Method for assisted synthesis of porous composite material by using assistant transfer byproduct

A technology of porous composite materials and by-products, which is applied in the field of preparing porous composite materials assisted by auxiliary transfer reaction by-products, can solve the problem of increasing the difficulty of mother liquor treatment, difficult new synthesis of mother liquor, unreasonable synthesis methods, etc. problems, to achieve the effect of easy conversion, thorough conversion, and low operating costs

Inactive Publication Date: 2019-11-22
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] As a kind of composite material in which the solvent participates in crystallization, the direct reuse of the mother liquor in the preparation process and how to transfer the by-products in time are still in the research stage. Needless to say, there are direct introduction of organic or inorganic bases into the reaction system to neutralize There are reports on materials related to the synthesis of by-product acids, but this method complicates the composition of the mother liquor, exacerbates the difficulty of sample washing and subsequent treatment of the mother liquor, and the mother liquor is also difficult to use for new synthesis. From the perspective of economy and environmental protection , the synthesis method of directly introducing additives is not reasonable

Method used

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  • Method for assisted synthesis of porous composite material by using assistant transfer byproduct

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Effect test

Embodiment 1

[0041] A method for assisting the synthesis of porous composite materials by using auxiliary agents to transfer by-products, specifically: measure 10 milliliters of deionized water and 10 milliliters of industrial alcohol respectively, and mix the two; weigh 3.624 grams of copper nitrate trihydrate and 2.102 Trimellitic acid; Add copper nitrate trihydrate to the aforementioned mixed solvent at 27°C, stir for 0.2 hours, then add trimesic acid, stir for 1.0 hour to form a reaction mixture, add 0.6 grams of sodium hydroxide solid at the bottom of the reaction kettle As an auxiliary agent, the container containing the reaction mixture is sealed in a self-pressurized reactor, and the sodium hydroxide is not in direct contact with the reaction mixture, heated to 110 ° C for 10 hours, cooled, filtered the sample in the container, and dried at room temperature to obtain the product. Collect the by-product sodium nitrate at the bottom of the kettle, which is formed by the reaction of so...

Embodiment 2

[0043] A kind of method that utilizes auxiliary agent to transfer by-product to assist the synthesis of porous composite material, specifically: measure 18 milliliters of deionized water, 5 milliliters of 95 ethanol, 5 milliliters of acetone, 5 milliliters of dimethyl ether and 5 milliliters of ether respectively, and put them Mix; weigh 0.9378 grams of aluminum nitrate nonahydrate, 0.5010 grams of aluminum acetate, 0.6047 grams of ferric nitrate, 0.4055 grams of ferric chloride and 2.102 grams of trimesic acid; add the weighed metal salt to the aforementioned mixed solvent at 30 °C , stirred for 0.5 hour, then added trimesic acid, stirred for 1.5 hours and mixed to form a reaction mixture, placed 1.4 grams of lithium hydroxide as an auxiliary agent at the bottom of the reaction kettle, then sealed the container of the reaction mixture in a self-pressurized reaction kettle, hydrogen Lithium oxide is not in direct contact with the reaction mixture, heated to 108 ° C for 10 hours...

Embodiment 3

[0045] A method for assisting the synthesis of porous composite materials by using auxiliary agents to transfer by-products, specifically: measure 20 milliliters of deionized water and 20 milliliters of ethanol respectively, and mix the two; add 3.624 grams of copper nitrate trihydrate to the aforementioned In the mixed solvent, stir for 0.2 hour, then add 2.102 gram of trimesic acid, stir for 1.0 hour and mix to form a reaction mixture, place 1.2 gram of sodium hydroxide solid at the bottom of the reaction kettle as an auxiliary agent, then the container containing the reaction mixture is sealed in an automatic In the pressure reaction kettle, sodium hydroxide does not directly contact with the reaction mixture, heated to 105 ° C for 10 hours, cooled and filtered to collect the sample in the container, and obtained the product after drying, and collected the by-product sodium nitrate at the bottom of the kettle, which is composed of solid hydrogen It is formed by the reaction ...

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Abstract

The invention discloses a method for assisted synthesis of a porous composite material by using an assistant transfer byproduct. According to the method, an alkaline auxiliary agent is placed in a reaction device and is not in direct contact with reactants, and the amount-of-substance ratio of the auxiliary agent to by-product acid is controlled, so that the porous composite material is obtained through heating treatment in a sealed reaction kettle; and the grain size and distribution of the composite framework material are regulated and controlled; meanwhile, by-product acid in the mother liquor steam is in contact with an alkaline additive to form salt to be fixed, the salt is not returned to the mother liquor anymore; the salt can be used as a by-product for sale, while the mother liquor is directly used as a solvent to dissolve the next batch of reaction raw materials. The whole reaction process is easy to operate, low in operation cost, zero in three-waste emission, high in yieldand easy to realize large-scale production.

Description

technical field [0001] The invention relates to a preparation method of a porous composite material, in particular to a preparation method for assisting the synthesis of a porous composite material by using auxiliary agent transfer reaction by-products. Background technique [0002] Porous composite materials are a kind of microporous functional materials with high specific surface area. Their surface properties, pore structure, and skeleton composition are variable, and can be modified according to the target requirements. The application potential in the fields of energy release, energy storage, optical devices, and chromatographic analysis has become increasingly huge, which has attracted attention and research from all walks of life around the world. [0003] At present, such materials can be synthesized by hydrothermal method, ultrasonic method, microwave method, solvothermal method, grinding method, etc. Taking the hydrothermal method as an example, a large amount of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/08C07F19/00C07F15/04C07F15/06C08G83/00C01D9/08C07C51/41C07C53/10C01D3/04B01D53/02B01J19/02
CPCB01D53/02B01D2257/504B01J19/02C01D3/04C07C51/412C07F1/08C07F15/025C07F15/045C07F15/065C08G83/008C07C53/10Y02C20/40
Inventor 薛春峰李晓红张潜刘刚郝晓刚
Owner TAIYUAN UNIV OF TECH
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