Polybenzoxazine aerogel and preparation method thereof

A technology of polybenzoxazine and benzoxazine, which is applied in the field of polybenzoxazine airgel and its preparation, can solve the problem of high cost, low shrinkage of polybenzoxazine and the influence of polybenzoxazine Airgel application and other problems, to achieve the effect of suppressing collapse, solving the problem of large linear shrinkage and low price

Pending Publication Date: 2022-02-08
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, the linear shrinkage rate of polybenzoxazine airgel prepared by the prior art is as high as 22%, and the cost of some methods is relatively high, which does not reflect the advantages of low shrinkage rate of polybenzoxazine, which seriously affects the polybenzoxazine airgel. Application of oxazine airgel

Method used

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  • Polybenzoxazine aerogel and preparation method thereof
  • Polybenzoxazine aerogel and preparation method thereof
  • Polybenzoxazine aerogel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] This embodiment adopts the preparation method proposed by the present invention to prepare polybenzoxazine airgel, such as figure 1 As shown, the steps are as follows:

[0032] 1) 10g BO-1 was dissolved in 30g ethyl acetate to obtain a benzoxazine monomer solution.

[0033] 2) Add 0.5 g of triethylenetetramine cross-linking agent to the benzoxazine monomer solution, stir at 25°C for 5 minutes, pour into a mold, and age at 120°C for 8 hours to obtain polybenzoxazine wet gel.

[0034] 3) Cool the obtained polybenzoxazine wet gel at room temperature for 24 hours, and keep it warm at 100° C. for 12 hours to obtain polybenzoxazine airgel with a low degree of reaction.

[0035] 4) Heat the polybenzoxazine airgel with a low degree of reaction to 200°C stepwise in the air (step heating program: 140°C for 2h; 160°C for 2h; 180°C for 2h; 200°C for 2h) , to obtain polybenzoxazine airgel.

[0036] The test result data of the polybenzoxazine airgel obtained in this embodiment ar...

Embodiment 2

[0038] In this embodiment, the preparation method proposed by the present invention is used to prepare polybenzoxazine airgel, and the steps are as follows:

[0039] 1) Dissolve 10g BO-2 in 30g toluene to obtain a benzoxazine monomer solution.

[0040] 2) Add 0.2 g of triethylamine cross-linking agent to the benzoxazine monomer solution, stir at 25°C for 5 minutes, pour into a mold, and age at 100°C for 96 hours to obtain polybenzoxazine wet gel .

[0041]3) The obtained polybenzoxazine wet gel was cooled at room temperature for 72 hours, and kept at 120° C. for 24 hours to obtain polybenzoxazine airgel with a low degree of reaction.

[0042] 4) Heat the polybenzoxazine airgel with a low degree of reaction to 200°C stepwise in the air (step heating program: 140°C for 12h; 160°C for 12h; 180°C for 12h; 200°C for 12h) , to obtain polybenzoxazine airgel.

[0043] The test result data of the polybenzoxazine airgel obtained in this embodiment are listed in Table 1.

Embodiment 3

[0045] In this embodiment, the preparation method proposed by the present invention is used to prepare polybenzoxazine airgel, and the steps are as follows:

[0046] 1) Dissolve 10g BO-3 in 30g toluene and xylene to obtain a benzoxazine monomer solution.

[0047] 2) Add 0.8 g of ethylenediamine cross-linking agent to the benzoxazine monomer solution, stir at 25°C for 5 minutes, pour into a mold, and age at 110°C for 48 hours to obtain polybenzoxazine wet gel .

[0048] 3) The obtained polybenzoxazine wet gel was cooled at room temperature for 48 hours, and then kept at 110° C. for 18 hours to obtain polybenzoxazine airgel with a low degree of reaction.

[0049] 4) Heat the polybenzoxazine airgel with a low degree of reaction to 200°C stepwise in the air (the stepwise heating program is: 140°C for 8 hours; 160°C for 8 hours; 180°C for 8 hours; 200°C for 8 hours) , to obtain polybenzoxazine airgel.

[0050] The test result data of the polybenzoxazine airgel obtained in this e...

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Abstract

The invention discloses polybenzoxazine aerogel and a preparation method thereof, and belongs to the technical field of aerogel materials. The preparation method comprises the steps of: dissolving a benzoxazine monomer in an organic solvent to obtain a benzoxazine monomer solution; adding an aliphatic polyamine cross-linking agent, mixing well, pouring the solution into a mold, heating for a gelation reaction, and aging to obtain polybenzoxazine wet gel; then carrying out normal pressure drying to obtain polybenzoxazine aerogel with a low reaction degree; and heating to 200 DEG C in air in a stepped manner, preserving heat for 2-12 hours at each temperature section, and cooling to room temperature to obtain polybenzoxazine aerogel. The linear shrinkage rate of the aerogel can be reduced, and the aerogel is good in thermal stability and easy to form.

Description

technical field [0001] The invention relates to a polybenzoxazine airgel and a preparation method thereof, belonging to the technical field of airgel materials. Background technique [0002] Polybenzoxazine resin is a new type of phenolic resin. Benzoxazine is the basic unit structure of polybenzoxazine resin polymerization. The full name is 3,4-dihydro-1,3-benzoxazine. A benzoheterocyclic six-membered ring containing oxygen and nitrogen atoms. Benzoxazine monomers can be ring-opened and polymerized at high temperature or under the action of catalysis to form a body-shaped cross-linked network structure. Polybenzoxazine resin has flexible molecular structure design. Compared with traditional phenolic resin, it has better thermal stability and mechanical properties. It also has the characteristics of easy molding, low moisture absorption and zero shrinkage after curing. The preparation of airgel materials is expected to solve the problems of large linear shrinkage (>14%)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/34C08J9/28C08G14/073
CPCC08J9/28C08G14/06C08J2361/34C08J2201/0502C08J2205/026
Inventor 刘韬刘圆圆高宇智郭慧王孟李文静赵英民张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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