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Preparation and application of light, heat-insulating and flame-retardant PIPD nanofiber aerogel

A nanofiber, airgel technology, applied in the direction of fiber chemical characteristics, textiles and papermaking, single-component synthetic polymer rayon, etc.

Inactive Publication Date: 2021-04-20
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Compared with PBO, poly 2,5-dihydroxy-1,4-phenylene pyridodiimidazole (PIPD) has higher compressive strength, excellent flame retardancy and interfacial bonding ability, while PIPD nanofibers aircondense Glue This sector has not been reported yet

Method used

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  • Preparation and application of light, heat-insulating and flame-retardant PIPD nanofiber aerogel
  • Preparation and application of light, heat-insulating and flame-retardant PIPD nanofiber aerogel
  • Preparation and application of light, heat-insulating and flame-retardant PIPD nanofiber aerogel

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Experimental program
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preparation example Construction

[0020] The invention provides a kind of preparation method of light weight, heat insulation, fire-retardant PIPD nanofiber airgel, comprising the following steps:

[0021] (1) Mix a certain amount of PIPD with mixed acid, and obtain PIPD nanofiber sol after ultrasonic treatment;

[0022] (2) The PIPD nanofiber sol is added with different proportions of proton-removing agents under stirring, and left to stand for a period of time under a constant temperature environment to obtain a stable gel;

[0023] (3) Soak the stable gel in a solvent for solvent exchange, then freeze-dry, and finally process at high temperature under an inert atmosphere to obtain PIPD nanofiber airgel.

[0024] In the present invention, the mass concentration of the PIPD in the mixed acid is 0.1-4wt%, more preferably 0.25-2wt%. The present invention preferably controls the mass concentration of PIPD in the mixed acid within the above-mentioned range, and can obtain uniform and completely dispersed PIPD na...

Embodiment 1

[0034] Weigh 0.1g of clean PIPD (intrinsic viscosity 9.7dL / g) into a 100ml single-necked flask, then add 18.6g of trifluoroacetic acid and 5.4g of methanesulfonic acid, seal it and place it in an ultrasonic cleaner at 35°C for ultrasonication to obtain PIPD Nanofiber sol.

[0035] Weigh 3.5g of methanesulfonic acid, 0.05g of deionized water, and 0.5g of ethyl acetate into a beaker, and stir evenly to obtain a proton-removing agent. Weigh 10g of PIPD nanofiber sol, pour the proton-removing agent into the PIPD nanofiber sol, stir at 1200rpm and pour it into the mold, then add enough deionized water to stabilize the mixed acid in the PIPD nanofiber gel. Replaced, and finally exchanged with tert-butanol solvent to obtain PIPD nanofiber wet gel.

[0036] The PIPD nanofiber wet gel was pre-frozen in a temperature-controlled refrigerator, then freeze-dried, then placed in a tube furnace, heated to 400 °C under a nitrogen atmosphere, and kept at a constant temperature for 30 minutes ...

Embodiment 2

[0039] Weigh 0.05g of clean PIPD (intrinsic viscosity 5.8dL / g) into a 100ml single-necked flask, then add 12g of trifluoroacetic acid, 7g of methanesulfonic acid, 1g of concentrated sulfuric acid, seal and place in an ultrasonic cleaner at 25°C Ultrasound to obtain PIPD nanofiber sol.

[0040] Weigh 2.8g of methanesulfonic acid, 0.13g of deionized water, 0.85g of ethyl acetate, and 0.05g of ethanol in a beaker, and stir evenly to obtain a proton-removing agent. Weigh 10g of PIPD nanofiber sol, pour the proton-removing agent into the PIPD nanofiber sol, stir at 1500rpm and pour it into the mold, then add enough phenol and water (w / w=5:1) to mix The solvent replaces the mixed acid in the PIPD nanofiber stable gel to obtain the PIPD nanofiber wet gel.

[0041] The PIPD nanofiber wet gel was pre-frozen in a temperature-controlled refrigerator, then freeze-dried, then placed in a tube furnace, heated to 350 °C under a nitrogen atmosphere, and kept at a constant temperature for 35 ...

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Abstract

The invention relates to the technical field of aerogel materials, and provides light, heat-insulating and flame-retardant PIPD nanofiber aerogel as well as preparation and application thereof. The PIPD nanofiber aerogel is prepared by taking high-molecular-weight PIPD as a raw material, stripping the PIPD into PIPD nanofibers by adopting an acid mixing method, and performing solvent exchange, freeze drying and high-temperature heat treatment in an inert atmosphere. The PIPD nanofiber aerogel is formed by assembling PIPD nanofibers serving as construction modules, the PIPD nanofibers are mutually staggered to form a layered network, and the layered network forms a honeycomb pore structure. The aerogel provided by the invention is adjustable in density of 6.90-17.95 kg / m < 3 >, high in porosity (80-99.8%), good in heat-insulating property, good in flame retardant property (UL-94, V-0 grade) and strong in interface bonding force, and can be used as a flame-retardant heat-insulating material. The preparation method provided by the invention is simple in steps and easy to implement.

Description

technical field [0001] The invention relates to the technical field of airgel materials, in particular to the preparation and application of a lightweight, heat-insulating and flame-retardant PIPD nanofiber airgel. Background technique [0002] A variety of heat insulation materials are widely used in military and civilian fields. In the context of today's high-performance materials that need to continuously meet the needs of special service environments, heat insulation materials that integrate light weight and high temperature resistance are also very important. [0003] Since Kistler successfully prepared "aerogels" in 1932, this type of material has attracted widespread attention because of its unique properties. Airgel is a nano-scale porous solid material with extremely high porosity, extremely low density, high specific surface area, ultra-high pore volume ratio, and low thermal conductivity. It can be used as a new type of thermal insulator. For example, the therma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08L79/04C08K5/42C08K5/101D01F6/58
Inventor 李欣欣陈康王嘉睿曾奥研罗元章高媛
Owner EAST CHINA UNIV OF SCI & TECH
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