CN110373003A - 一种增强型碳纤维短纤复合板的制备方法 - Google Patents
一种增强型碳纤维短纤复合板的制备方法 Download PDFInfo
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- CN110373003A CN110373003A CN201910505518.3A CN201910505518A CN110373003A CN 110373003 A CN110373003 A CN 110373003A CN 201910505518 A CN201910505518 A CN 201910505518A CN 110373003 A CN110373003 A CN 110373003A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 122
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- 239000011347 resin Substances 0.000 claims abstract description 25
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
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- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 claims description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 7
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 6
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- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 6
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- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
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- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
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- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 3
- 150000003505 terpenes Chemical class 0.000 claims description 3
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
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- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 abstract description 6
- 239000004566 building material Substances 0.000 abstract description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
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- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 241000274582 Pycnanthus angolensis Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- 150000001412 amines Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 229910003460 diamond Inorganic materials 0.000 description 1
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- MHUWZNTUIIFHAS-CLFAGFIQSA-N dioleoyl phosphatidic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(COP(O)(O)=O)OC(=O)CCCCCCC\C=C/CCCCCCCC MHUWZNTUIIFHAS-CLFAGFIQSA-N 0.000 description 1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
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- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 1
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- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 239000011120 plywood Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/02—Polyglycidyl ethers of bis-phenols
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2445/00—Characterised by the use of homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic ring system; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2457/00—Characterised by the use of unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C08J2457/02—Copolymers of mineral oil hydrocarbons
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2493/00—Characterised by the use of natural resins; Derivatives thereof
- C08J2493/04—Rosin
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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Abstract
本发明公开了一种增强型碳纤维短纤复合板的制备方法,属于建筑材料技术领域。本发明将碳纤维与氢氧化钠溶液混合,浸泡,过滤,冷冻粉碎,过筛,洗涤,干燥,得预处理碳纤维;将预处理碳纤维,二沉池污泥,蔗糖,水混合发酵,接着滴加和硝酸铁溶液,搅拌混合,过滤,干燥,炭化,即得改性碳纤维;按重量份数计,将40~60份环氧树脂,20~30份稀释剂,15~20份改性碳纤维,5~8份固化剂,5~8份植物精油,5~8份增稠树脂,3~5份改性添加料,搅拌混合,注模,压制成型,脱模,即得增强型碳纤维短纤复合板。本发明提供的增强型碳纤维短纤复合板具有优异的力学性能。
Description
技术领域
本发明公开了一种增强型碳纤维短纤复合板的制备方法,属于建筑材料技术领域。
背景技术
传统的冷藏车箱板、豪华房车面板、物流车面板等为实现保温,所使用的板材通常是采用钢结构加聚氨酯泡沫复合形成,而因钢结构导热系数大,使得其保温效果欠佳,同时钢材密度大,给车子本身增加了能耗,时间长了宜发生腐蚀。碳纤维因其质量比金属铝轻,但其强度要高于钢铁,且其具有耐腐蚀、高模量的特性,常被用于制作成板材,采用碳纤维布浸渍环氧树脂胶制成,其具有抗拉强度高的特点,同时还提高了抗压、抗弯、抗扭、抗剪切强度,但是,因该板材几乎完全采用了碳纤维,导致其碳纤维材料的使用量大大增加,增加了生产成本。
而现有的碳纤维板材的制作方法,通常是采用的模压成型,采用模压成型的方法在制作碳纤维板材时存在以下缺点:不能有效避免复合板中各材料层间存在气泡,导致复合板的致密性得不到保证,同时一般在制作过程完成后使用时,为了防腐,还需在复合板的表面涂抹一层油漆,在长期露天使用过程中,油漆易发生开裂。碳纤维是指在惰性气氛中,由有机纤维或者沥青纤维经过高温碳化而成的碳素纤维,该纤维分子结构介于金刚石和石墨之间,含碳量超过90%的多环结构,目前商业和军事用碳纤维按照原料的不同可以分为三大类,分别为:黏胶基、沥青基以及聚丙烯腈基碳纤维。联合碳化物公司在1959年开展了对碳纤维的研究,开发并生产了黏胶基碳纤维,同时期,A.Shindo采用聚丙烯腈纤维为基础原料,发明了生产聚丙烯腈基碳纤维的方法,几乎同时间,某研究院优化了聚丙烯腈基碳纤维的技术方案和工艺条件,实现了高性能聚丙烯腈基碳纤维的工业化制造,联合碳化物公司在1970年又研究开发了高性能沥青基碳纤维,此后,碳纤维的制造工艺取得了飞速的发展,其中聚丙烯腈基碳纤维由于其生产工艺简单,产品性能稳定,力学性能优异,在制造工艺上取得了长足的进步,已发展成为如今碳纤维工业的主流。做为一种高性能纤维,碳纤维具有低密度、强度高、热膨胀系数小、耐高温、摩擦系数小、导电性好、耐高温等突出特点,密度是钢的四分之一,强度是钢的5~6倍。此外,碳纤维的化学特性也非常优秀,具有耐酸碱性好,抗辐射,耐油,抗放射等特性。
碳纤维由于其一系列的优异性能被用作高性能复合材料的主要增强材料。碳纤维复合材料因为具有轻质高强等优良性能,在航空航天、土木建筑、清洁能源等领域都取得了广泛的应用,成为未来材料发展的重要方向。目前传统的碳纤维短纤复合板还存在力学性能无法进一步提升的问题,因此还需对其进行研究。
发明内容
本发明主要解决的技术问题是:针对传统增强型碳纤维短纤复合板力学性能不佳的问题,提供了一种增强型碳纤维短纤复合板的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
(1)将碳纤维与氢氧化钠溶液按质量比1:10~1:20混合,浸泡,过滤,冷冻粉碎,过筛,洗涤,干燥,得预处理碳纤维;
(2)按重量份数计,将20~30份预处理碳纤维,2~3份二沉池污泥,1~2份蔗糖,30~50份水混合发酵,接着滴加碳纤维质量0.2~0.3倍的尿素溶液和碳纤维质量0.2~0.3倍的硝酸铁溶液,搅拌混合,过滤,干燥,炭化,即得改性碳纤维;
(3)按重量份数计,将40~60份环氧树脂,20~30份稀释剂,15~20份改性碳纤维,5~8份固化剂,5~8份植物精油,5~8份增稠树脂,3~5份改性添加料,搅拌混合,注模,压制成型,脱模,即得增强型碳纤维短纤复合板。
步骤(3)所述环氧树脂为环氧树脂E51,环氧树脂E44或环氧树脂E20中任意一种。
步骤(3)所述稀释剂为甲苯,二甲苯,丙酮或乙醇中的任意一种。
步骤(3)所述固化剂为二己基三胺、二乙氨基丙胺或三乙烯四胺中的任意一种。
步骤(3)所述植物精油为迷迭香精油,薰衣草精油,玫瑰花精油,茉莉花精油,茶花精油或雪莲精油中的任意一种。
步骤(3)所述增粘树脂为松香,石油树脂或萜烯树脂中任意一种。
步骤(3)所述改性添加料的制备过程为:将海泡石与四氧化三铁按质量比10:1~20:1粉碎,过筛,焙烧,得预处理海泡石,按重量份数计,将30~40份预处理海泡石,10~20份硅烷偶联剂KH-550,20~30份无水乙醇,40~60份水混合,接着滴加盐酸调节pH至3.8~4.0,恒温搅拌反应,过滤,洗涤,干燥,即得改性添加料。
步骤(1)所述碳纤维还可以为改性碳纤维;所述改性碳纤维的改性过程为:
(1)将碳纤维和浓度为4g/L的多巴胺溶液按质量比为1:4~1:8混合后,以3~5mL/min速率持续通入空气10~20min后,得碳纤维分散液;
(2)将碳纤维分散液和质量分数为8~10%的氯化亚铁溶液混合后,加热搅拌反应,再经离心分离,真空冷冻干燥后,球磨,得球磨料,即为改性碳纤维;
所述碳纤维选用长度为10~20mm,直径为3~8μm的碳纤维短纤。
步骤(2)所述水中还可以加入蔗糖等质量的硫代硫酸钠。
本发明的有益效果是:
(1)本发明通过添加改性碳纤维和改性添加料,首先,在制备过程中,碳纤维经过氢氧化钠溶液浸泡,再经过冷冻球磨,使得碳纤维表面出现大量的缺陷或沟壑,接着,将预处理碳纤维,二沉池污泥,蔗糖,水混合发酵,碳纤维表面存在的大量缺陷或沟壑为细菌的繁殖提供了场所,接着通过添加硝酸铁溶液,由于细菌细胞表面带负电荷,使其能够大量的富集体系中的铁离子,在保温炭化过程中,改性碳纤维表面的有机质炭化,同时产生焦油,随着温度的升高,体系中铁离子被还原成单质铁,在使用过程中,改性碳纤维中渗出的焦油能够改善其与基体树脂间的界面结合,从而使得体系的力学性能得到提升,同时,改性碳纤维表面包裹的单质铁能够吸引含四氧化三铁的改性添加料,改性添加料中的海泡石能够在极性溶剂中分散成海泡石纤维束,海泡石纤维束通过磁力附着在改性填料表面,使得改性填料表面的粗糙度得到进一步的提升,从而使得纤维间更易缠结咬合,从而使得体系的力学性能得到进一步的提升;
(2)本发明技术方案旨在解决利用碳纤维制备的板材力学性能不佳的问题,通过改变纤维的表面物理结构,以实现纤维和纤维之间,尤其是碳纤维短纤和短纤之间的结合方式的改变,由传统工艺中较弱的相互作用转变为缠结咬合,该结合方式主要依赖于碳纤维表面物理结构的改善,而通过对碳纤维进一步改性后,再进行后续处理,有利于更进一步的改善碳纤维的表面状况,使其更利于生成缠结咬合的机械结构,该改性过程中,主要依赖多巴胺的还原作用,使体系中亚铁离子转变为纳米结构的单质铁粉,再以此铁粉为硬质核心,在球磨过程中,改善碳纤维的表面结构。
具体实施方式
将碳纤维和浓度为4g/L的多巴胺溶液按质量比为1:4~1:8混合后,以3~5mL/min速率持续通入空气10~20min后,得碳纤维分散液;将碳纤维分散液和质量分数为8~10%的氯化亚铁溶液混合后,加热搅拌反应,再经离心分离,真空冷冻干燥后,球磨,得球磨料,即为改性碳纤维;所述碳纤维选用长度为10~20mm,直径为3~8μm的碳纤维短纤;将海泡石海泡石与四氧化三铁按质量比10:1~20:1置于球磨机中球磨粉碎,过120目的筛,得细化海泡石,接着将细化海泡石置于马弗炉中,于温度为650~750℃条件下,焙烧2~3h,得预处理海泡石,按重量份数计,将30~40份预处理海泡石,10~20份硅烷偶联剂KH-550,20~30份无水乙醇,40~60份水置于1号烧杯中,于转速为300~500r/min条件下,搅拌混合40~60min,接着向1号烧杯中滴加质量分数为10~20%的盐酸调节pH至3.8~4.0,接着将1号烧杯置于数显测速恒温磁力搅拌器中,于温度为60~80℃,转速为400~600r/min条件下,恒温搅拌反应1~2h,得混合浆液,再将混合浆液过滤,得1号滤饼,接着将1号滤饼用去离子水洗涤3~5次洗涤,接着将洗涤后的1号滤饼置于烘箱中,于温度为105~110℃条件下,干燥至恒重,即得改性添加料;将改性碳纤维与质量分数为30~35%的氢氧化钠溶液按质量比1:10~1:20置于反应釜中,于转速为300~500r/min条件下,搅拌混合浸泡2~3h后,过滤,得滤渣,接着将滤渣置于液氮中,得冷冻块,接着将冷冻块置于球磨机中球磨粉碎,过300目的筛,得球磨料,接着将球磨料用去离子水洗涤3~5次,接着将洗涤后的球磨料置于烘箱中,于温度为105~110℃条件下,干燥至恒重,得预处理碳纤维;按重量份数计,将20~30份预处理碳纤维,2~3份二沉池污泥,1~2份蔗糖,30~50份水置于发酵釜中,并加入蔗糖等质量的硫代硫酸钠,于温度为30~35℃,转速为100~200r/min条件下,混合发酵3~5天,接着向发酵釜中滴加碳纤维质量0.2~0.3倍质量分数为10~20%的尿素溶液和碳纤维质量0.2~0.3倍质量分数为10~20%的硝酸铁溶液,于转速为600~800r/min条件下,搅拌混合40~60in后,过滤,得2号滤饼,接着将2号滤饼置于烘箱中,于温度为105~110℃条件下,干燥至恒重,得干燥2号滤饼,接着将干燥2号滤饼置于炭化炉中,并以60~90mL/min速率向炉内充入氮气,于温度为1050~1150℃条件下,炭化1~2h后,随炉降至室温,即得改性碳纤维;按重量份数计,将40~60份环氧树脂,20~30份稀释剂,15~20份改性碳纤维,5~8份固化剂,5~8份植物精油,5~8份增稠树脂,3~5份改性添加料置于混料机中,于转速为600~800r/min条件下,搅拌混合40~60min,得混合浆料,接着向模具表面喷洒甲基硅油,接着将混合浆料注入模具中,接着将模具置于成型中,于温度为150~165℃,压力为2~3MPa条件下,压制成型后,脱模,即得增强型碳纤维短纤复合板。所述环氧树脂为环氧树脂E51,环氧树脂E44或环氧树脂E20中任意一种。所述稀释剂为甲苯,二甲苯,丙酮或乙醇中的任意一种。所述固化剂为二己基三胺、二乙氨基丙胺或三乙烯四胺中的任意一种。所述植物精油为迷迭香精油,薰衣草精油,玫瑰花精油,茉莉花精油,茶花精油或雪莲精油中的任意一种。所述增粘树脂为松香,石油树脂或萜烯树脂中任意一种。
实例1
将碳纤维和浓度为4g/L的多巴胺溶液按质量比为1:8混合后,以5mL/min速率持续通入空气20min后,得碳纤维分散液;将碳纤维分散液和质量分数为10%的氯化亚铁溶液混合后,加热搅拌反应,再经离心分离,真空冷冻干燥后,球磨,得球磨料,即为改性碳纤维;所述碳纤维选用长度为10~20mm,直径为3~8μm的碳纤维短纤;将海泡石海泡石与四氧化三铁按质量比20:1置于球磨机中球磨粉碎,过120目的筛,得细化海泡石,接着将细化海泡石置于马弗炉中,于温度为750℃条件下,焙烧3h,得预处理海泡石,按重量份数计,将40份预处理海泡石,20份硅烷偶联剂KH-550,30份无水乙醇,60份水置于1号烧杯中,于转速为500r/min条件下,搅拌混合60min,接着向1号烧杯中滴加质量分数为20%的盐酸调节pH至4.0,接着将1号烧杯置于数显测速恒温磁力搅拌器中,于温度为80℃,转速为600r/min条件下,恒温搅拌反应2h,得混合浆液,再将混合浆液过滤,得1号滤饼,接着将1号滤饼用去离子水洗涤5次洗涤,接着将洗涤后的1号滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,即得改性添加料;将改性碳纤维与质量分数为35%的氢氧化钠溶液按质量比1:20置于反应釜中,于转速为500r/min条件下,搅拌混合浸泡3h后,过滤,得滤渣,接着将滤渣置于液氮中,得冷冻块,接着将冷冻块置于球磨机中球磨粉碎,过300目的筛,得球磨料,接着将球磨料用去离子水洗涤5次,接着将洗涤后的球磨料置于烘箱中,于温度为110℃条件下,干燥至恒重,得预处理碳纤维;按重量份数计,将30份预处理碳纤维,3份二沉池污泥,2份蔗糖,50份水置于发酵釜中,并加入蔗糖等质量的硫代硫酸钠,于温度为35℃,转速为200r/min条件下,混合发酵5天,接着向发酵釜中滴加碳纤维质量0.3倍质量分数为20%的尿素溶液和碳纤维质量0.3倍质量分数为20%的硝酸铁溶液,于转速为800r/min条件下,搅拌混合60in后,过滤,得2号滤饼,接着将2号滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,得干燥2号滤饼,接着将干燥2号滤饼置于炭化炉中,并以90mL/min速率向炉内充入氮气,于温度为1150℃条件下,炭化2h后,随炉降至室温,即得改性碳纤维;按重量份数计,将60份环氧树脂,30份稀释剂,20份改性碳纤维,8份固化剂,8份植物精油,8份增稠树脂,5份改性添加料置于混料机中,于转速为800r/min条件下,搅拌混合60min,得混合浆料,接着向模具表面喷洒甲基硅油,接着将混合浆料注入模具中,接着将模具置于成型中,于温度为165℃,压力为3MPa条件下,压制成型后,脱模,即得增强型碳纤维短纤复合板。所述环氧树脂为环氧树脂E51。所述稀释剂为甲苯。所述固化剂为二己基三胺。所述植物精油为迷迭香精油。所述增粘树脂为松香。
实例2
将海泡石海泡石与四氧化三铁按质量比20:1置于球磨机中球磨粉碎,过120目的筛,得细化海泡石,接着将细化海泡石置于马弗炉中,于温度为750℃条件下,焙烧3h,得预处理海泡石,按重量份数计,将40份预处理海泡石,20份硅烷偶联剂KH-550,30份无水乙醇,60份水置于1号烧杯中,于转速为500r/min条件下,搅拌混合60min,接着向1号烧杯中滴加质量分数为20%的盐酸调节pH至4.0,接着将1号烧杯置于数显测速恒温磁力搅拌器中,于温度为80℃,转速为600r/min条件下,恒温搅拌反应2h,得混合浆液,再将混合浆液过滤,得1号滤饼,接着将1号滤饼用去离子水洗涤5次洗涤,接着将洗涤后的1号滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,即得改性添加料;按重量份数计,将60份环氧树脂,30份稀释剂,20份碳纤维,8份固化剂,8份植物精油,8份增稠树脂,5份改性添加料置于混料机中,于转速为800r/min条件下,搅拌混合60min,得混合浆料,接着向模具表面喷洒甲基硅油,接着将混合浆料注入模具中,接着将模具置于成型中,于温度为165℃,压力为3MPa条件下,压制成型后,脱模,即得增强型碳纤维短纤复合板。所述环氧树脂为环氧树脂E51。所述稀释剂为甲苯。所述固化剂为二己基三胺。所述植物精油为迷迭香精油。所述增粘树脂为松香。
实例3
将海泡石海泡石与四氧化三铁按质量比20:1置于球磨机中球磨粉碎,过120目的筛,得细化海泡石,接着将细化海泡石置于马弗炉中,于温度为750℃条件下,焙烧3h,得预处理海泡石,按重量份数计,将40份预处理海泡石,20份硅烷偶联剂KH-550,30份无水乙醇,60份水置于1号烧杯中,于转速为500r/min条件下,搅拌混合60min,接着向1号烧杯中滴加质量分数为20%的盐酸调节pH至4.0,接着将1号烧杯置于数显测速恒温磁力搅拌器中,于温度为80℃,转速为600r/min条件下,恒温搅拌反应2h,得混合浆液,再将混合浆液过滤,得1号滤饼,接着将1号滤饼用去离子水洗涤5次洗涤,接着将洗涤后的1号滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,即得改性添加料;将碳纤维与质量分数为35%的氢氧化钠溶液按质量比1:20置于反应釜中,于转速为500r/min条件下,搅拌混合浸泡3h后,过滤,得滤渣,接着将滤渣置于液氮中,得冷冻块,接着将冷冻块置于球磨机中球磨粉碎,过300目的筛,得球磨料,接着将球磨料用去离子水洗涤5次,接着将洗涤后的球磨料置于烘箱中,于温度为110℃条件下,干燥至恒重,得预处理碳纤维;按重量份数计,将30份预处理碳纤维,3份二沉池污泥,2份蔗糖,50份水置于发酵釜中,于温度为35℃,转速为200r/min条件下,混合发酵5天,接着向发酵釜中滴加碳纤维质量0.3倍质量分数为20%的尿素溶液和碳纤维质量0.3倍质量分数为20%的硝酸铁溶液,于转速为800r/min条件下,搅拌混合60in后,过滤,得2号滤饼,接着将2号滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,得干燥2号滤饼,接着将干燥2号滤饼置于炭化炉中,并以90mL/min速率向炉内充入氮气,于温度为1150℃条件下,炭化2h后,随炉降至室温,即得改性碳纤维;按重量份数计,将60份环氧树脂,30份稀释剂,20份改性碳纤维,8份固化剂,8份增稠树脂,5份改性添加料置于混料机中,于转速为800r/min条件下,搅拌混合60min,得混合浆料,接着向模具表面喷洒甲基硅油,接着将混合浆料注入模具中,接着将模具置于成型中,于温度为165℃,压力为3MPa条件下,压制成型后,脱模,即得增强型碳纤维短纤复合板。所述环氧树脂为环氧树脂E51。所述稀释剂为甲苯。所述固化剂为二己基三胺。所述增粘树脂为松香。
实例4
将碳纤维与质量分数为35%的氢氧化钠溶液按质量比1:20置于反应釜中,于转速为500r/min条件下,搅拌混合浸泡3h后,过滤,得滤渣,接着将滤渣置于液氮中,得冷冻块,接着将冷冻块置于球磨机中球磨粉碎,过300目的筛,得球磨料,接着将球磨料用去离子水洗涤5次,接着将洗涤后的球磨料置于烘箱中,于温度为110℃条件下,干燥至恒重,得预处理碳纤维;按重量份数计,将30份预处理碳纤维,3份二沉池污泥,2份蔗糖,50份水置于发酵釜中,于温度为35℃,转速为200r/min条件下,混合发酵5天,接着向发酵釜中滴加碳纤维质量0.3倍质量分数为20%的尿素溶液和碳纤维质量0.3倍质量分数为20%的硝酸铁溶液,于转速为800r/min条件下,搅拌混合60in后,过滤,得2号滤饼,接着将2号滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,得干燥2号滤饼,接着将干燥2号滤饼置于炭化炉中,并以90mL/min速率向炉内充入氮气,于温度为1150℃条件下,炭化2h后,随炉降至室温,即得改性碳纤维;按重量份数计,将60份环氧树脂,30份稀释剂,20份改性碳纤维,8份固化剂,8份植物精油,8份增稠树脂置于混料机中,于转速为800r/min条件下,搅拌混合60min,得混合浆料,接着向模具表面喷洒甲基硅油,接着将混合浆料注入模具中,接着将模具置于成型中,于温度为165℃,压力为3MPa条件下,压制成型后,脱模,即得增强型碳纤维短纤复合板。所述环氧树脂为环氧树脂E51。所述稀释剂为甲苯。所述固化剂为二己基三胺。所述植物精油为迷迭香精油。所述增粘树脂为松香。
对比例:无锡某新材料有限公司生产的增强型碳纤维短纤复合板。
将实例1至4所得增强型碳纤维短纤复合板和对比例产品进行性能检测,具体检测方法如下:
采用CMT4204型微机控制电子万能试验机测试上述增强型碳纤维短纤复合板的界面剪切强度。具体检测结果如表1所示:
表1:性能检测表
| 检测内容 | 实例1 | 实例2 | 实例3 | 实例4 | 对比例 |
| 界面剪切强度/MPa | 84.8 | 60.4 | 56.8 | 57.2 | 39.2 |
由表1检测结果可知,本发明所得增强型碳纤维短纤复合板具有优异的力学性能。
Claims (9)
1.一种增强型碳纤维短纤复合板的制备方法,其特征在于具体指步骤如下:
(1)将碳纤维与氢氧化钠溶液按质量比1:10~1:20混合,浸泡,过滤,冷冻粉碎,过筛,洗涤,干燥,得预处理碳纤维;
(2)按重量份数计,将20~30份预处理碳纤维,2~3份二沉池污泥,1~2份蔗糖,30~50份水混合发酵,接着滴加碳纤维质量0.2~0.3倍的尿素溶液和碳纤维质量0.2~0.3倍的硝酸铁溶液,搅拌混合,过滤,干燥,炭化,即得改性碳纤维;
(3)按重量份数计,将40~60份环氧树脂,20~30份稀释剂,15~20份改性碳纤维,5~8份固化剂,5~8份植物精油,5~8份增稠树脂,3~5份改性添加料,搅拌混合,注模,压制成型,脱模,即得增强型碳纤维短纤复合板。
2.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(3)所述环氧树脂为环氧树脂E51,环氧树脂E44或环氧树脂E20中任意一种。
3.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(3)所述稀释剂为甲苯,二甲苯,丙酮或乙醇中的任意一种。
4.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(3)所述固化剂为二己基三胺、二乙氨基丙胺或三乙烯四胺中的任意一种。
5.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(3)所述植物精油为迷迭香精油,薰衣草精油,玫瑰花精油,茉莉花精油,茶花精油或雪莲精油中的任意一种。
6.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(3)所述增粘树脂为松香,石油树脂或萜烯树脂中任意一种。
7.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(3)所述改性添加料的制备过程为:将海泡石与四氧化三铁按质量比10:1~20:1粉碎,过筛,焙烧,得预处理海泡石,按重量份数计,将30~40份预处理海泡石,10~20份硅烷偶联剂KH-550,20~30份无水乙醇,40~60份水混合,接着滴加盐酸调节pH至3.8~4.0,恒温搅拌反应,过滤,洗涤,干燥,即得改性添加料。
8.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(1)所述碳纤维还可以为改性碳纤维;所述改性碳纤维的改性过程为:
(1)将碳纤维和浓度为4g/L的多巴胺溶液按质量比为1:4~1:8混合后,以3~5mL/min速率持续通入空气10~20min后,得碳纤维分散液;
(2)将碳纤维分散液和质量分数为8~10%的氯化亚铁溶液混合后,加热搅拌反应,再经离心分离,真空冷冻干燥后,球磨,得球磨料,即为改性碳纤维;
所述碳纤维选用长度为10~20mm,直径为3~8μm的碳纤维短纤。
9.根据权利要求1所述一种增强型碳纤维短纤复合板的制备方法,其特征在于:步骤(2)所述水中还可以加入蔗糖等质量的硫代硫酸钠。
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