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A kind of preparation method of aluminum phosphorus microporous molecular sieve

A technology of microporous molecular sieve and aluminum phosphorus, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of long stirring time, deposition, small stirring torque, etc., and achieve convenient product processing and good application Foreground, wide applicability effect

Inactive Publication Date: 2017-04-26
SHANXI DATONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, conventional stirring uses magnetic stirring in beakers or flasks. The stirring torque is relatively small, and the uniformity of the silicon source, aluminum source, and phosphorus source can not be controlled or the stirring time is too long, which often causes crystals to stick or deposit at the bottom of the reactor. , so that the synthesis rate of microporous molecular sieves (that is, the porosity) is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Select the XFD-1.5 flotation machine, add 70mL deionized water and 38g phosphoric acid (85% purity) into the flotation cell of the flotation machine, turn on the flotation machine stirrer, the stirring speed is 1650r / min, and turn on the flotation Select the intake valve of the machine and adjust the intake volume to 0.05m 3 / h. Add 20.7g of triethylamine dropwise into the flotation cell of the flotation machine, and continue stirring for 5-10min. Then add 53.3g of aluminum isopropoxide (98% purity) dropwise into the flotation cell of the flotation machine and stir for 60min. Add 900mL of 0.46mol / L HF (40% purity) solution into the flotation cell of the flotation machine and stir for 2h. Then move the sol into a polytetrafluoroethylene reaction kettle, and put it in an oven for crystallization at 180°C for 6 hours, then take it out, wash the product to be neutral, filter, and dry to obtain a solid product to obtain AlPO 4 -5 microporous molecular sieve material with ...

Embodiment 2

[0033] Select the XFD-1.5 flotation machine, add 1000mL deionized water and 143g phosphoric acid (85% purity) into the flotation cell of the flotation machine, turn on the flotation machine stirrer, the stirring speed is 1650r / min, and turn on the flotation Select the intake valve of the machine and adjust the intake volume to 0.1m 3 / h. Add 120g of dipropylamine dropwise into the flotation cell of the flotation machine, and continue stirring for 5-10min. Then slowly add 78g of aluminum hydroxide into the flotation cell of the flotation machine and stir for 30min. Add 10mL of 18mol / L HF solution into the flotation cell of the flotation machine and stir for 1.5h. Then move the sol into a polytetrafluoroethylene reaction kettle, and put it in an oven for crystallization at 150°C for 10 hours, then take it out, wash the product to be neutral, filter, and dry to obtain a solid product to obtain AlPO 4 -11 microporous molecular sieve material with a porosity of 91%.

Embodiment 3

[0035] Select the XFD-1.5 flotation machine, add 400mL deionized water and 73g phosphoric acid (85% purity) into the flotation cell of the flotation machine, turn on the flotation machine stirrer, the stirring speed is 1650r / min, and turn on the flotation Select the intake valve of the machine and adjust the intake volume to 0.05m 3 / h. Add 154g of aluminum isopropoxide (98% purity) dropwise into the flotation cell of the flotation machine and stir for 60min. Then add 44.5g of silicon dioxide powder into the flotation cell of the flotation machine and stir for 15min. Add 139.8g of dipentylamine dropwise into the flotation cell of the flotation machine, continue to stir for 10min, and adjust the pH value to 7.5 with HCl. Then move the sol into a polytetrafluoroethylene reaction kettle, and place it in an oven for crystallization at 180°C for 10 hours, then take it out, wash the product to be neutral, filter, and dry to obtain a solid product to obtain a SAPO-31 microporous mo...

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Abstract

The invention relates to a preparation method of a phosphorous-aluminum microporous molecular sieve and belongs to the technical field of porous material preparation. A phosphorous-aluminum microporous material is synthesized by a flotation machine, and sol is uniformly dispersed through high-speed stirring and bubbling, so that the phosphorous-aluminum microporous molecular sieve with the high pore forming rate is prepared. The sol is uniformly dispersed through high-speed stirring in the synthesis process, for abundant unformed sol, sol-gel forms regular micropores in a short time through outgoing of bubbles, and formation of compact imporous substances is avoided; the synthesis method is simple to operate, products are convenient to treat, and the synthesis technology is easy to popularize.

Description

technical field [0001] The invention relates to a method for preparing a phosphorus-aluminum microporous molecular sieve, which belongs to the technical field of porous material preparation. Background technique [0002] Microporous zeolite was discovered by Swedish scientist A.F.Cronstedt as early as 1756. In the 1940s, Barrer R. M. successfully synthesized zeolite molecular sieves through alkali and silicate under hydrothermal conditions. In 1961, the quaternary ammonium base was introduced into the zeolite synthesis system, and the microporous zeolite molecular sieve was synthesized with the directing agent or template agent. The material has the characteristics of regular structure, fixed pore type, large specific surface area and strong adsorption capacity. Traditional silica-alumina microporous molecular sieves such as A-type, X-type, Y-type and ZSM-5 can be synthesized under alkaline conditions. And by acidic conditions especially F - Aluminophosphorus microporous...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08
CPCC01B37/08C01B39/54
Inventor 吕存琴张继龙刘建红郭永晋春乔永生杨国臣
Owner SHANXI DATONG UNIV