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Method for producing ordered mesoporous polymer, material with carbon element and composite material in macro amount

A composite material and polymer technology, applied in the fields of mesoporous polymers, carbon materials and composite materials, can solve the problems of low space utilization, complicated operation, long reaction cycle, etc., to simplify the production process, optimize the production conditions, produce Efficient effect

Inactive Publication Date: 2008-08-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this way, there are still many limitations in this method: for example, it is necessary to scrape and collect the product from the surface of the glass substrate, and then carry out subsequent processing; in the process of solvent volatilization and high temperature thermal polymerization, the utilization rate of space is low; the recovery rate of the product is not good, etc. Wait
For this reason, it has also been proposed to use the aqueous solution co-assembly method to prepare mesoporous polymer materials first, and then prepare mesoporous carbon materials by carbonization, but this method has a long reaction cycle and complicated operation.
These shortcomings have formed obstacles to the large-scale industrial production and wide application of mesoporous polymers, carbon materials and composite materials.
So far, there are no reports on the large-scale preparation of ordered mesoporous polymers, carbon materials and composite materials

Method used

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  • Method for producing ordered mesoporous polymer, material with carbon element and composite material in macro amount
  • Method for producing ordered mesoporous polymer, material with carbon element and composite material in macro amount
  • Method for producing ordered mesoporous polymer, material with carbon element and composite material in macro amount

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1, taking phenol and formaldehyde to form a phenolic resin polymer precursor as an example, its preparation is as follows: 305g of phenol is melted at 40-42°C, then 52g of sodium hydroxide solution with a concentration of 25% by mass is added and stirred evenly, Then add 530g of formaldehyde solution with a mass percentage concentration of 37%, and polymerize in a water bath at 65-75°C for 70 minutes. After cooling to room temperature, neutralize to neutral with 32g of concentrated hydrochloric acid. Water was removed by pressure distillation to obtain 520 g of polymer precursor (phenolic resin) (molecular weight 200-500). The obtained polymer precursor (phenolic resin) was dissolved in 780 g of ethanol to obtain an ethanol solution with a mass percent concentration of 40% of the polymer precursor (phenolic resin) used in the reaction.

Embodiment 2

[0044] Example 2, using the triblock copolymer F127 as the structure directing agent system, the steps of preparing the mesoporous carbon material are as follows: 20g F127 is uniformly dispersed in 200g ethanol; The ethanol solution was mixed, and the reaction sol was obtained after magnetic stirring at 30°C for 60 minutes, and then the reaction sol was attached to a volume of 1800cm 3 , the density is 0.02g / cm 3 Polyether polyurethane sponge. The solvent was evaporated for 6 hours at 32°C. The obtained sponge was thermally polymerized in an oven at 100° C. for 20 hours to obtain 75 g of a material composed of F127 / polymer / sponge (99% yield). Its small-angle X-ray scattering spectrum (SAXS) is attached figure 1 As shown, it has a two-dimensional hexagonal channel structure. Then put the sponge in a nitrogen-protected tube furnace and bake at 620° C. for 3 hours with a heating rate of 1° C. / min to obtain 30 g of mesoporous carbon material. The small-angle X-ray scattering ...

Embodiment 3

[0045] Example 3, using tri-block copolymer F127 as a structure directing agent, the steps of synthesizing mesoporous polymer materials and carbon materials are as follows: 100g F127 is uniformly dispersed in 1500g ethanol; then mixed with 200g phenolic resin polymer precursor 500g of ethanol solution was mixed, and the reaction sol was prepared after stirring with a magnetic stirrer at 25°C for 90 minutes; then the reaction sol was attached to a volume of 14000cm 3 , the density is 0.02g / cm 3 The solvent was evaporated at 30° C. for 7 hours on a polyether polyurethane sponge. The obtained sponge was placed in an oven at 100° C. for static thermal polymerization treatment for 24 hours to obtain 580 g of a material composed of F127 / polymer / sponge (99% yield). The sponge is then placed in a vacuum tube furnace and roasted at 350° C. for 3.5 hours (vacuum degree is -0.1 MPa), and the heating rate is 1° C. / min to remove the surfactant template agent, and obtain 297 g of mesoporou...

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Abstract

The invention relates to a method of mass preparation of orderly mesoporous macromolecule, carbon material and composite material, belonging to the technical field of the macromolecule and nanometer material. With polyurethane sponge as frame, nonionic surface-active material as structural guide, macromolecule precursor as carbon source and inorganic silicon source and other materials as addition agent, through hot polymerization and carburetion, mesoporous macromolecule with orderly continuous mesoporous porous channel, high specific surface area and large hole volume, carbon material and composite material are prepared in large quantity. The method of mass preparation of orderly mesoporous macromolecule, carbon material and composite material has the advantages of low cost, time and labor saving, easy recovery of products, thus facilitating industrial production.

Description

technical field [0001] The invention belongs to the field of macromolecules, nanomaterials and porous molecular sieve materials, and in particular relates to a method for macromolecular preparation of mesoporous macromolecules, carbon materials and composite materials with ordered pore structure by using cheap polyurethane sponge as a skeleton support . technical background [0002] Ordered mesoporous materials obtained by self-assembly of surfactants have large specific surface area and pore volume, uniform and adjustable pore size and skeleton composition, and controllable morphology. It has broad application prospects and has been widely valued by people. In the large family of mesoporous materials, ordered mesoporous carbon materials are more attractive. In addition to the above-mentioned excellent properties, mesoporous carbon materials show broad application prospects in electric double layer supercapacitors, solar cells, lithium-ion batteries, fuel cells and other f...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B31/08
Inventor 薛春峰屠波赵东元
Owner FUDAN UNIV
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