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Rapid preparation method for A-type nano zeolite molecular sieve

A zeolite molecular sieve and nanotechnology, which is applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of long preparation period of nano A-type zeolite molecular sieve, shorten the synthesis period, inhibit the polycondensation rate, The effect of shortening the time

Inactive Publication Date: 2015-03-11
KUNMING UNIV OF SCI & TECH TECH IND SALES MANAGEMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the preparation cycle of nano-type A zeolite molecular sieve is too long, and propose a simple and rapid method for synthesizing nano-type A zeolite molecular sieve

Method used

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  • Rapid preparation method for A-type nano zeolite molecular sieve
  • Rapid preparation method for A-type nano zeolite molecular sieve
  • Rapid preparation method for A-type nano zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) by SiO 2 :Al 2 o 3 : Na 2 O: (TMA) 2 O: H 2 The molar ratio of O is 10.95: 1.8: 0.45: 14: 690. Weigh the reaction raw materials corresponding to the above substances, such as ethyl orthosilicate, aluminum isopropoxide, sodium hydroxide, tetramethylammonium hydroxide, deionized water, spare;

[0031] (2) Divide 27ml of deionized water in step (1) into two parts, one part accounts for 2 / 3 of the total volume, and the other part accounts for 1 / 3 of the total volume, and the volume accounts for 2 / 3 under stirring at 40°C Slowly add 2.29g of aluminum isopropoxide to 18ml of deionized water, and add 2.8g of sodium hydroxide solution with a concentration of 1mol / L, 15.9g of tetramethylammonium hydroxide (TMAOH 5H 2 (0), fully stir, prepare solution A;

[0032] (3) Add hydrochloric acid solution to 9ml of deionized water accounting for 1 / 3 of the volume, the pH of the solution after adding hydrochloric acid is = 5, and then slowly mix 7.1g of tetraethyl orthosilicate...

Embodiment 2

[0036] (1) by SiO 2 :Al 2 o 3 : Na 2 O: (TMA) 2 O: H 2 The molar ratio of O is 12.2: 1.89: 0.56: 15: 780. Weigh the reaction raw materials corresponding to the above substances, such as tetraethyl orthosilicate, aluminum powder, sodium hydroxide, tetramethylammonium hydroxide, deionized water, spare;

[0037] (2) Divide 36ml of deionized water in step (1) into two parts, one part accounts for 2 / 3 of the total volume, and the other part accounts for 1 / 3 of the total volume, and the volume accounts for 2 / 3 under stirring at 30°C Slowly add 0.38g of aluminum powder to 24ml of deionized water, and add it in one hour, then add 4.15g of sodium hydroxide solution with a concentration of 1mol / L, 21.5g of tetramethylammonium hydroxide (TMAOH·5H 2 (0), fully stir, prepare solution A;

[0038] (3) Add nitric acid solution to 12ml of deionized water accounting for 1 / 3 of the volume, the pH of the solution after adding nitric acid is 1, and then slowly mix 9.3g of tetraethyl orthosi...

Embodiment 3

[0042] (1) by SiO 2 :Al 2 o 3 : Na 2 O: (TMA) 2 O: H 2 The molar ratio of O is 5:1:0.2:10:500, and the reaction raw materials corresponding to the above substances are weighed orthosilicate ethyl ester, gibbsite, sodium hydroxide, tetramethylammonium hydroxide, deionized water, etc., spare;

[0043] (2) Divide 33ml of deionized water in step (1) into two parts, one part accounts for 2 / 3 of the total volume, and the other part accounts for 1 / 3 of the total volume, and the volume accounts for 2 / 3 under stirring at 35°C Slowly add 0.76g gibbsite in 22ml of deionized water, add 1.95g concentration and be 1mol / L sodium hydroxide solution, 17.4g tetramethylammonium hydroxide (TMAOH·5H 2 (0), fully stir, prepare solution A;

[0044] (3) Add sulfuric acid solution to 11ml of deionized water accounting for 1 / 3 of the volume, the pH of the solution after adding sulfuric acid is 3, and then slowly mix 4.91g of ethyl orthosilicate at a rate of 0.3ml / min under magnetic stirring at r...

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Abstract

The invention discloses a rapid preparation method of nanometer A-type zeolite molecular sieve. In this method, a certain amount of aluminum source is added to deionized water, and then sodium hydroxide and organic template agent tetramethylammonium hydroxide are added; Add ethyl orthosilicate that has been catalytically hydrolyzed by an acid solution with pH=1-5; stir and age the above mixture at room temperature for 1-10 hours, and then put it into a hydrothermal synthesis kettle for crystallization at 70-120°C 3 -15h, and then undergo ultrasonic, centrifugal, drying, calcination and other steps to prepare type A nano zeolite molecular sieve; this preparation method is simple, greatly shortens the reaction time, and the particle size of the prepared nano type A zeolite molecular sieve can reach less than 100nm and the particle size is The diameter distribution is uniform.

Description

technical field [0001] The invention belongs to the field of preparation of nanometer zeolite molecular sieves, in particular to a method for synthesizing nanometer type A zeolite molecular sieves in a short period. Background technique [0002] As far as solid physics is concerned, when the particle size is reduced to below 100nm, it enters the category of nanomaterials, which will show the small size effect and surface effect that conventional size particles do not have. Compared with molecular sieves of conventional size, nanoscale molecular sieves have a larger outer surface area and more active centers on the outer surface, so that more active adsorption sites are exposed, which is beneficial to the realization of molecular sieve catalytic and adsorption performance. At present, there are two methods for artificially synthesizing nanoscale molecular sieves: one is to increase the low-temperature aging time; the other is to reduce the crystallization temperature. These ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/14
Inventor 刘艳娜白璞孙彦琳赵文波李艳红龙丽李桦军
Owner KUNMING UNIV OF SCI & TECH TECH IND SALES MANAGEMENT
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