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Solvent-free and kilogram-scale preparation method for regular mesoporous phenol-formaldehyde resin

A phenolic resin, kilogram technology, applied in the field of material science, can solve the problems of cumbersome preparation process, unfavorable industrial production, high synthesis cost, and achieve the effects of green preparation process, improved surface alkalinity, and good adsorption activity

Inactive Publication Date: 2019-02-01
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, the present invention aims at the production technical defects such as high synthesis cost, cumbersome preparation process, solvent and strong acid or strong base catalyst unfavorable for industrial production, etc., through a simple, fast, green and solvent-free one-step synthesis method, thereby realizing a kind of Solvent, method for preparing regular mesoporous phenolic resin at kilogram level

Method used

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  • Solvent-free and kilogram-scale preparation method for regular mesoporous phenol-formaldehyde resin
  • Solvent-free and kilogram-scale preparation method for regular mesoporous phenol-formaldehyde resin
  • Solvent-free and kilogram-scale preparation method for regular mesoporous phenol-formaldehyde resin

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Embodiment 1

[0029] This embodiment provides a solvent-free regular mesoporous polymer with m-aminophenol as the phenolic organic compound, terephthalaldehyde as the aldehyde compound, and F127 as the block template polymer.

[0030] Its preparation method comprises the following steps:

[0031] Weigh 2.2g of block copolymer template, 0.47g of m-aminophenol and 0.64g of terephthalaldehyde in 50ml of polytetrafluoroethylene lining. Drying oven, curing at 140°C for 24 hours, the curing temperature rising rate is 5°C / min, the obtained sample is transferred to a tube furnace, and carbonized at 360°C for 5 hours under a nitrogen atmosphere, the carbonization heating rate is 5°C / min, and the removed The regular mesoporous polymer after removing the templating agent is denoted as OMP-A.

Embodiment 2

[0033] This embodiment provides a solvent-free regular mesoporous polymer with m-aminophenol as the phenolic organic compound, terephthalaldehyde as the aldehyde compound, and F127 as the block template polymer.

[0034] Its preparation method comprises the following steps:

[0035] Weigh 11g of block copolymer template, 2.35g of m-aminophenol and 3.2g of terephthalaldehyde in 50ml of polytetrafluoroethylene lining. box, cured at 140°C for 24 hours, the curing temperature rise rate was 5°C / min, the obtained sample was transferred to a tube furnace, and carbonized at 360°C for 5 hours under a nitrogen atmosphere, the carbonization temperature rise rate was 5°C / min, and the removal The regular mesoporous polymer after the template is denoted as OMP-B.

Embodiment 3

[0037] This embodiment provides a solvent-free regular mesoporous polymer with m-aminophenol as the phenolic organic compound, terephthalaldehyde as the aldehyde compound, and F127 as the block template polymer.

[0038] Its preparation method comprises the following steps:

[0039] Weigh 22g of block copolymer template, 4.3g of m-aminophenol and 6.1g of terephthalaldehyde in 100ml of polytetrafluoroethylene lining. Box, cured at 140°C for 24 hours, the curing temperature rise rate was 5°C / min, the obtained sample was transferred to a tube furnace, and carbonized at 360°C for 5 hours under a nitrogen atmosphere, the carbonization temperature rise rate was 5°C / min, and the template was removed The regular mesoporous polymer after curing is denoted as OMP-C.

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Abstract

The invention provides a solvent-free and kilogram-scale preparation method for regular mesoporous phenol-formaldehyde resin. A phenolic organic compound and an aldehyde organic compound are adopted as the raw materials, a block copolymer is taken as the template, and a simple, fast and solvent-free one-step synthesis method is utilized to realize amplified preparation of mesoporous phenol-formaldehyde resin. At the same time, by optimizing the experimental parameters, laboratory gram-scale preparation is successfully expanded to kilogram-scale material preparation, and the prepared material maintains a highly regular mesoporous structure and the doping of nitrogen heteroatoms. By optimizing the structural parameters of the material, the amplification prepared material in the invention shows excellent adsorption performance (a hydrogen sulfide adsorption capacity up to 3.2-5.3mmol / g under a 0DEG C condition) in hydrogen sulfide gas adsorption performance test. The method provided by the invention is of important practical significance for realizing green and large-scale preparation of regular mesoporous phenol-formaldehyde resin and application of the resin to selective desorptionof hydrogen sulfide.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to a solvent-free method for preparing regular mesoporous phenolic resin at the kilogram level. Background technique [0002] Due to its high specific surface area, adjustable pore size, unique organic framework, and regular pore structure, regular mesoporous polymers have broad applications in high-tech fields such as heterogeneous catalysis, gas adsorption, biomedicine, and nanodevices. Application prospects. At present, regular mesoporous polymers are mainly phenolic resins and their derivatives, which have low preparation cost, controllable surface wettability and excellent acid and alkali resistance, which have attracted widespread attention and have been successfully applied in many researches. field. [0003] So far, regular mesoporous phenolic resins usually use solvent evaporation-induced self-assembly (EISA) or high-temperature hydrothermal synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/26C08G8/04B01J20/26B01J20/30B01D53/02C08L61/06
CPCB01D53/02B01J20/262B01J2220/4812C08G8/04C08J9/26C08J2201/046C08J2361/06
Inventor 刘福建阚巡赵思萌曹彦宁米金星江莉龙
Owner FUZHOU UNIV
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