Method for quickly preparing nano thermal insulation material by supercritical drying

A nano-insulation material and supercritical drying technology, which is applied in the processing of textile materials, equipment configuration for processing textile materials, spraying/spraying of textile materials, etc., can solve the problem of increasing the production cost of nano-insulation materials, low solution recovery rate, Long drying time and other issues, to avoid the volatilization of organic solvents and personnel contact with volatiles, the process is simple, and the effect of saving equipment investment

Pending Publication Date: 2020-10-16
中化学华陆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the supercritical carbon dioxide drying method needs to continuously heat, cool, and compress carbon dioxide. The equipment is complicated, the energy consumption is high, the time for pressurization, replacement drying, and pressure relief is long, and the requirements for operators are high. It is difficult to achieve automation, and The water in the wet gel felt is not easily extracted by carbon dioxide, thus greatly increasing the production cost of nano-insulation materials
However, the preparation of nano-insulation materials by normal pressure drying, due to pore shrinkage and gel cracking during the drying process, the properties of the prepared nano-insulation materials cannot meet the requirements of use, and the drying time is long and the recovery rate of the solution is low, so gradually Be eliminated

Method used

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  • Method for quickly preparing nano thermal insulation material by supercritical drying
  • Method for quickly preparing nano thermal insulation material by supercritical drying
  • Method for quickly preparing nano thermal insulation material by supercritical drying

Examples

Experimental program
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Effect test

Embodiment 1

[0033] See figure 1 , figure 2 , The present invention provides a method for quickly preparing nano thermal insulation materials by supercritical drying. The entire process flow from front to back includes hydrolysis solution preparation, lye configuration, gel solution mixing, spray impregnation, cycle impregnation, and heating Gel, heating and drying, complete drying.

[0034] The fiber felt web 13 fixed on the web loading and unloading tray 23 is hoisted and put into the supercritical drying kettle 8, the cloth pipe 10 is connected with the feed pipe of the drying kettle using a quick-connect clamp, and the drying kettle lid 11 is covered.

[0035] Ethyl orthosilicate and methyl triethoxy silicon are mixed at a molar ratio of 1:1, and then used as a silicone source, and ethanol, water, and oxalic acid are added to the hydrolysate preparation tank 1 in a molar ratio of 1:20:4:0.02. Stir and raise the temperature to 50°C for 4 hours. After being pumped by the first delivery pump ...

Embodiment 2

[0046] The difference from Example 1 is that the mixed silicon source is replaced with methyl orthosilicate and methyl trimethoxy silicon mixed in a ratio of 1:1, and the catalyst acid is replaced with a mixed acid with a molar ratio of hydrochloric acid and hydrofluoric acid of 1:2. After replacing ethanol with methanol, mix according to the molar ratio of silicon source: alcohol: water: acid=1:18:4.5:0.02 to form a hydrolysis solution. The hydrolysis temperature is between 40 and 55°C, and other conditions remain basically unchanged. Supercritical drying is changed to methanol supercritical drying. The produced aerogel has better elasticity and lower thermal conductivity.

Embodiment 3

[0048] The difference from the first embodiment is that the fiber felt and the 5mm thick spacer (PP material hexagonal mesh) are rolled together, so that there is a larger gap between the fiber felt layer and the layer, and the supercritical temperature The holding time is shortened to 30min, which speeds up the drying speed. After drying, it is necessary to rewind the nano heat insulation material and recycle the spacer. The prepared nano heat insulation material has a stable surface structure and good appearance quality. At the same time, the method is also suitable for changing supercritical alcohol drying to supercritical carbon dioxide drying to prepare nano thermal insulation materials.

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Abstract

The invention discloses a method for quickly preparing a nano thermal insulation material by supercritical drying. The method combines liquid preparation, dipping, gelation and drying. After fiber felt rolls are directly immersed in a drying kettle for molding and solidification, the fiber felt rolls are directly heated to dry with supercritical methanol or ethanol, so as to achieve complete sealing to prepare the nano thermal insulation material. The method omits the curing and molding step of fiber felt, injects gel solution into the drying kettle, uses the adsorption performance of the fiber felt to remove the excess gel, and directly performs supercritical drying after gelation. The method has simple process, is easy to realize complete automation, saves much equipment investment, at the same time avoids a large amount of organic solvent volatilization and personnel contact with volatiles, and the waste heat recovery in the production process can save energy to the greatest extent.

Description

Technical field [0001] The invention relates to a method for quickly preparing nano thermal insulation materials by supercritical drying. Background technique [0002] In the preparation process of silicon oxide nano heat insulation material, the currently known preparation method of nano heat insulation material usually adopts aerogel and fiber mat fiber composite, and then adds spacers and soaks and ages, or performs hydrophobic modification process again, and then performs Supercritical carbon dioxide drying. The commonly used method for compounding fiber felt and gel liquid is gel tank whole roll soaking method, or unwinding-dipping-heating curing-adding septum winding method. [0003] After immersing the fiber web by the gel tank dipping method, a large amount of gel liquid forms a bulk aerogel around the fiber felt, which is broken and dropped after rewinding and adding a septum, forming a large amount of waste gel, and the operation engineering A large number of people are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06B1/02D06B9/06D06B15/00D06B23/20D06M11/79
CPCD06B1/02D06B9/06D06B15/00D06B23/20D06M11/79Y02P70/62
Inventor 赵耀耀徐妥夫杨志国郭卫疆康程陈维平
Owner 中化学华陆新材料有限公司
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