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Pure inorganic microporous desiccant and synthetic method thereof

A synthesis method and desiccant technology, applied in the field of inorganic microporous new material desiccant, can solve the problems of rare reports of heteropolyacid microporous materials, and achieve the effects of high molecular weight, large molecular volume and enhanced adsorption capacity

Inactive Publication Date: 2015-12-30
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the metal-organic porous framework (MOF) material is a research hotspot of microporous materials. This kind of microporous materials have the reversible property of adsorption / desorption, and are widely used in the fields of gas storage, separation and catalysis. However, pure inorganic heterogeneous Rare reports on acid microporous materials

Method used

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  • Pure inorganic microporous desiccant and synthetic method thereof
  • Pure inorganic microporous desiccant and synthetic method thereof
  • Pure inorganic microporous desiccant and synthetic method thereof

Examples

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preparation example Construction

[0024] A synthetic method of pure inorganic microporous desiccant, comprising the following steps:

[0025] (1) Weigh 55mmol of Na 2 WO 4 ·2H 2 O18.2g was placed in a 100mL beaker, dissolved in 30mL distilled water, and under stirring at room temperature, 16.5mL of 4.0M hydrochloric acid was added dropwise to obtain solution A;

[0026] (2) Weigh 5mmolNa 2 SiO 3 1.1 g was dissolved in 10 mL of distilled water to obtain solution B;

[0027] (3) solution B is poured into solution A to obtain solution C;

[0028] (4) Under vigorous stirring, adjust the pH of solution C to 5.0-6.0 with 4.0M HCl, and then stir at room temperature for 100 min;

[0029] (5) under electromagnetic stirring then, add 9.0g solid KCl to the solution of step (4), separate out a large amount of white solid after 15min, vacuum pump suction filtration, place drying at room temperature to obtain white solid K 8 SiW 11 O 39 ;

[0030] (6) Weigh K with a weight of 1.0g 8 SiW 11 O 39 ·14H 2 O was di...

Embodiment 2

[0040] The remaining conditions are the same as in Example 1, the difference is that in step (8), the aqueous solution of 4mL2.0MKCl was added dropwise at a rate of 50 drops per minute, stirred at room temperature for 30min, filtered, and the filtrate was allowed to stand at room temperature for two days to separate out colorless tetragonal crystals , the yield was 84.2%.

Embodiment 3

[0042] The remaining conditions are the same as in Example 1, the difference is that in step (8), the aqueous solution of 6mL of 2.0MKCl was added dropwise at a rate of 50 drops per minute, stirred at room temperature for 30min, filtered, and the filtrate was allowed to stand at room temperature for two days to separate out colorless tetragonal crystals , the yield was 84.5%.

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Abstract

The invention discloses a pure inorganic microporous desiccant and a synthetic method thereof. The chemical formula of the desiccant is K3HSiW12O40.16H2O, the molecular weight is 3343.59, a space group is Pm3<->m, cell parameters: shown as an equation, Dc=4.605g.cm<-3>, and Z=1, the synthetic method comprises the steps of weighing Na2WO4.2H2O and dissolving the Na2WO4.2H2O into water, and dropwise adding hydrochloric acid to obtain a solution A; weighing Na2SiO3 and dissolving the Na2SiO3 into distilled water so as to obtain a solution B; mixing the solution A and the solution B and adjusting the pH value of a mixed solution by using HCl, adding solid KCl into the mixed solution, separating out a white solid, performing suction filtration, and drying so as to obtain K8SiW11O39.14H2O; then dissolving the K8SiW11O39.14H2O into distilled water to obtain a solution; adjusting the pH by using diluted hydrochloric acid, dropwise adding an aqueous solution containing KCl, stirring for 30min at room temperature, standing for two days in a filtrate chamber, separating out a colorless square shaped crystal; the pure inorganic microporous desiccant is simple in the synthetic method, pure in products, high in productive rate, clear and definite in composition and structure, good in heat stability, free of corrosivity and pollution to environment, can quickly adsorb water vapour in air and water in an organic solvent, and can be recycled and reused after being dried at 150 DEG C.

Description

technical field [0001] The invention belongs to an inorganic microporous new material desiccant, and relates to the synthesis of Keggin-type silicotungstic acid salts, in particular to a pure inorganic microporous desiccant and a synthesis method thereof, more specifically K 3 HSiW 12 O 40 ·16H 2 Preparation method and crystal structure of O compound. Background technique [0002] The commonly used desiccants are silica gel, concentrated sulfuric acid, anhydrous calcium chloride, anhydrous magnesium sulfate, etc. The solid desiccant is in irregular shape except the silica gel which is granular. The particle distribution range is very wide, and there are a considerable number of powdery particles. Silica gel has a three-dimensional spatial network structure, which belongs to an amorphous structure. It has the advantages of good hygroscopic performance, economical and practical, and easy to use. However, it is easy to break after absorbing a large amount of water, which li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/00B01D53/28
Inventor 刘雪梅于洪江徐海升韦海龙
Owner XI'AN PETROLEUM UNIVERSITY
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