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Titanium-contained silicon-aluminum phosphate molecular sieve and synthesis thereof

A titanium silicoaluminophosphate, molecular sieve technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problem of lack of cation exchange performance and catalytic reaction performance, and achieve high ethylene selectivity, high low carbon The effect of olefin selectivity

Active Publication Date: 2011-01-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve (USP4310440) invented by UCC Corporation in the United States in the early 1980s. It is electrically neutral, so it has no cation exchange performance and catalytic reaction performance

Method used

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  • Titanium-contained silicon-aluminum phosphate molecular sieve and synthesis thereof
  • Titanium-contained silicon-aluminum phosphate molecular sieve and synthesis thereof
  • Titanium-contained silicon-aluminum phosphate molecular sieve and synthesis thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add 117.53 grams of hydrated alumina and 368.21 grams of deionized water into the gelling kettle placed in a 60°C water bath, mix and stir for 30 minutes to make it evenly mixed, add 147.58 grams of phosphoric acid into the gelling kettle and stir and mix for 30 minutes, Add 30.66 grams of titanium tetrachloride solution (containing 99.7% by weight of TiCl 4 , Beijing Yili Fine Chemicals Co., Ltd.). After stirring evenly for 2 hours, add 96.13 grams of silica sol, and after stirring for 1 hour, add 368.21 grams of deionized water and stir for 1 hour, then add 118.21 grams of diethylamine, continue stirring and mixing for 1 hour, and the colloid is aged at room temperature for 20 Hours, 6.27 grams of SRM-2 molecular sieve powder was added to the above-mentioned gelling kettle, and fully stirred for 2 hours to prepare a reaction mixture. Part of the reaction mixture was packaged into a stainless steel crystallization kettle, the temperature was raised to 130°C and stirre...

Embodiment 2

[0053] Add 1121.49 grams of silica sol, 117.53 grams of hydrated alumina and 293.56 grams of deionized water into a gelling kettle placed in a 70°C water bath, mix and stir for 30 minutes, add 221.36 grams of phosphoric acid into the gelling kettle and stir for 2 hours, Add 8.14 grams of titanium oxide (98%, Shanghai Guanghua Science and Technology Co., Ltd.) and continue to stir for 1 hour, 177.31 grams of diethylamine is added to the above-mentioned gelling kettle, after stirring for 10 minutes, add 245.33 grams of di-n-propylamine, continue After stirring for 1 hour, the colloid was statically aged at 40° C. for 15 hours, and 48.49 grams of SRM-2 molecular sieve powder was added and stirred thoroughly for 2 hours to prepare a reaction mixture. Part of the reaction mixture was packaged into a stainless steel crystallization kettle, and the temperature was raised to 185° C. under autogenous pressure for 48 hours to crystallize with stirring. Then filter, wash, and dry the cry...

Embodiment 3

[0061] First put 100 grams of deionized water into a beaker in a water bath at 50°C, stir at a constant speed for 30 minutes, then slowly add a mixture of 13.89 grams of tetra-n-butyl titanate and 11.09 grams of absolute ethanol dropwise into the water for hydrolysis , and the hydrolyzed product is used for later use. Then add the mixed solution of 184.47 grams of phosphoric acid and 298.74 grams of deionized water into the gelling kettle placed in a water bath at 50°C, mix and stir for 30 minutes, add 117.53 grams of hydrated alumina, and continue stirring for 2 hours. Add the hydrolyzate of n-butyl ester and ethanol mixture into the gelling kettle, continue to stir for 1 hour, add 147.75 grams of diethylamine, stir for 1 hour, add 160.22 grams of silica sol, stir fully for 2 hours, and make a reaction The mixture, the colloid is statically aged at 5-90° C. for 5-80 hours, and 37.24 grams of SRM-2 molecular sieve raw powder is added. Part of the reaction mixture was packaged...

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Abstract

The invention discloses a titanium-contained silicon-aluminum phosphate molecular sieve and a synthetic method thereof, wherein the molecular sieve is characterized in that X-ray diffraction data before roasting for removing a template agent at least contains a diffraction peak shown in a table 1, and the X-ray diffraction data after roasting for removing the template agent at least contains the diffraction peak of a table 2; and the molecular sieve is obtained according to the following steps of: mixing and gelatinizing the compound of an aluminum source, a phosphorus source, a silicon source and metallic titanium as well as an organic template agent at the temperature of 5-100 DEG C, aging the obtained colloid for 5-80 hours at the temperature of 5-90 DEG C, adding 0.1-15wt% of crystal seed on a dry basis, and then carrying out hydrothermal crystallization for 4-500 hours at the temperature of 100-250 DEG C. A catalyst using the molecular sieve provided by the invention as an activecomponent can be used for the conversion reaction of oxygen-contained organic compounds.

Description

technical field [0001] The invention relates to a titanium-containing silicoaluminophosphate molecular sieve and its synthesis. Background technique [0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve (USP4310440) invented by UCC Corporation in the United States in the early 1980s. It is electrically neutral, so it has no cation exchange performance and catalytic reaction performance. Aluminum phosphate molecular sieves are a series of molecular sieves with unique XRD characteristic spectra and data. Among them, there are molecular sieves with the same crystal structure as the existing aluminum silicate molecular sieves, and there are also new structures that are not found in the existing aluminum silicate molecular sieves. of molecular sieves. [0003] Introducing silicon into the framework of aluminum phosphate molecular sieves will become silicoaluminophosphate molecular sieves, that is, SAPO series molecular sieves (UCC, USP4440871). Neg...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
Inventor 许吓清李黎声张凤美王卫东秦凤明
Owner CHINA PETROLEUM & CHEM CORP