Synthetic fiber felt-polymer aerogel composite material and preparation and application thereof, and high-temperature-resistant emergency oil wick and preparation and application thereof
The emergency oil core made of synthetic fiber felt and polymer aerogel composite material solves the problem of poor high temperature resistance of existing emergency oil cores, and realizes continuous oil supply under high temperature conditions, thus extending the stable operation time of the transmission system.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- LANZHOU INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
- Filing Date
- 2025-01-15
- Publication Date
- 2026-05-29
AI Technical Summary
Existing emergency oil cores have poor high-temperature resistance, which causes transmission components to heat up and fail rapidly after losing lubrication, increasing the difficulty of equipment design and manufacturing, and making them unsuitable for transmission systems with special spatial dimensions.
The core is made of synthetic fiber felt and polymer aerogel composite material, including polyimide aerogel, polyether ether ketone aerogel or polyphenylene sulfide aerogel, through impregnation and cross-linking reaction, and lubricating oil is adsorbed to form a high-temperature resistant emergency oil core.
The high-temperature resistance of the emergency oil core has been improved, enabling it to continuously supply lubricating oil under high-temperature conditions, extending the stable operation time of the transmission system and reducing the risk of equipment downtime.
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Figure CN119798991B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of emergency oil core technology, and in particular to a synthetic fiber felt-polymer aerogel composite material and its preparation and application, and a high-temperature resistant emergency oil core and its preparation and application. Background Technology
[0002] The safe and continuous operation of the lubrication system for transmission components is crucial. Without lubrication, the transmission components will quickly enter a dry-running state. This leads to continuous temperature increases, exacerbating the seizing and failure of the transmission components. To avoid this, an additional lubrication system and device are typically installed, which undoubtedly increases the overall design and manufacturing complexity of the equipment and adds to the weight of the entire transmission system, making it difficult to meet the requirements of some transmission systems with special space constraints. Therefore, developing an emergency lubrication core can effectively avoid this problem. Existing technology discloses a polyurethane emergency lubrication core, but polyurethane emergency lubrication cores have poor high-temperature resistance. Summary of the Invention
[0003] In view of this, the purpose of this invention is to provide a synthetic fiber felt-polymer aerogel composite material, its preparation and application, and a high-temperature resistant emergency oil core, its preparation and application. The synthetic fiber felt-polymer aerogel composite material provided by this invention exhibits good high-temperature resistance. By forming the core of the synthetic fiber felt-polymer aerogel composite material and adsorbing base oil, the resulting emergency oil core possesses excellent high-temperature resistance.
[0004] To achieve the above-mentioned objectives, the present invention provides the following technical solution:
[0005] The present invention provides a synthetic fiber felt-polymer aerogel composite material, comprising a synthetic fiber felt and a polymer aerogel filling the pores of the synthetic fiber felt, wherein the polymer aerogel comprises polyimide aerogel, polyetheretherketone aerogel or polyphenylene sulfide aerogel.
[0006] Preferably, the pore size of the synthetic fiber felt is 10-100 μm and the porosity is 20-80%.
[0007] Preferably, when the polymer aerogel is a polyimide aerogel, the polyimide aerogel is prepared from a polyimide aerogel solution; the raw materials for preparing the polyimide aerogel solution include the following components: diamine monomer, dianhydride monomer, crosslinking agent, dehydrating agent, catalyst, and organic solvent;
[0008] The total mass of the diamine monomer, dianhydride monomer, and crosslinking agent accounts for 5 to 20% of the total mass of the diamine monomer, dianhydride monomer, crosslinking agent, and organic solvent.
[0009] Preferably, the molar ratio of the diamine monomer to the crosslinking agent is 1:0 to 0.07, and the molar amount of the crosslinking agent is not 0.
[0010] Preferably, the diamine monomer comprises one or more of 4,4'-diaminodiphenyl ether, p-phenylenediamine, 4,4'-diaminodiphenylmethane, 4,4'-diaminobenzophenone, and 4,4'-diaminodicyclohexylmethane;
[0011] The dianhydride monomers include one or more of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride, pyromellitic dianhydride, hexafluorodianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride, diphenyl methyl ether tetracarboxylic dianhydride, and bisphenol A type dianhydride;
[0012] The crosslinking agent includes one or more of hexamethylene diisocyanate trimer (N3300), tris(4-aminophenyl)amine, 1,3,5-tris(4-aminophenyl)benzene, and 1,3,5-tris(4-aminophenyl)triazine.
[0013] Preferably, the dehydrating agent comprises acetic anhydride;
[0014] The catalyst includes pyridine;
[0015] The organic solvent includes N,N-dimethylacetamide.
[0016] This invention also provides a method for preparing the synthetic fiber felt-polymer aerogel composite material described in the above technical solution, comprising the following steps:
[0017] The synthetic fiber felt was immersed in a polymer aerogel solution. After complete immersion, the synthetic fiber felt was removed and drained, and then a crosslinking reaction was carried out to obtain the synthetic fiber felt-polymer aerogel composite material.
[0018] The present invention also provides a high-temperature resistant emergency oil core, comprising a core and lubricating oil adsorbed in the core; the core is made of the synthetic fiber felt-polymer aerogel composite material described in the above technical solution.
[0019] This invention also provides a method for preparing the high-temperature resistant emergency oil core described in the above technical solution, comprising the following steps:
[0020] The core is immersed in lubricating oil to obtain the high-temperature resistant emergency oil core;
[0021] The oil immersion temperature is 50–120°C, the time is 8–48 hours, and the oil immersion is carried out under vacuum conditions.
[0022] The present invention also provides the application of the synthetic fiber felt-polymer aerogel composite material or the high-temperature resistant emergency oil core described above in the transmission system.
[0023] The present invention provides a synthetic fiber felt-polymer aerogel composite material, comprising a synthetic fiber felt and a polymer aerogel filling the pores of the synthetic fiber felt, wherein the polymer aerogel comprises polyimide aerogel, polyetheretherketone aerogel or polyphenylene sulfide aerogel.
[0024] The synthetic fiber felt-polymer aerogel composite material provided by this invention combines high-temperature resistant synthetic fiber felt with high-temperature resistant polymer aerogel (polyimide aerogel, polyetheretherketone aerogel, or polyphenylene sulfide aerogel), thus improving the high-temperature resistance of the composite material. Specifically, the synthetic fiber felt possesses high-temperature resistance; the polymer aerogel not only has good temperature resistance but also provides abundant porous structures to store lubricating oil. Using the synthetic fiber felt-polymer aerogel composite material provided by this invention as the core, an emergency oil core can be prepared. This core can not only withstand the temperature rise caused by continuous poor lubrication but also provide a continuous and stable supply of lubricating oil, thereby preventing rapid failure of moving parts in a short period and ensuring stable operation for a certain period. The synthetic fiber felt-polymer aerogel composite material provided by this invention exhibits excellent high-temperature resistance.
[0025] Furthermore, this invention limits the total mass of the diamine monomer, dianhydride monomer, and crosslinking agent to 5-20% of the total mass of the diamine monomer, dianhydride monomer, crosslinking agent, and organic solvent, i.e., the solid content is 5-20%; and the molar ratio of the diamine monomer to the crosslinking agent is 1:0-0.07, and the molar amount of the crosslinking agent is not 0. This ensures that the polyimide aerogel still has an excellent oil penetration rate after being subjected to high temperatures. Using the above-mentioned synthetic fiber felt-polymer aerogel composite material as the core, the prepared emergency oil core can continuously and stably provide lubricating oil to the bearing under the action of centrifugal force during the rotation of the shaft when the transmission system's oil supply and lubrication system cannot work normally. Compared with other oil core materials, it prolongs the stable operation of the transmission system for a certain period of time, provides more operating space for the staff, and reduces the risk of equipment downtime. Attached Figure Description
[0026] Figure 1 The oil seepage rate of the emergency oil cores obtained in Examples 1-12;
[0027] Figure 2 Thermal decomposition curves of commercially available wool felt, wool felt-polyurethane composite material, synthetic fiber felt, and synthetic fiber felt-PI aerogel composite material obtained in Example 2 are shown.
[0028] Figure 3 The oil seepage rate of the emergency oil core obtained in Example 2 before and after high-temperature treatment. Detailed Implementation
[0029] The present invention provides a synthetic fiber felt-polymer aerogel composite material, comprising a synthetic fiber felt and a polymer aerogel filling the pores of the synthetic fiber felt, wherein the polymer aerogel comprises polyimide aerogel, polyetheretherketone aerogel or polyphenylene sulfide aerogel.
[0030] In this invention, unless otherwise specified, all raw materials used are preferably commercially available products.
[0031] The synthetic fiber felt-polymer aerogel composite material provided by this invention includes a synthetic fiber felt. The pore size of the synthetic fiber felt is preferably 10–100 μm, specifically 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, or 100 μm; the porosity is preferably 20–80%, specifically 20%, 30%, 40%, 50%, 60%, 70%, 75%, or 80%. In this invention, the material of the synthetic fiber felt is preferably one or more of meta-aramid (Nomex), para-aramid (Kevlar), polyphenylene ether, and polyimide, more preferably meta-aramid (Nomex).
[0032] The synthetic fiber felt-polymer aerogel composite material provided by this invention includes a polymer aerogel filling the pores of the synthetic fiber felt. The polymer aerogel includes polyimide aerogel, polyetheretherketone aerogel, or polyphenylene sulfide aerogel, preferably polyimide aerogel. In this invention, when the polymer aerogel is a polyimide aerogel, the polyimide aerogel is preferably prepared from a polyimide aerogel solution. The raw materials for preparing the polyimide aerogel solution preferably include the following components: diamine monomer, dianhydride monomer, crosslinking agent, dehydrating agent, catalyst, and organic solvent.
[0033] In this invention, the diamine monomer preferably includes one or more of 4,4'-diaminodiphenyl ether (ODA), p-phenylenediamine, 4,4'-diaminodiphenylmethane (MDA), 4,4'-diaminobenzophenone (DABP), and 4,4'-diaminodicyclohexylmethane (PACM), and more preferably 4,4'-diaminodiphenyl ether (ODA).
[0034] In this invention, the dianhydride monomer preferably includes one or more of 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), pyromellitic dianhydride (PMDA), hexafluorodianhydride (6FDA), 3,3',4,4'-benzophenone tetracarboxylic dianhydride (BTDA), diphenyl methyl ether tetracarboxylic dianhydride, and bisphenol A dianhydride (BEPA), and more preferably 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA).
[0035] In this invention, the crosslinking agent preferably includes one or more of hexamethylene diisocyanate trimer (N3300), tris(4-aminophenyl)amine, 1,3,5-tris(4-aminophenyl)benzene and 1,3,5-tris(4-aminophenyl)triazine, and more preferably N3300.
[0036] In this invention, the dehydrating agent preferably includes acetic anhydride.
[0037] In this invention, the catalyst preferably comprises pyridine.
[0038] In this invention, the organic solvent preferably includes N,N-dimethylacetamide (DMAc).
[0039] In this invention, the molar ratio of the diamine monomer and the dianhydride monomer is preferably 1:1.1.
[0040] In this invention, the molar ratio of the diamine monomer to the crosslinking agent is preferably 1:0 to 0.07, and the molar amount of the crosslinking agent is not 0. More preferably, it is 1:0.001 to 0.07, even more preferably, it is 1:0.01 to 0.07, and specifically preferably, it is 1:0.0678, 1:0.0387 or 1:0.0136.
[0041] In this invention, the total mass of the diamine monomer, dianhydride monomer, and crosslinking agent preferably accounts for 5-20% (which may be referred to as solid content) of the total mass of the diamine monomer, dianhydride monomer, crosslinking agent, and organic solvent, specifically preferably 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20%.
[0042] In this invention, the degree of crosslinking of the polyimide aerogel solution is preferably 20% to 100%, specifically preferably 100%, 60%, or 20%. In this invention, the degree of crosslinking of the polyimide aerogel solution is preferably calculated according to the following formula:
[0043]
[0044] In this invention, the degree of crosslinking and solid content affect the degree of crosslinking and pore structure of the diamine monomer and dianhydride monomer, thereby affecting the lubricant release rate of the obtained synthetic fiber felt-polymer aerogel composite material.
[0045] In this invention, the molar ratio of the dianhydride monomer to the dehydrating agent is preferably 1:4 to 16, and more preferably 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15 or 1:16.
[0046] In this invention, the molar ratio of the dianhydride monomer to the catalyst is preferably 1:4 to 16, and more preferably 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15 or 1:16.
[0047] In this invention, the method for preparing the polyimide aerogel solution is preferably described in the section on the preparation method of the synthetic fiber felt-polymer aerogel composite material, and will not be repeated here.
[0048] This invention also provides a method for preparing the synthetic fiber felt-polymer aerogel composite material described in the above technical solution, comprising the following steps:
[0049] The synthetic fiber felt was immersed in a polymer aerogel solution. After complete immersion, the synthetic fiber felt was removed and drained, and then a crosslinking reaction was carried out to obtain the synthetic fiber felt-polymer aerogel composite material.
[0050] In this invention, the synthetic fiber felt is preferably pretreated before use. The pretreatment preferably includes cutting, washing, and drying in sequence. This invention does not specifically limit the cutting process, and those skilled in the art can set it according to actual needs. The washing reagent is preferably ethanol. This invention does not specifically limit the number of washings or the amount of washing reagent, as long as impurities can be removed cleanly.
[0051] In this invention, when the polymer aerogel is a polyimide aerogel, the method for preparing the polyimide aerogel solution preferably includes the following steps:
[0052] Under nitrogen atmosphere, diamine monomer is weighed and dissolved in an organic solvent, and then dianhydride monomer and crosslinking agent are added sequentially to obtain a mixed system; a dehydrating agent and a catalyst are added sequentially to the mixed system to obtain the polyimide aerogel solution.
[0053] In this invention, the dianhydride monomer is preferably added in multiple portions, preferably 1 to 7 times, specifically 1, 2, 3, 4, 5, 6, or 7 times; when the number of portions is greater than or equal to 2, the amount added each time is preferably equal. After the dianhydride monomer is added, this invention preferably further includes stirring (referred to as the first stirring), the first stirring time being preferably 8 to 24 hours, specifically 8 hours, 12 hours, 16 hours, 18 hours, 20 hours, or 24 hours.
[0054] After the crosslinking agent is added, the present invention preferably further includes stirring (referred to as second stirring). The time for the second stirring is not specifically limited, but it is sufficient until the crosslinking agent is completely dissolved. In the present invention, the solid content of the mixed system is preferably 5-20%, specifically preferably 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20%. The solid content of the mixed system refers to the total mass of the diamine monomer, dianhydride monomer, and crosslinking agent, preferably accounting for 5-20% of the total mass of the diamine monomer, dianhydride monomer, crosslinking agent, and organic solvent.
[0055] After the dehydrating agent is added, the present invention preferably further includes stirring (referred to as third stirring). The present invention does not specifically limit the time of the third stirring, but only until the dehydrating agent is completely dissolved.
[0056] After the catalyst is added, the present invention preferably further includes stirring (referred to as the fourth stirring). The present invention does not specifically limit the time of the fourth stirring, as long as the catalyst is completely dissolved.
[0057] In this invention, the impregnation temperature is preferably room temperature, meaning that neither additional heating nor cooling is required; the impregnation time is not specifically limited, as long as complete impregnation is achieved. In this invention, complete impregnation means that the synthetic fiber felt is completely immersed in the polymer aerogel solution.
[0058] In this invention, "draining" means that no more polyimide aerogel solution drips down.
[0059] In this invention, after draining, a synthetic fiber felt-polymer aerogel solution composite material is preferably obtained, wherein the mass fraction of the polymer aerogel solution in the synthetic fiber felt-polymer aerogel solution composite material is 50-90%, specifically preferably 50%, 55%, 57%, 59%, 60%, 63%, 65%, 70%, 75%, 80%, 81%, 85%, or 90%.
[0060] In this invention, the crosslinking reaction is preferably carried out under sealed conditions, the temperature of the crosslinking reaction is preferably room temperature, and the time is preferably 8 to 48 hours, specifically 8 hours, 10 hours, 12 hours, 16 hours, 24 hours, 30 hours, 36 hours, 40 hours, 42 hours or 48 hours.
[0061] After the crosslinking reaction, the present invention preferably further includes: sequentially washing with N,N-dimethylacetamide and washing with acetone to obtain the synthetic fiber felt-polymer aerogel composite material; the washing method of N,N-dimethylacetamide washing and acetone washing is preferably immersion washing, and the present invention does not specifically limit the number of times N,N-dimethylacetamide washing and acetone washing are performed, as long as the material is clean.
[0062] In this invention, the preferred method for storing the synthetic fiber felt-polymer aerogel composite material is to immerse it in acetone.
[0063] The present invention also provides a high-temperature resistant emergency oil core, comprising a core and lubricating oil adsorbed in the core; the core is made of the synthetic fiber felt-polymer aerogel composite material described in the above technical solution.
[0064] The high-temperature resistant emergency oil core provided by the present invention includes a core, which is made of the synthetic fiber felt-polymer aerogel composite material described in the above technical solution.
[0065] The high-temperature resistant emergency oil core provided by this invention includes lubricating oil adsorbed in the core. In this invention, the lubricating oil preferably includes one or more of the following: base oil PAO, Pegasus II, RIPP555, white oil, and transformer oil.
[0066] This invention also provides a method for preparing the high-temperature resistant emergency oil core described in the above technical solution, comprising the following steps:
[0067] The core is immersed in lubricating oil to obtain the high-temperature resistant emergency oil core.
[0068] In this invention, the oil immersion temperature is 50–120°C, preferably 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, or 120°C; the time is 8–48 hours, preferably 8 hours, 12 hours, 15 hours, 24 hours, 30 hours, 36 hours, 42 hours, or 48 hours; the oil immersion is preferably carried out under vacuum conditions, and the vacuum degree is preferably 20–10000 Pa, preferably 20 Pa, 100 Pa, 500 Pa, 1000 Pa, 2000 Pa, 4000 Pa, 5000 Pa, 7000 Pa, or 10000 Pa.
[0069] This invention provides the application of the synthetic fiber felt-polymer aerogel composite material and the high-temperature resistant emergency oil core described above in a transmission system.
[0070] This invention does not impose specific limitations on the application of the synthetic fiber felt-polymer aerogel composite material and the high-temperature resistant emergency oil core; those skilled in the art can make settings according to actual needs.
[0071] The following detailed descriptions, in conjunction with embodiments, illustrate the synthetic fiber felt-polymer aerogel composite material and its preparation and application, as well as the high-temperature resistant emergency oil core and its preparation and application. However, these descriptions should not be construed as limiting the scope of protection of this invention.
[0072] Example 1
[0073] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 22.96 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in three equal portions, stir for 18 h, add 0.35 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 20.0%. Add 4.50 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 3.50 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0074] 2. Cut the synthetic fiber felt (specifically, meta-aramid (Nomex), with a pore size of 50 μm and a porosity of 75%) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in a polyimide (PI) aerogel solution until it is completely soaked, remove it and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polyimide aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 90%. Seal and store for 48 hours, then soak and clean it with DMAc and acetone for 72 hours respectively to obtain the synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0075] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 120℃ and 20Pa for 48 hours to obtain an emergency oil core.
[0076] Example 2
[0077] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 32.5 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add a total of 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in 5 equal portions. Stir for 15 h, then add 0.35 g of N3300. After N3300 dissolves, a mixed system with a solid content of 15.0% is obtained. Add 9.00 g of acetic anhydride to the mixed system. After it is completely dissolved, add 7.00 g of pyridine and stir until homogeneous to obtain a polyimide aerogel solution for later use.
[0078] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of polyimide aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 81%. Seal and store for 12 hours, then soak and clean it with DMAc and acetone for 12 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0079] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 50℃ and 100Pa for 8 hours to obtain an emergency oil core.
[0080] Example 3
[0081] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 51.7 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in 6 equal portions, stir for 12 h, add 0.35 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 10.0%. Add 13.5 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 10.5 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0082] 2. Cut the synthetic fiber felt (same as in Example 1) into the desired shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 70%. Seal and store for 12 hours, then soak and clean it with DMAc and acetone for 24 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0083] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil, and then vacuum immersed in oil at 80℃ and 500Pa for 24h to obtain an emergency oil core.
[0084] Example 4
[0085] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 109.1 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in 7 equal portions, stir for 8 h, add 0.35 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 5.0%. Add 18.00 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 14.00 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0086] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 59%. Seal and store for 24 hours. Soak and clean it with DMAc and acetone for 24 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0087] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 90℃ and 10000Pa for 24 hours to obtain an emergency oil core.
[0088] Example 5
[0089] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 22.36 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in four equal portions, stir for 10 h, add 0.20 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 20.0%. Add 4.50 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 3.50 g of pyridine and stir evenly to obtain a polyimide aerogel solution for later use.
[0090] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 85%. Seal and store for 24 hours, then soak and clean it with DMAc and acetone for 12 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0091] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 100℃ and 5000Pa for 24 hours to obtain an emergency oil core.
[0092] Example 6
[0093] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 31.67 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in 6 equal portions, stir for 24 h, add 0.20 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 15.0%. Add 9.00 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 9.00 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0094] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 75%. Seal and store for 10 hours, then soak and clean it with DMAc and acetone for 60 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0095] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 110℃ and 2000Pa for 30 hours to obtain an emergency oil core.
[0096] Example 7
[0097] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 50.13 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in four equal portions, stir for 8 h, add 0.20 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 10.0%. Add 13.50 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 10.50 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0098] 2. Cut the synthetic fiber felt (same as in Example 1) into the desired shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 63%. Seal and store for 48 hours, then soak and clean it with DMAc and acetone for 24 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0099] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 70℃ and 4000Pa for 48 hours to obtain an emergency oil core.
[0100] Example 8
[0101] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 106.21 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in three equal portions, stir for 18 h, add 0.20 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 5.0%. Add 18.00 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 14.00 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0102] 2. Cut the synthetic fiber felt (same as in Example 1) into the desired shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 55%. Seal and store for 40 hours, then soak and clean it with DMAc and acetone for 60 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0103] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 80℃ and 7000Pa for 40 hours to obtain an emergency oil core.
[0104] Example 9
[0105] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 21.84 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in one go, stir for 8 h, add 0.07 g of N3300, and after N3300 dissolves, a mixed system is obtained with a solid content of 20.0%. Add 4.50 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 3.50 g of pyridine, stir evenly, and a polyimide aerogel solution is obtained for later use.
[0106] 2. Cut the synthetic fiber felt (same as in Example 1) into the desired shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 70%. Seal and store for 36 hours. Soak and clean it with DMAc and acetone for 36 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0107] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 120℃ and 1000Pa for 45 hours to obtain an emergency oil core.
[0108] Example 10
[0109] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 30.94 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in two equal portions, stir for 16 h, add 0.07 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 15.0%. Add 9.00 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 9.00 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0110] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 63%. Seal and store for 40 hours, then soak and clean it with DMAc and acetone for 20 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0111] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 70℃ and 20Pa for 20 hours to obtain an emergency oil core.
[0112] Example 11
[0113] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 49.14 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in three equal portions, stir for 12 h, add 0.07 g of N3300, and after N3300 dissolves, obtain a mixed system with a solid content of 10.0%. Add 13.50 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 10.50 g of pyridine, stir evenly, and obtain a polyimide aerogel solution for later use.
[0114] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 57%. Seal and store for 8 hours, then soak and clean it with DMAc and acetone for 20 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0115] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil, and then vacuum-immersed in oil at 65℃ and 500Pa for 30h to obtain an emergency oil core.
[0116] Example 12
[0117] 1. Weigh 2.05 g of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 103.74 g of anhydrous N,N-dimethylacetamide (DMAc). Under nitrogen atmosphere, add 3.24 g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride (BPDA) in four equal portions, stir for 24 h, add 0.07 g of N3300, and wait for N3300 to dissolve to obtain a mixed system with a solid content of 5.0%. Add 18.00 g of acetic anhydride to the mixed system, and after it is completely dissolved, add 14.00 g of pyridine and stir evenly to obtain a polyimide aerogel solution for later use.
[0118] 2. Cut the synthetic fiber felt (same as in Example 1) into the required shape, clean it with ethanol and dry it. Immerse the cleaned felt in the polyimide aerogel solution until it is completely soaked, take it out and drain it to obtain a synthetic fiber felt-polyimide aerogel solution composite material. The mass fraction of the polymer aerogel solution in the synthetic fiber felt-polyimide aerogel solution composite material is 50%. Seal and store for 48 hours. Soak and clean it with DMAc and acetone for 24 hours respectively to obtain a synthetic fiber felt-PI aerogel composite material. Finally, soak it in acetone solvent for later use.
[0119] The synthetic fiber felt-PI aerogel composite material was taken out and immersed in lubricating oil. It was then vacuum-immersed in oil at 70℃ and 1000Pa for 48 hours to obtain an emergency oil core.
[0120] The parameters and raw material usage in Examples 1 to 12 are shown in Table 1.
[0121] Table 1. Crosslinking degree and solid content of different embodiments
[0122]
[0123]
[0124] The present invention calculates the oil content of the emergency oil core by weighing the synthetic fiber felt-PI aerogel composite material obtained in each embodiment before and after oil immersion. The results are shown in Table 2.
[0125] The oil supply performance (oil leakage rate) of the obtained emergency oil core was tested through a high-speed oil slinging experiment. The results are shown in Table 2 and... Figure 1 As shown.
[0126] Table 2. Oil content and seepage rate of emergency oil cores in different embodiments.
[0127]
[0128] Figure 1 The oil seepage rate of the emergency oil cores obtained in Examples 1-12 is calculated from... Figure 1As shown in Table 2, comparing Examples 1-4 reveals that decreasing solid content leads to a gradual increase in oil content, but also results in an excessively rapid oil seepage rate. The optimal oil seepage rate is observed at a solid content of 15%, with the fastest seepage rate across all time periods. Comparing Examples 1-4 with Examples 5-12 shows that decreasing cross-linking degree not only leads to a decrease in oil content but also a decrease in the oil seepage rate of the emergency oil core. Considering both oil content and seepage rate, Example 2 demonstrates the best overall performance.
[0129] To verify the high-temperature resistance of the synthetic fiber felt-polymer aerogel composite material, this invention used thermogravimetric analysis to test the thermal decomposition curves of commercially available wool felt, wool felt-polyurethane composite material, synthetic fiber felt, and the synthetic fiber felt-PI aerogel composite material obtained in Example 2. The results are as follows: Figure 2 As shown, from Figure 2 It can be seen that the synthetic fiber felt-PI aerogel composite material provided by the present invention has a decomposition temperature as high as 420℃ compared with the wool felt-polyurethane composite material sold on the market.
[0130] Meanwhile, the oil seepage rate of the emergency oil core obtained in Example 2 after treatment at 150°C for 24 hours was compared, and the results are as follows: Figure 3 As shown, Figure 3 The oil seepage rate of the emergency oil core obtained in Example 2 before and after high-temperature treatment is shown. Figure 3 As shown, after high-temperature treatment, the oil seepage rate remained stable and did not decrease.
[0131] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A synthetic fiber felt-polymer aerogel composite material, comprising a synthetic fiber felt and a polymer aerogel filling the pores of the synthetic fiber felt, wherein the polymer aerogel is a polyimide aerogel; The synthetic fiber felt has a pore size of 10~100μm and a porosity of 20~80%; The polyimide aerogel is prepared from a polyimide aerogel solution; the raw materials for preparing the polyimide aerogel solution include the following components: diamine monomer, dianhydride monomer, crosslinking agent, dehydrating agent, catalyst and organic solvent; The total mass of the diamine monomer, dianhydride monomer, and crosslinking agent accounts for 11-20% of the total mass of the diamine monomer, dianhydride monomer, crosslinking agent, and organic solvent. The degree of crosslinking of the polyimide aerogel solution is 20-100%; The degree of crosslinking of the polyimide aerogel solution is calculated according to the following formula: 。 2. The synthetic fiber felt-polymer aerogel composite material according to claim 1, characterized in that, The molar ratio of the diamine monomer to the crosslinking agent is 1:0 to 0.07, and the molar amount of the crosslinking agent is not 0.
3. The synthetic fiber felt-polymer aerogel composite material according to claim 1, characterized in that, The diamine monomer includes one or more of 4,4'-diaminodiphenyl ether, p-phenylenediamine, 4,4'-diaminodiphenylmethane, 4,4'-diaminobenzophenone and 4,4'-diaminodicyclohexylmethane; The dianhydride monomers include one or more of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride, pyromellitic dianhydride, hexafluorodianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride, diphenyl methyl ether tetracarboxylic dianhydride, and bisphenol A type dianhydride; The crosslinking agent includes one or more of hexamethylene diisocyanate trimer, tris(4-aminophenyl)amine, 1,3,5-tris(4-aminophenyl)benzene, and 1,3,5-tris(4-aminophenyl)triazine.
4. The synthetic fiber felt-polymer aerogel composite material according to claim 1, characterized in that, The dehydrating agent includes acetic anhydride; The catalyst includes pyridine; The organic solvent includes N,N-dimethylacetamide.
5. The method for preparing the synthetic fiber felt-polymer aerogel composite material according to any one of claims 1 to 4, characterized in that, Includes the following steps: The synthetic fiber felt was immersed in a polymer aerogel solution. After complete immersion, the synthetic fiber felt was removed and drained, and then a crosslinking reaction was carried out to obtain the synthetic fiber felt-polymer aerogel composite material.
6. A high-temperature resistant emergency oil core, characterized in that, It includes a core and lubricating oil adsorbed in the core; the core is made of the synthetic fiber felt-polymer aerogel composite material according to any one of claims 1 to 4.
7. The method for preparing the high-temperature resistant emergency oil core according to claim 6, characterized in that, Includes the following steps: The core is immersed in lubricating oil to obtain the high-temperature resistant emergency oil core; The oil immersion temperature is 50~120℃, the time is 8~48h, and the oil immersion is carried out under vacuum conditions.
8. The application of the synthetic fiber felt-polymer aerogel composite material according to any one of claims 1 to 4 or the high-temperature resistant emergency oil core according to claim 6 in a transmission system.