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Modified oxide hybrid phenolic aldehyde thermal insulation material and preparation method thereof

A technology of thermal insulation materials and oxides, applied in the direction of coating, etc., can solve the problems that affect the service life and storage life of high-performance thermal insulation materials, cannot fundamentally solve the problems of absorbing and enriching gaseous water, and the huge difference in surface reactivity , to achieve the effect of stable and controllable weight gain, wide and cheap sources of raw materials, and excellent moisture-proof performance

Pending Publication Date: 2021-12-21
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the known reports related to the waterproof modification of phenolic materials, the hydrophobic treatment of the material is mainly achieved by compounding a hydrophobic coating on the outer surface of the material. This treatment can prevent liquid water from interacting with the The contact of phenolic insulation materials prevents the material from absorbing liquid water, but it cannot fundamentally solve the problem of absorbing and enriching gaseous water on the surface of the pores inside the material
At the same time, due to the huge difference in surface reactivity between multiple components, the modification methods that are applicable to each other will also interfere with each other when used at the same time
Therefore, the use and storage life of the above-mentioned high-performance thermal insulation materials in large-scale, highly integrated thermal protection systems are affected

Method used

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preparation example Construction

[0032] In a first aspect, the present invention provides a method for preparing a modified oxide hybrid phenolic heat insulating material, the method comprising the following steps:

[0033] (1) Preparation of modifying agent: mixing the modifying agent with an optional solvent to prepare a modifying agent with hydrophobic modification function;

[0034] (2) Modification reaction: introducing the modifier into the oxide hybrid phenolic heat insulation material to keep warm for modification reaction;

[0035](3) Drying: After the modification reaction is completed, excess modifying reagents are removed by heating under in-situ conditions to obtain a modified oxide hybrid phenolic heat insulating material with moisture-proof performance.

[0036] In some preferred embodiments, in step (1), the modifying reagent comprises a first modifying reagent and a second modifying reagent, and the first modifying reagent is selected from formula (1) or formula ( 2) One or more reagents of ...

Embodiment 1

[0061] The size is 500mm×500mm×30mm, the density is 0.5g / cm 3 , a commercially available unmodified oxide hybrid phenolic airgel composite sheet with a thermal conductivity of 0.06W / (m·K) at room temperature is placed in a tank with a height of 800mm and a diameter of 800mm to keep the atmosphere Keep warm at 60°C for 4 hours in the connected state. While maintaining the same temperature, evacuate the inside of the tank to a vacuum, then inhale the modifier containing 94g of dimethyl carbonate and 94g of trimethylmethoxysilane, close the tank and continue to keep warm at 60°C for 12h, and then take out the plate , 90 ° C blast drying for 6h. The surface of the obtained material is in a hydrophobic state, the weight of the material increases by 2% (the mass change rate is tested after 120°C oven treatment for 2 hours, the same below), the moisture absorption rate is 0.40%, and the thermal conductivity change at room temperature is <1%.

Embodiment 2

[0063] The size is 500mm×500mm×30mm, the density is 0.5g / cm 3 , a commercially available unmodified oxide hybrid phenolic airgel composite sheet with a thermal conductivity of 0.06W / (m·K) at room temperature is placed in a tank with a height of 800mm and a diameter of 800mm to keep the atmosphere Keep warm at 60°C for 4 hours in the connected state. While maintaining the same temperature, evacuate the inside of the tank to a vacuum, then inhale a mixture containing 94g of dimethyl carbonate, 94g of trimethylmethoxysilane and 187.5g of acetone, then close the tank and continue to keep warm at 60°C for 12h, then put The plates were taken out and air-dried at 90°C for 6 hours. The surface of the material is in a hydrophobic state, the weight gain of the material is 2.5%, the moisture absorption rate is 0.35%, and the thermal conductivity at room temperature does not change <1%.

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Abstract

The invention belongs to the technical field of thermal protection, and discloses a modified oxide hybrid phenolic aldehyde thermal insulation material and a preparation method thereof. The method comprises the following steps: (1) preparing a modifying agent: mixing a modifying reagent with an optional solvent to prepare a modifying agent with a hydrophobic modification function; (2) carrying out a modification reaction: introducing the modifying agent into an oxide hybrid phenolic aldehyde thermal insulation material, and carrying out heat preservation to carry out modification reaction; and (3) drying: after the modification reaction is completed, under an in-situ condition, removing redundant reagents and by-products in a heating manner to obtain the oxide hybrid phenolic aldehyde thermal insulation material with the moisture-proof performance. According to the invention, the thermal insulation property of the thermal insulation material is almost not affected adversely, the thermal insulation material is endowed with excellent moisture resistance, and after modification treatment, the mass gain percentage is smaller than or equal to 3%, the mass moisture absorption rate is smaller than or equal to 1% and / or the heat conductivity change is smaller than 1%.

Description

technical field [0001] The invention relates to the technical field of heat protection, in particular to a modified oxide hybrid phenolic heat insulating material and a preparation method thereof. Background technique [0002] The description of the background technology of the present invention belongs to the relevant technology related to the present invention, and is only used to illustrate and facilitate the understanding of the content of the present invention. prior art prior to the filing date. [0003] Porous thermal insulation materials represented by phenolic thermal insulation materials, especially oxide hybrid phenolic thermal insulation materials, have many advantages such as ablation resistance, light weight, excellent thermal insulation performance, stable performance, and low cost. It is widely used in aerospace, deep space exploration and civil thermal insulation fields. However, this type of material has high porosity, rich internal pore structure, large ...

Claims

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Application Information

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IPC IPC(8): C08J9/36C08L61/06
CPCC08J9/36C08J2361/06
Inventor 黄红岩李文静刘圆圆张贝贝高翠雪张昊赵英民
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH