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Normal-pressure drying preparation method of low-density high-strength phenolic resin aerogel with extremely low shrinkage rate

A phenolic resin, atmospheric drying technology, applied in the field of low-density and high-strength phenolic resin aerogel drying under atmospheric pressure, can solve problems such as shrinkage and cracking, and achieve the effect of large porosity and low density

Active Publication Date: 2021-06-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention aims at the problem that the phenolic resin aerogel prepared from thermoplastic phenolic resin and hexamethylenetetramine will shrink and crack obviously during the normal pressure drying process

Method used

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  • Normal-pressure drying preparation method of low-density high-strength phenolic resin aerogel with extremely low shrinkage rate
  • Normal-pressure drying preparation method of low-density high-strength phenolic resin aerogel with extremely low shrinkage rate
  • Normal-pressure drying preparation method of low-density high-strength phenolic resin aerogel with extremely low shrinkage rate

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0034] In this example, two kinds of phenolic resin aerogels with thermosetting phenolic resin and without thermosetting phenolic resin were prepared respectively. The specific implementation is as follows:

[0035] (1) Add 1.5g of powdered thermoplastic phenolic resin and 0.214g of powdered thermosetting phenolic resin into 10ml of ethylene glycol solution as the first group (containing thermosetting phenolic resin), and add 1.714g of powdered thermoplastic phenolic resin , added to 10ml of ethylene glycol solution as the second group (without thermosetting phenolic resin, and the total content of phenolic resin resin in the two groups of solutions should be the same), put the two groups of phenolic resin solutions on a heating platform at 150°C and heat for 30min After cooling, 0.214 g of hexamethylenetetramine was added to the two groups of solutions, and dissolved by ultrasonic vibration for 3 hours to obtain the precursor solution;

[0036] (2) Pour the prepared precurso...

Embodiment 2

[0041] This implementation case tests and compares the compressive properties of several phenolic resin airgels with different contents of thermosetting phenolic resin or hexamethylenetetramine (such as Figure 5 shown), the stronger the compressive capacity of the phenolic resin airgel, the stronger the ability to resist drying shrinkage under normal pressure, and the compressive stress-strain curve can further prove that the added thermosetting phenolic resin can enhance the airgel skeleton strength The way to resist the shrinking capillary force generated during the drying process. The specific implementation is as follows:

[0042] (1) Weigh 5 groups of thermoplastic phenolic resins with a mass of 1.5g respectively, add 0.428g of thermosetting phenolic resin to the first 3 groups, and add 0.214g of thermosetting phenolic resin to the remaining group (that is, group 4). For phenolic resin, add 0.642g of thermosetting phenolic resin to the last remaining group (namely Group...

Embodiment approach

[0049] In this example, a precursor solution (containing thermosetting phenolic resin) with a lower concentration of phenolic resin was used to prepare a low-density, high-strength phenolic resin aerogel with extremely low shrinkage ( Image 6 ), the specific implementation is as follows:

[0050] (1) Add 1.166g of powdered thermoplastic phenolic resin and 0.334g of powdered thermosetting phenolic resin to 10ml of ethylene glycol, and place it on a heating platform at 150°C for 30 minutes, and add 0.2332g of it after cooling Hexamethylenetetramine, and assisted dissolution by ultrasonic vibration for 2h, to obtain the precursor solution;

[0051] (2) Pour the prepared precursor solution into an airtight container, incubate in a heating box at 120°C for 1 hour, and incubate at 150°C for 3 hours to obtain a phenolic resin wet gel;

[0052] (3) Take out the cross-linked phenolic resin wet gel and soak it in 50ml of absolute ethanol, and place it on a heating platform at 150°C for ...

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Abstract

The invention belongs to the technical field of aerogel preparation, and particularly relates to a normal-pressure drying preparation method of low-density high-strength phenolic resin aerogel with an extremely low shrinkage rate. The invention aims to solve the problems that phenolic resin aerogel prepared by taking thermoplastic phenolic resin as a raw material is obviously shrunk and cracked in a normal-pressure drying process and the drying time is too long. A certain proportion of thermosetting phenolic resin is added into a thermoplastic phenolic resin solution to serve as an aerogel reinforcing agent, hexamethylene tetramine serves as a cross-linking agent, and the low-density and high-strength phenolic resin aerogel which is almost free of shrinkage can be prepared under the normal-pressure drying condition. The method has the advantages that the problems that phenolic resin wet gel is obviously shrunk and cracked in the normal-pressure drying process, and the time is too long are solved. The preparation method is simple in process, green, safe, low in cost and high in efficiency. The prepared phenolic resin aerogel does not generate observable deformation and shrinkage, and can realize near-net forming according to application requirements.

Description

technical field [0001] The invention belongs to the technical field of airgel preparation, and in particular relates to a method for preparing low-density and high-strength phenolic resin airgel under normal pressure and drying with extremely low shrinkage. Background technique [0002] As a three-dimensional porous solid material, airgel has extremely low density, high porosity and specific surface area, so it has excellent thermal insulation, sound insulation, adsorption, catalysis and other properties. It has a wide range of applications in electricity. Phenolic resin is a low-flammability material with excellent temperature resistance, and has the advantages of low smoke rate and low toxicity in high-temperature environments. Phenolic resin aerogels can be used in fire-resistant, sound-insulating and heat-insulating layers of buildings and ablation and heat-insulating layers of spaceship return cabins. In addition, due to the high carbon residue rate of phenolic resin ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08L61/06C08K5/3477
CPCC08J9/28C08J2205/026C08J2361/06C08J2461/06C08K5/3477
Inventor 沙建军沙如意苏成代吉祥祖宇飞
Owner DALIAN UNIV OF TECH
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