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Preparation method of three-dimensional fiber-based aerogel material and product thereof

A fiber-based and aerogel technology, applied in chemical instruments and methods, colloid chemistry, colloid chemistry, etc., can solve the problems of narrow selection of raw materials, difficulty in reflecting the advantages of fiber structure and functional characteristics, and complex preparation processes, etc., to achieve Good flexibility and connectivity, good structural controllability, simple preparation process

Active Publication Date: 2015-05-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the above method, the fibers are added to the precursor of the inorganic sol as a filling material, and the prepared airgel is still a particle-type airgel in essence, and the fibers only exist as a reinforcing component in the material structure, so that the material is difficult to obtain. Demonstrates the advantages and functional properties of the fiber structure
In addition, the above methods all need to prepare the inorganic precursor sol first, which leads to the disadvantages of complex preparation process, long time-consuming, narrow range of raw material selection, etc.
Japanese patent P2006-75235A discloses a preparation method of a cellulose acetate fiber / polylactic acid composite airgel material, in which polylactic acid forms a composite nano-airgel with the fiber in the form of spraying, and the material structure is still a kind of polylactic acid The airgel material is formed by the aggregation of tiny lactic acid particles, and the spraying method is difficult to realize the uniform composite of polylactic acid particles and fibers, and the pore structure of the material is difficult to control
Foreign literature [Highly conductive and stretchable conductors fabricated from bacterial cellulose.[J].NPG Asia Materials2012,4,e19] reported a method of directly drying bacterial cellulose to prepare fiber-based airgel materials, but this method can only It is suitable for bacterial cellulose raw materials, which are difficult to break through the structure of bacterial cellulose raw materials in terms of material size, and because bacterial cellulose fibers have extremely strong hydrophilicity and hydrogen bonding, they have poor mechanical strength, no resilience, and moisture absorption. Defects such as post-deformation
Therefore, the methods disclosed in the above-mentioned patents are difficult to realize the controllable preparation of full-fiber structural airgel materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of a three-dimensional fiber-based airgel material, the specific steps are:

[0034] The first step: dispersing cotton fibers with an average diameter of 10 μm and an aspect ratio of 5000 in water to form a homogeneous suspension; in the suspension, the mass fraction of fibers is 0.01%;

[0035] Step 2: aging the suspension at 20°C for 13 hours to make the suspension form a coagulated block;

[0036] The third step: using supercritical drying method to remove the solidified water in the solidified block to form uncrosslinked fiber-based airgel;

[0037] Step 4: subject the uncrosslinked fiber-based airgel to thermal crosslinking treatment for 2 hours to obtain a three-dimensional fiber-based airgel material bonded and fixed at interlaced points of fibers, and the volume density of the three-dimensional fiber-based airgel material is 0.1mg / cm 3 , the average pore diameter of the three-dimensional fiber-based airgel material is 2000 μm, and the spec...

Embodiment 2

[0039] A preparation method of a three-dimensional fiber-based airgel material, the specific steps are:

[0040] The first step: dispersing viscose fibers with an average diameter of 20 μm and an aspect ratio of 40,000 and silk fibroin fibers with an average diameter of 10 μm and an aspect ratio of 40,000 in ethanol to form a homogeneous suspension; In the turbid liquid, the mass fraction of fiber is 0.1%;

[0041] The second step: freeze the suspension at -196°C for 14 minutes to make the suspension form a coagulated block;

[0042] Step 3: Freeze-drying is used to remove the solidified ethanol in the solidified block to form an uncrosslinked fiber-based airgel;

[0043] The fourth step: subject the uncrosslinked fiber-based airgel to ultrasonic crosslinking treatment for 30 minutes to obtain a three-dimensional fiber-based airgel material bonded and fixed at interlaced points of fibers, and the volume density of the three-dimensional fiber-based airgel material is 1mg / cm ...

Embodiment 3

[0045] A preparation method of a three-dimensional fiber-based airgel material, the specific steps are:

[0046] Step 1: Disperse silk fibers with an average diameter of 10 μm and an aspect ratio of 30,000, cupro fibers with an average diameter of 20 μm and an aspect ratio of 20,000 in water, and glass fibers with an average diameter of 10 μm and an aspect ratio of 30,000 Dispersed in propanol, then the two are mixed to form a homogeneous suspension; in the suspension, the mass fraction of fiber is 5%;

[0047] Step 2: Freeze the suspension at -196°C for 10 minutes to make the suspension form a coagulated block;

[0048] The third step: vacuum drying is used to remove the solidified water and propanol in the solidified block to form an uncrosslinked fiber-based airgel;

[0049] Step 4: subject the uncrosslinked fiber-based airgel to cross-linking treatment by microwave irradiation for 2 hours to obtain a three-dimensional fiber-based airgel material bonded and fixed at interl...

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PUM

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Abstract

The invention relates to a preparation method of a three-dimensional fiber-based aerogel material and a product thereof. The preparation method comprises the following steps of: firstly dispersing fibers in solvents which do not have fiber solubility to form turbid liquid; secondly curing the turbid liquid to form cured pieces; thirdly removing cured solvents in the cured pieces to form non-crosslinked fiber-based aerogel; and finally carrying out crosslinking stabilization treatment on the non-crosslinked fiber-based aerogel to obtain the fiber crossing point bonded and fixed three-dimensional fiber-based aerogel material. The product is a three-dimensional network-shaped material formed through mutual penetration and stagger of fibers. The fiber crossing points are effectively interconnected through non-hydrogen-bond bonding. The three-dimensional fiber-based aerogel material has volume density of 0.1-500mg / cm<3>, average pore size of 0.01-2000mu m and specific surface area of 0.2-2000m<2> / g. The preparation method and the product have the advantages that the preparation process is simple; the raw material limitations are less; and the aerogel product has good flexibility and connectivity and has broad application prospects in numerous fields.

Description

technical field [0001] The invention relates to a preparation method of a three-dimensional fiber-based airgel material and its products, in particular to a three-dimensional fiber-based airgel material obtained from a one-dimensional fiber through a three-dimensional network reconstruction method and a preparation method thereof. Background technique [0002] Airgel is a highly dispersed solid material formed by replacing the liquid in the gel with gas, and it is one of the solid materials with the lowest density known so far. Airgel can be divided into inorganic aerogel, organic aerogel and inorganic / organic composite aerogel according to different components. The preparation method is mainly through the combination of sol-gel technology and supercritical drying technology to obtain the colloid Or a three-dimensional porous network material constructed by the mutual aggregation of tiny polymer particles. Airgel materials have the advantages of high porosity, large specifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/00
Inventor 丁彬斯阳葛建龙唐晓敏黄美玲朱婕俞建勇
Owner DONGHUA UNIV
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