A kind of preparation method of sio2/cellulose tough aerogel fiber

Abstract

The invention relates to a preparing method for SiO2 / cellulose tough aerogel fibers. The preparing method comprises the steps that silicate or silanol sol is prepared into a spinning solution, a cellulose solution is added, then the mixture is injected into an H2SO4 / Na2SO4 solution for a reaction for wet method spinning, and orthosilicic acid / silicate / cellulose fibers are obtained; the fibers are wound and steeped into an H2SO4 / Na2SO4 solution for aging at the room temperature, the fibers are washed with deionized water to be neutral, solvent replacement is carried out, the fibers are dried, and the SiO2 / cellulose tough aerogel fibers are obtained. The method has the advantages that raw materials are cheap and easy to obtain, the reaction process is simple, and spinnability is good. The prepared continuous SiO2 / cellulose tough aerogel fibers contain abundant holes, have a high specific surface area and are resistant to high temperatures and chemical corrosion; meanwhile, the fibers are adjustable in specific surface area and have certain toughness, the application range of the aerogel fibers can be enlarged, and higher practical value is achieved.

Description

technical field

[0001] The invention belongs to the field of preparation of airgel fibers, in particular to a SiO 2 / The preparation method of cellulose tenacity airgel fiber. Background technique

[0002] Aerogel (aerogel) refers to the medium filled in the space network structure in the gel is not a solvent but a gas, a special gel with a solid appearance, because there is almost no solvent component inside, so it is also called xerogel . Airgel is a low-density nanoporous amorphous solid material with a unique structure. The solid phase forms a spatial network structure, and the network structure and the pore structure between the networks are at the nanoscale. Because of its unique structure, airgel also has many unique properties, such as high porosity, high specific surface area, strong adsorption, low density, low acoustic impedance, low thermal conductivity, low refraction, etc.

[0003] SiO 2 The high specific surface area of ​​airgel can provide a large number ...

Examples

Embodiment 1

[0033] Use composite solvent 9wt% NaOH / 5wt% thiourea / 5wt% urea to prepare microcrystalline cellulose solution as cellulose solvent, cellulose solution and modulus are 2, the sodium water glass of 50 degrees Baume is mixed, cellulose solution The volume ratio with sodium water glass is 1:9. The mixed solution is used as spinning dope, with H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.8mol / L, Na 2 SO 4 The concentration is 0.8mol / L) as a coagulation bath for reactive wet spinning. The orthosilicic acid / silicate / cellulose fibers formed in the coagulation bath were wound at a winding speed of 0.1 m / s. The wound fiber is immersed in H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.01mol / L, Na 2 SO 4 The concentration is 0.8mol / L) for 10 days for aging to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fiber is transformed, and the cellulose is further solidified at the same time, and ...

Embodiment 2

[0035] Use composite solvent 9wt% NaOH / 5wt% thiourea / 5wt% urea as cellulose solvent to prepare microcrystalline cellulose solution, cellulose solution is mixed with solution obtained by direct heating of sodium silicate nonahydrate, cellulose solution and silicic acid The volume ratio of sodium solution is 5:5. The mixed solution is used as spinning dope, with H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.8mol / L, Na 2 SO 4 The concentration is 0.8mol / L) as a coagulation bath for reactive wet spinning. The orthosilicic acid / silicate / cellulose fibers formed in the coagulation bath were wound at a winding speed of 2 m / s. The wound fiber is immersed in H 2 SO 4 / Na 2 SO 4 solution (concentration of sulfuric acid solution is 0.01mol / L, Na 2 SO 4 The concentration is 0.8mol / L) for 2 days for aging to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fiber is transformed, and the cellulose is further solidified at ...

Embodiment 3

[0037] Use composite solvent 9wt% NaOH / 5wt% thiourea / 5wt% urea to prepare microcrystalline cellulose solution as cellulose solvent, the cellulose solution is mixed with the potassium water glass that modulus is 23,35 Baume degree, cellulose solution The volume ratio to potassium water glass is 6:4. The mixed solution is used as spinning dope, with H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.8mol / L, Na 2 SO 4 The concentration is 0.8mol / L) as a coagulation bath for reactive wet spinning. The orthosilicic acid / silicate / cellulose fibers formed in the coagulation bath were wound at a winding speed of 0.5 m / s. The wound fiber is immersed in H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.01mol / L, Na 2 SO 4 The concentration is 0.8mol / L) for 10 days for aging to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fiber is transformed, and the cellulose is further solidified at the same t...

technical field

[0001] The invention belongs to the field of preparation of airgel fibers, in particular to a SiO 2 / The preparation method of cellulose tenacity airgel fiber. Background technique

[0002] Aerogel (aerogel) refers to the medium filled in the space network structure in the gel is not a solvent but a gas, a special gel with a solid appearance, because there is almost no solvent component inside, so it is also called xerogel . Airgel is a low-density nanoporous amorphous solid material with a unique structure. The solid phase forms a spatial network structure, and the network structure and the pore structure between the networks are at the nanoscale. Because of its unique structure, airgel also has many unique properties, such as high porosity, high specific surface area, strong adsorption, low density, low acoustic impedance, low thermal conductivity, low refraction, etc.

[0003] SiO 2 The high specific surface area of ​​airgel can provide a large number ...

Examples

Embodiment 1

[0033] Use composite solvent 9wt% NaOH / 5wt% thiourea / 5wt% urea to prepare microcrystalline cellulose solution as cellulose solvent, cellulose solution and modulus are 2, the sodium water glass of 50 degrees Baume is mixed, cellulose solution The volume ratio with sodium water glass is 1:9. The mixed solution is used as spinning dope, with H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.8mol / L, Na 2 SO 4 The concentration is 0.8mol / L) as a coagulation bath for reactive wet spinning. The orthosilicic acid / silicate / cellulose fibers formed in the coagulation bath were wound at a winding speed of 0.1 m / s. The wound fiber is immersed in H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.01mol / L, Na 2 SO 4 The concentration is 0.8mol / L) for 10 days for aging to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fiber is transformed, and the cellulose is further solidified at the same time, and ...

Embodiment 2

[0035] Use composite solvent 9wt% NaOH / 5wt% thiourea / 5wt% urea as cellulose solvent to prepare microcrystalline cellulose solution, cellulose solution is mixed with solution obtained by direct heating of sodium silicate nonahydrate, cellulose solution and silicic acid The volume ratio of sodium solution is 5:5. The mixed solution is used as spinning dope, with H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.8mol / L, Na 2 SO 4 The concentration is 0.8mol / L) as a coagulation bath for reactive wet spinning. The orthosilicic acid / silicate / cellulose fibers formed in the coagulation bath were wound at a winding speed of 2 m / s. The wound fiber is immersed in H 2 SO 4 / Na 2 SO 4 solution (concentration of sulfuric acid solution is 0.01mol / L, Na 2 SO 4 The concentration is 0.8mol / L) for 2 days for aging to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fiber is transformed, and the cellulose is further solidified at ...

Embodiment 3

[0037] Use composite solvent 9wt% NaOH / 5wt% thiourea / 5wt% urea to prepare microcrystalline cellulose solution as cellulose solvent, the cellulose solution is mixed with the potassium water glass that modulus is 23,35 Baume degree, cellulose solution The volume ratio to potassium water glass is 6:4. The mixed solution is used as spinning dope, with H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.8mol / L, Na 2 SO 4 The concentration is 0.8mol / L) as a coagulation bath for reactive wet spinning. The orthosilicic acid / silicate / cellulose fibers formed in the coagulation bath were wound at a winding speed of 0.5 m / s. The wound fiber is immersed in H 2 SO 4 / Na 2 SO 4 Solution (concentration of sulfuric acid solution is 0.01mol / L, Na 2 SO 4 The concentration is 0.8mol / L) for 10 days for aging to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fiber is transformed, and the cellulose is further solidified at the same t...

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