Preparation method for phenolic aerogel

An aerogel and phenolic technology, applied in the field of preparation of phenolic aerogel, can solve the problems of unfavorable large-scale industrial production, long preparation period, expensive drying equipment and the like

Inactive Publication Date: 2019-11-19
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a long preparation cycle, needs to use a reactor for gel reaction, and expensive drying equipment, which is not conducive to large-scale industrial production

Method used

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  • Preparation method for phenolic aerogel
  • Preparation method for phenolic aerogel

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[0021] The invention provides a preparation method of the phenolic airgel with simple preparation process and low cost. The method is: a. Use phenols, aldehydes and amines as raw materials, add a basic catalyst, and add acid to adjust the pH value. b. Add accelerator, etherification agent, and water as solvent to adjust pH. c After the sol-gel reaction, the wet gel is obtained by curing, and the aqueous solution is replaced by an organic solvent, and dried to obtain the phenolic aerogel.

[0022] Described phenolic airgel can be prepared as follows:

[0023] Described aldehydes are any in liquid formaldehyde, paraformaldehyde, acetaldehyde, preferably liquid formaldehyde.

[0024] The basic catalyst is any one of NaOH, ethanolamine and diethanolamine.

[0025] The conditions for obtaining the mixture in step a: the reaction temperature is 55°C, the time is 0.5-1h; the molar ratio n 酚 :n 胺 :n 醛 =1:3:8.

[0026] The phenols are any one of phenol, resorcinol and phlorogluc...

Embodiment 1

[0034] The molar ratio of each component is n 苯酚 :n 三聚氰胺 :n 甲醛 =1:3:8, W (苯酚+三聚氰胺+甲醛) :W 水 =1:2

[0035] In a water bath at 55°C, add 68g of 37% liquid formaldehyde, 100g of distilled water, add 1g of triethanolamine, stir and mix, measure the pH and adjust the pH to 8.57 with 20% dilute hydrochloric acid (10g concentrated hydrochloric acid + 40g water). Then add 10g phenol and 40g melamine, react at 55°C, turn transparent and start to cool down to 50°C, stir steadily for 30min, cool down to 45°C, add 20% dilute hydrochloric acid dropwise to adjust to 7.75. Add 10g of methanol and 1g of ammonium persulfate, continue to react at 43-45°C for 30min, cool down to 30°C and discharge. At this time, the pH was adjusted to 1.04 with concentrated hydrochloric acid, and the solution was left to age for 3 days with the mouth closed, and the solution began to appear gelatinous. The obtained wet gel was soaked in tert-butanol to replace the water therein, and placed in a freeze dryer...

Embodiment 2

[0037] The molar ratio of each component is n 间苯二酚 :n 乙二胺 :n 甲醛 =1:3:8, W (间苯二酚+乙二胺+甲醛) :W 水 =1:2

[0038] In a water bath at 55°C, add 24g of paraformaldehyde, 104g of deionized water, 1g of diethanolamine, stir and mix, measure the pH, and adjust the pH to 8.50 with 20% dilute hydrochloric acid (10g of concentrated hydrochloric acid + 40g of water). Then add 10g of resorcinol and 18g of ethylenediamine and react at 55°C. After it becomes transparent, start to cool down to 50°C. Stir steadily for 30 minutes. Measure the pH after cooling down to 45°C. Add 20% dilute hydrochloric acid dropwise to adjust to 7.70. Add 10g of ethanol and 1g of potassium persulfate, continue to react at 43-45°C for 30min, cool down to 30°C and discharge. At this time, the pH was adjusted to 1.01 with concentrated hydrochloric acid, and the solution was left to age for 3 days with the mouth closed, and the solution began to appear gelatinous. The obtained wet gel was soaked in acetone to repla...

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Abstract

The invention provides a preparation method for a phenolic aerogel. The phenolic aerogel is prepared from a template polymer, phenols, amines and aldehydes through water blending, crosslinking and drying, and belongs to the field of material preparation technology. The preparation method for the phenolic aerogel of the invention comprises the following successive steps: a, mixing phenols, aldehydes, amines, a catalyst, an initiator and the like in water, and carrying out heating in a water bath; b, adding the template polymer, adjusting a pH value, carrying out a sol-gel reaction, and performing standing and ageing so as to obtain a wet gel; and c, immersing the obtained gel in an organic solvent for replacement, and carrying out drying to obtain the organic phenolic aerogel. The preparation method of invention has mild reaction conditions, prepares the aerogel under low-temperature heating conditions, is simple to operate, is safe and reliable, and uses easily-available and cheap rawmaterials.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a preparation method of phenolic airgel. Background technique [0002] Compared with traditional foam materials, aerogels have high research value because of their special properties, such as higher surface area, higher porosity, and lower density. Aerogels can be divided into two categories: inorganic aerogels and organic aerogels. Since silica aerogels were first prepared by Kislter in 1931, aerogels have been used in various fields. Airgel materials, organic aerogels have better sound insulation and heat insulation properties. In the late 1980s, Pekala synthesized phenolic resin (RF) aerogels for the first time. Airgel materials can meet the national standard GB8624-2012 "Classification of Combustion Performance of Building Materials and Products" A-level non-combustible standard, even if it is swallowed by fire, there is no open flame, no molten drop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08G14/12C08G14/10C08G14/073C08L61/34
CPCC08G14/06C08G14/10C08G14/12C08J9/28C08J2201/0482C08J2205/026C08J2361/34
Inventor 胡立红李卓尚倩倩宋飞潘政薄采颖周永红
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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