosphate aluminum with 85% solid content glue.

[0047] Move the phosphoraluminum glue to a 100ml crystallization kettle, add 30g tetraethylammonium hydroxide, 5.2g triethylamine, 3g acidic silica sol with a mass fraction of 30% and 17g water, stir evenly, seal the reaction kettle, and crystallize The conditions are divided into steps of aging at room temperature for 10 hours, crystallization at 150°C for 10 hours, and crystallization at 200°C for 40 hours. After the temperature of the kettle drops to room temperature, take out the crystallized product, filter or centrifuge, wash with deionized water until neutral, and place it at 100-110 ℃ in a constant temperature drying oven, and finally placed in a muffle furnace and heated...

Embodiment 2

[0050] Weigh 7g of SB powder and dissolve it in 25g of deionized water, stir rapidly for 1 hour, mix with the solution obtained by adding 9.2g of 85% analytical pure orthophosphoric acid into 30g of deionized water and stir evenly, dry in a constant temperature dryer at 120°C to obtain a solid content of 85% Phosphor aluminum glue.

[0051] Move the phosphoraluminum glue to a 100ml crystallization kettle, add 30g tetraethylammonium hydroxide and 3g acidic silica sol with a mass fraction of 30%, stir evenly, seal the reaction kettle, and crystallize according to room temperature aging for 10h, 140°C Crystallization for 10h and 170°C crystallization for 70h in stages. After the kettle temperature drops to room temperature, take out the crystallized product, filter or centrifuge and wash it with deionized water until it becomes neutral. The product is dried in a constant temperature drying oven at 100-110°C, and finally put into a muffle furnace and heated to 550°C for constant t...

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Abstract

The invention discloses a preparation method of a SAPO-34 molecular sieve, which is characterized by comprising the following steps: (1) uniformly mixing a phosphorus source and an aluminum source according to the mol ratio of (0.6-1.2)P2O5:Al2O3:(20-60)H2O, and drying to obtain phosphorus aluminum dry glue A with the solid content of not lower than 60%; (2) uniformly contacting and mixing the phosphorus aluminum dry glue A with a template and a silicon source to obtain a mixture B, wherein the addition amount of the template agent is 1-2.5 mol on the basis of 1 mol of Al2O3 in the phosphorus aluminum dry glue A, and the addition amount of the silicon source is 0.1-1 mol on the basis of SiO2; and (3) putting the mixture B in a closed reaction kettle, sectionally crystallizing under autogenous pressure, and recovering the product.

Description

technical field [0001] The present invention relates to a preparation method of SAPO-34 molecular sieve, more specifically to a preparation method of hydrothermal synthesis of SAPO-34 molecular sieve. Background technique [0002] SAPO-34 molecular sieve is a phosphorus silicon aluminum molecular sieve developed by United Carbide Chemical Company in 1984. It is an eight-membered ring chabazite CHA structure and belongs to the cubic crystal system. The pore diameter is about 0.43nm, which is comparable to the molecular diameter of ethylene and propylene. Similarly, SAPO-34 molecular sieve has suitable acid strength, pore structure and good hydrothermal stability, and exhibits excellent catalytic performance in methanol to light olefins (MTO). [0003] There are many methods for the synthesis of SAPO-34 molecular sieves, such as hydrothermal synthesis, microwave synthesis, liquid phase synthesis, gas phase transfer synthesis and so on. Wherein the most commonly used is the hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 杨冬清王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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