Anisotropic lamellar inorganic fiber aerogel materials and preparation method thereof

Patent metadata

Field	Value
Publication number	US-11857937-B2
Application number	US-202016980376-A
Country	US
Kind code	B2
Filing date	Apr 21, 2020
Priority date	May 7, 2019
Publication date	Jan 2, 2024
Grant date	Jan 2, 2024

Abstract

The present disclosure provides an anisotropic lamellar inorganic fiber aerogel material and a preparation method thereof. The method includes: mixing a polymer solution, an inorganic precursor and a chloride to obtain a spinning precursor solution; blow spinning the spinning precursor solution to obtain a composite fiber aerogel; calcinating the composite fiber aerogel to obtain the anisotropic lamellar inorganic fiber aerogel material. Therefore, the method has advantages of simplicity, easy operation, low cost, high efficiency and easy industrialized production. The inorganic fiber aerogel materials prepared by the above method are composed of multi-layer stacked fibers and have an anisotropic lamellar structure, which can be cut into any desired shape, and stacked to any desired thickness. In addition, the inorganic fiber aerogel materials have good flexibility and compressibility, excellent fire resistance, good high and low temperature resistance and superior thermal insulation, which greatly expands their application field.

First claim

What is claimed is:

1. A method for preparing an anisotropic lamellar inorganic fiber aerogel material, comprising:
mixing a polymer solution, an inorganic precursor and a chloride to obtain a spinning precursor solution;
blow spinning the spinning precursor solution to obtain a composite fiber aerogel; and
calcinating the composite fiber aerogel to obtain the anisotropic lamellar inorganic fiber aerogel material.

2. The method according to claim 1 , wherein the polymer solution comprises polymer material and a solvent, wherein a mass ratio of the polymer material to the solvent is in a range of 2:100 to 30:100.

3. The method according to claim 2 , wherein the mass ratio of the polymer material to the solvent is in a range of 4:100 to 20:100.

4. The method according to claim 1 , wherein the spinning precursor solution further comprises a catalyst.

5. The method according to claim 4 , wherein the spinning precursor solution comprises:
2 to 30 parts by weight of the polymer material;
100 parts by weight of the solvent;
0.5 to 100 parts by weight of the inorganic precursor;
0.001 to 1 part by weight of the catalyst; and
1 to 100 parts by weight of the chloride.

6. The method according to claim 4 , wherein the polymer material is selected from at least one of polyvinyl alcohol, polyethylene glycol, polyurethane, polyacrylic acid, polyvinyl pyrrolidone, cellulose acetate, methyl cellulose, carboxymethyl cellulose, polyvinylidene fluoride, polymethyl methacrylate, polyacrylamide, polyethylene oxide, polylactic acid, polyamide, polycaprolactone, polyvinyl butyral, polyaniline, polyimide and polycarbonate;
optionally, the solvent is selected from at least one of water, formic acid, tetrahydrofuran, acetone, butanone, n-hexane, cyclohexane, n-heptane, acetonitrile, N-methylpyrrolidone, 1,2-propanediol, chloroform, dichloromethane, 1,2-dichloroethane, methanol, ethanol, isopropanol, tert-butanol, n-butanol, toluene, xylene, ethylenediamine, dimethyl sulfoxide, N,N-dimethylformamide, N,N-dimethylacetamide and carbon tetrachloride;
optionally, the inorganic precursor is selected from at least one of zirconium oxychloride, zirconium acetate, aluminum isopropoxide, zirconium n-propoxide, tetraethyl orthosilicate, and tetramethyl orthosilicate;
optionally, the catalyst is selected from at least one of phosphoric acid, sulphuric acid, hydrochloric acid, nitric acid, formic acid, acetic acid, hydrofluoric acid, perchloric acid, trifluoroacetic acid, citric acid, oxalic acid and maleic acid.

7. The method according to claim 4 , wherein the chloride is selected from at least one of lithium chloride, sodium chloride, potassium chloride, rubidium chloride, cesium chloride, beryllium chloride, magnesium chloride, calcium chloride, strontium chloride, barium chloride, radium chloride, zinc chloride, copper chloride, nickel chloride, cobalt chloride, iron chloride, ferrous chloride, manganese chloride, chromic chloride, vanadium chloride, titanium tetrachloride, scandium chloride, aluminum chloride, gallium chloride, indium chloride, thallium chloride, tin chloride, lead chloride, cadmium chloride, palladium chloride, rhodium chloride, ruthenium chloride, zirconium chloride, hafnium chloride, osmium trichloride, platinum chloride, gold chloride and mercuric chloride.

8. The method according to claim 4 , wherein compressed air is used to blow the spinning precursor solution from a spinneret of a blow spinning device, and in blow spinning, an extrusion speed of the spinning precursor solution is in a range of 0.1 to 15 mL/h, a distance between the spinneret and a receiver is in a range of 20 to 100 cm, and a flow rate of the compressed air is in a range of 1 to 50 m/s.

9. The method according to claim 8 , wherein in blow spinning, the extrusion speed of the spinning precursor solution is in a range of 1 to 5 mL/h, the distance between the spinneret and the receiver is in a range of 30 to 60 cm, and the flow rate of the compressed air is in a range of 3 to 5 m/s.

10. The method according to claim 4 , wherein a calcination temperature is in a range of 500° C. to 2000° C. at a heating rate of 0.1 to 10° C./min, maintained for a time period of 0 to 24 h, and cooled down to room temperature.

11. The method according to claim 10 , wherein the calcination temperature is in a range of 800° C. to 1100° C. at a heating rate of 5° C./min, maintained for a time period of 1 to 5 h, and cooled down to room temperature.

12. The method according to claim 1 , wherein the chloride is selected from at least one of lithium chloride, sodium chloride, potassium chloride, rubidium chloride, cesium chloride, beryllium chloride, magnesium chloride, calcium chloride, strontium chloride, barium chloride, radium chloride, zinc chloride, copper chloride, nickel chloride, cobalt chloride, iron chloride, ferrous chloride, manganese chloride, chromic chloride, vanadium chloride, titanium tetrachloride, scandium chloride, aluminum chloride, gallium chloride, indium chloride, thallium chloride, tin chloride, lead chloride, cadmium chloride, palladium chloride, rhodium chloride, ruthenium chloride, zirconium chloride, hafnium chloride, osmium trichloride, platinum chloride, gold chloride and mercuric chloride.

13. The method according to claim 1 , wherein compressed air is used to blow the spinning precursor solution from a spinneret of a blow spinning device, and in blow spinning, an extrusion speed of the spinning precursor solution is in a range of 0.1 to 15 mL/h, a distance between the spinneret and a receiver is in a range of 20 to 100 cm, and a flow rate of the compressed air is in a range of 1 to 50 m/s.

14. The method according to claim 13 , wherein in blow spinning, the extrusion speed of the spinning precursor solution is in a range of 1 to 5 mL/h, the distance between the spinneret and the receiver is in a range of 30 to 60 cm, and the flow rate of the compressed air is in a range of 3 to 5 m/s.

15. The method according to claim 1 , wherein a calcination temperature is in a range of 500° C. to 2000° C. at a heating rate of 0.1 to 10° C./min, maintained for a time period of 0 to 24 h, and cooled down to room temperature.

16. The method according to claim 15 , wherein the calcination temperature is in a range of 800° C. to 1100° C. at a heating rate of 5° C./min, maintained for a time period of 1 to 5 h, and cooled down to room temperature.

Assignees

• Univ Tsinghua

Inventors

• Wu Hui
• Jia Chao

Classifications

• B01J13/0091 Primary

  Preparation of aerogels, e.g. xerogels · CPC title

• C01B33/20

  Silicates (persilicates C01B15/14 {; containing aluminium C01B33/26}) · CPC title

• C01B33/26 Primary

  Aluminium-containing silicates {, i.e. silico-aluminates} · CPC title

• C01G25/006

  Compounds containing zirconium, with or without oxygen or hydrogen, and containing two or more other elements · CPC title

• C01G49/0018

  Mixed oxides or hydroxides, (C01G49/0009 takes precedence) · CPC title