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Method for conversion of dry powder for synthesis of porous composite framework material

A technology of skeleton materials and synthesis methods, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as increased environmental pollution, reduced yield, increased cost, etc., and achieves low operating costs and reaction promotion Large force, reduced operating energy consumption and cost

Inactive Publication Date: 2018-10-23
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that a large amount of solvents are used in the synthesis process of the current porous composite framework material, and the reactants are easily dissolved in the solvent, resulting in a decrease in yield, an increase in cost, and an increase in environmental pollution, the present invention provides a dry powder conversion synthesis porous composite framework The material method does not need to add solvent or liquid reactants to prepare the reaction mixture. The reactants are in the form of powder, granular or block, and then processed in the steam generated by the heating of the liquid phase at the bottom of the reaction vessel to obtain a porous composite skeleton material.

Method used

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  • Method for conversion of dry powder for synthesis of porous composite framework material
  • Method for conversion of dry powder for synthesis of porous composite framework material
  • Method for conversion of dry powder for synthesis of porous composite framework material

Examples

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Effect test

Embodiment 1

[0016] Example 1: A method of dry powder conversion to synthesize a porous composite framework material. Copper nitrate trihydrate is the coordination metal source in the porous composite framework material, and trimesic acid is the ligand of the porous composite framework material. Accurately weigh 0.0061 One mole of copper nitrate trihydrate and 0.004 mole of trimesic acid, the molar ratio of coordination metal source to ligand is 3.05:2, mix copper nitrate trihydrate and trimesic acid at room temperature and grind and stir for 10 minutes to form a dry material , and then transfer the mixed material into a polytetrafluoroethylene container with a height of about 30 mm.

[0017] Add 2ml of deionized water and 1.4ml of ethanol at the bottom of the reaction kettle with a volume of 100ml; put the polytetrafluoroethylene container containing the reaction materials into the reaction kettle, the dry materials in the reaction kettle will not be in direct contact with the liquid phase...

Embodiment 2

[0019] Example 2: A method of dry powder conversion to synthesize a porous composite framework material, copper carbonate is the coordination metal source in the porous composite framework material, trimesic acid is the ligand of the porous composite framework material, and 0.0061 moles of carbonic acid are accurately weighed respectively Copper and 0.004 moles of trimesic acid, the molar ratio of the coordination metal source and the ligand is 3.05:2, copper carbonate and trimesic acid are ground separately at room temperature, stirred for 5 minutes and mixed evenly to form a dry material, and the dry material is mixed in the following manner: Extrusion mixing, pneumatic mixing or impulse mixing, manual mixing and transfer of the mixed material into a Teflon container approximately 30mm high.

[0020] Add 1ml of deionized water and 2.0ml of industrial alcohol at the bottom of the reactor with a volume of 100ml; put the polytetrafluoroethylene container containing the reaction ...

Embodiment 3

[0021] Example 3: A method of dry powder conversion to synthesize a porous composite framework material. Nickel nitrate is the coordination metal source in the porous composite framework material, and trimesic acid is the ligand of the porous composite framework material. Accurately weigh 0.0061 moles of nitric acid respectively Nickel and 0.0244 moles of trimesic acid, the molar ratio of the coordination metal source and the ligand is 0.5:2, nickel nitrate and trimesic acid are respectively ball milled at room temperature and stirred for 5 minutes to form a dry material. The dry material is mixed in the following manner: Extrusion material mixing, pneumatic mixing or impulsive mixing, using a mechanical device for mixing, the mechanical device is any one of a blender, kneader, mixer, jet mixer or static mixer; then the mixed material Transfer to a Teflon container about 20 mm high.

[0022]Add 1.2ml mineral water and 1.8ml modified ethanol at the bottom of the reaction kettle...

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Abstract

The invention belongs to the technical field of preparation of porous composite materials, and provides a method for conversion of dry powder for synthesis of a porous composite framework material inorder to solve the problem in the prior art that a large amount of a solvent is used in the synthesis process of a porous composite framework material, yield is reduced, cost is increased and environmental pollution is increased. The method comprises the following steps: using metal salt or metal base as a coordinated metal source and using a carboxylic acid organic compound as a ligand; grinding,stirring and uniformly mixing the coordinated metal source and the ligand at room temperature to form a dry material; presetting a liquid phase at the bottom of a reaction kettle with the dry material in the container not directly contacting with the liquid phase; heating the reaction kettle, letting liquid vapor be contacted with the dry material to carry out a reaction, cooling and collecting asample in the container, and drying at room temperature to obtain a porous composite framework material. The method has advantages of zero emission of waste liquids, high yield, no washing, low operational cost, easy operation, low labor intensity, environmental protection and economic feasibility, and is easy to achieve large-scale intensive production. The obtained large granular composite framework material has higher adsorption capacity in terms of gas adsorption.

Description

technical field [0001] The invention belongs to the technical field of porous composite material preparation, and in particular relates to a method for synthesizing a porous composite framework material through dry powder conversion. During the preparation of the reaction mixture in this method, there is no need to add any solvents, liquid reactants or substances that are liquid at 1 standard atmospheric pressure (or local atmospheric pressure) and below 200°C, and the reaction mixture does not need to be made into a solution or colloid, and it is in the form of dry powder or The granular form can be converted in steam or mixed gas to obtain porous composite skeleton materials. Background technique [0002] Porous composite framework materials are a class of high specific surface functional materials with variable surface properties, pore structures, metal ions, adjustable framework composition, and specific chemical modification according to final application requirements. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C63/26C07C63/307
CPCC07C51/418C07C63/26C07C63/307
Inventor 薛春峰李晓红王恩阳杜晓郝晓刚
Owner TAIYUAN UNIV OF TECH
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