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Method for synthesizing silicoaluminophosphate molecular sieve SAPO-11 at normal pressure

A technology of SAPO-11 and silicoaluminophosphate, which is applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali exchange phosphate, etc., can solve the problems of inconvenient synthesis and high price of ionic liquids

Inactive Publication Date: 2012-11-21
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, ionic liquids are not very convenient to synthesize, and the price is relatively high; eutectic mixtures have similar properties to ionic liquids, and can also be used as solvents for the synthesis of molecular sieves, which are convenient and cheaper to prepare

Method used

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  • Method for synthesizing silicoaluminophosphate molecular sieve SAPO-11 at normal pressure
  • Method for synthesizing silicoaluminophosphate molecular sieve SAPO-11 at normal pressure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 20.0 grams of pentaerythritol and 40.0 grams of tetrabutylammonium bromide, grind and mix them, place them in a 150 mL beaker, heat them on a hot plate to melt them, and stir them until a transparent liquid is formed to obtain a eutectic mixture. Add 3.89 grams of phosphoric acid dropwise to the eutectic mixture, stir well, then add 7.1 grams (30.0%) of acidic silica sol, then add 0.50 grams of hydrofluoric acid (40.0%), and add 3.1 grams of di-n-propylamine to the eutectic In the mixture, stir evenly; slowly add 2.85 grams of Shandong aluminum powder from the aluminum source to the above mixed solution, continue to stir the resulting mixed sol for half an hour; transfer the above mixed sol to a 150 ml round bottom flask, use a heating mantle to heat, and stir magnetic , The condenser is connected to the flask with water cooling, at 180 o C crystallized for 12 hours. Then the reactant was cooled to room temperature, 50 ml of deionized water was added and stirred, a...

Embodiment 2~5

[0035] The specific steps and synthesis conditions are similar to Example 1, but the crystallization temperature is 160, 170, 180, 190 o C, the crystallization time is 24 hours.

Embodiment 6

[0037] The specific steps and synthesis conditions are similar to those in Example 1, but the eutectic mixture is made of 15 grams of pentaerythritol and 45 grams of tetrabutylammonium bromide. The crystallization reaction is carried out in a 150 ml static reactor, and the constant temperature is 180 in a rotating oven. o C crystallized for 12 hours.

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Abstract

The invention provides a method for synthesizing a silicoaluminophosphate molecular sieve SAPO-11 at normal pressure. The method is characterized in that the main process comprises the following steps of 1) preparation of eutectic mixture: fully grinding and mixing quaternary ammonium salt and organic acid or organic alcohol in a mortar with a mol ratio of 0.1 to 1.0; placing the mixture in a beaker, heating the beaker at a temperature of 80-180 DEG C to melt the mixture into transparent liquid, so as to obtain the eutectic mixture; 2) preparation of crystallization reaction mixture: adding phosphorus source, silicon source, mineralizing agent, template agent and aluminum source into the molten eutectic mixture in sequence, uniformly stirring the mixture at a mixing temperature range from 80 to 150 DEG C to form a reaction mixture; 3) crystallizing the reaction mixture prepared by step 2); and 4) water cooling the reactant reacted in step 3) to a room temperature, washing and separating the mixture, and drying and baking the washed and separated mixture, wherein the washed filtrate is recovered after rotary evaporation.

Description

technical field [0001] The invention belongs to the field of inorganic synthesis, and relates to a method for synthesizing molecular sieves; more precisely, it relates to an ionothermal synthesis method of silicoaluminophosphate molecular sieve (SAPO-11) in eutectic mixture. Background technique [0002] Aluminum phosphate molecular sieves are a new generation of molecular sieves (USP4310440) developed by Union Carbide in the early 1980s following the silica-alumina molecular sieves. AlPO 4 -11 molecular sieve (skeleton topological structure code named AEL), which contains a one-dimensional ten-membered ring straight pore structure, with an elliptical orifice and a size of 0.39×0.63 nm. The silicoaluminophosphate SAPO (MAPO) molecular sieve introduced by silicon (or other metal heteroatoms M) has an acidic site in the framework, thus expanding the use of the molecular sieve, especially in the alkane hydroisomerization reaction, carrying noble metals SAPO-11 molecular siev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 裴仁彦李孝国于海滨费亚南李佳孙国方张耀日隋芝宇张永惠赵甲肖寒
Owner CHINA NAT OFFSHORE OIL CORP
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