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Slurry state synthetic method for porous composite framework material

A framework material and synthesis method technology, applied in chemical instruments and methods, preparation of organic compounds, copper-organic compounds, etc., can solve the problems that the slurry method is not used to synthesize inorganic-organic composite framework materials, and the solvent is in a blank stage. Achieve the effect of eliminating the discharge of metal ions and organic ligands, facilitating adsorption and storage, and avoiding washing

Inactive Publication Date: 2018-02-09
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] As an inorganic-organic composite framework material that requires solvents to participate in crystallization, the consumption of solvent and the control of crystal size in the preparation process are still in the blank stage, and there is no literature on the synthesis of inorganic-organic composite framework materials using the slurry method.

Method used

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  • Slurry state synthetic method for porous composite framework material
  • Slurry state synthetic method for porous composite framework material
  • Slurry state synthetic method for porous composite framework material

Examples

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Effect test

Embodiment 1

[0022] Example 1: A method for synthesizing a porous composite framework material in a slurry state, comprising the following steps: (1) selecting a solvent: the solvent is a mixture of 1.6 ml of deionized water and 1.4 ml of ethanol;

[0023] (2) Accurately weigh 0.0061 moles of copper nitrate trihydrate as the metal precursor, and accurately weigh 0.004 moles of trimesic acid as the organic ligand of the porous composite framework material;

[0024] (3) At room temperature, add copper nitrate trihydrate to the solvent prepared in step (1), stir for 10 minutes, then add trimesic acid, stir for 2 hours to form a slurry, seal it in a self-pressurized reactor, and heat to 110 °C for 10 h, and dried at room temperature to obtain a granular product.

[0025] The granular product that obtains is photographed, and optical photo shows that the size of most of particles is about about 140 microns (as Image 6 shown), the XRD pattern shows that its crystallinity is high, and the growt...

Embodiment 2

[0026] Embodiment 2: A method for synthesizing a porous composite skeleton material in a slurry state, comprising the following steps: (1) selecting a solvent: the solvent is a mixture of 1.0 ml of deionized water and 2.0 ml of industrial alcohol;

[0027] (2) Accurately weigh 0.0061 mole of copper sulfate as the metal precursor, and accurately weigh 0.004 mole of trimesic acid as the organic ligand of the porous composite framework material;

[0028] (3) At room temperature, add copper sulfate to the solvent prepared in step (1), stir for 10 minutes, then add trimesic acid, stir for 2 hours to form a slurry, seal it in a self-pressurized reactor, and heat it to 100°C for reaction After 16 hours, dry at room temperature to obtain a granular product.

[0029]The test of the product shows that the optical photos show that its size is about 130 microns, the specific surface area is about 1690 square meters per gram, the pore volume is about 0.53 cubic centimeters per gram, the po...

Embodiment 3

[0030] Embodiment 3: A method for synthesizing a porous composite skeleton material in a slurry state, comprising the following steps: (1) selecting a solvent: the solvent is mixed with 1.2 ml of deionized water and 1.8 ml of ethylene glycol;

[0031] (2) Accurately weigh 0.0061 mole of copper chloride as the metal precursor, and accurately weigh 0.004 mole of trimesic acid as the organic ligand of the porous composite framework material;

[0032] (3) At room temperature, add copper chloride to the solvent prepared in step (1), stir for 10 minutes, then add trimesic acid, stir for 2 hours to form a slurry, seal it in a self-pressurized reactor, and heat to 110°C After reacting for 13 hours, the granular product can be obtained by drying at room temperature.

[0033] The test of the product shows that the optical photos show that its size is about 110 microns, the specific surface area is about 1601 square meters per gram, the pore volume is about 0.50 cubic centimeters per gra...

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Abstract

The invention belongs to the technical field of preparation of porous composite materials, and provides a slurry state synthetic method for a porous composite framework material. The mass ratio of a solvent to a solid reactant is controlled, so that the reactant is at different saturations, an inorganic-organic composite framework material is obtained through heating in a sealed container, and thecrystal size and distribution of the composite framework material are regulated and controlled. Under a room temperature, an inorganic metal source is dispersed into the solvent, and then mixed witha polycarboxylic acid organic compound to form a slurry material, and the slurry material is sealed in a self-pressurized reaction kettle, the obtained material is heated to 70-170 DEG C, a reaction is performed for 0.5-240 hours, drying is performed at the room temperature, and therefore the porous composite framework material is obtained. According to the invention, the crystal size is controllable, and the method provides a novel synthetic route for controlling the particle size of the composite framework material; the yield is higher, washing is not needed, the operating costs are low, theoperation is easy, the emission is zero, the method is green, environmentally friendly, economical and practicable, and the large-scale intensive production is easy to realize; and the obtained large-particle composite framework material has a higher adsorption capacity in the gas adsorption aspect.

Description

technical field [0001] The invention belongs to the technical field of preparation of porous composite materials, and in particular relates to a slurry-state synthesis method of porous composite skeleton materials. The method uses a very small amount of solvent, and the reactants are transformed in a slurry state to obtain porous composite materials with different particle sizes. Background technique [0002] Porous composite materials are a new type of microporous high specific surface functional materials. The surface properties, pore structure, and central metal ion coordination form are changeable, and specific chemical modifications can be carried out according to the final application requirements. With the research in recent years, it has great application potential in the fields of gas storage and separation, drug storage and release, energy storage, optical devices, chromatographic analysis, etc. . [0003] At present, methods for synthesizing such materials inclu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/08C07F3/06C07F15/04C07F15/06C07F15/02C07F5/06C07F19/00C07C63/307C07C51/41C08G83/00B01J20/22B01J20/30B01D53/02
CPCB01D53/02B01D2253/204B01J20/226C07C51/418C07C63/307C07F1/005C07F3/003C07F5/069C07F15/025C07F15/045C07F15/065C08G83/008
Inventor 薛春峰李晓红王恩阳杨复娟郝晓刚王俊文
Owner TAIYUAN UNIV OF TECH
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