A kind of pure inorganic microporous desiccant and its synthesis method
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A synthesis method and desiccant technology are applied in the field of inorganic microporous material desiccant, which can solve the problems of rare reports of heteropolyacid microporous materials, and achieve the effects of high molecular weight, broad application value and large molecular volume.
Inactive Publication Date: 2017-03-22
XI'AN PETROLEUM UNIVERSITY
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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
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[0024] A kind of synthetic method of pure inorganic microporous desiccant, comprises the following steps:
[0025] (1) Weigh 55mmol of Na 2 WO 4 2H 2 O 18.2g was placed in a 100mL beaker, dissolved in 30mL of distilled water, stirred at room temperature, and 16.5mL of 4.0M hydrochloric acid was added dropwise to prepare solution A;
[0026] (2) Weigh 5mmol Na 2 SiO 3 0.61g was dissolved in 10mL distilled water to prepare 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) Then, under electromagnetic stirring, 9.0 g of solid KCl was added to the solution of step (4), and a large amount of white solids were precipitated after 15 minutes, which were filtered by a vacuum pump, placed at room temperature and dried to obtain white solid KCl. 8 SiW 11 o 39 ;
[0030] (6) Weigh K with a weight...
Embodiment 2
[0040] The remaining conditions are the same as in Example 1, the difference is that in step (8), 4 mL of 2.0 MKCl aqueous solution is added dropwise at a rate of 50 drops per minute, stirred at room temperature for 30 min, filtered, and the filtrate is allowed to stand at room temperature for two days, and colorless square crystals are precipitated , and the yield was 84.2%.
Embodiment 3
[0042] The remaining conditions are the same as in Example 1, except that in step (8), 6 mL of 2.0 MKCl aqueous solution is added dropwise at a rate of 50 drops per minute, stirred at room temperature for 30 min, filtered, and the filtrate is allowed to stand at room temperature for two days, and a colorless square crystal is precipitated , and 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 inorganic microporous material desiccant, relates to the synthesis of Keggin type silicotungstate, in particular to a pure inorganic microporous desiccant and its synthesis method, more specifically K 3 wxya 12 o 40 16H 2 The preparation method and crystal structure of O compound. Background technique [0002] At present, commonly used desiccants include silica gel, concentrated sulfuric acid, anhydrous calcium chloride, anhydrous magnesium sulfate, etc. Except for silica gel which is granular, the solid desiccant is irregular in shape, with a wide range of particle distribution and a considerable number of powder particles, which is inconvenient to use and becomes paste after moisture absorption, which is prone to leakage. Silica gel has a three-dimensional space network structure and is an amorphous structure. It has the advantages of good hygroscopicity, economical and practical, and convenient use. However, it is easy t...
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