Aerogel composite material and method of manufacturing aerogel composite material, and aerogel particle
Patent Information
- Authority / Receiving Office
- EP · EP
- Patent Type
- Applications
- Current Assignee / Owner
- OWENS CORNING INTELLECTUAL CAPITAL LLC
- Filing Date
- 2024-11-22
- Publication Date
- 2026-07-08
AI Technical Summary
Existing methods for manufacturing aerogel composite materials face high costs, energy consumption, and limitations in scalability, particularly with the supercritical drying method, while atmospheric pressure drying methods struggle to produce composite materials in situ.
The application of an alternating electric field to impregnate aerogel particles into porous fiber materials, utilizing silicon hydroxyl functional groups (Si-OH) and specific infrared absorption peaks, allows for uniform distribution and low-cost, low-energy production of aerogel composites.
This method enables efficient, low-cost, and energy-efficient production of aerogel composites with improved thermal insulation and reduced fallout rates, avoiding structural damage to aerogel particles and enhancing their performance.
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Figure US2024057025_28052026_PF_FP_ABST
Abstract
Description
AEROGEL COMPOSITE MATERIAL AND METHOD OF MANUFACTURING AEROGEL COMPOSITE MATERIAL, AND AEROGEL PARTICLECROSS-REFERENCE TO RELATED APPLICATION(S)
[0001] This application claims priority to Chinese Patent Application No. 202411657775.6 filed on November 19, 2024, the disclosure of which is incorporated by reference herein in its entirety.BACKGROUND
[0002] The present invention relates to the technical field of aerogel, and in particular to an aerogel composite material and a method of manufacturing an aerogel composite material, and aerogel particle.
[0003] Aerogel composite material is a new advanced material, which is made by the combination of nano aerogel particle and fiber materials through a special process. It has the characteristics of light weight, heat insulation with high efficiency, fire prevention and is eco-friendly, and is widely used in construction, petroleum, aerospace and other fields.
[0004] At present, aerogel composite material is mainly manufactured by a supercritical drying method or an atmospheric pressure drying method. The supercritical drying method is to replace the solvent in the sol-gel pre-impregnated in the fiber material by using the special properties of supercritical fluid (such as carbon dioxide), so as to achieve the transformation of sol-gel to aerogel, and make the aerogel grow in situ in the fiber material to manufacture the aerogel composite materials. However, the supercritical drying method requires supercritical conditions. The cost of supercritical drying equipment is large, the process operation is complicated, the process energy consumption is very high, and the selection for precursor has certain restrictions.
[0005] The atmospheric pressure drying method converts sol-gel into aerogel under atmospheric pressure at room temperature or atmospheric pressure at high temperature by doing a large amount of hydrophobic modification in advance. The atmospheric pressure drying method has low equipment cost and low energy consumption. However, the limitation on further industrialization of the atmospheric pressure drying method is that it can only produce aerogel powder on a large scale, and cannot prepare aerogel composite materials in situ.
[0006] To provide a secondary composite technology with low process input cost, low production energy consumption, simple preparation process, excellent distribution effect of aerogel powder and good pore structure and properties is an urgent technical problem that needs to be solved in this field.SUMMARY
[0007] A series of simplified concepts is introduced into the portion of Summary, which would be further illustrated in the portion of the detailed description. The Summary of the present invention does not mean attempting to define the key feature and essential technical feature of the claimed technical solution, let alone determining the protection scope thereof.
[0008] The present invention provides an aerogel composite material, comprising: a porous fiber material; and an aerogel particle distributed within the porous fiber material, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; wherein the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3, and the average particle size of the aerogel particle is less than or equal to 500pm.
[0009] In a specific embodiment, the aerogel particle, distributed within the porous fiber material, is impregnated into the porous fiber material by applying an alternating electric filed; the voltage of the alternating electric field ranges from 0.1KV to 50KV, and the frequency ranges from 1HZ to 800HZ; the application time of the alternating electric field ranges from 30 seconds to 5 minutes.
[0010] In a specific embodiment, the density of the aerogel particle ranges from 0.03g / cm3to O. lg / cm3, and the average particle size of the aerogel particle is less than or equal to 50pm.
[0011] In a specific embodiment, the porous fiber material is selected from a glass fiber felt, a glass fiber non-woven fabric, a glass fiber textile fabric, a ceramic fiber felt, a paper, a polyurethane fiber felt, a carbon fiber felt, a polypropylene fiber felt, a polypropylene and glass fiber composite felt, and a combination of the above.
[0012] In a specific embodiment, the areal density of the glass fiber non-woven fabric is between 20g / m2and 500g / m2; the thickness is between 0.3mm and 4mm; and the air permeability is between 200L / m2 / s and 3000L / m2 / s.
[0013] In a specific embodiment, the areal density of the glass fiber non-woven fabric is between 50g / m2and 150g / m2; the thickness is between 0.5mm and 1.5mm; and the air permeability is between 500L / m2 / s and 2000L / m2 / s.
[0014] In a specific embodiment, the areal density of the glass fiber non-woven fabric is between 90g / m2and 135g / m2; the thickness is between 0.8mm and 1.3mm; and the air permeability is between 1100L / m2 / s and 1800L / m2 / s.
[0015] In a specific embodiment, the polypropylene and glass fiber composite felt is made by blending a polypropylene fiber with a glass fiber; the density of the polypropylene andglass fiber composite felt is between 20kg / m3and 200kg / m3; and the thickness is between 1mm and 20mm.
[0016] In a specific embodiment, the density of the polypropylene and glass fiber composite felt is between 50kg / m3and 150kg / m3, and the thickness is between 3mm and 10mm.
[0017] In a specific embodiment, an additive for inhibiting thermal radiation is added to the aerogel particle, and the additive is selected from at least one of silicon carbide, boron carbide, titanium oxide and boron nitride; the weight ratio of the additive to the aerogel particle ranges from lwt% to 15wt%.
[0018] In a specific embodiment, the weight ratio of the additive to the aerogel particle ranges from 5wt% to 12wt%.
[0019] In a specific embodiment, the weight ratio of the aerogel particle to the aerogel composite material ranges from lwt% to 50wt%.
[0020] The present invention further provides a method of manufacturing the aerogel composite material discussed above, wherein the method comprises the following steps: impregnating aerogel particle into a porous fiber material by applying an alternating electric field, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; wherein the voltage of the alternating electric field ranges from 0.1KV to 200KV, and the frequency ranges from 0.1HZ to 800HZ; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3; and the average particle size of the aerogel particle is less than or equal to 500pm.
[0021] In a specific embodiment, the application time of the alternating electric field ranges from 30 seconds to 5 minutes.
[0022] In a specific embodiment, a step is further comprised to apply the aerogel particle to a surface of the porous fiber material and / or applying the aerogel particle to a loader that is at least partially subject to the alternating electric field.
[0023] In a specific embodiment, the porous fiber material and the aerogel particle are arranged between a lower electrode and an upper electrode, and the electrode is electrically insulated from each other through a dielectric and connected to a power supply such that the porous fiber material and the aerogel particle are subject to the alternating electric field.
[0024] In a specific embodiment, the density of the aerogel particle ranges from 0.03g / cm3to O. lg / cm3, and the average particle size of the aerogel particle is less than or equal to 50pm.
[0025] In a specific embodiment, the porous fiber material is selected from a glass fiberfelt, a glass fiber non-woven fabric, a glass fiber textile fabric, a ceramic fiber felt, a paper, a polyurethane fiber felt, a carbon fiber felt, a polypropylene fiber felt, a polypropylene and glass fiber composite felt, and a combination of the above.
[0026] In a specific embodiment, the areal density of the glass fiber non-woven fabric is between 20g / m2and 500g / m2; the thickness is between 0.3mm and 4mm; and the air permeability is between 200L / m2 / s and 3000L / m2 / s.
[0027] In a specific embodiment, the areal density of the glass fiber non-woven fabric is between 50g / m2and 150g / m2; the thickness is between 0.5mm and 1.5mm; and the air permeability is between 500L / m2 / s and 2000L / m2 / s.
[0028] In a specific embodiment, the areal density of the glass fiber non-woven fabric is between 90g / m2and 135g / m2; the thickness is between 0.8mm and 1.3mm; and the air permeability is between 1100L / m2 / s and 1800L / m2 / s.
[0029] In a specific embodiment, the polypropylene and glass fiber composite felt is made by blending a polypropylene fiber with a glass fiber; the density of the polypropylene and glass fiber composite felt is between 20kg / m3and 200kg / m3; and the thickness is between 1mm and 20mm.
[0030] In a specific embodiment, the density of the polypropylene and glass fiber composite felt is between 50kg / m3and 150kg / m3, and the thickness is between 3mm and 10mm.
[0031] In a specific embodiment, an additive for inhibiting thermal radiation is added to the aerogel particle, and the additive is selected from at least one of silicon carbide, boron carbide, titanium oxide and boron nitride; the weight ratio of the additive to the aerogel particle ranges from lwt% to 15wt%.
[0032] In a specific embodiment, the weight ratio of the additive to the aerogel particle ranges from 5wt% to 12wt%.
[0033] The present invention further provides aerogel particle, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3; and the average particle size of the aerogel particle is less than or equal to 500pm.
[0034] The present invention provides an aerogel composite material. One of the innovations of the aerogel composite material provided by the invention is that the alternating electric field is applied to the process of preparing the aerogel composite material, so that the aerogel composite material of the invention has more prominent technical advantages compared with the aerogel composite material manufactured by the supercritical drying method or theslurry impregnation method in prior art or other prior arts. For example, compared to the supercritical drying method, there is no need to use a complex supercritical equipment and high energy consumption to produce supercritical fluid, and the aerogel composite material can be manufactured while meeting the requirements for the uniformity of distribution of aerogel particle by only needing to use the aerogel powder prepared by the alternating electric field of a simple structure and atmospheric pressure drying method, with simple manufacturing process, low input cost and low energy consumption. Compared to the aerogel slurry impregnation method, the aerogel composite material has better performance because it does not require solvent impregnation and thereby avoids the destruction of the structure of the aerogel particle. At the same time, the process does not include the use of solvents and drying, which reduces a lot of energy consumption.
[0035] In addition, aerogel powder is impregnated into porous fiber materials by alternating electric field, and the aerogel particle has a large impregnation amount and is uniform such that the aerogel composite material has better thermal insulation properties, with simple process and low production cost.
[0036] The present invention further discloses aerogel particle. The aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1. The fallout rate of the aerogel composite material manufactured by using the aerogel particle is significantly improved.BRIEF DESCRIPTION OF THE DRAWINGS
[0037] The following drawings are hereby incorporated as part of the present invention for the understanding of the present invention. The embodiments are illustrated and described in the drawings in order to explain the principles of the present invention.
[0038] In the drawings:
[0039] FIG. 1 is an electron micrograph photograph of a vertical cross-section of the aerogel composite material according to Example 1 of the present invention;
[0040] FIG. 2a is an electron micrograph photograph of a vertical cross-section of the aerogel composite material according to Example 2 of the present invention;
[0041] FIG. 2b is an electron micrograph photograph of a front side of the aerogel composite material according to Example 2 of the present invention;
[0042] FIG. 2c is an electron micrograph photograph of a back side of the aerogel composite material according to Example 2 of the present invention;
[0043] FIG. 3a is an electron micrograph photograph of a vertical cross-section of the aerogel composite material according to Comparative Example 1 of the present invention;
[0044] FIG. 3b is an electron micrograph photograph of a front side of the aerogel composite material according to Comparative Example 1 of the present invention;
[0045] FIG. 3c is an electron micrograph photograph of a back side of the aerogel composite material according to Comparative Example 1 of the present invention;
[0046] FIG. 4a is an electron micrograph photograph of a vertical cross-section of the aerogel composite material according to Comparative Example 2 of the present invention;
[0047] FIG. 4b is an electron micrograph photograph of a front side of the aerogel composite material according to Comparative Example 2 of the present invention;
[0048] FIG. 4c is an electron micrograph photograph of a back side of the aerogel composite material according to Comparative Example 2 of the present invention;
[0049] FIG. 5 shows a reference chart for testing powder fallout rate by a nitrile glove friction test method; and
[0050] FIG. 6 shows the infrared spectrum of different types of aerogel particles in Example 4 of the present invention.DETAILED DESCRIPTION
[0051] In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. However, it is obvious to those skilled in this art that the present invention may be implemented without one or more of these details. Some technical features well-known in this art are not described in other examples in order to avoid confusion with the present invention.
[0052] In order to thoroughly understand the present invention, a detailed description will be provided in the following description to elaborate the aerogel composite material and the method of manufacturing the aerogel composite material of the present invention. Obviously, the implementation of the present invention is not limited to the specific details familiar to those skilled in the art. The preferred embodiments of the present invention are described in detail as follows. However, in addition to these detailed descriptions, the present invention may have other embodiments.
[0053] It shall be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments of the present invention. As used herein, the singular forms are intended to include the plural forms as well, unless the context clearly indicates otherwise.
[0054] The exemplary embodiments according to the present invention will now be described in detail with reference to the drawings. However, these exemplary embodiments can be implemented in various forms but should not be construed as being limited to theembodiments set forth herein. It is to be understood that these embodiments are provided to make the disclosure of the invention thorough and complete, and that the ideas of these exemplary embodiments are fully communicated to those of ordinary skill in the art.
[0055] To at least partially solve the problem, a first aspect of the present invention provides an aerogel composite material. One of the innovations of the aerogel composite material provided by the invention is that the alternating electric field is applied to the process of preparing the aerogel composite material, so that the aerogel composite material of the invention has more prominent technical advantages compared with the aerogel composite material manufactured by the supercritical drying method or the slurry impregnation method in prior art or other prior art. For example, compared to the supercritical drying method, there is no need to use a complex supercritical equipment and high energy consumption to produce supercritical fluid, and the aerogel composite material can be manufactured while meeting the requirements of the uniformity of distribution of aerogel particle by only needing to use the aerogel powder prepared by the alternating electric field with a simple structure and atmospheric pressure drying method, with simple manufacturing process, low input cost and low energy consumption. Compared to the aerogel slurry impregnation method, the aerogel composite material has better performance because it does not require solvent impregnation and thereby avoids the destruction of the structure of the aerogel particle. At the same time, the process does not include the use of solvents and drying, which reduces a lot of energy consumption.
[0056] Specifically, the aerogel composite material disclosed in the present invention may include a porous fiber material and aerogel particle distributed within the porous fiber material. By applying the alternating electric field to the porous fiber material, the aerogel particle is impregnated not only into the porous fiber material, but also is impregnated more uniformly. With reference to FIG. 1 and FIG. 2a, the electron micrograph photographs of the aerogel composite material of Examples 1 and 2 in vertical cross section are shown. Compared to FIG. 3a and FIG. 4a of Comparative Examples, it can be seen that the aerogel particle in the aerogel composite material of the invention is more evenly distributed and has a relatively large amount of impregnation. In multiple embodiments, the weight ratio of the aerogel particle to the aerogel composite material may range from 1 wt% to 50 wt%.
[0057] An alternating electric field refers to an electric field whose magnitude and direction change with time. It is produced by an alternating current power supply, in which the charge oscillates sometimes positively and sometimes negatively, causing a change in the electric field. The alternating electric field is characterized by periodic changes, and its frequency describes the rate of change in Hertz (Hz). The voltage range of the alternatingelectric field of the invention can be 0.1KV to 50KV, the frequency range can be 1HZ to 800HZ, and the application time of the alternating electric field can be 30 seconds to 5 minutes. Those skilled in the art can adjust any of the above parameters according to the actual needs of use and product conditions in the production process.
[0058] The density of the aerogel particle of the aerogel composite material of the present invention can range from 0.01g / cm3to 0.5g / cm3, and the average particle size of the aerogel particle is less than or equal to 500 pm. Preferably, the density of the aerogel particle can range from 0.03g / cm3to O. lg / cm3, and the average particle size of the aerogel particle is less than or equal to 50pm. For example, the aerogel particle may be JIOS aerogel Company AeroVa® aerogel particle (Chinese patent CN103771428B and U.S. Patent Application Publication No. 2022 / 0306833 are incorporated by reference as a whole into this specification).
[0059] The porous fiber material can be selected from a glass fiber felt, a glass fiber non-woven fabric, a glass fiber textile fabric, a ceramic fiber felt, a paper, a polyurethane fiber felt, a carbon fiber felt, a polypropylene fiber felt, a polypropylene and glass fiber composite felt, and a combination of the above. Preferably, the porous fiber material can use the glass fiber non-woven fabric, whose areal density can be between 20g / m2and 500g / m2, thickness can be between 0.3mm and 4mm, and air permeability can be between 200L / m2 / s and 3000L / m2 / s. Further preferably, the areal density can be between 50g / m2and 150g / m2, the thickness can be between 0.5mm and 1.5mm, and the air permeability can be between 500L / m2 / s and 2000L / m2 / s, or the areal density is between 90g / m2and 135g / m2, the thickness is between 0.8mm and 1.3mm, and the air permeability is between 1100L / m2 / s and 1800L / m2 / s.
[0060] As another preferred embodiment, the polypropylene and glass fiber composite felt with the density between 50kg / m3and 150kg / m3and thicknesses between 3mm and 10mm may also be selected for the porous fiber material. It should be noted that the present invention is not limited to the varieties of the porous fiber material specifically enumerated, as long as the fibrous material with porosity known to the person skilled in the art or the material equivalent to the porous fiber material that can accommodate the aerogel particle is within the protection scope limited by the invention.
[0061] In order to improve the thermal insulation and insulation properties of aerogel composite materials, an additive for inhibiting thermal radiation can also be added to the aerogel particle. For example, the additive may be selected from at least one of silicon carbide, boron carbide, titanium oxide and boron nitride. The weight ratio of the additive to the aerogel particle may range from lwt% to 15wt%. Preferably, the weight ratio of the additive to the aerogel particle ranges from 5wt% to 12wt%.
[0062] A second aspect of the present invention further provides a method of manufacturing the aerogel composite material, wherein the method may fundamentally comprise the following steps:
[0063] Feeding: The aerogel particle is applied to the surface of the porous fiber material and / or onto a loader that is at least partially subject to an alternating electric field. For example, the loader may be a conveyor belt or a rotary feeder, or the like. The conveyor belt may be located above the porous fiber material and at least partially located in the alternating electric field. The aerogel particle may be transported through the conveyor belt, and the aerogel particle located on the conveyor belt may be impregnated into the porous fiber material when the alternating electric field is applied.
[0064] Treatment: The aerogel particle is impregnated into the porous fiber material by applying an alternating electric field, where the voltage range of the alternating electric field can be 0.1KV to 200KV, and the frequency ranges from 0.1HZ to 800HZ; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3, and the average particle size of the aerogel particle is less than or equal to 500 pm. The application time of the alternating electric field ranges from 30 seconds to 5 minutes.
[0065] In an optional embodiment, the porous fiber material and the aerogel particle are arranged between a lower electrode and an upper electrode, and the electrodes are electrically insulated from each other through a dielectric and connected to a power supply such that the porous fiber material and the aerogel particle are subject to the alternating electric field.
[0066] Further, in order to better describe the aerogel composite material and the method of manufacturing the aerogel composite material provided by the present invention, the invention provides a plurality of Examples and Comparative Examples to illustrate that the invention has more prominent technical advantages compared with the prior art.Example 1 :
[0067] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, and porosity > 90%.
[0068] Owens Corning Company glass fiber non-woven fabric, gram weight: 125g / m2, thickness: 1.25mm, and air permeability: 1300 ~ 1350L / m2 / s (the test standard for air permeability is GB / T 5453).
[0069] High voltage alternating electric field: Consist of two electrodes. One electrode is grounded, and the other electrode is powered by high voltage alternating current. The maximum voltage is ±15kv, sine wave, and frequency is 600HZ.
[0070] Implementation process: The aerogel particle is evenly spread on the glass fibernon-woven fabric, placed between the high voltage alternating electric fields, and electrified such that that the powder is fully oscillated in it for 2 minutes and will be impregnated into the middle pores of the non-woven fabric.
[0071] Results: The final weight ratio of the aerogel particle to the whole material is 42wt%. FIG. 1 is the electron micrograph photograph of the vertical cross-section of the aerogel composite material in Example 1. It can be seen that the aerogel particle is uniformly impregnated into the pores of the non-woven fabric from the upper surface to the lower surface of the porous fiber material. Due to the large impregnation amount and uniform impregnation of the aerogel particle, the aerogel composite material has good thermal insulation performance. Example 2:
[0072] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Owens Corning Company glass fiber non-woven fabric, gram weight: 100g / m2, thickness: 1mm, and air permeability: 1700~1750L / m2 / s.
[0073] High voltage alternating electric field: Consist of two electrodes. One electrode is grounded, and the other electrode is powered by high voltage alternating current. The maximum voltage is ±20kv, sine wave, and frequency is 600HZ.
[0074] Implementation process: The aerogel particle is evenly spread on the glass fiber non-woven fabric, placed between the high voltage alternating electric fields, and electrified such that that the powder is fully oscillated in it for 2 minutes and will be impregnated into the middle pores of the non-woven fabric.
[0075] Results: The final weight ratio of the aerogel particle to the whole material is 32wt%. FIGS. 2a, 2b, and 2c are respectively electron micrograph photographs of the vertical cross-section, front side, and back side of the aerogel composite material in Example 2.
[0076] Compared with FIG. 3a and FIG. 4a of Comparative Examples, it can be seen that the aerogel particle in the aerogel composite material of Example 2 is evenly distributed and the amount of impregnation is relatively large. Compared with FIG. 3b and FIG. 4b of Comparative Examples, it can be seen that the aerogel particle on the front side of the aerogel composite material in Example 2 is evenly distributed and the amount of impregnation is relatively large. From the distribution of the aerogel particle on the back of the aerogel composite material in the Comparative Examples shown in FIG. 3c and FIG. 4c, it can be seen that there is basically no aerogel particle due to insufficient impregnation amount and uneven distribution of the aerogel particle. However, the aerogel particle on the back of the aerogel composite material in Example 2 is evenly distributed, with relatively large impregnation amount.Example 3 :
[0077] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Silicon carbide powder, particle size: 0.5pm~0.7pm, density: 0.8 ~ 0.9g / cm3, etc. Owens Corning Company glass fiber non-woven fabric, gram weight: 100g / m2, thickness: 1mm, and air permeability: 1700~1750L / m2 / s.
[0078] High voltage alternating electric field: Consist of two electrodes. One electrode is grounded, and the other electrode is powered by high voltage alternating current. The maximum voltage is ±20kv, sine wave, and frequency is 600HZ.
[0079] Implementation process: The aerogel particle and silicon carbide particle are evenly dispersed and spread on the glass fiber non-woven fabric in the ratio of 9: 1, placed between high voltage alternating electric fields, and electrified such that the powder is fully oscillated in it for 2 minutes and will be impregnated into the middle pores of the non-woven fabric.
[0080] Results: The final weight ratio of the aerogel and silicon carbide particle to the whole material is 41wt%.Example 4:
[0081] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Glass fiber and polypropylene fiber blended felt, density: ~ 90 kg / m3, thickness: ~ 6mm, and air permeability: 380~420L / m2 / s.
[0082] High voltage alternating electric field: Consist of two electrodes. One electrode is grounded, and the other electrode is powered by high voltage alternating current. The maximum voltage is ±14kv, sine wave, and frequency is 600HZ.
[0083] Implementation process: The aerogel particle is evenly spread on the glass fiber non-woven fabric, placed between the high voltage alternating electric fields, and electrified such that the powder is fully oscillated in it for 2 minutes and will be impregnated into the middle pores of the non-woven fabric.
[0084] Results: The final weight ratio of the aerogel particle to the whole material is 35wt%.Comparative Example 1 :
[0085] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Owens Corning Company glass fiber non-woven fabric, gram weight: 125g / m2, thickness: 1.25mm, and air permeability: 1300 ~ 1350L / m2 / s.
[0086] Electrostatic spraying: Electrostatic high voltage: 20KV, electrostatic current:40pA, powder pressure: 210KPa, atomization pressure: 70KPa, and powder bucket fluidizationpressure: 35KPa.
[0087] Implementation process: The non-woven fabric is placed on the horizontal desktop. The electrostatic spraying device is connected to a powder barrel and electrified. The parameters are adjusted. The switch is turned on to evenly coat the aerogel particle on the non-woven fabric, three times in total.
[0088] Results: The final weight ratio of the aerogel particle to the whole material is 12wt%. FIGS. 3a, 3b, and 3c are respectively electron micrograph photographs of the vertical cross-section, front side and back side of the aerogel composite material in Comparative Example 1.Comparative Example 2:
[0089] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; glass fiber and polypropylene fiber blended felt, gram weight: 540g / m2, thickness: 6mm, and air permeability: 380~420L / m2 / s.
[0090] Electrostatic spraying: Electrostatic high voltage: 20KV, electrostatic current: 40pA, powder pressure: 210KPa, atomization pressure: 70KPa, and powder bucket fluidization pressure: 35KPa.
[0091] Implementation process: The blended felt is placed on the horizontal desktop. The electrostatic spraying device is connected to a powder barrel and electrified. The parameters are adjusted. The switch is turned on to evenly coat the aerogel particle on the non-woven fabric, three times in total.
[0092] Results: The final weight ratio of the aerogel particle to the whole material is 8wt%. FIGS. 4a, 4b, and 4c are respectively electron micrograph photographs of the vertical cross-section, front side and back side of the aerogel composite material in Comparative Example 2.Comparative Example 3 :
[0093] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Owens Corning Company needle felt, gram weight: 900g / m2, density: 60kg / m2, thickness: ~ 15mm, air permeability: 100-300L / m2 / s; and Solvent: ethanol.
[0094] Implementation process: The aerogel particle is stirred and dispersed in solvent ethanol to prepare a dispersion liquid with the mass concentration of 10wt% and the viscosity of 18.1cP. The dispersion liquid is added to the glass fiber felt, and the negative pressure is pumped to make the dispersion liquid fully impregnated. The glass fiber felt is naturally dried at room temperature for 24 hours, and then put into a 200°C oven for 12 hours.
[0095] Results: The final weight ratio of the aerogel particle to the whole material is 22wt%. The data of specific surface area of aerogel after immersion of the dispersion liquid and drying are shown in Table 1.Comparative Example 4:
[0096] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Owens Corning Company needle felt, gram weight: 900g / m2, density: 60kg / m2, thickness: ~ 15mm, air permeability: 100-300L / m2 / s; and Solvent: n-hexane.
[0097] Implementation process: The aerogel particle is stirred and dispersed in solvent n-hexane to prepare a dispersion liquid with the mass concentration of 10wt% and the viscosity of 6.24cP. The dispersion liquid is added to the glass fiber felt, and the negative pressure is pumped to make the dispersion liquid fully impregnated. The glass fiber felt is naturally dried at room temperature for 24 hours, and then put into a 200°C oven for 12 hours.
[0098] Results: The final weight ratio of the aerogel particle to the whole material is 21wt%. The data of specific surface area of aerogel after immersion of the dispersion liquid and drying are shown in Table 1.Comparative Example 5:
[0099] Material: JIOS aerogel Company AeroVa® aerogel particle, particle size: D50< 50pm, density: 0.03-0. lg / cm3, porosity > 90%; Owens Corning Company glass fiber non-woven fabric, gram weight: - 60g / m2, thickness: - 0.6mm, air permeability: 3000 - 3100L / m2 / s; and Solvent: 75% water +25% ethanol.
[0100] Implementation process: The aerogel particle is stirred and dispersed in solvent to prepare a dispersion liquid with the mass concentration of 10wt% and the viscosity of 12.1cP. The dispersion liquid is added to the glass fiber felt, and the negative pressure is pumped to make the dispersion liquid fully impregnated. The glass fiber felt is naturally dried at room temperature for 24 hours, and then put into a 200°C oven for 12 hours.
[0101] Results: The final weight ratio of the aerogel particle to the whole material is 20wt%. The data of specific surface area of aerogel after immersion of the dispersion liquid and drying are shown in Table 1.
[0102] Table 1 shows the pore structure changes of Comparative Examples 3, 4 and 5 after solvent treatment of the aerogel particle. Compared with untreated AeroVa® aerogel particle, the aerogels samples in Comparative Examples 3, 4 and 5 all show a decrease in specific surface area to varying degrees, and the porosity, or pore volume, decreases significantly, indicating that the nanopore in the aerogel particle is damaged in different degrees.The collapse of the inner space of the nanopore causes the pore volume to become smaller and the specific surface area to decrease. The present invention prevents the problem that the structure of the aerogel particle is destroyed by solution treatment due to direct impregnation of the aerogel particle into the porous fiber material through the alternating electric field, such that the aerogel composite material of the invention has better performance.Table 1
[0103] In another aspect of the present invention, the inventor found that during subsequent packaging, transportation and use, the aerogel particle is prone to fall out from the aerogel composite material product, which in turn affects the performance and use effect of the aerogel composite material, and the fallen aerogel particle is also prone to pollute the environment.
[0104] In order to at least partially solve the above problems, reduce the fallout rate of the aerogel composite material, and thereby enhance the performance of the aerogel composite material, the inventors have found through a large number of studies and experiments that the use of aerogel particles with specific functional groups can at least partially solve the above technical problems.
[0105] The inventor has found through a large number of studies and experiments that if the aerogel particle used contains the silicon hydroxyl functional group (Si-OH) and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1, the fallout rate of the product prepared using such aerogel particle is significantly reduced, and the thermal insulating properties of the aerogel composite material are significantly improved. The method of preparing the product comprises, as defined in Examples 1-4 above, impregnating the aerogel particle into the porous fiber material by applying an alternating electric field to the porous fiber material.
[0106] It should be noted here that there is currently no unified national (China) or international standard to define the fallout rate or to specify a method for testing the rate. Especially in the field of aerogel products, there are not even any companies that disclose theirown standards and test methods either. Based on this situation, in order to show the technical effect brought by the present invention, the inventor himself has defined a test method to express the powder fallout rate, which is used to evaluate the powder fallout rate of the experimental examples and comparative examples in the embodiments, thereby reflecting that the powder fallout rate of the aerogel composite material manufactured by the technology disclosed in the present invention will be significantly reduced.
[0107] The test method is the nitrile glove friction test method, where the tester wears nitrile gloves (e.g., TOUCHNTUFF® 92-600) of composite standard GB 4806.9-2016 or ASTM D3578, and then slides and rubs the aerogel composite material with the size of A4 paper (210mm x 297mm) from left to right (or from right to left) three times. The amount of aerogel particle adsorbed on the nitrile glove is then observed and scored on a scale of 1 to 5 based on the amount adsorbed. Referring to FIG. 5, which shows the amount of aerogel particle adsorbed on the nitrile gloves after wiping different aerogel composite materials respectively, it can be seen that the amount of aerogel adsorbed on the left 1 figure is the most, with a score of 1, and the amount of aerogel adsorbed on the right 1 figure is the least, with a score of 5, i.e., the higher the score, the lower the powder fallout rate. The samples can basically be scored between 1 and 5 points. Through such comparative observation, it can also reflect that different samples have different powder fallout rates.
[0108] Furthermore, the present invention specifically discloses a method of manufacturing the aerogel composite material, wherein the method may comprise the following steps: impregnating aerogel particle into a porous fiber material by applying an alternating electric field, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; the voltage of the alternating electric field ranges from 0.1KV to 200KV, and the frequency ranges from 0.1HZ to 800HZ; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3, and the average particle size of the aerogel particle is less than or equal to 500pm.Example 5:Table 2
[0109] Samples 51 to 54 as well as samples 55 and 56 are treated with the same processing conditions and substrates, i.e., the same conditions except for the different aerogel powder particles used. As can be seen from Table 2, when the aerogel particle used contains the silicon hydroxyl functional group (Si-OH), the powder fallout rate of the aerogel composite material obtained by impregnating the aerogel particle into the CR33NI glass fiber non-woven felt or DL-2.6 thick felt through the same process conditions is significantly improved compared to the samples with the aerogel particle that does not contain the silicon hydroxyl functional group (Si-OH). For example, Sample 51 has a powder loss score of 1.0 and Sample 53 has a powder loss score of 5.0.
[0110] On the other hand, referring to FIG. 6, the infrared spectrum of the aerogel particle corresponding to the samples with significantly improved powder fallout rate has at least one absorption peak between 780cm'1and 820cm'1. For example, the LM aerogel particle has one absorption peak at 796cm'1; the Alison-Q aerogel particle has one absorption peak at 796cm'1; and the JIOS AEROVA®D50-500 aerogel particle has one absorption peak at 806cm'1. It can be seen that when the aerogel powder has an absorption peak between 780cm'1and 820cm'1, more specifically at 800 ± 10cm'1, the product prepared from this aerogel powder has a lower fallout rate. On the one hand, the absorption peak in this range may be formed due to the presence of the silicon hydroxyl functional group (Si-OH), and on the other, it is not excluded that it is formed by the combined effect of the other types of functional groups. In short, the presence of the silicon hydroxyl functional group (Si-OH) and the infrared spectrum with at least one absorption peak between 780cm'1and 820cm'1are two conditions that define the juxtaposition of probabilistic aerogel particles.
[0111] The detection conditions for infrared spectrum in this Example are as follows:
[0112] Spectrometer: Nicolet 6700 infrared spectrometer, ThermoFisher, USA;
[0113] Detector: DTGS KBr;
[0114] Resolution: 4.000,525 to 4000;
[0115] Sampling accessories: Smart iTR, ThermoFisher, USA.
[0116] In an optional embodiment, the aerogel particle containing the silicon hydroxyl functional group (Si-OH) and having the infrared spectrum with at least one absorption peak between 780cm'1and 820cm'1can be directly applicable to the method defined in any of the preceding embodiments, i.e., the aerogel particles in the preceding Examples 1-4 can be replaced with aerogel particles of this type. The voltage range of the alternating electric field, the selection of the porous fiber material, the additives in the aerogel particles, and the manner of applying the aerogel particles can be referred to in the description of the foregoing embodiments and will not be repeated herein.
[0117] The present invention further discloses aerogel particle. The aerogel particle contains the silicon hydroxyl functional group (Si-OH), and the infrared photoelectron spectroscopy of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3; and the average particle size of the aerogel particle is less than or equal to 500pm.
[0118] The present invention has been described through the above-mentioned embodiments, but it should be understood that the above-mentioned embodiments are only for the purpose of illustration and description, and are not intended to limit the present invention to the scope of the described embodiments. Furthermore, those skilled in the art can understand that the present invention is not limited to the above embodiments, and more variations and modifications can be made according to the teachings of the present invention. These variations and modifications fall within the protection scope of the present invention as defined in the appended claims and their equivalents.
Claims
WHAT IS CLAIMED IS:
1. An aerogel composite material, comprising: a porous fiber material; aerogel particle distributed within the porous fiber material, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm-l and 820cm-l; wherein the density of the aerogel particle ranges from 0.01g / cm3 to 0.5g / cm3, and the average particle size of the aerogel particle is less than or equal to 500pm.
2. The aerogel composite material of claim 1, wherein the aerogel particle, distributed within the porous fiber material, is impregnated into the porous fiber material by applying an alternating electric filed; the voltage of the alternating electric field ranges from 0.1KV to 50KV, and the frequency ranges from 1HZ to 800HZ; the application time of the alternating electric field ranges from 30 seconds to 5 minutes.
3. The aerogel composite material of claim 1, wherein the density of the aerogel particle ranges from 0.03g / cm3to O. lg / cm3, and the average particle size of the aerogel particle is less than or equal to 50pm.
4. The aerogel composite material of claim 1, wherein the porous fiber material is selected from a glass fiber felt, a glass fiber non-woven fabric, a glass fiber textile fabric, a ceramic fiber felt, a paper, a polyurethane fiber felt, a carbon fiber felt, a polypropylene fiber felt, a polypropylene and glass fiber composite felt, and a combination of the above.
5. The aerogel composite material of claim 4, wherein the areal density of the glass fiber non-woven fabric is between 20g / m2and 500g / m2; the thickness is between 0.3mm and 4mm; and the air permeability is between 200L / m2 / s and 3000L / m2 / s.
6. The aerogel composite material of claim 5, wherein the areal density of the glass fiber non-woven fabric is between 50g / m2and 150g / m2; the thickness is between 0.5mm and 1.5mm; and the air permeability is between 500L / m2 / s and 2000L / m2 / s.
7. The aerogel composite material of claim 6, wherein the areal density of the glass fiber non-woven fabric is between 90g / m2and 135g / m2; the thickness is between 0.8mm and 1.3mm; and the air permeability is between 1100L / m2 / s and 1800L / m2 / s.
8. The aerogel composite material of claim 4, wherein the polypropylene and glass fiber composite felt is made by blending a polypropylene fiber with a glass fiber; the density of the polypropylene and glass fiber composite felt is between 20kg / m3and 200kg / m3; and the thickness is between 1mm and 20mm.
9. The aerogel composite material of claim 8, wherein the density of the polypropylene and glass fiber composite felt is between 50kg / m3and 150kg / m3, and the thickness is between 3mm and 10mm.
10. The aerogel composite material of claim 1, wherein an additive for inhibiting thermal radiation is added to the aerogel particle, and the additive is selected from at least one of silicon carbide, boron carbide, titanium oxide and boron nitride; the weight ratio of the additive to the aerogel particle ranges from lwt% to 15wt%.
11. The aerogel composite material of claim 10, wherein the weight ratio of the additive to the aerogel particle ranges from 5wt% to 12wt%.
12. The aerogel composite material of claim 1, wherein the weight ratio of the aerogel particle to the aerogel composite material ranges from lwt% to 50wt%.
13. A method of manufacturing the aerogel composite material of any of claims 1 to 12, wherein the method comprises the following steps: impregnating aerogel particle into a porous fiber material by applying an alternating electric field, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3; and the average particle size of the aerogel particle is less than or equal to 500pm; wherein the voltage of the alternating electric field ranges from 0.1KV to 200KV, and the frequency ranges from 0.1HZ to 800HZ.
14. The method of claim 13, wherein the application time of the alternating electric field ranges from 30 seconds to 5 minutes.
15. The method of claim 13, a step is further comprised to apply the aerogel particle to a surface of the porous fiber material and / or applying the aerogel particle to a loader that is at least partially subject to the alternating electric field.
16. The method of claim 13, wherein the porous fiber material and the aerogel particle are arranged between a lower electrode and an upper electrode, and the electrode is electrically insulated from each other through a dielectric and connected to a power supply such that the porous fiber material and the aerogel particle are subject to the alternating electric field.
17. The method of claim 13, wherein the density of the aerogel particle ranges from 0.03g / cm3to O. lg / cm3, and the average particle size of the aerogel particle is less than or equal to 50pm.
18. The method of claim 13, wherein the porous fiber material is selected from a glass fiber felt, a glass fiber non-woven fabric, a glass fiber textile fabric, a ceramic fiber felt, a paper, a polyurethane fiber felt, a carbon fiber felt, a polypropylene fiber felt, a polypropylene and glass fiber composite felt, and a combination of the above.
19. The method of claim 18, wherein the areal density of the glass fiber non-woven fabric is between 20g / m2and 500g / m2; the thickness is between 0.3mm and 4mm; and the air permeability is between 200L / m2 / s and 3000L / m2 / s.
20. The method of claim 19, wherein the areal density of the glass fiber non-woven fabric is between 50g / m2and 150g / m2; the thickness is between 0.5mm and 1.5mm; and the air permeability is between 500L / m2 / s and 2000L / m2 / s.
21. The method of claim 20, wherein the areal density of the glass fiber non-woven fabric is between 90g / m2and 135g / m2; the thickness is between 0.8mm and 1.3mm; and the air permeability is between 1100L / m2 / s and 1800L / m2 / s.
22. The method of claim 18, wherein the polypropylene and glass fiber composite felt is made by blending a polypropylene fiber with a glass fiber; the density of the polypropylene and the glass fiber composite felt is between 20kg / m3and 200kg / m3; and the thickness is between 1mm and 20mm.
23. The method of claim 22, wherein the density of the polypropylene and glass fiber composite felt is between 50kg / m3and 150kg / m3, and the thickness is between 3mm and 10mm.
24. The method of claim 13, wherein an additive for inhibiting thermal radiation is added to the aerogel particle, and the additive is selected from at least one of silicon carbide, boron carbide, titanium oxide and boron nitride; the weight ratio of the additive to the aerogel particle ranges from lwt% to 15wt%.
25. The method of claim 24, wherein the weight ratio of the additive to the aerogel particle ranges from 5wt% to 12wt%.
26. Aerogel particle, wherein the aerogel particle contains a silicon hydroxyl functional group (Si-OH), and the infrared spectrum of the aerogel particle has at least one absorption peak between 780cm'1and 820cm'1; the density of the aerogel particle ranges from 0.01g / cm3to 0.5g / cm3; and the average particle size of the aerogel particle is less than or equal to 500pm.