Composition for preparing aerogel, aerogel as well as preparation method and application of aerogel
By using a composition containing components such as silica and rekinocyanide, the problems of insufficient electrostatic conduction and thermal stability of the existing aerogel are solved, and the effect of efficient release of electrostatic charge and high temperature stability is achieved.
Patent Information
- Application Number
- CN202311564966.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-22
- Publication Date
- 2025-05-23
AI Technical Summary
The electrostatic conductivity and thermal stability of existing aerogel materials are insufficient, making it difficult to effectively release the electrostatic charge on the surface of energy storage devices and maintain the structure stability at high temperatures.
Aerogel is prepared by specific reaction and mixing steps to enhance its electrostatic conduction properties and thermal stability using a composition comprising silica, rekinocyanol, formaldehyde, melamine, phenolic resin, furfural, composite conductive powder and solvating agent.
The prepared aerogel has low surface resistivity and excellent electrostatic conduction properties, which can effectively release the electrostatic charge in energy storage devices and maintain the structure stable at high temperatures. It is suitable for applications such as energy storage devices.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of aerogel materials, and in particular to a composition for preparing aerogel, aerogel and a preparation method and application thereof. Background Art
[0002] Aerogel, also known as dry gel, is a nanoporous material with pores filled with gaseous dispersion medium. It is known as the lightest solid in the world. Aerogel has the advantages of high porosity, high specific surface area, low density, and low thermal conductivity, and has attracted widespread attention. Due to these excellent properties of aerogel, it can be used in energy storage devices, thermal insulation materials, and space probes. There are many types of aerogels. The most widely studied and applied one is silica aerogel, which is a lightweight nanoporous amorphous solid material with a spatial network structure composed of cross-linked colloidal particles or polymer molecules.
[0003] At present, the conductivity of most common aerogels is poor, and most of the existing technologies focus on the thermal conductivity and specific surface area of silica aerogels, but not much research has been done on the electrostatic conductivity of aerogel materials.
[0004] In the field of energy storage devices, a large amount of static charge will accumulate when the energy storage devices collide and rub against the outside world. These static charges will accumulate on the surface. If they are not released, electric sparks will appear on the surface of the energy storage device, causing major accidents. Summary of the invention
[0005] The purpose of the present invention is to overcome the problems of poor electrostatic conductivity and poor thermal stability of aerogels in the prior art, and to provide a composition for preparing aerogels, aerogels, and a preparation method and application thereof. The aerogels described in the present invention have low surface resistivity and excellent thermal stability. When used in energy storage devices, they can well release static electricity accumulation on the surface of the energy storage devices, thereby ensuring the safe operation of the energy storage devices.
[0006] In order to achieve the above object, the present invention provides a composition for preparing aerogel, wherein the composition contains silicon dioxide, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, composite conductive powder and a solvent.
[0007] Preferably, the composition further contains N-hydroxymethyl acrylamide, dihydroxybenzoic acid, epoxy resin and defoaming agent.
[0008] Preferably, the composite conductive powder is obtained by mixing carbon nanotubes and metal oxides;
[0009] Preferably, in the composite conductive powder, the weight ratio of carbon nanotubes to metal oxides is 1-30:1.
[0010] Preferably, the ratio of the sum of the weight of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder is 100:5-20;
[0011] Preferably, the weight ratio of the composite conductive powder to the solvent is 1:1-5.
[0012] Preferably, the weight ratio of hydroquinone, formaldehyde and melamine is 1:1.2-2:1-2.
[0013] Preferably, the weight ratio of the composite conductive powder to the silicon dioxide is 0.5-3:1.
[0014] A second aspect of the present invention provides a method for preparing an aerogel, the method comprising the following steps:
[0015] (1) mixing the composite conductive powder with a solvent;
[0016] (2) in the presence of a catalyst, mixing hydroquinone, formaldehyde, melamine, phenolic resin and furfural to react;
[0017] (3) mixing the material obtained in step (2) with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoaming agent in sequence;
[0018] (4) The material obtained in step (3) is mixed with silicon dioxide, and then the pH value is adjusted to 1-3, followed by heat treatment.
[0019] Preferably, in step (2), the reaction conditions include: temperature of 60-100° C. and time of 1-12 h.
[0020] Preferably, in step (2), the catalyst is selected from NaOH, KOH, H 2 SO 4 or HCl.
[0021] Preferably, in step (3), the mixing conditions include: temperature of 20-100° C. and time of 2-12 h.
[0022] Preferably, in step (3), the atmosphere during the mixing is an inert atmosphere;
[0023] Preferably, the inert atmosphere is selected from a nitrogen atmosphere, an argon atmosphere or a helium atmosphere.
[0024] Preferably, the ratio of the sum of the weight of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder is 100:5-20;
[0025] Preferably, the weight ratio of the composite conductive powder to the solvent is 1:1-5;
[0026] Preferably, the weight ratio of hydroquinone, formaldehyde and melamine is 1:1.2-2:1-2;
[0027] Preferably, the composite conductive powder is obtained by mixing carbon nanotubes and metal oxides;
[0028] Preferably, the weight ratio of the carbon nanotubes to the metal oxide is 1-30:1.
[0029] Preferably, the weight ratio of the composite conductive powder to the silicon dioxide is 0.5-3:1.
[0030] Preferably, the temperature of the heat treatment is 40-80° C., and the time of the heat treatment is 1-4 hours.
[0031] A third aspect of the present invention provides an aerogel prepared by the above preparation method.
[0032] A fourth aspect of the present invention provides the above composition for preparing aerogel or use of the above aerogel in an energy storage device.
[0033] The aerogel prepared by using the composition of the present invention has a lower surface resistivity and better electrostatic conductivity, and can well release the static charge in the energy storage element. In addition, the aerogel of the present invention also has excellent thermal stability, and can still maintain structural stability after the temperature exceeds 500°C, and has a broader application prospect. DETAILED DESCRIPTION
[0034] The specific embodiments of the present invention are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.
[0035] The endpoints and any values of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, the endpoint values of each range and the individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.
[0036] The invention provides a composition for preparing aerogel, wherein the composition contains silicon dioxide, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, composite conductive powder and a solvent.
[0037] In the present invention, a polymer of phenolic resin can be prepared through the coordination of hydroquinone, formaldehyde, melamine, phenolic resin and furfural, so that the carbon skeleton of the prepared aerogel is more stable and has better thermal stability.
[0038] In the present invention, the silicon dioxide is used to maintain the stability of the prepared aerogel skeleton, so that the prepared aerogel is not prone to collapse during use, thereby ensuring the normal use of the aerogel.
[0039] In the present invention, the composite conductive powder is used to increase the conductivity of the aerogel, so that the prepared aerogel can be better applied in the field of energy storage devices. The solvent is used to fully dissolve and disperse the composite conductive powder, so as to facilitate better subsequent application.
[0040] In the present invention, the composition further contains N-hydroxymethyl acrylamide, dihydroxybenzoic acid, epoxy resin and defoamer. Specifically, the N-hydroxymethyl acrylamide and dihydroxybenzoic acid are solvents used by the reactants, which are used to dissolve the reactants to facilitate the reaction to prepare aerogel; the defoamer is a common functional auxiliary agent in the art, which is used to defoam the reaction system.
[0041] In the present invention, the composition may further contain titanium dioxide slurry to promote uniform mixing of materials.
[0042] In a preferred embodiment, the composite conductive powder is obtained by mixing carbon nanotubes with metal oxides. Specifically, the metal oxides may be any type of metal oxides commonly used in the art, for example, Fe 2 O 3 , CuO, MgO, ZnO and PtO 2 One or more of the following.
[0043] In a preferred embodiment, in the composite conductive powder, the weight ratio of carbon nanotubes to metal oxides is 1-30: 1, preferably 3-10: 1. Specifically, the weight ratio of carbon nanotubes to metal oxides is 1: 1, 5: 1, 10: 1, 15: 1, 20: 1, 25: 1 or 30: 1.
[0044] In a preferred embodiment, the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder is 100:5-20, preferably 100:5-16. Specifically, the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder can be 100:5, 100:10, 100:15 or 100:20.
[0045] In a preferred embodiment, the weight ratio of the composite conductive powder to the solvent is 1:1-5, preferably 1:1-3. Specifically, the weight ratio of the composite conductive powder to the solvent may be 1:1, 1:2, 1:3, 1:4 or 1:5.
[0046] In a preferred embodiment, the weight ratio of hydroquinone, formaldehyde and melamine is 1:1.2-2:1-2. In the present invention, the amount of phenolic resin and furfural is not limited.
[0047] In a preferred embodiment, the weight ratio of the composite conductive powder to the silicon dioxide is 0.5-3: 1, preferably 0.5-2: 1. Specifically, the weight ratio of the composite conductive powder to the silicon dioxide can be 0.5: 1, 1: 1, 1.5: 1, 2: 1, 2.5: 1 or 3: 1.
[0048] In a specific embodiment, the weight ratio of N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoaming agent is 0.1-5:0.5-10:1:0.1-5:1-15:0.01-1, preferably 1-3:1-5:1:1-3:2-6:0.1-0.6.
[0049] The present invention further provides a method for preparing an aerogel, the method comprising the following steps:
[0050] (1) mixing the composite conductive powder with a solvent;
[0051] (2) in the presence of a catalyst, mixing hydroquinone, formaldehyde, melamine, phenolic resin and furfural to react;
[0052] (3) mixing the material obtained in step (2) with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoaming agent in sequence;
[0053] (4) The material obtained in step (3) is mixed with silicon dioxide, and then the pH value is adjusted to 1-3, followed by heat treatment.
[0054] In a specific embodiment, in step (1), the composite conductive powder and the solvent can be mixed by ultrasonic mixing or stirring mixing to uniformly disperse the composite conductive powder in the solvent.
[0055] In a specific embodiment, the solvent is a common organic solvent in the art that can dissolve and disperse, and is used to fully disperse the composite conductive powder in the composition to ensure uniform mixing and reaction. It can be a common solvent auxiliary agent in the art that can play a dissolving role, for example, it can be ether, acetone, xylene, methanol, or methyl sulfoxide.
[0056] In a specific embodiment, in step (2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted to obtain a more stable carbon skeleton structure.
[0057] In a specific embodiment, in step (2), the catalyst is selected from NaOH, KOH, H 2 SO 4 or HCl.
[0058] In a preferred embodiment, the ratio of the sum of the weight of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst is 100:1-5.
[0059] In the present invention, in step (2), the catalyst can be directly dissolved in a mixed system of hydroquinone, formaldehyde, melamine, phenolic resin and furfural, followed by a reaction.
[0060] In a preferred embodiment, in step (2), the reaction conditions include: a temperature of 60-100°C and a reaction time of 1-12 hours. Specifically, the reaction temperature may be 60°C, 70°C, 80°C, 90°C or 100°C; and the reaction time may be 1 hour, 2 hours, 5 hours, 8 hours, 10 hours or 12 hours.
[0061] In a specific embodiment, in step (3), the material obtained in step (2) is sequentially mixed with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoaming agent. The mixed materials will react during the mixing process. The specific mixing temperature is the temperature at which the reaction occurs, and the mixing time is the time for the overall reaction to occur.
[0062] In a specific embodiment, the weight ratio of N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoaming agent is 0.1-5:0.5-10:1:0.1-5:1-15:0.01-1, preferably 1-3:1-5:1:1-3:2-6:0.1-0.6.
[0063] In a specific embodiment, the defoamer can be a common defoamer type in the art, for example, a silicone oil defoamer. The epoxy resin can be a common commercial product, for example, an epoxy resin purchased from Dow, Hexion Chemical Company, Huntsman, and BASF.
[0064] In a specific embodiment, in step (3), the mixing conditions include: a temperature of 20-100°C and a time of 2-12 hours. Specifically, the mixing temperature can be 20°C, 30°C, 40°C, 50°C, 60°C, 70°C, 80°C, 90°C or 100°C; and the mixing time can be 2h, 5h, 8h, 10h or 12h.
[0065] In a preferred embodiment, in step (3), the mixing atmosphere is an inert atmosphere; the inert atmosphere is selected from a nitrogen atmosphere, an argon atmosphere or a helium atmosphere.
[0066] In a preferred embodiment, the composite conductive powder is obtained by mixing carbon nanotubes with metal oxides. Specifically, the metal oxides may be any type of metal oxides commonly used in the art, for example, Fe 2 O 3 , CuO, MgO, ZnO and PtO 2 One or more of the following.
[0067] In a preferred embodiment, the weight ratio of carbon nanotubes to metal oxides is 1-30: 1, preferably 3-10: 1. Specifically, the weight ratio of carbon nanotubes to metal oxides is 1: 1, 5: 1, 10: 1, 15: 1, 20: 1, 25: 1 or 30: 1.
[0068] In a preferred embodiment, the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder is 100:5-20, preferably 100:5-16. Specifically, the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder can be 100:5, 100:10, 100:15 or 100:20.
[0069] In a preferred embodiment, the weight ratio of the composite conductive powder to the solvent is 1:1-5, preferably 1:1-3. Specifically, the weight ratio of the composite conductive powder to the solvent may be 1:1, 1:2, 1:3, 1:4 or 1:5.
[0070] In a preferred embodiment, the weight ratio of hydroquinone, formaldehyde and melamine is 1:1.2-2:1-2. In the present invention, the amount of phenolic resin and furfural is not limited.
[0071] In a preferred embodiment, the weight ratio of the composite conductive powder to the silicon dioxide is 0.5-3: 1, preferably 0.5-2: 1. Specifically, the weight ratio of the composite conductive powder to the silicon dioxide can be 0.5: 1, 1: 1, 1.5: 1, 2: 1, 2.5: 1 or 3: 1.
[0072] In a preferred embodiment, the heat treatment temperature is 40-80°C, and the heat treatment time is 1-4 hours. Specifically, the heat treatment temperature can be 40°C, 50°C, 60°C, 70°C or 80°C; and the heat treatment time can be 1 hour, 2 hours, 3 hours or 4 hours.
[0073] The present invention further provides an aerogel prepared by the above preparation method. The aerogel further enhances the electrostatic conductivity of the aerogel by using composite conductive powder, and is compounded by a skeleton generated by the reaction of silicon dioxide and hydroquinone, formaldehyde, melamine, phenolic resin and furfural, so that the skeleton of the prepared aerogel is stronger and the stability performance at high temperature is more excellent.
[0074] The present invention may also provide the above composition for preparing aerogel or use of the above aerogel in an energy storage device.
[0075] The present invention will be described in detail below through examples, but the protection scope of the present invention is not limited thereto.
[0076] The experimental methods in the following examples, unless otherwise specified, are all conventional methods in the art. The experimental materials used in the following examples, unless otherwise specified, are all commercially available.
[0077] The solvent used in the examples and comparative examples is methanol; the defoaming agent selected is Tween 80.
[0078] Example 1
[0079] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:0.5:1:1:1.5:1.5:1.5:1.5:2:3:1:2:4:0.5;
[0080] The preparation method of aerogel comprises the following steps:
[0081] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and CuO in a weight ratio of 5:1) with a solvent;
[0082] (2) in the presence of a catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst KOH is 100:2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 60° C. and a reaction time of 5 h;
[0083] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 65° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0084] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 1, and then the obtained material is heat treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0085] Example 2
[0086] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:1:1:1:1.5:1.5:1.5:1.5:2:3:1:2:4:0.5;
[0087] The preparation method of aerogel comprises the following steps:
[0088] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and MgO in a weight ratio of 10:1) with a solvent;
[0089] (2) in the presence of catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of catalyst KOH is 100:2.5), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 70° C. and a reaction time of 5.5 h;
[0090] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 82° C., the mixing time is 5 h, and the mixing atmosphere is nitrogen atmosphere;
[0091] (4) The material obtained in step (3) is uniformly mixed with silicon dioxide, and then the pH value of the mixed material is adjusted to 1.5, and then the obtained material is heat-treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0092] Example 3
[0093] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, and the weight ratio is 1:0.5:1:1:2:1.5:1.5:1.5:2:3:1:2:4:0.5;
[0094] The preparation method of aerogel comprises the following steps:
[0095] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and ZnO in a weight ratio of 8:1) with a solvent;
[0096] (2) in the presence of a catalyst NaOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst NaOH is 100:3), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 85° C. and a reaction time of 6.5 h;
[0097] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 75° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0098] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 2, and then the obtained material is heat-treated for 3 hours at a temperature of 80° C. After the heat treatment, an aerogel material can be obtained.
[0099] Example 4
[0100] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, and the weight ratio is 1:1:1:1:2:1.5:1.5:1.5:2:3:1:2:4:0.5;
[0101] The preparation method of aerogel comprises the following steps:
[0102] (1) Composite conductive powder (composed of carbon nanotubes and Co 3 O 4 Mix the mixture in a weight ratio of 9:1 with a solvent and mix well;
[0103] (2) in the presence of a catalyst HCl (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst HCl is 100:2.5), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 80° C. and a reaction time of 7 h;
[0104] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 90° C., the mixing time is 5 h, and the mixing atmosphere is argon atmosphere;
[0105] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 2, and then the obtained material is heat-treated for 3 hours at a temperature of 80° C. After the heat treatment, an aerogel material can be obtained.
[0106] Example 5
[0107] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:1:1:1:1.5:1:1.5:1.5:2:3:1:2:4:0.5;
[0108] The preparation method of aerogel comprises the following steps:
[0109] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and ZnO in a weight ratio of 8:1) with a solvent;
[0110] (2) in the presence of a catalyst HCl (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst HCl is 100:3), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 90° C. and a reaction time of 8 h;
[0111] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 80° C., the mixing time is 5 h, and the mixing atmosphere is nitrogen atmosphere;
[0112] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 2.8, and then the obtained material is heat treated for 3 hours at a temperature of 80° C. After the heat treatment, an aerogel material can be obtained.
[0113] Example 6
[0114] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:1:1:1:1.5:1.5:1:1.5:2:3:1:2:4:0.5;
[0115] The preparation method of aerogel comprises the following steps:
[0116] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and CuO in a weight ratio of 5:1) with a solvent;
[0117] (2) in the presence of a catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst KOH is 100:2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 60° C. and a reaction time of 5 h;
[0118] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 65° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0119] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 1, and then the obtained material is heat treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0120] Example 7
[0121] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:1:1:1:1.5:1.5:1.5:1:2:3:1:2:4:0.5;
[0122] The preparation method of aerogel comprises the following steps:
[0123] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and CuO in a weight ratio of 5:1) with a solvent;
[0124] (2) in the presence of a catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst KOH is 100:2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 60° C. and a reaction time of 5 h;
[0125] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 65° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0126] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 1, and then the obtained material is heat treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0127] Example 8
[0128] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:0.5:1:1:1.5:1.5:1.5:1.5:2:3:1:2:10:0.5;
[0129] The preparation method of aerogel comprises the following steps:
[0130] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and CuO in a weight ratio of 5:1) with a solvent;
[0131] (2) in the presence of a catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst KOH is 100:2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 60° C. and a reaction time of 5 h;
[0132] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 65° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0133] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 1, and then the obtained material is heat treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0134] Example 9
[0135] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:1:1:1:1.5:1.5:1.5:1.5:2:3:1:2:10:0.5;
[0136] The preparation method of aerogel comprises the following steps:
[0137] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and CuO in a weight ratio of 5:1) with a solvent;
[0138] (2) in the presence of a catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst KOH is 100:2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 60° C. and a reaction time of 5 h;
[0139] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 65° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0140] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 1, and then the obtained material is heat treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0141] Example 10
[0142] The composition for preparing aerogel comprises: silicon dioxide, composite conductive powder, solvent, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin, defoamer, with a weight ratio of 1:0.5:1:1:1.5:1.5:1.5:1.5:2:3:1:2:4:1;
[0143] The preparation method of aerogel comprises the following steps:
[0144] (1) mixing a composite conductive powder (obtained by mixing carbon nanotubes and CuO in a weight ratio of 5:1) with a solvent;
[0145] (2) in the presence of a catalyst KOH (the ratio of the sum of the weights of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the catalyst KOH is 100:2), hydroquinone, formaldehyde, melamine, phenolic resin and furfural are mixed and reacted at a reaction temperature of 60° C. and a reaction time of 5 h;
[0146] (3) the material obtained in step (2) is mixed in sequence with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoamer, the mixing temperature is 65° C., the mixing time is 6 h, and the mixing atmosphere is nitrogen atmosphere;
[0147] (4) The material obtained in step (3) is mixed evenly with silicon dioxide, and then the pH value of the mixed material is adjusted to 1, and then the obtained material is heat treated for 3 hours at a temperature of 70° C. After the heat treatment, an aerogel material can be obtained.
[0148] Comparative Example 1
[0149] The method of Example 1 was followed, except that the composite conductive agent was replaced with an equal weight of silicon dioxide.
[0150] Comparative Example 2
[0151] The method of Example 1 was followed, except that no silicon dioxide was used for the preparation.
[0152] Test Case
[0153] The properties of the aerogels prepared in the examples and comparative examples were tested.
[0154] Specific surface area: The specific surface area of the aerogel was tested by the BET method, and the results are shown in Table 1;
[0155] Surface resistivity: The electrical conductivity of the aerogel was tested using a resistivity tester, and the results are shown in Table 1;
[0156] Thermal conductivity: The thermal conductivity of aerogel was tested using a thermal conductivity meter, and the results are shown in Table 1;
[0157] Thermal stability temperature: The thermal stability temperature of the aerogel material was tested using a thermogravimetric analyzer, where the thermal stability temperature refers to the temperature at which the weight of the material remains constant at high temperature during the thermogravimetric test. The results are shown in Table 1.
[0158] Table 1
[0159]
[0160]
[0161] It can be seen from the results in Table 1 that the aerogel of the present invention has excellent electrical conductivity and thermal stability, can be better used in energy storage devices to release the accumulated static charge, and has broader application prospects.
[0162] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.
Claims
1. A composition for preparing an aerogel, It is characterized in that The composition contains silicon dioxide, hydroquinone, formaldehyde, melamine, phenolic resin, furfural, composite conductive powder and a solvent.
2. The composition according to claim 1, It is characterized in that The composition also contains N-hydroxymethyl acrylamide, dihydroxybenzoic acid, epoxy resin and defoaming agent.
3. The composition according to claim 1, It is characterized in that The composite conductive powder is obtained by mixing carbon nanotubes and metal oxides; Preferably, in the composite conductive powder, the weight ratio of carbon nanotubes to metal oxides is 1-30:
1.
4. The composition according to claim 1, It is characterized in that The ratio of the sum of the weight of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder is 100:5-20; Preferably, the weight ratio of the composite conductive powder to the solvent is 1:1-5.
5. The composition according to claim 1, It is characterized in that The weight ratio of hydroquinone, formaldehyde and melamine is 1:1.2-2:1-2.
6. The composition according to claim 1, It is characterized in that The weight ratio of the composite conductive powder to the silicon dioxide is 0.5-3:
1.
7. A method for preparing an aerogel, It is characterized in that The preparation method comprises the following steps: (1) mixing the composite conductive powder with a solvent; (2) in the presence of a catalyst, mixing hydroquinone, formaldehyde, melamine, phenolic resin and furfural to react; (3) mixing the material obtained in step (2) with the material obtained in step (1), N-hydroxymethyl acrylamide, p-cresol, m-cresol, dihydroxybenzoic acid, epoxy resin and defoaming agent in sequence; (4) The material obtained in step (3) is mixed with silicon dioxide, and then the pH value is adjusted to 1-3, followed by heat treatment.
8. The method for preparing aerogel according to claim 7, It is characterized in that In step (2), the reaction conditions include: temperature of 60-100° C. and time of 1-12 h.
9. The method for preparing the aerogel according to claim 7. It is characterized in that In step (2), the catalyst is selected from NaOH, KOH, H 2 SO 4 or HCl.
10. The method for preparing aerogel according to claim 7, It is characterized in that In step (3), in step (3), the mixing conditions include: temperature of 20-100° C. and time of 2-12 h.
11. The method for preparing aerogel according to claim 7 or 10, It is characterized in that In step (3), the atmosphere during the mixing is an inert atmosphere; Preferably, the inert atmosphere is selected from a nitrogen atmosphere, an argon atmosphere or a helium atmosphere.
12. The method for preparing aerogel according to claim 7, It is characterized in that The ratio of the sum of the weight of hydroquinone, formaldehyde, melamine, phenolic resin and furfural to the weight of the composite conductive powder is 100:5-20; Preferably, the weight ratio of the composite conductive powder to the solvent is 1:1-5; Preferably, the weight ratio of hydroquinone, formaldehyde and melamine is 1:1.2-2:1-2; Preferably, the composite conductive powder is obtained by mixing carbon nanotubes and metal oxides; Preferably, the weight ratio of the carbon nanotubes to the metal oxide is 1-30:
1.
13. The method for preparing aerogel according to claim 7, It is characterized in that The weight ratio of the composite conductive powder to the silicon dioxide is 0.5-3:
1.
14. The method for preparing aerogel according to claim 7, It is characterized in that The temperature of the heat treatment is 40-80° C., and the time of the heat treatment is 1-4 hours.
15. An aerogel prepared by the method for preparing aerogel according to any one of claims 7 to 14.
16. Use of the composition for preparing aerogel according to any one of claims 1 to 6 or the aerogel according to claim 15 in an energy storage device.