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Polysilazane-zirconium dioxide composite aerogel material as well as preparation method and application thereof

A technology of composite aerogel and polysilazane, which is applied in the production of bulk chemicals, etc., to achieve the effect of simple process, high porosity and low density

Inactive Publication Date: 2018-03-09
TIANJIN CHENGJIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports on the preparation of precursor polysilazane-zirconia composite aerogels using precursor polysilazane (PSN) polymer as silicon source

Method used

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  • Polysilazane-zirconium dioxide composite aerogel material as well as preparation method and application thereof
  • Polysilazane-zirconium dioxide composite aerogel material as well as preparation method and application thereof
  • Polysilazane-zirconium dioxide composite aerogel material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step (1) Disperse 0.40g polysilazane (PSN) precursor containing vinyl side chains and Si-H bonds with a number average molecular weight of 1000 in 0.40g toluene, and add 0.05g tetrabutyl zirconate (TBT ) and 0.50g divinylbenzene (DVB), stir rapidly, and then transfer the prepared mixed dilute solution to the polytetrafluoroethylene lining of the hydrothermal reaction kettle, and seal it; the reaction kettle filled with the mixed solution is placed React in a drying oven at 180°C for 3 hours. After cooling to room temperature, a wet gel is obtained. Add toluene into the beaker containing the wet gel to submerge the wet gel test piece, and let it stand for 24 hours before use.

[0033] Step (2) Transfer the product in step (1) to a carbon dioxide supercritical extraction device, immerse in liquid carbon dioxide for about 1 hour, and then perform supercritical drying at a drying temperature and pressure of 45° C. and 8 MPa, respectively, for 6 hours.

[0034] The specific ...

Embodiment 2

[0036] Step (1) disperse 0.40g polysilazane (PSN) precursor containing vinyl side chains and Si-H bonds with a number average molecular weight of 1000 in 0.40g toluene, and add 0.10g tetrabutyl zirconate (TBT ) and 0.60g divinylbenzene (DVB), stir rapidly, and then transfer the prepared mixed dilute solution to the polytetrafluoroethylene lining of the hydrothermal reaction kettle, and seal it; the reaction kettle filled with the mixed solution is placed React in a drying oven at 160°C for 6 hours. After cooling to room temperature, a wet gel is obtained. Add toluene into the beaker containing the wet gel to submerge the wet gel test piece, and let it stand for 36 hours before use.

[0037] Step (2) The product in step (1) was transferred to a carbon dioxide supercritical extraction device, immersed in liquid carbon dioxide for about 0.5h, and then supercritically dried at a drying temperature and pressure of 40°C and 9MPa for 7h.

[0038] The specific surface area, porosity a...

Embodiment 3

[0040] Step (1) disperse 0.40g polysilazane (PSN) precursor containing vinyl side chain and Si-H bond with number average molecular weight 1000 in 0.40g toluene, add 0.20g tetrabutyl zirconate (TBT ) and 0.80g divinylbenzene (DVB), stir rapidly, then transfer the prepared mixed dilute solution to the polytetrafluoroethylene lining of the hydrothermal reaction kettle, and seal it; the reaction kettle filled with the mixed solution is placed React in a drying oven at 200°C for 1 hour, and cool to room temperature to obtain a wet gel. Add toluene into the beaker containing the wet gel to submerge the wet gel test piece, and let it stand for 32 hours before use.

[0041] Step (2) Transfer the product in step (1) to a carbon dioxide supercritical extraction device, immerse in liquid carbon dioxide for about 2 hours, and then carry out supercritical drying at a drying temperature and pressure of 50° C. and 7 MPa for 8 hours.

[0042] The specific surface area, porosity and density o...

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Abstract

The invention discloses a polysilazane-zirconium dioxide composite aerogel material as well as a preparation method and application thereof. The preparation method comprises the following steps: dispersing a polysilazane precursor in methylbenzene, successively adding zirconium n-butoxide and divinyl benzene, rapidly and uniformly stirring, obtaining a mixed dilute solution, transferring the mixeddilute solution into a hydrothermal reaction kettle, sealing the hydrothermal reaction kettle, placing the reaction kettle with the mixed dilute solution in a drying box, performing the reaction, cooling to room temperature to obtain wet gel, and standing the wet gel in a beaker with the methylbenzene; and transferring a product of the step 1 into a carbon dioxide supercritical extraction apparatus, soaking in liquid carbon dioxide, supercritically drying, and obtaining the polysilazane-zirconium dioxide composite aerogel material. The polysilazane-zirconium dioxide composite aerogel materialis a novel nano porous composite material, has high porosity, high specific surface area and low density; and the preparation condition is mild, and the process is simple and controllable.

Description

technical field [0001] The invention relates to a precursor polysilazane-zirconia composite airgel material and a preparation method thereof, belonging to the field of preparation technology of nanoporous materials. Background technique [0002] Airgel is a kind of solid nanoporous material with a three-dimensional network structure composed of nanoparticles or polymer molecules. It is formed by wet gel while maintaining its pore and space network structure. The product obtained by replacing the liquid in its interstices with air. Airgel is currently the solid material with the smallest density and thermal conductivity in the world. The density can be as low as 0.0029g / m3, and the vacuum thermal conductivity at room temperature can reach 0.001W / mK. The special structure of airgel makes it have the advantages of light weight and high-efficiency heat insulation at the same time. It can be widely used in the fields of heat, light, sound, electricity, mechanics and so on. One ...

Claims

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Application Information

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IPC IPC(8): C08L83/16C08K3/22C08G77/62C08J9/28
CPCC08G77/62C08J9/28C08J2383/16C08K3/22C08K2003/2244C08L83/16Y02P20/54
Inventor 刘洪丽邓青怡李洪彦李婧李亚静刘志华
Owner TIANJIN CHENGJIAN UNIV
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