A method for post-loading nanometals to prepare continuous SIO2/nanometal airgel fibers with catalytic properties

Abstract

The invention relates to a method for preparing continuous SiO2 / nano-metal airgel fibers with catalytic properties by loading nano-metal. The method includes: preparing silicate or silanol sol into a spinning stock solution; adding an acidic solution to the coagulation tank as a coagulation bath; injecting the spinning stock solution into the coagulation bath and performing reaction wet spinning to obtain orthosilicic acid / silicon The acid salt fiber is rolled, then aged, washed with deionized water until neutral, and then immersed in the metal salt solution. After taking it out, take out the surface solvent, immersed in the reducing agent, washed with deionized water until neutral, and use deionized water to remove the fiber. Replace with ionized water or ethanol and dry. In the method of the present invention, the raw materials are cheap and easy to obtain, the reaction process is simple, and the spinnability is good. The obtained airgel fiber has abundant holes, high specific surface area, high temperature resistance, and chemical corrosion resistance. At the same time, the fiber specific surface area, nanometal loading capacity Adjustable.

Description

technical field

[0001] The invention belongs to the field of preparation of airgel fibers, in particular to a continuous SiO with catalytic performance prepared by post-loading nano metal 2 / Nanometal airgel fiber method. Background technique

[0002] In a chemical reaction, a substance that can change the chemical reaction rate of the reactants (both increase and decrease) without changing the chemical balance, and whose quality and chemical properties have not changed before and after the chemical reaction is called a catalyst. In actual production, catalysts tend to be more expensive. In order to reduce the amount of catalyst as much as possible and improve the efficiency of the catalyst, it is often necessary to enlarge its specific surface and make it into nanoparticles. In order to support the active components and make the catalyst have specific physical properties, the catalyst is often loaded on a porous material with open pores that can realize the internal trans...

Examples

Embodiment 1

[0031] 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, the fibers were washed with deionized water until neutral. SiO will be obtained 2 The porous fibers were immersed in 0.01mol / L AgNO 3 In the solution for 10min, take it out, remove the surface solvent, and immerse in 0.05mol / L NaBH 4 Solution (need to use NaOH to adjust the pH to 12) for 10min, remove the surface solvent, repeat AgNO 3 The solution and the reducing agent solution are i...

Embodiment 2

[0033] Potassium water glass with a modulus of 3 and 35 Baume degrees is used as the spinning stock solution, and 0.2mol / L dilute sulfuric acid solution is 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, the fibers were washed with deionized water until neutral. The obtained SiO2 porous fiber was immersed in 0.01mol / L CuSO 4 In the solution for 10 minutes, take it out, remove the surface solvent, and immerse in 0.1mol / L ascorbic acid solution (need to use H 2 SO 4 Adjust the pH to 3) for 10min, remove the surface solvent, repeat CuSO 4 The solution and the reducing agent solutio...

Embodiment 3

[0035] 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, the fibers were washed with deionized water until neutral. SiO will be obtained 2 The porous fibers were immersed in 0.01mol / L AgNO 3 In the solution for 10 minutes, take it out, remove the surface solvent, immerse in 0.05mol / L hydrazine hydrate solution (need to use NaOH to adjust the pH to 10) for 10 minutes, remove the surface solvent, repeat AgNO 3 The solution and the reducing agent sol...

technical field

[0001] The invention belongs to the field of preparation of airgel fibers, in particular to a continuous SiO with catalytic performance prepared by post-loading nano metal 2 / Nanometal airgel fiber method. Background technique

[0002] In a chemical reaction, a substance that can change the chemical reaction rate of the reactants (both increase and decrease) without changing the chemical balance, and whose quality and chemical properties have not changed before and after the chemical reaction is called a catalyst. In actual production, catalysts tend to be more expensive. In order to reduce the amount of catalyst as much as possible and improve the efficiency of the catalyst, it is often necessary to enlarge its specific surface and make it into nanoparticles. In order to support the active components and make the catalyst have specific physical properties, the catalyst is often loaded on a porous material with open pores that can realize the internal trans...

Examples

Embodiment 1

[0031] 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, the fibers were washed with deionized water until neutral. SiO will be obtained 2 The porous fibers were immersed in 0.01mol / L AgNO 3 In the solution for 10min, take it out, remove the surface solvent, and immerse in 0.05mol / L NaBH 4 Solution (need to use NaOH to adjust the pH to 12) for 10min, remove the surface solvent, repeat AgNO 3 The solution and the reducing agent solution are i...

Embodiment 2

[0033] Potassium water glass with a modulus of 3 and 35 Baume degrees is used as the spinning stock solution, and 0.2mol / L dilute sulfuric acid solution is 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, the fibers were washed with deionized water until neutral. The obtained SiO2 porous fiber was immersed in 0.01mol / L CuSO 4 In the solution for 10 minutes, take it out, remove the surface solvent, and immerse in 0.1mol / L ascorbic acid solution (need to use H 2 SO 4 Adjust the pH to 3) for 10min, remove the surface solvent, repeat CuSO 4 The solution and the reducing agent solutio...

Embodiment 3

[0035] 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, the fibers were washed with deionized water until neutral. SiO will be obtained 2 The porous fibers were immersed in 0.01mol / L AgNO 3 In the solution for 10 minutes, take it out, remove the surface solvent, immerse in 0.05mol / L hydrazine hydrate solution (need to use NaOH to adjust the pH to 10) for 10 minutes, remove the surface solvent, repeat AgNO 3 The solution and the reducing agent sol...