A kind of preparation method of toughness sio2 airgel fiber with post-treatment of isocyanate

Abstract

The invention relates to a preparation method of tough SiO2 aerogel fibers post-processed through isocyanate. The preparation method comprises steps as follows: a spinning solution is prepared from silicate or silanol sol; an acid solution is used for a coagulating bath; the spinning solution is added to the coagulating bath, the mixture has a reaction, wet spinning is performed, orthosiliconic acid / silicate fibers are obtained, wound, aged, washed, soaked in a tetrahydrofuran solution of isocyanate for 48 h, then taken out and washed with acetone, solvent replacement is performed through water or ethanol, and the tough SiO2 aerogel fibers are obtained after drying. The method has the characteristics that the raw materials are cheap and easy to obtain, the reaction process is simple, and the spinnability is good; the SiO2 aerogel fibers are toughened through high polymers, the prepared tough SiO2 aerogel fibers have rich pores, a high specific surface area and certain toughness and is high-temperature-resistant and chemical-corrosion resistant, and the specific surface area of the fibers is adjustable.

Description

technical field

[0001] The invention belongs to the field of preparation of airgel fibers, in particular to a tough SiO with isocyanate post-treatment 2 Preparation method of 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 ...

Examples

Embodiment 1

[0032] Sodium water glass with a modulus of 2 and 50 Baume degrees was used as the spinning stock solution, and 0.8 mol / L dilute sulfuric acid solution was used as the coagulation bath to carry out reactive wet spinning. The orthosilicic acid / silicate fiber formed in the coagulation bath was wound at a winding speed of 0.1 m / s. The wound fiber was immersed in 0.005mol / L dilute sulfuric acid for 10 days for aging, so as to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fibers are transformed, and a large number of holes are formed at the same time. After aging, wash 3 times with acetone. After washing, place the fiber in a tetrahydrofuran solution of toluene diisocyanate for 48 hours. Toluene diisocyanate and SiO 2 The hydroxyl group on the skeleton reacts. After the reaction is completed, wash with acetone, replace the solution in the fiber with deionized water, and freeze-dry to obtain tough SiO 2 Airgel fibers. The spinning process is very s...

Embodiment 2

[0034] Potassium water glass with a modulus of 3 and 35 degrees Baume was used as the spinning stock solution, and 0.2mol / L dilute sulfuric acid solution was used as the coagulation bath to carry out reactive wet spinning. The orthosilicic acid / sodium silicate fiber formed in the coagulation bath was wound at a winding speed of 0.5 m / s. The wound fiber was immersed in 0.005mol / L dilute sulfuric acid for 10 days for aging, so as to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fibers are transformed, and a large number of holes are formed at the same time. After aging, wash 5 times with acetone. After washing, place the fiber in a tetrahydrofuran solution of toluene diisocyanate for 48 hours. Toluene diisocyanate and SiO 2 The hydroxyl group on the skeleton reacts. After the reaction is completed, wash with acetone, replace the solution in the fiber with deionized water, and freeze-dry to obtain SiO 2 Airgel fibers. Occasionally, there is a ph...

Embodiment 3

[0036] Potassium water glass with a modulus of 3 and 35 degrees Baume was used as the spinning stock solution, and 0.8 mol / L dilute sulfuric acid solution was used as the coagulation bath to carry out reactive wet spinning. The orthosilicic acid / potassium silicate fiber formed in the coagulation bath was wound at a winding speed of 1 m / s. The wound fiber was immersed in 0.1mol / L dilute sulfuric acid for 5 days for aging, and the transformation from orthosilicic acid / silicate fiber to SiO 2 The fibers are transformed, and a large number of holes are formed at the same time. After aging, wash 3 times with acetone. After washing, place the fiber in a tetrahydrofuran solution of toluene diisocyanate for 48 hours. Toluene diisocyanate and SiO 2 The hydroxyl group on the skeleton reacts. After the reaction is completed, wash with acetone, replace the solution in the fiber with deionized water, and freeze-dry to obtain SiO 2 Airgel fibers. Occasionally, there is a phenomenon of br...

technical field

[0001] The invention belongs to the field of preparation of airgel fibers, in particular to a tough SiO with isocyanate post-treatment 2 Preparation method of 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 ...

Examples

Embodiment 1

[0032] Sodium water glass with a modulus of 2 and 50 Baume degrees was used as the spinning stock solution, and 0.8 mol / L dilute sulfuric acid solution was used as the coagulation bath to carry out reactive wet spinning. The orthosilicic acid / silicate fiber formed in the coagulation bath was wound at a winding speed of 0.1 m / s. The wound fiber was immersed in 0.005mol / L dilute sulfuric acid for 10 days for aging, so as to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fibers are transformed, and a large number of holes are formed at the same time. After aging, wash 3 times with acetone. After washing, place the fiber in a tetrahydrofuran solution of toluene diisocyanate for 48 hours. Toluene diisocyanate and SiO 2 The hydroxyl group on the skeleton reacts. After the reaction is completed, wash with acetone, replace the solution in the fiber with deionized water, and freeze-dry to obtain tough SiO 2 Airgel fibers. The spinning process is very s...

Embodiment 2

[0034] Potassium water glass with a modulus of 3 and 35 degrees Baume was used as the spinning stock solution, and 0.2mol / L dilute sulfuric acid solution was used as the coagulation bath to carry out reactive wet spinning. The orthosilicic acid / sodium silicate fiber formed in the coagulation bath was wound at a winding speed of 0.5 m / s. The wound fiber was immersed in 0.005mol / L dilute sulfuric acid for 10 days for aging, so as to realize the transformation from orthosilicic acid / silicate fiber to SiO 2 The fibers are transformed, and a large number of holes are formed at the same time. After aging, wash 5 times with acetone. After washing, place the fiber in a tetrahydrofuran solution of toluene diisocyanate for 48 hours. Toluene diisocyanate and SiO 2 The hydroxyl group on the skeleton reacts. After the reaction is completed, wash with acetone, replace the solution in the fiber with deionized water, and freeze-dry to obtain SiO 2 Airgel fibers. Occasionally, there is a ph...

Embodiment 3

[0036] Potassium water glass with a modulus of 3 and 35 degrees Baume was used as the spinning stock solution, and 0.8 mol / L dilute sulfuric acid solution was used as the coagulation bath to carry out reactive wet spinning. The orthosilicic acid / potassium silicate fiber formed in the coagulation bath was wound at a winding speed of 1 m / s. The wound fiber was immersed in 0.1mol / L dilute sulfuric acid for 5 days for aging, and the transformation from orthosilicic acid / silicate fiber to SiO 2 The fibers are transformed, and a large number of holes are formed at the same time. After aging, wash 3 times with acetone. After washing, place the fiber in a tetrahydrofuran solution of toluene diisocyanate for 48 hours. Toluene diisocyanate and SiO 2 The hydroxyl group on the skeleton reacts. After the reaction is completed, wash with acetone, replace the solution in the fiber with deionized water, and freeze-dry to obtain SiO 2 Airgel fibers. Occasionally, there is a phenomenon of br...

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