CN105568693A - 一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 - Google Patents
一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 Download PDFInfo
- Publication number
- CN105568693A CN105568693A CN201610151275.4A CN201610151275A CN105568693A CN 105568693 A CN105568693 A CN 105568693A CN 201610151275 A CN201610151275 A CN 201610151275A CN 105568693 A CN105568693 A CN 105568693A
- Authority
- CN
- China
- Prior art keywords
- powder
- parts
- preparation
- carbon fiber
- sizing agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000004513 sizing Methods 0.000 title claims abstract description 35
- 239000004593 Epoxy Substances 0.000 title claims abstract description 33
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 34
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229940043237 diethanolamine Drugs 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 16
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 17
- 239000004917 carbon fiber Substances 0.000 abstract description 17
- 229920005989 resin Polymers 0.000 abstract description 15
- 239000011347 resin Substances 0.000 abstract description 15
- 239000011159 matrix material Substances 0.000 abstract description 14
- 239000000835 fiber Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 1
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 1
- 238000010790 dilution Methods 0.000 description 6
- 239000012895 dilution Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 4
- 238000009955 starching Methods 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明公开了一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法，属于碳纤维上浆剂制备技术领域。本发明将氧化锆和氧化铝粉末混合，与去离子水搅拌，球磨处理，干燥得复合陶瓷粉末，经两次炭化，与环氧树脂、无水乙醇混合保温后，滴加二乙醇胺、盐酸溶液保温反应，旋转蒸发后，与二乙醇胺、去离子水混合，旋转蒸发制得环氧上浆剂。本发明的有益效果是：本发明制备步骤简单，所得产品与基体树脂的粘结性和润湿性好；有效促进纤维与基体树脂之间的化学结合，提高其界面结合强度。
Description
技术领域
本发明涉及一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法，属于碳纤维上浆剂制备技术领域。
背景技术
碳纤维作为国防军工用的高科技材料，近年来，在民用领域得到广泛应用。碳纤维的性能直接决定着复合材料制品的性能。碳纤维伸长率低且脆，加工过程中受到反复弯曲、摩擦容易造成单丝断裂和毛丝。上浆剂的作用是保护碳纤维表面处理（特别是臭氧处理或等离子体处理）后产生的表面活性，避免纤维表面吸附空气中的水分和灰尘；有利于改善纤维与基体树脂的粘合力及后加工性能；提高纤维丝束的抱合力，在单丝表面成膜防止毛丝的产生。
目前碳纤维常用的上浆剂有环氧树脂型乳液上浆剂，将环氧树脂与乙二醇单乙醚按一定比例搅拌混合稀释，稀释后的环氧树脂与乳化剂按比例加热融化混合均匀，高速搅拌，转速为8000r/min，在高速搅拌下，缓慢加入45℃的温水，体系粘度逐渐增加，在相转变期停止加水，继续高速搅拌，完成转相后，可快速将剩余水加入，乳液总固含量质量分数为45%。搅拌时间为1h，得到混合均匀的白色乳状液。环氧树脂乳液型上浆剂，不含或者极少含有有机溶剂，不在导辊残余树脂，工艺性较好。但是大部分乳化剂与基体树脂的结合性较差，随主浆料涂覆与碳纤维表面后，不利于纤维与基体树脂之间的化学结合，导致其界面结合强度降低。
发明内容
本发明所要解决的技术问题：针对环氧树脂乳液型上浆剂中乳化剂与基体树脂的粘结性和润湿性较差，随主浆料涂覆于碳纤维表面后，不利于纤维与基体树脂之间的化学结合，导致其界面结合强度降低的弊端，提供了一种将氧化锆和氧化铝粉末混合，与去离子水搅拌，球磨处理，干燥得复合陶瓷粉末，经两次炭化，与环氧树脂、无水乙醇混合保温后，滴加二乙醇胺、盐酸溶液保温反应，旋转蒸发后，与二乙醇胺、去离子水混合，旋转蒸发制得环氧上浆剂的方法。本发明制备步骤简单，所得产品与基体树脂的粘结性和润湿性好。
为解决上述技术问题，本发明采用如下所述的技术方案是：
（1）按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3～4h，随后将其至于65～80℃下干燥6～8h，制备得复合陶瓷粉末；
（2）将上述制备的复合陶瓷粉末置于150～270℃马弗炉中进行初步炭化，控制炭化时间为2～3h，待初步炭化完成后，按8℃/min的速率程序升温至650～800℃，保温炭化8～10h，随后静置冷却至20～30℃，制备得混合煅烧陶瓷粉末；
（3）按重量份数计，分别称量35～55份无水乙醇、15～25份上述制备的混合煅烧陶瓷粉末和30～40份环氧树脂于三口烧瓶中，在55～60℃下保温加热1～2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；
（4）待滴加完成后，继续保温反应2～3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10～15min，随后继续保温加热反应30～45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；
（5）按重量份数计，分别量取45～65份去离子水、15～25份二乙醇胺和20～30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2～5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
本发明的应用方法：将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到2.5～3.0%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在115～125℃下烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了78～82%，断裂伸长率提高了1.0～1.2%，拉伸强度为3.28～3.42GPa，毛丝量减少了90%以上，值得推广与使用。
本发明与其他方法相比，有益技术效果是：
（1）本发明制备步骤简单，所得产品与基体树脂的粘结性和润湿性好；
（2）有效促进纤维与基体树脂之间的化学结合，提高其界面结合强度。
具体实施方式
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3～4h，随后将其至于65～80℃下干燥6～8h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于150～270℃马弗炉中进行初步炭化，控制炭化时间为2～3h，待初步炭化完成后，按8℃/min的速率程序升温至650～800℃，保温炭化8～10h，随后静置冷却至20～30℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量35～55份无水乙醇、15～25份上述制备的混合煅烧陶瓷粉末和30～40份环氧树脂于三口烧瓶中，在55～60℃下保温加热1～2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应2～3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10～15min，随后继续保温加热反应30～45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取45～65份去离子水、15～25份二乙醇胺和20～30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2～5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
实例1
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3h，随后将其至于65℃下干燥6h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于150℃马弗炉中进行初步炭化，控制炭化时间为2h，待初步炭化完成后，按8℃/min的速率程序升温至650℃，保温炭化8h，随后静置冷却至20℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量35份无水乙醇、25份上述制备的混合煅烧陶瓷粉末和40份环氧树脂于三口烧瓶中，在55℃下保温加热1h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应2h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10min，随后继续保温加热反应30min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取45份去离子水、25份二乙醇胺和30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到2.5%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在115℃的干燥炉烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了78%，断裂伸长率提高了1.0%，拉伸强度为3.28GPa，毛丝量减少了90.3%，值得推广与使用。
实例2
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理4h，随后将其至于72℃下干燥7h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于210℃马弗炉中进行初步炭化，控制炭化时间为3h，待初步炭化完成后，按8℃/min的速率程序升温至720℃，保温炭化9h，随后静置冷却至25℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量45份无水乙醇、20份上述制备的混合煅烧陶瓷粉末和35份环氧树脂于三口烧瓶中，在58℃下保温加热2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为13min，随后继续保温加热反应37min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取55份去离子水、20份二乙醇胺和25份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为3%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到2.8%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在120℃的干燥炉烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了80%，断裂伸长率提高了1.1%，拉伸强度为3.35GPa，毛丝量减少了90.8%，值得推广与使用。
实例3
首先按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理4h，随后将其至于80℃下干燥8h，制备得复合陶瓷粉末；然后将上述制备的复合陶瓷粉末置于270℃马弗炉中进行初步炭化，控制炭化时间为3h，待初步炭化完成后，按8℃/min的速率程序升温至800℃，保温炭化10h，随后静置冷却至30℃，制备得混合煅烧陶瓷粉末；再按重量份数计，分别称量55份无水乙醇、15份上述制备的混合煅烧陶瓷粉末和30份环氧树脂于三口烧瓶中，在60℃下保温加热2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；待滴加完成后，继续保温反应3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为15min，随后继续保温加热反应45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；最后按重量份数计，分别量取65份去离子水、15份二乙醇胺和20份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
将本发明制得的煅烧陶瓷粉体改性碳纤维环氧上浆剂稀释到3.0%，稀释后放入上浆槽中，将碳纤维在上浆槽中经过压辊挤压进行上浆，随后在125℃的干燥炉烘干，再经收丝架卷绕制得成品，即可。该环氧上浆剂与基体树脂的粘结性和润湿性好，碳纤维界面结合强度提高了82%，断裂伸长率提高了1.2%，拉伸强度为3.42GPa，毛丝量减少了91.2%，值得推广与使用。
Claims (1)
1.一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法，其特征在于具体制备步骤为：
（1）按质量比1:1，将氧化锆与氧化铝粉末搅拌混合，在球磨机中搅拌混合，制备得混合粉体，按质量比1:5，将上述制备的混合粉体与去离子水搅拌混合，再在球磨机上球磨处理3～4h，随后将其至于65～80℃下干燥6～8h，制备得复合陶瓷粉末；
（2）将上述制备的复合陶瓷粉末置于150～270℃马弗炉中进行初步炭化，控制炭化时间为2～3h，待初步炭化完成后，按8℃/min的速率程序升温至650～800℃，保温炭化8～10h，随后静置冷却至20～30℃，制备得混合煅烧陶瓷粉末；
（3）按重量份数计，分别称量35～55份无水乙醇、15～25份上述制备的混合煅烧陶瓷粉末和30～40份环氧树脂于三口烧瓶中，在55～60℃下保温加热1～2h，随后对其滴加无水乙醇质量1/8的二乙醇胺，控制滴加速度为2mL/min；
（4）待滴加完成后，继续保温反应2～3h后，继续滴加与二乙醇胺质量相同的0.8mol/L的盐酸溶液，控制滴加时间为10～15min，随后继续保温加热反应30～45min，再旋转蒸发至原体积的1/9，制备得改性环氧树脂；
（5）按重量份数计，分别量取45～65份去离子水、15～25份二乙醇胺和20～30份上述制备的改性环氧树脂，将其搅拌混合并旋转蒸发至固含量为2～5%，即可制得一种煅烧陶瓷粉体改性碳纤维环氧上浆剂。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610151275.4A CN105568693B (zh) | 2016-03-17 | 2016-03-17 | 一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610151275.4A CN105568693B (zh) | 2016-03-17 | 2016-03-17 | 一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105568693A true CN105568693A (zh) | 2016-05-11 |
| CN105568693B CN105568693B (zh) | 2017-10-27 |
Family
ID=55879286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610151275.4A Active CN105568693B (zh) | 2016-03-17 | 2016-03-17 | 一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105568693B (zh) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108035143A (zh) * | 2017-12-29 | 2018-05-15 | 陕西科技大学 | 一种同时提高碳纤维环氧复合材料界面强度和韧性的方法 |
| CN108547151A (zh) * | 2018-03-30 | 2018-09-18 | 王景硕 | 一种水性环氧树脂碳纤维上浆剂 |
| CN110079993A (zh) * | 2019-04-28 | 2019-08-02 | 陕西科技大学 | 一种二氧化锆/氧化石墨烯表面改性碳纤维的方法 |
| CN110158317A (zh) * | 2019-05-30 | 2019-08-23 | 叶小文 | 一种高结合型碳纤维环氧上浆剂的制备方法 |
| CN110590386A (zh) * | 2019-10-11 | 2019-12-20 | 武汉理工大学 | 一种碳纤维混杂保护方法及其耐烧蚀复合材料制备 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382864A (zh) * | 2002-06-12 | 2002-12-04 | 弘生集团有限公司 | 一种纺织浆料组合物 |
| CN102212967A (zh) * | 2011-04-06 | 2011-10-12 | 东华大学 | 一种碳纳米管改性的碳纤维乳液上浆剂及其制备方法 |
| CN105178026A (zh) * | 2015-10-29 | 2015-12-23 | 山东日新复合材料有限公司 | 一种水溶性碳纤维上浆剂及其制备方法和应用 |
-
2016
- 2016-03-17 CN CN201610151275.4A patent/CN105568693B/zh active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382864A (zh) * | 2002-06-12 | 2002-12-04 | 弘生集团有限公司 | 一种纺织浆料组合物 |
| CN102212967A (zh) * | 2011-04-06 | 2011-10-12 | 东华大学 | 一种碳纳米管改性的碳纤维乳液上浆剂及其制备方法 |
| CN105178026A (zh) * | 2015-10-29 | 2015-12-23 | 山东日新复合材料有限公司 | 一种水溶性碳纤维上浆剂及其制备方法和应用 |
Non-Patent Citations (3)
| Title |
|---|
| 李超等: "水性环氧树脂碳纤维上浆剂的研制与性能分析", 《产业用纺织品》 * |
| 杨禹等: "纳米SiO2改性炭纤维乳液上浆剂的性能评价", 《复合材料学报》 * |
| 罗益锋: "国外PAN原丝及碳纤维专利分析报告（2）", 《高科技纤维与应用》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108035143A (zh) * | 2017-12-29 | 2018-05-15 | 陕西科技大学 | 一种同时提高碳纤维环氧复合材料界面强度和韧性的方法 |
| CN108035143B (zh) * | 2017-12-29 | 2020-05-12 | 陕西科技大学 | 一种同时提高碳纤维环氧复合材料界面强度和韧性的方法 |
| CN108547151A (zh) * | 2018-03-30 | 2018-09-18 | 王景硕 | 一种水性环氧树脂碳纤维上浆剂 |
| CN110079993A (zh) * | 2019-04-28 | 2019-08-02 | 陕西科技大学 | 一种二氧化锆/氧化石墨烯表面改性碳纤维的方法 |
| CN110079993B (zh) * | 2019-04-28 | 2021-09-17 | 陕西科技大学 | 一种二氧化锆/氧化石墨烯表面改性碳纤维的方法 |
| CN110158317A (zh) * | 2019-05-30 | 2019-08-23 | 叶小文 | 一种高结合型碳纤维环氧上浆剂的制备方法 |
| CN110590386A (zh) * | 2019-10-11 | 2019-12-20 | 武汉理工大学 | 一种碳纤维混杂保护方法及其耐烧蚀复合材料制备 |
| CN110590386B (zh) * | 2019-10-11 | 2022-06-17 | 武汉理工大学 | 一种碳纤维混杂保护方法及其耐烧蚀复合材料制备 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105568693B (zh) | 2017-10-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105568693A (zh) | 一种煅烧陶瓷粉体改性碳纤维环氧上浆剂的制备方法 | |
| CN108585672A (zh) | 一种水性环氧复合水泥砂浆自流平地坪及制备方法 | |
| CN107163894A (zh) | 一种高强度快干防水胶粘剂及其制备方法 | |
| CN102926198A (zh) | 一种纺织浆料 | |
| CN106220774A (zh) | 一种聚苯乙烯/石墨烯纳米复合材料的制备方法 | |
| CN105036568A (zh) | 一种稳定型玄武岩连续纤维浸润剂 | |
| CN104194415A (zh) | 一种疏水亲油改性的合成云母及其制备方法 | |
| CN107200516A (zh) | 一种改性玄武岩纤维增强火山渣轻集料混凝土及制备方法 | |
| CN108773997A (zh) | 一种玄武岩短切纤维生产工艺 | |
| CN104446075B (zh) | 一种玄武岩短切纤维分散剂及其应用方法 | |
| CN106810863A (zh) | 一种pbo纤维环氧树脂复合材料及其制备方法 | |
| CN100412262C (zh) | 有机硅织物平滑剂的制备方法 | |
| CN108659411A (zh) | 一种硅酸钙填充含氟聚合物复合材料及其制备方法 | |
| CN104673087A (zh) | 一种建筑用防剥落防水涂料及其制备方法 | |
| CN104650728A (zh) | 一种耐磨耐擦洗防水涂料及其制备方法 | |
| CN106189612A (zh) | 一种太阳能选择性吸热涂料 | |
| CN107522494A (zh) | 一种碳化硅微粉的改性方法 | |
| CN100383077C (zh) | 水泥助磨剂及其制备方法 | |
| CN104672965A (zh) | 一种附着力强抗裂性好的防水涂料及其制备方法 | |
| CN108409236A (zh) | 一种单组份室内墙体修补材料及其制备方法 | |
| CN107460779A (zh) | 一种玻纤合成树脂改性的装饰板及其制备方法 | |
| CN107903405A (zh) | 一种自乳化水性环氧合成乳液的制备工艺 | |
| CN107057494A (zh) | 一种耐刮擦保温涂料及其制备方法 | |
| CN110054858A (zh) | 一种硅烷改性碳化硅纤维及其制备方法 | |
| CN104944805A (zh) | 一种玄武岩纤维浸润剂 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Weijun Inventor before: Chou Yingying Inventor before: Sheng Yanhua Inventor before: Gao Liqun |
|
| CB03 | Change of inventor or designer information | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20170919 Address after: 224400 No. 42, salt Hing Road, Jiangsu, Yancheng City Applicant after: YANCHENG YONGYUE NEW MATERIALS CO., LTD. Address before: 221500, Changzhou, Jiangsu Province, North West villa town, East Village Committee, 87 East Bridge Applicant before: Chou Yingying |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 224000 Building 1, No. 55 Zhengtong Road, Zhangzhuang office, Yandu District, Yancheng City, Jiangsu Province Patentee after: Jiangsu Yongyue New Material Co.,Ltd. Address before: 224400 No. 42, Yanxing Road, Yancheng City, Jiangsu Province Patentee before: YANCHENG YONGYUE NEW MATERIALS Co.,Ltd. |
|
| CP03 | Change of name, title or address |