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CN-117945413-B - Durable fingerprint pollution-preventing low-density transparent silica aerogel and preparation method and application thereof

CN117945413BCN 117945413 BCN117945413 BCN 117945413BCN-117945413-B

Abstract

The invention relates to a durable fingerprint pollution-preventing low-density transparent silica aerogel and a preparation method and application thereof. The method comprises the steps of sequentially calcining low-density transparent silica aerogel, initially humidifying the low-density transparent silica aerogel in a constant temperature and humidity box and performing controllable humidification treatment in a vacuum drying box, performing gas-phase fingerprint pollution prevention modification on the wet activated low-density transparent silica aerogel and a modified liquid containing a perfluorinated silane reagent and ammonia methanol, and performing thermal vacuum treatment on the gas-phase fingerprint pollution prevention modified low-density transparent silica aerogel to obtain durable fingerprint pollution prevention low-density transparent silica aerogel. The method of the invention does not influence the intrinsic structure, the light weight characteristic and the transparent function of the aerogel, the coating is not easy to fall off due to the strong combination effect of the coating and the matrix based on chemical reaction, even if the surface layer of the aerogel is damaged, the newly exposed surface layer is still covered with the perfluorinated coating, and the method has excellent durable fingerprint pollution prevention effect.

Inventors

  • ZHANG WANLIN
  • LI WENJING
  • CHENG PIAO
  • LIAO YALONG
  • HUANG HONGYAN
  • LEI CHAOSHUAI

Assignees

  • 航天特种材料及工艺技术研究所

Dates

Publication Date
20260512
Application Date
20240123
Priority Date
20231129

Claims (17)

  1. 1. A method for preparing durable fingerprint-contamination-preventing low-density transparent silica aerogel, which is characterized by comprising the following steps: (1) Providing a low density transparent silica aerogel; (2) Calcining the low-density transparent silica aerogel sequentially, primarily humidifying the low-density transparent silica aerogel in a constant temperature and humidity box and performing controllable humidifying treatment in a vacuum drying box to obtain the wet activated low-density transparent silica aerogel; (3) Carrying out gas-phase fingerprint pollution prevention modification on the wet activated low-density transparent silica aerogel and a modified liquid containing a perfluorinated silane reagent and ammonia methanol to obtain the fingerprint pollution prevention low-density transparent silica aerogel; (4) And performing durable reinforcement treatment on the low-density transparent silica aerogel with fingerprint pollution resistance to obtain the low-density transparent silica aerogel with durable fingerprint pollution resistance.
  2. 2. The method of claim 1, wherein in step (2): The calcination is carried out in a muffle furnace, the temperature of the calcination is 300-500 ℃, and the time of the calcination is 0.1-2 h.
  3. 3. The method of claim 1, wherein in step (2): The constant temperature and humidity box is subjected to preliminary humidity treatment for 5-120 min under the conditions that the temperature is 25-40 ℃ and the humidity is 20-50%.
  4. 4. A method of preparation according to claim 3, wherein in step (2): the constant temperature and humidity box is subjected to primary humidity treatment for 20min under the conditions that the temperature is 25-40 ℃ and the humidity is 35%.
  5. 5. The method of claim 1, wherein in step (2): The controllable humidification treatment of the vacuum drying oven is heat preservation treatment for 1-8 hours under the conditions that the temperature is 25-40 ℃ and the absolute pressure is not more than 50 Pa.
  6. 6. The method according to claim 5, wherein in step (2): The controllable humidification treatment of the vacuum drying oven is heat preservation treatment for 3 hours under the conditions that the temperature is 25-40 ℃ and the absolute pressure is not more than 50 Pa.
  7. 7. The method of claim 1, wherein in step (3): The perfluoro silane reagent is 1H, 2H-perfluoro octyl triethoxy silane, 1H, 2H-perfluoro decyl triethoxy silane one or more of 1H, 2H-perfluorooctyl trimethoxysilane, 1H, 2H-perfluorodecyl trimethoxysilane.
  8. 8. The method of claim 1, wherein in step (3): the molar ratio of the perfluorinated silane reagent to the ammonia in the ammonia methanol is 1 (0.002-0.05), and/or The mass ratio of the substance amount of the perfluorinated silane reagent to the low-density transparent silica aerogel is 0.001-0.03 mol/g.
  9. 9. The method of claim 8, wherein in step (3): the molar ratio of the perfluorinated silane reagent to ammonia in the ammonia methanol is 1:0.02.
  10. 10. The method of claim 8, wherein in step (3): The mass ratio of the substance of the perfluorosilane reagent to the low-density transparent silica aerogel is 0.005mol/g.
  11. 11. The method of claim 1, wherein in step (3): the gas-phase fingerprint pollution prevention modification is carried out for 1-48 h under the condition of 60-120 ℃.
  12. 12. The method of claim 11, wherein in step (3): The gas-phase fingerprint pollution prevention modification is carried out for 12 hours under the condition of 90 ℃.
  13. 13. The method of claim 1, wherein in step (4): The durability enhancing treatment is carried out for 1-48 hours under the conditions that the temperature is 100-180 ℃ and the absolute pressure is not more than 0.0007 Pa.
  14. 14. The method of claim 13, wherein in step (4): The endurance strengthening treatment is a treatment under conditions of a temperature of 150 ℃ and an absolute pressure of not more than 0.0007Pa for 24 hours.
  15. 15. A durable fingerprint contamination resistant low density transparent silica aerogel made by the method of any of claims 1 to 14.
  16. 16. The durable fingerprint contamination resistant low density transparent silica aerogel of claim 15, wherein the durable fingerprint contamination resistant low density transparent silica aerogel has one or more of the following properties: The durable fingerprint pollution prevention low-density transparent silica aerogel has good hydrophobic and oleophobic characteristics, can effectively reduce fingerprint marks or stains generated when touching the surface of the aerogel, and shows excellent fingerprint pollution prevention performance; the light transmittance of the durable fingerprint pollution prevention low-density transparent silica aerogel is basically unchanged before and after fingerprint pollution prevention modification; The durable fingerprint pollution-preventing low-density transparent silica aerogel has pollution resistance from the surface to the inside, and after the aerogel surface layer is destroyed, the newly exposed surface layer still has good fingerprint pollution resistance; the durable fingerprint-contamination-preventing low-density transparent silica aerogel has low total mass loss and condensable volatile in a vacuum environment, and cannot cause environmental pollution in a closed use environment.
  17. 17. Use of the durable fingerprint contamination resistant low density transparent silica aerogel produced by the production process of any one of claims 1 to 14 in the new generation deep space exploration field, high energy physics field, building field or electronics field.

Description

Durable fingerprint pollution-preventing low-density transparent silica aerogel and preparation method and application thereof Technical Field The invention belongs to the technical field of nano porous materials, and particularly relates to a durable fingerprint pollution prevention low-density transparent silica aerogel and a preparation method and application thereof. Background The low-density transparent silica aerogel is a high-performance aerogel material with light weight and high transparency, and the high light transmittance of the aerogel can be widely applied to deep space detection tasks, high-energy physics and high-efficiency energy-saving transparent windows for buildings, which are represented by capturing cosmic dust. However, due to the low density and high porosity structure, the mechanical properties of the low density transparent silica aerogel are poor, and in actual use, the low density transparent silica aerogel is often required to be manually and carefully assembled into the protective frame, so that frequent touching of the aerogel is unavoidable, stains such as fingerprints are inevitably left on the surface of the aerogel in the touching process, the stains are more obviously visually presented by grease in the fingerprints, and the stains are not easy to clean after being polluted, which seriously affects the transparency and the attractiveness of the aerogel, and the actual application of the aerogel is affected. Therefore, developing a low density transparent silica aerogel having fingerprint contamination prevention functional properties has significant economic value. One of the key keys of the anti-fingerprint is that the constructed coating is a super-amphiphobic system, so that grease of the fingerprint is not easy to adhere, and the anti-fingerprint effect is achieved. Many prior art reports on the formation of anti-fingerprint coating on the surface of a substrate and a manufacturing method thereof, for example, chinese patent application CN112189061a describes a new method for coating a metal substrate with an anti-fingerprint coating by coating the metal substrate with a water-soluble silicone coating mixture, chinese patent application CN114507475A relates to an anti-fingerprint coating composed of a silane functional polymer, a polymer containing a fluoropolyether group and an organic solvent, chinese patent application CN115079316a describes a durable lubricating anti-fingerprint coating composed of a perfluoropolyether chain and a manufacturing method thereof, chinese patent application CN115124910a describes an anti-fingerprint liquid fluorine-containing coating material composed of perfluoropolyether, methyl nonafluorobutylether and nano calcium carbonate, and chinese patent application CN116515097A, CN115216001A, CN113788942a adopts complex synthesis to prepare fluorinated polyether siloxane, fluorine-containing siloxane compound, fluorine-containing polyether siloxane and other fluoride as the anti-fingerprint coating, respectively, to improve the anti-fouling performance of the surface of the substrate. However, the anti-fingerprint coating methods reported so far are not suitable for special substrates such as low density transparent silica aerogel, especially in certain special places in aerospace where high control of the condensable volatile content is required. The problems of the prior reported fingerprint-proof coating method are that firstly, the low-density silica aerogel has the characteristic of high porosity, fluorine-containing compounds and organic solvents are adopted as coating compounds, the fluorine-containing compounds and the organic solvents are easy to penetrate into the low-density silica aerogel when the low-density silica aerogel is sprayed or brushed, the porous structure of the aerogel is damaged, secondly, additives such as nano particles are often added in the method in the prior art, or the thickness of the coating is thicker, the high transparency of the aerogel is adversely affected, thirdly, the bonding capability of the coating and the silica aerogel is relatively weak, the abrasion resistance is insufficient and the fingerprint-proof performance is reduced after the coating is used for a long time, fourthly, the prior fingerprint-proof coating is easy to release volatile matters under high vacuum degree, the long-term use in a closed spacecraft system is not facilitated, and fifth, once the surface coating of the aerogel is damaged by adopting the reported methods, the newly exposed surface layer does not have the fingerprint-proof characteristic. Therefore, there is a need to develop a durable anti-fingerprint pollution coating for low-density transparent silica aerogel, which does not have any adverse effect on the characteristics of intrinsic porous structure, high transparency, light weight and the like of the material, has the characteristics of wear resistance and long-term applicability of anti-fingerprint pollution