CN112940251A - 一种宽温域下聚酰亚胺润滑材料及其制备方法 - Google Patents
一种宽温域下聚酰亚胺润滑材料及其制备方法 Download PDFInfo
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- CN112940251A CN112940251A CN202110157451.6A CN202110157451A CN112940251A CN 112940251 A CN112940251 A CN 112940251A CN 202110157451 A CN202110157451 A CN 202110157451A CN 112940251 A CN112940251 A CN 112940251A
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- polyimide
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- wide temperature
- dianhydride
- lubricating material
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 68
- 239000004642 Polyimide Substances 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 40
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 9
- 239000011593 sulfur Substances 0.000 claims abstract description 9
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 8
- 239000011737 fluorine Substances 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims description 47
- 239000002904 solvent Substances 0.000 claims description 30
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 28
- 150000004985 diamines Chemical class 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- 239000002981 blocking agent Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229920005575 poly(amic acid) Polymers 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- NSGXIBWMJZWTPY-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropane Chemical compound FC(F)(F)CC(F)(F)F NSGXIBWMJZWTPY-UHFFFAOYSA-N 0.000 claims description 7
- 239000004952 Polyamide Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 229920002647 polyamide Polymers 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
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- UPGRRPUXXWPEMV-UHFFFAOYSA-N 5-(2-phenylethynyl)-2-benzofuran-1,3-dione Chemical compound C=1C=C2C(=O)OC(=O)C2=CC=1C#CC1=CC=CC=C1 UPGRRPUXXWPEMV-UHFFFAOYSA-N 0.000 claims description 5
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 claims description 5
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 4
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- KNDQHSIWLOJIGP-UMRXKNAASA-N (3ar,4s,7r,7as)-rel-3a,4,7,7a-tetrahydro-4,7-methanoisobenzofuran-1,3-dione Chemical compound O=C1OC(=O)[C@@H]2[C@H]1[C@]1([H])C=C[C@@]2([H])C1 KNDQHSIWLOJIGP-UMRXKNAASA-N 0.000 claims description 3
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
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- FYYYKXFEKMGYLZ-UHFFFAOYSA-N 4-(1,3-dioxo-2-benzofuran-5-yl)-2-benzofuran-1,3-dione Chemical compound C=1C=C2C(=O)OC(=O)C2=CC=1C1=CC=CC2=C1C(=O)OC2=O FYYYKXFEKMGYLZ-UHFFFAOYSA-N 0.000 claims description 2
- VQVIHDPBMFABCQ-UHFFFAOYSA-N 5-(1,3-dioxo-2-benzofuran-5-carbonyl)-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(C(C=2C=C3C(=O)OC(=O)C3=CC=2)=O)=C1 VQVIHDPBMFABCQ-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
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- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Natural products C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 2
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- NNKQLUVBPJEUOR-UHFFFAOYSA-N 3-ethynylaniline Chemical compound NC1=CC=CC(C#C)=C1 NNKQLUVBPJEUOR-UHFFFAOYSA-N 0.000 claims 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
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- ICNFHJVPAJKPHW-UHFFFAOYSA-N 4,4'-Thiodianiline Chemical compound C1=CC(N)=CC=C1SC1=CC=C(N)C=C1 ICNFHJVPAJKPHW-UHFFFAOYSA-N 0.000 description 4
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 125000006160 pyromellitic dianhydride group Chemical group 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- NVKGJHAQGWCWDI-UHFFFAOYSA-N 4-[4-amino-2-(trifluoromethyl)phenyl]-3-(trifluoromethyl)aniline Chemical group FC(F)(F)C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F NVKGJHAQGWCWDI-UHFFFAOYSA-N 0.000 description 1
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- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
本发明公开了一种宽温域下不同分子结构聚酰亚胺润滑材料。本发明通过在聚酰亚胺分子结构中分别引入含氟或含硫基团，以提高其化学活性，促进界面摩擦化学反应的发生。摩擦过程中生成的高稳定性转移膜可提高摩擦界面润滑性，降低宽温域环境中含氟及含硫聚酰亚胺的摩擦系数和磨损率，进而提高其工程应用中的可靠性和使用寿命。同时，合成工艺中降低反应温度、缩短反应时间对材料的摩擦学性能影响不大，可进一步节约能耗。
Description
技术领域
本发明涉及一种宽温域下聚酰亚胺润滑材料，属于润滑技术领域。
背景技术
随着我国航空航天事业的发展，对空间摩擦系统的可靠性和稳定性的要求越来越高，例如空间轴承及其保持架等摩擦学部件的摩擦与润滑问题，通常涉及环境介质、高低温、高速度、高真空、高应力、强辐射等特殊工作条件，要求润滑材料免维护且长期在宽温域(-150~150℃)下保持良好的润滑效果。然而，长期在高低温下服役，并反复经历高低温交变循环，对聚合物复合材料的耐温性能、力学强度、高低温摩擦学性能等提出了严苛的要求。
聚酰亚胺(PI)由于其热稳定性好、自润滑效果好、机械强度高等优异性能，在机械工程、轨道交通、智能制造等领域应用较广。然而，常规分子结构聚酰亚胺的摩擦系数和磨损率相对较高，难以长时间在极端工况下服役。
基于上述情况，设计发明一种适用于宽温域下的润滑材料就显得尤为必要。
发明内容
为解决常规分子结构聚酰亚胺摩擦系数和磨损率相对较高，难以长时间在极端工况下服役的问题，本申请提出了一种宽温域下的聚酰亚胺润滑材料。通过对聚酰亚胺进行结构设计，引入化学活性较高的氟原子或硫原子，旨在促进聚酰亚胺与金属对偶之间摩擦化学反应的发生，提高转移膜与金属对偶之间的界面结合。生成的高稳定性转移膜，可避免摩擦系统的直接接触，提高界面润滑性，降低摩擦磨损，进而提高系统的可靠性和使用寿命。
为了实现上述目的，本申请采取的技术方案如下：
一种宽温域下聚酰亚胺润滑材料，在聚酰亚胺中引入硫或氟制备而成，且聚酰亚胺的分子量控制在3000-5000g/mol。
所述的宽温域下聚酰亚胺润滑材料的制备方法，具体包括以下步骤：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体与封端剂完全溶解；
3）将二酐单体加入到步骤1）所得的混合溶液中，室温、氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
4）将步骤2）得到的聚酰胺酸粘稠溶液均匀涂抹于载体表面，放入恒温加热台上50~60℃处理大约4h使溶剂全部蒸发；然后放入管式炉中，80~100℃保温1h，100~120℃、180~200℃、280~300℃分别保温1h，得到聚酰亚胺膜润滑材料。在50-60℃下蒸发溶剂，样品固化，可以缩短反应时间；四个温度梯度均发生了亚胺化，梯度升温能使亚胺化更完全，避免了升温过快导致聚合物裂解。
步骤1）中所述的溶剂选自N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮中的一种。
步骤1）中所述的二胺单体选自4,4'-二氨基二苯醚、4,4'-二氨基二苯硫醚、4,4'-二氨基-2,2'-双三氟甲基联苯、4,4'-二氨基二苯砜中的任意两种配比组合。
步骤1）中所述的封端剂选自4-苯乙炔基苯酐、降冰片烯二酸酐、3-乙炔苯胺中的一种或几种。反应体系引入封端剂可得到热固性聚酰亚胺，能够进一步提高润滑材料的耐温性能和耐磨性能。
步骤2）中所述的二酐单体选自3,3',4,4'-联苯四甲酸二酐、2,3,3',4'-联苯四甲酸二酐、均苯四甲酸二酐、2,2'-双(3,4-二羧酸)六氟丙烷二酐、4,4'-联苯醚二酐、3,3'4,4'-二苯甲酮四羧酸二酐中的任意一种或者任意两种及以上的复配组合。
步骤3）中所述的载体选自轴承钢、不锈钢、铝板、玻璃、陶瓷、硅片中的一种或几种。
所述二胺单体在溶剂中的浓度为0.124-0.513 mol/L。
本技术制备的聚酰亚胺润滑材料通过引入封端剂可得到交联型的热固性结构，提高材料的力学性能和高温耐磨性。分子结构中引入化学活性较高的氟原子或硫原子，能够促进聚合物与金属对偶之间摩擦化学反应的发生，进而生成结构稳定的转移膜，提高摩擦系统的可靠性和服役寿命。
附图说明
图1为不同分子结构的聚酰亚胺润滑材料硬度与模量。
具体实施方式
下面通过具体实施例进一步说明本发明，但本实施例并不用于限制本发明，凡是采用本发明的相似方法及其相似变化，均应列入本发明的保护范围。所述试剂和原料，如无特殊说明，均从商业途径获得。
实施例1
一种宽温域下聚酰亚胺润滑材料，该材料通过以下步骤来制备：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体完全溶解；
2）将二酐单体加入到步骤1）所得的混合溶液中，氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
3）将步骤2）得到的聚酰胺酸粘稠溶液均匀涂抹于载体表面，放入恒温加热台上50~60℃处理大约4h使溶剂全部蒸发；然后放入管式炉中，80~100℃保温1h，100~120℃、180~200℃、280~300℃分别保温1h，相对温和地升温使得聚酰胺酸亚胺化为聚酰亚胺，得到宽温域下聚酰亚胺润滑材料。
所述的溶剂选自N-甲基吡咯烷酮；
所述的二胺单体选自4,4'-二氨基二苯醚、4,4'-二氨基二苯硫醚，两者配比为5：1；
所述的封端剂选自4-苯乙炔基苯酐；
所述的二酐单体选自3,3', 4,4'-联苯四甲酸二酐；
所述的载体选自轴承钢；
所制备聚酰亚胺的分子量控制在4000g/mol。
本发明所述二胺单体N-甲基吡咯烷酮溶液的浓度为0.513mol/L。
实施例2
一种宽温域下聚酰亚胺润滑材料，该材料通过以下步骤来制备：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体完全溶解；
2）将二酐单体加入到步骤1）所得的混合溶液中，氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
3）将步骤2）得到的聚酰胺酸粘稠溶液中加入异喹啉，以促进亚胺化反应,然后按以下程序逐渐升温固化：80℃保温1h，120℃、180℃、220℃分别保温1h。反应完毕，将溶液过滤、洗涤，固体用研钵磨碎，在索氏提取器中分别用四氢吠喃、丙酮、乙醇萃取，直至黄色溶液完全退色为止。120℃下真空干燥24h，得到宽温域下聚酰亚胺粉末材料。
所述的溶剂选自N-甲基吡咯烷酮；
所述的二胺单体选自4,4'-二氨基二苯醚、4,4'-二氨基二苯硫醚，两者配比为5：1；
所述的封端剂选自4-苯乙炔基苯酐；
所述的二酐单体选自3,3', 4,4'-联苯四甲酸二酐；
所述的载体选自轴承钢；
所制备聚酰亚胺的分子量控制在4000g/mol。
本发明所述二胺单体N-甲基吡咯烷酮溶液的浓度为0.513mol/L。
实施例3
一种宽温域下聚酰亚胺润滑材料，该材料通过以下步骤来制备：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体与封端剂完全溶解；
2）将二酐单体加入到步骤1）所得的混合溶液中，氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
3）将步骤2）得到的聚酰胺酸粘稠溶液均匀涂抹于载体表面，放入恒温加热台上50~60℃处理大约4h使溶剂全部蒸发；然后放入管式炉中，80~100℃保温1h，100~120℃、180~200℃、280~300℃分别保温1h，相对温和地升温使得聚酰胺酸亚胺化为聚酰亚胺，得到宽温域下聚酰亚胺润滑材料。
所述的溶剂选自N-甲基吡咯烷酮；
所述的二胺单体选自4,4'-二氨基二苯砜、4,4'-二氨基二苯硫醚，两者配比为1：1；
所述的封端剂选自4-苯乙炔基苯酐；
所述的二酐单体选自3,3', 4,4'-联苯四甲酸二酐，2,2'-双(3,4-二羧酸)六氟丙烷二酐，两者配比为2：1；
所述的载体选自轴承钢；
所制备聚酰亚胺的分子量控制在4000g/mol。
本发明所述二胺单体N-甲基吡咯烷酮溶液的浓度为0.329 mol/L。
实施例4
一种宽温域下聚酰亚胺润滑材料，该材料通过以下步骤来制备：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体与封端剂完全溶解；
2）将二酐单体加入到步骤1）所得的混合溶液中，氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
3）将步骤2）得到的聚酰胺酸粘稠溶液均匀涂抹于载体表面，放入恒温加热台上50~60℃处理大约4h使溶剂全部蒸发；然后放入管式炉中，80~100℃保温1h，100~120℃、180~200℃、280~300℃分别保温1h，相对温和地升温使得聚酰胺酸亚胺化为聚酰亚胺，得到宽温域下聚酰亚胺润滑材料。
所述的溶剂选自N,N-二甲基乙酰胺；
所述的二胺单体选自4,4'-二氨基二苯硫醚、4,4'-二氨基-2,2'-双三氟甲基联苯，两者配比为1：1；
所述的封端剂选自降冰片烯二酸酐；
所述的二酐单体选自均苯四甲酸二酐、2,2'-双(3,4-二羧酸)六氟丙烷二酐，2,2'-双(3,4-二羧酸)六氟丙烷二酐，三者配比为3：2：1；
所述的载体选自轴承钢；
所制备聚酰亚胺的分子量控制在4000g/mol。
本发明所述二胺单体N-甲基吡咯烷酮溶液的浓度为0.124 mol/L。
实施例5
一种宽温域下聚酰亚胺润滑材料，该材料通过以下步骤来制备：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体与封端剂完全溶解；
2）将二酐单体加入到步骤1）所得的混合溶液中，氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
3）将步骤2）得到的聚酰胺酸粘稠溶液均匀涂抹于载体表面，放入恒温加热台上50~60℃处理大约4h使溶剂全部蒸发；然后放入管式炉中，80~100℃保温1h，100~120℃、180~200℃、280~300℃分别保温1h，相对温和地升温使得聚酰胺酸亚胺化为聚酰亚胺，得到宽温域下聚酰亚胺润滑材料。
所述的溶剂选自N-甲基吡咯烷酮；
所述的二胺单体选自4'-二氨基二苯硫醚、4,4'-二氨基二苯砜，两者配比为1：1；
所述的封端剂选自3-乙炔苯胺；
所述的二酐单体选自均苯四甲酸二酐、2,2'-双(3,4-二羧酸)六氟丙烷二酐，两者配比为1：4；
所述的载体选自轴承钢；
所制备聚酰亚胺的分子量控制在4000g/mol。
本发明所述二胺单体N-甲基吡咯烷酮溶液的浓度为0.462 mol/L。
本发明采用MDZ-1GL型高/低温、真空摩擦磨损试验机对实施例1-5进行旋转摩擦实验。聚酰亚胺材料为下式样圆盘，轴承钢为上式样对偶球，实施例2中的粉末样品通过热压成型得到块体材料。摩擦实验测试条件为：大气环境，试验持续1.0h，加载力50.0N，速度0.5m/s。所得结果见附表1与附表2。聚合物的体积磨损率(mm3/N·m)通过Rtec-MFT3000型多功能摩擦磨损试验机附带的白光三维扫描仪扫描并计算得出。
本发明所制备的宽温域下不同分子结构的聚酰亚胺润滑材料对比结果发现，聚酰亚胺粉末和膜材料的摩擦学性能，力学性能有一定区别。由于含氟、含硫分子结构促进摩擦界面摩擦化学反应的发生，摩擦过程中生成的高稳定性转移膜可提高摩擦界面的润滑性，因此，分子结构中硫和氟的比例越大，材料的摩擦学性能越好，证实了宽温域下聚酰亚胺的摩擦磨损具有明显的结构依赖性。
表1 宽温域下不同分子结构的聚酰亚胺润滑材料摩擦系数
| -100℃ | -50℃ | 25℃ | 50℃ | 100℃ | |
| 实施例1 | 0.48 | 0.61 | 0.82 | 0.58 | 0.46 |
| 实施例2 | 0.46 | 0.59 | 0.78 | 0.50 | 0.50 |
| 实施例3 | 0.23 | 0.22 | 0.22 | 0.25 | 0.24 |
| 实施例4 | 0.059 | 0.12 | 0.15 | 0.17 | 0.15 |
| 实施例5 | 0.045 | 0.10 | 0.12 | 0.15 | 0.09 |
表2宽温域下不同分子结构的聚酰亚胺润滑材料磨损率(10-6mm3/N·m)
| -100℃ | -50℃ | 25℃ | 50℃ | 100℃ | |
| 实施例1 | 0.54 | 0.64 | 1.92 | 2.82 | 3.15 |
| 实施例2 | 0.58 | 0.60 | 1.82 | 2.92 | 2.95 |
| 实施例3 | 0.44 | 0.20 | 0.95 | 1.10 | 2.12 |
| 实施例4 | 0.22 | 0.19 | 0.87 | 0.2 | 0.4 |
| 实施例5 | 0.12 | 0.11 | 0.58 | 0.15 | 0.3 |
从表1、表2可以看出，实施例5得到宽温域下含硫分子结构聚酰亚胺润滑材料的摩擦系数和磨损率最低。相同条件下，实施例1中硫和氟的含量最低的聚酰亚胺摩擦系数和磨损率最高。此外，实施例3和4得到的复合材料的摩擦性能都优于实施例1中聚酰亚胺的摩擦性能。
采用纳米压痕仪(G200, Keysight, USA)测试了材料的机械性能，如图1所示，说明含氟、硫分子引入可显著提高聚酰亚胺材料的机械性能。
Claims (9)
1.一种宽温域下聚酰亚胺润滑材料，其特征在于，在聚酰亚胺中引入硫或氟制备而成，且聚酰亚胺的分子量控制在3000-5000g/mol。
2.制备如权利要求1所述的宽温域下聚酰亚胺润滑材料，其特征在于，具体包括以下步骤：
1）向反应容器中加入溶剂，称取二胺单体与封端剂加入溶剂中，超声加搅拌5min至二胺单体与封端剂完全溶解；
3）将二酐单体加入到步骤1）所得的混合溶液中，室温、氮气条件下搅拌反应8h取出，得到聚酰胺酸粘稠溶液；
4）将步骤2）得到的聚酰胺酸粘稠溶液均匀涂抹于载体表面，放入恒温加热台上50~60℃处理大约4h使溶剂全部蒸发；然后放入管式炉中，80~100℃保温1h，100~120℃、180~200℃、280~300℃分别保温1h，得到聚酰亚胺膜润滑材料。
3.如权利要求2所述的宽温域下聚酰亚胺润滑材料的制备方法，其特征在于，步骤1）中所述的溶剂选自N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮中的一种。
4.如权利要求2所述的宽温域下聚酰亚胺润滑材料的制备方法，其特征在于，步骤1）中所述的二胺单体选自4,4'-二氨基二苯醚、4,4'-二氨基二苯硫醚、4,4'-二氨基-2,2'-双三氟甲基联苯、4,4'-二氨基二苯砜中的任意两种配比组合。
5.如权利要求2所述的宽温域下聚酰亚胺润滑材料的制备方法，其特征在于，步骤1）中所述的封端剂选自4-苯乙炔基苯酐、降冰片烯二酸酐、3-乙炔苯胺中的一种或几种。
6.如权利要求2所述的宽温域下聚酰亚胺润滑材料的制备方法，其特征在于，步骤2）中所述的二酐单体选自3,3',4,4'-联苯四甲酸二酐、2,3,3',4'-联苯四甲酸二酐、均苯四甲酸二酐 、2,2'-双(3,4-二羧酸)六氟丙烷二酐、4,4'-联苯醚二酐、3,3'4,4'-二苯甲酮四羧酸二酐中的任意一种或者任意两种及以上的复配组合。
7.如权利要求2所述的宽温域下聚酰亚胺润滑材料的制备方法，其特征在于，步骤3）中所述的载体选自轴承钢、不锈钢、铝板、玻璃、陶瓷、硅片中的一种或几种。
8.如权利要求2所述的宽温域下聚酰亚胺润滑材料的制备方法，其特征在于，所述二胺单体在溶剂中的浓度为0.124-0.513 mol/L。
9.如权利要求1所述的宽温域下聚酰亚胺润滑材料，其特征在于，具体形式为膜或者粉末。
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| CN115160783A (zh) * | 2022-07-28 | 2022-10-11 | 西南科技大学 | 适用于宽温域聚脲/聚酰亚胺共聚物自润滑复合材料及其制备方法 |
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