CN114875678A - 多功能导电纱线及其制备方法 - Google Patents
多功能导电纱线及其制备方法 Download PDFInfo
- Publication number
- CN114875678A CN114875678A CN202210520176.4A CN202210520176A CN114875678A CN 114875678 A CN114875678 A CN 114875678A CN 202210520176 A CN202210520176 A CN 202210520176A CN 114875678 A CN114875678 A CN 114875678A
- Authority
- CN
- China
- Prior art keywords
- conductive yarn
- fiber
- modified graphene
- graphene
- multifunctional conductive
- 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.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229920002972 Acrylic fiber Polymers 0.000 claims abstract description 55
- 239000000835 fiber Substances 0.000 claims abstract description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 30
- 229910021389 graphene Inorganic materials 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 16
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- LBSXSAXOLABXMF-UHFFFAOYSA-N 4-Vinylaniline Chemical compound NC1=CC=C(C=C)C=C1 LBSXSAXOLABXMF-UHFFFAOYSA-N 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical group CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 5
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000037452 priming Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229920000767 polyaniline Polymers 0.000 abstract description 23
- 239000010410 layer Substances 0.000 abstract description 22
- 239000004744 fabric Substances 0.000 abstract description 16
- 239000002344 surface layer Substances 0.000 abstract description 7
- 230000004044 response Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 230000006750 UV protection Effects 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 230000000977 initiatory effect Effects 0.000 description 5
- 238000005096 rolling process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000006384 oligomerization reaction Methods 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007761 roller coating Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- -1 4-aminostyrene modified graphene Chemical class 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000006467 substitution reaction 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
- D06M15/61—Polyamines polyimines
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
-
- 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
- D06M11/73—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 carbon or compounds thereof
- D06M11/74—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 carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- 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
- D06M13/325—Amines
- D06M13/332—Di- or polyamines
-
- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
-
- 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
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D10B2321/10—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Carbon And Carbon Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明涉及多功能导电纱线及其制备方法,属于导电面料技术领域。该导电纱线以腈纶纤维为基础纤维,在表层附着改性石墨烯层,改性石墨烯层的表面聚合有聚苯胺层,电荷由改性石墨烯快速导出,再由聚苯胺均匀释放,具有响应快、导电性优异的特点;本发明中使用的改性石墨烯呈褶皱状,与活化腈纶纤维有更多的结合位点,与聚苯胺有更大接触面积,提高改性石墨烯与活化腈纶纤维和聚苯胺的结合强度;此外,本发明中用两步法在纤维表层形成聚苯胺层,使得聚苯胺层残留较多的盐酸,为聚苯胺导电提供更多的质子,从而提高导电性。
Description
技术领域
本发明属于导电面料技术领域,具体地,涉及多功能导电纱线及其制备方法。
背景技术
导电纤维广泛用于抗静电衣料、防尘工作服,在半导体工业、电子精密エ业、医学、生物科学等领域有广阔的市场;
导电纤维及织物的制备工艺繁多,现有技术中应用较多的导线纤维主要有以下几类:
金属丝导电纤维:将导电性良好的金属基材通过反复模拉制成金属丝,将金属丝与织物纤维混纺制成复合纤维,利用金属丝的导电性实现导电功能,该类导电纤维纺织性能差、柔软性能差,应用在穿戴织物上不舒适。
掺杂型导电纤维:在纺丝纤维胶料中添加导电粒子,或者通过低温碳化在纤维中形成可导电炭黑,从而达到导电的效果,由于导电粒子在纤维中的分布均匀程度难以控制,难以形成连续的导电通道,导致该类导电纤维的导电性能难以提升。
原位聚合高分子导电纤维:在纤维的表层附着导电高分子材料,通过原位聚合法在纤维表层形成导电层,从而使得纤维具有导电性能,该类纤维中高分子材料与纤维的结合强度较低,耐擦洗性能差。
发明内容
为了解决背景技术中提到的技术问题,本发明的目的在于提供多功能导电纱线及其制备方法。
本发明的目的可以通过以下技术方案实现:
多功能导电纱线的制备方法,具体包括以下步骤:
步骤S1:取二乙烯三胺与去离子水混溶,向反应釜中加入腈纶纤维,再投加混溶液浸没腈纶纤维,升温至95±5℃保温反应120-180min,取出腈纶纤维用水和无水乙醇交替洗涤,干燥后得到活化腈纶纤维;通过二乙烯三胺对腈纶纤维改性,在腈纶纤维的分子侧链上接枝上含有氨基的基团,对腈纶纤维进行活化,改变其表面惰性;
步骤S2:取改性石墨烯超声分散于去离子水中制成分散液,将活化腈纶纤维投加到分散液中二浸二轧,之后烘干,重复浸泡、烘干,将改性石墨烯附着在活化腈纶纤维的表面,得到石墨烯复合腈纶纤维;
步骤S3:取苯胺、过硫酸铵、盐酸溶液、去离子水和乳化剂加入反应器中,在5-10℃恒温水浴中搅拌反应25-32min,得到预聚涂料,将石墨烯复合腈纶纤维浸入预聚涂料中,之后取出流平,得到浸涂纤维;
步骤S4:取过硫酸铵缓慢加入稀硝酸溶液中搅拌溶解得到引发液,将浸涂纤维浸入引发液中,在20-30℃浸泡反应1-1.5h,预聚涂料再聚合,形成聚苯胺层,之后取出纤维用水冲洗,得到多功能导电纱线。
进一步地,步骤S1中二乙烯三胺和去离子水的用量体积比为1:8-10。
进一步地,步骤S2中分散液中改性石墨烯的含量为80-100g/L。
进一步地,步骤S2中活化腈纶纤维在分散液中的浸轧温度为65-80℃,每道次浸泡时间为10-20min。
进一步地,步骤S3中苯胺、过硫酸铵、盐酸溶液、去离子水和乳化剂的用量比为1L:4.7-6.3g:18-25mL:1.5-2L:30-50mL;盐酸溶液的浓度为0.5mol/L,乳化剂为十二烷基苯磺酸。
进一步地,步骤S4中过硫酸铵和稀硝酸溶液的用量比为20-25g:1L,稀硝酸溶液的质量分数为3%。
进一步地,改性石墨烯由以下步骤制备:
步骤A1:将氧化石墨烯粉末超声分散于DMF中,形成均匀的氧化石墨烯分散液;
步骤A2:向氧化石墨烯分散液加入4-氨基苯乙烯,滴加氢氧化钠溶液调节pH值为9,回流反应8h,反应后抽滤,对滤饼洗涤至洗涤水接近中性,再次抽滤、干燥,得到改性石墨烯。
进一步地,氧化石墨烯粉末和DMF的用量比为120-150g:1L。
进一步地,氧化石墨烯分散液和4-氨基苯乙烯的用量比为1L:16-20mL。
多功能导电纱线,包括芯部的腈纶纤维,腈纶纤维的表面包覆有改性石墨烯,改性石墨烯的表面包覆有聚苯胺。
本发明的有益效果:
1.本发明制备的导电纱线以腈纶纤维为基础纤维,在表层附着改性石墨烯层,改性石墨烯层的表面聚合有聚苯胺层,石墨烯具有优异的导电性,聚苯胺也具有一定的导电性,当摩擦产生静电或者接触到带电体时,电荷由改性石墨烯快速导出,再由聚苯胺均匀释放,具有响应快、导电性优异的特点,石墨烯层还具有良好的抗紫外线的作用,使可应用在抗静电且需要抗紫外线的织物中。
2.本发明中采用4-氨基苯乙烯改性氧化石墨烯,氧化石墨烯上的环氧基、羧基等与4-氨基苯乙烯的氨基发生亲核取代反应,在空间位阻作用下,石墨烯呈褶皱状,活化腈纶纤维表面粗糙且接枝有氨基,褶皱状的石墨烯提供了更多的反应位点,提高改性石墨烯与纤维的结合强度,同样也提高与聚苯胺层的结合强度,另一方面增大与聚苯胺层的接触面积,有利于快速导电。
3.本发明中采用两步法在纤维表层形成聚苯胺层,先通过苯胺在少量过硫酸铵的情况下进行低聚,提高反应液的粘度,使得预聚涂料可均匀挂附在改性石墨烯表面,预聚涂料中添加较多量的盐酸为聚苯胺的导电提供质子,然后在含有较高浓度过硫酸铵的引发液中催化聚合,外层的低聚苯胺先聚合,减少预聚涂料中的盐酸析出,从而保证聚苯胺层残留较多的盐酸,从而提高导电性。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
本实施例制备一种改性石墨烯,具体实施过程如下:
步骤A1:将240g氧化石墨烯粉末超声分散于2L的DMF中,形成均匀的氧化石墨烯分散液;
步骤A2:向氧化石墨烯分散液加入32mL 4-氨基苯乙烯,滴加质量分数为10%的氢氧化钠溶液调节pH值为9,回流反应8h,反应后抽滤,对滤饼洗涤至洗涤水接近中性,最后抽滤,对滤饼采用60℃干燥箱中干燥2h,得到改性石墨烯。
实施例2
本实施例制备一种改性石墨烯,具体实施过程如下:
步骤A1:将300g氧化石墨烯粉末超声分散于2L的DMF中,形成均匀的氧化石墨烯分散液;
步骤A2:向氧化石墨烯分散液加入40mL 4-氨基苯乙烯,滴加质量分数为10%的氢氧化钠溶液调节pH值为9,回流反应8h,反应后抽滤,对滤饼洗涤至洗涤水接近中性,最后抽滤,对滤饼采用60℃干燥箱中干燥2h,得到改性石墨烯。
实施例3
本实施例制备一种多功能导电纱线,具体实施过程如下:
步骤S1:取1L二乙烯三胺与8L去离子水混溶,向反应釜中加入腈纶纤维,再投加混溶液浸没腈纶纤维,升温至95±5℃保温反应120min,取出腈纶纤维用水和无水乙醇交替洗涤1次,之后将沥干后的纤维放入干燥箱中,设置干燥温度为70℃干燥2h,得到活化腈纶纤维;通过二乙烯三胺对腈纶纤维改性,在腈纶纤维的分子侧链上接枝上含有氨基的基团,对腈纶纤维进行活化,改变其表面惰性;
步骤S2:取160g实施例1制备的改性石墨烯超声分散于2L去离子水中制成分散液,将活化腈纶纤维投加到分散液中二浸二轧,控制浸轧温度为65℃,每道次浸泡时间为20min,浸轧后在70℃干燥箱中烘干1h,重复浸轧烘干1次,将改性石墨烯附着在活化腈纶纤维的表面,石墨烯复合腈纶纤维;
步骤S3:取1L苯胺、4.7g过硫酸铵、18mL浓度为0.5mol/L的盐酸溶液、1.5L去离子水和30mL十二烷基苯磺酸加入反应器中,在5℃恒温水浴中搅拌反应32min,得到预聚涂料,将石墨烯复合腈纶纤维浸入预聚涂料中,完全浸没后取出流平,得到浸涂纤维;
步骤S4:取40g过硫酸铵缓慢加入2L质量分数为3%的稀硝酸溶液中搅拌溶解得到引发液,将浸涂纤维浸入引发液中,在30℃浸泡反应1.5h,预聚涂料再聚合,形成聚苯胺层,之后取出纤维用水冲洗,得到多功能导电纱线。
实施例4
本实施例制备一种多功能导电纱线,具体实施过程如下:
步骤S1:取1L二乙烯三胺与10L去离子水混溶,向反应釜中加入腈纶纤维,再投加混溶液浸没腈纶纤维,升温至95±5℃保温反应180min,取出腈纶纤维用水和无水乙醇交替洗涤1次,之后将沥干后的纤维放入干燥箱中,设置干燥温度为70℃干燥2h,得到活化腈纶纤维;通过二乙烯三胺对腈纶纤维改性,在腈纶纤维的分子侧链上接枝上含有氨基的基团,对腈纶纤维进行活化,改变其表面惰性;
步骤S2:取200g实施例2制备的改性石墨烯超声分散于2L去离子水中制成分散液,将活化腈纶纤维投加到分散液中二浸二轧,控制浸轧温度为80℃,每道次浸泡时间为10min,浸轧后在70℃干燥箱中烘干1h,重复浸轧烘干1次,将改性石墨烯附着在活化腈纶纤维的表面,石墨烯复合腈纶纤维;
步骤S3:取1L苯胺、6.3g过硫酸铵、25mL浓度为0.5mol/L的盐酸溶液、2L去离子水和50mL十二烷基苯磺酸加入反应器中,在10℃恒温水浴中搅拌反应25min,得到预聚涂料,将石墨烯复合腈纶纤维浸入预聚涂料中,完全浸没后取出流平,得到浸涂纤维;
步骤S4:取50g过硫酸铵缓慢加入2L质量分数为3%的稀硝酸溶液中搅拌溶解得到引发液,将浸涂纤维浸入引发液中,在30℃浸泡反应1h,预聚涂料再聚合,形成聚苯胺层,之后取出纤维用水冲洗,得到多功能导电纱线。
对比例1
本对比例制备一种多功能导电纱线,具体实施过程与实施例3相同,将步骤S2中的改性石墨烯替换为相同分量的氧化石墨烯,其余步骤均相同。
对比例2
本对比例制备一种多功能导电纱线,具体实施过程与实施例3相同,将步骤S1中的活化腈纶纤维替换为相同分量的未处理腈纶纤维,其余步骤均相同。
将实施例3、对比例1和对比例2制得的导电纱线采用纺织机纺织成面料,参照GB/T3921-2008标准,对面料进行皂洗,皂洗50次后采用光学显微镜观察面料表层的脱落情况,具体数据如表1所示:
表1
实施例3 | 对比例1 | 对比例2 | |
脱落情况 | 无可见脱落 | 几乎全部脱落 | 沿纤维凸起脱落 |
由表1数据可知,本发明制备的多功能导电纱线应用在织物上有良好的耐擦洗性能。
对比例3
本对比例制备一种多功能导电纱线,具体实施过程如下:
步骤S1:制备活化腈纶纤维,制备方法与实施例4相同;
步骤S2:取85g实施例2制备的改性石墨烯超声分散于2L去离子水中,采用分散有改性石墨烯的去离子水替换实施例4中的步骤S3的去离子水,其他操作相同,制备得到预聚涂料;之后采用与实施例4相同的方法制备多功能导电纱线。
对比例4
本对比例采用实施例4制备的石墨烯复合腈纶纤维制备一种多功能导电纱线,实施方法如下:
取1L苯胺、22g过硫酸铵、25mL浓度为0.5mol/L的盐酸溶液、2L去离子水和50mL十二烷基苯磺酸加入反应器中,在10℃恒温水浴中搅拌反应20min,得到低聚涂料,采用辊涂法在石墨烯复合腈纶纤维表面辊涂一层低聚涂料,之后将纤维牵丝过80℃的隧道式干燥箱,控制干燥时间为5min,冷却后得到多功能导电纱线。
将实施例3、实施例4、对比例3和对比例4制得的多功能导电纱线采用纺织机纺织成面料,参照GB/T24249-2009标准,使用织物感应式静电测试仪对试样布料进行测试,参照GB/T18830-2009标准,对试样布料进行抗紫外线测试,具体测试数据如表2所示:
表2
静电电压/V | 半衰期/s | UPF值 | |
实施例3 | 525 | 2.1 | 932 |
实施例4 | 497 | 1.9 | 955 |
对比例3 | 727 | 4.3 | 142 |
对比例4 | 643 | 7.6 | 928 |
由表2数据可知,采用实施例4的纱线制备的面料静电电压为497V,半衰期仅仅有1.9s,具有优异的导电性能,其UPF为955,具有优异的抗紫外线能力;对比例3中,改性石墨烯分散在聚苯胺层内部,部分区域分散效果差,没有形成连续结构,故而导电性较差,抗紫外线能力也较差;对比例4中,采用一步法制成聚苯胺层,在固化过程中盐酸易析出,聚苯胺层中含有的盐酸量较少,在导电过程中无法提供充足的质子,故而导电性较差。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (9)
1.多功能导电纱线的制备方法,其特征在于,包括以下步骤:
步骤S1:取二乙烯三胺与去离子水混溶后浸泡腈纶纤维,控制浸泡温度为95±5℃,浸泡时间为120-180min,之后洗涤、干燥得到活化腈纶纤维;
步骤S2:取改性石墨烯分散于去离子水中,将活化腈纶纤维在分散液中重复浸轧、烘干,得到石墨烯复合腈纶纤维;
步骤S3:取苯胺、过硫酸铵、盐酸溶液、去离子水和乳化剂在5-10℃下搅拌反应得到预聚涂料,将石墨烯复合腈纶纤维浸入预聚涂料中,之后取出流平,得到浸涂纤维;
步骤S4:取过硫酸铵溶于稀硝酸溶液中得到引发液,将浸涂纤维浸入引发液中,在20-30℃浸泡反应1-1.5h,之后取出冲洗得到多功能导电纱线。
2.根据权利要求1所述的多功能导电纱线的制备方法,其特征在于,步骤S1中二乙烯三胺和去离子水的用量体积比为1:8-10。
3.根据权利要求1所述的多功能导电纱线的制备方法,其特征在于,步骤S2中改性石墨烯和去离子水的用量比为80-100g:1L。
4.根据权利要求1所述的多功能导电纱线的制备方法,其特征在于,步骤S3中苯胺、过硫酸铵、盐酸溶液、去离子水和乳化剂的用量比为1L:4.7-6.3g:18-25mL:1.5-2L:30-50mL,盐酸溶液的浓度为0.5mol/L,乳化剂为十二烷基苯磺酸。
5.根据权利要求1所述的多功能导电纱线的制备方法,其特征在于,步骤S4中过硫酸铵和稀硝酸溶液的用量比为20-25g:1L,稀硝酸溶液的质量分数为3%。
6.根据权利要求1所述的多功能导电纱线的制备方法,其特征在于,改性石墨烯由以下步骤制备:
步骤A1:将氧化石墨烯粉末超声分散于DMF中,形成均匀的氧化石墨烯分散液;
步骤A2:向氧化石墨烯分散液加入4-氨基苯乙烯,滴加氢氧化钠溶液调节pH值为9,回流反应8h,反应后抽滤并对滤饼洗涤、干燥,得到改性石墨烯。
7.根据权利要求6所述的多功能导电纱线的制备方法,其特征在于,氧化石墨烯粉末和DMF的用量比为120-150g:1L。
8.根据权利要求6所述的多功能导电纱线的制备方法,其特征在于,氧化石墨烯分散液和4-氨基苯乙烯的用量比为1L:16-20mL。
9.多功能导电纱线,其特征在于,由权利要求1-8任意一项所述的方法制备而成。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210520176.4A CN114875678A (zh) | 2022-05-12 | 2022-05-12 | 多功能导电纱线及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210520176.4A CN114875678A (zh) | 2022-05-12 | 2022-05-12 | 多功能导电纱线及其制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114875678A true CN114875678A (zh) | 2022-08-09 |
Family
ID=82676096
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210520176.4A Pending CN114875678A (zh) | 2022-05-12 | 2022-05-12 | 多功能导电纱线及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114875678A (zh) |
Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104313873A (zh) * | 2014-10-11 | 2015-01-28 | 江南大学 | 一种石墨烯/聚苯胺自组装柔性导电织物的制备方法 |
KR101489174B1 (ko) * | 2013-10-25 | 2015-02-03 | 한국원자력연구원 | 기능화된 그래핀의 제조방법과 이에 따라 제조된 기능화된 그래핀 |
CN105821653A (zh) * | 2016-04-18 | 2016-08-03 | 邯郸派瑞电器有限公司 | 一种聚丙烯腈抗菌纤维的制备方法 |
US9434826B2 (en) * | 2015-01-05 | 2016-09-06 | The Boeing Company | Graphene-augmented carbon fiber for aerospace composites |
CN106183316A (zh) * | 2016-07-08 | 2016-12-07 | 东华大学 | 一种柔性导电复合织物及其制备和应用 |
WO2018166477A1 (zh) * | 2017-03-15 | 2018-09-20 | 山东圣泉新材料股份有限公司 | 一种改性纤维制品、制备方法及其用途 |
CN109003837A (zh) * | 2018-07-23 | 2018-12-14 | 成都新柯力化工科技有限公司 | 一种用于智能纺织品的复合电极材料及制备方法 |
CN109930377A (zh) * | 2019-02-20 | 2019-06-25 | 常州市海若纺织品有限公司 | 一种聚苯胺复合长效导电涤纶纤维的制备方法 |
CN111118907A (zh) * | 2019-12-28 | 2020-05-08 | 宜禾股份有限公司 | 一种应用于防护服的聚苯胺芳纶复合导电纤维的制备工艺 |
CN111172745A (zh) * | 2020-01-21 | 2020-05-19 | 黑龙江科技大学 | 一种石墨烯、聚苯胺和涤纶复合导电纤维的制备方法 |
US20200281497A1 (en) * | 2017-09-13 | 2020-09-10 | Allegheny Singer Research Institute | Conductive Fiber with Polythiophene Coating |
CN112900076A (zh) * | 2021-01-31 | 2021-06-04 | 福建沃凯丝化纤有限公司 | 一种多功能涤纶纤维及其制备方法 |
WO2021114321A1 (zh) * | 2019-12-13 | 2021-06-17 | 中国科学院深圳先进技术研究院 | 一种柔性导电纤维膜材料及其制备方法 |
-
2022
- 2022-05-12 CN CN202210520176.4A patent/CN114875678A/zh active Pending
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101489174B1 (ko) * | 2013-10-25 | 2015-02-03 | 한국원자력연구원 | 기능화된 그래핀의 제조방법과 이에 따라 제조된 기능화된 그래핀 |
CN104313873A (zh) * | 2014-10-11 | 2015-01-28 | 江南大学 | 一种石墨烯/聚苯胺自组装柔性导电织物的制备方法 |
US9434826B2 (en) * | 2015-01-05 | 2016-09-06 | The Boeing Company | Graphene-augmented carbon fiber for aerospace composites |
CN105821653A (zh) * | 2016-04-18 | 2016-08-03 | 邯郸派瑞电器有限公司 | 一种聚丙烯腈抗菌纤维的制备方法 |
CN106183316A (zh) * | 2016-07-08 | 2016-12-07 | 东华大学 | 一种柔性导电复合织物及其制备和应用 |
WO2018166477A1 (zh) * | 2017-03-15 | 2018-09-20 | 山东圣泉新材料股份有限公司 | 一种改性纤维制品、制备方法及其用途 |
US20200281497A1 (en) * | 2017-09-13 | 2020-09-10 | Allegheny Singer Research Institute | Conductive Fiber with Polythiophene Coating |
CN109003837A (zh) * | 2018-07-23 | 2018-12-14 | 成都新柯力化工科技有限公司 | 一种用于智能纺织品的复合电极材料及制备方法 |
CN109930377A (zh) * | 2019-02-20 | 2019-06-25 | 常州市海若纺织品有限公司 | 一种聚苯胺复合长效导电涤纶纤维的制备方法 |
WO2021114321A1 (zh) * | 2019-12-13 | 2021-06-17 | 中国科学院深圳先进技术研究院 | 一种柔性导电纤维膜材料及其制备方法 |
CN111118907A (zh) * | 2019-12-28 | 2020-05-08 | 宜禾股份有限公司 | 一种应用于防护服的聚苯胺芳纶复合导电纤维的制备工艺 |
CN111172745A (zh) * | 2020-01-21 | 2020-05-19 | 黑龙江科技大学 | 一种石墨烯、聚苯胺和涤纶复合导电纤维的制备方法 |
CN112900076A (zh) * | 2021-01-31 | 2021-06-04 | 福建沃凯丝化纤有限公司 | 一种多功能涤纶纤维及其制备方法 |
Non-Patent Citations (3)
Title |
---|
于荣荣;田明伟;曲丽君;刘洋洋;赵珊珊;迟淑丽;杜敏芝;: "石墨烯复合纤维与纺织品的功能", 染整技术, no. 06, pages 14 - 19 * |
卢神州: "《纺织化学TEXTILE CHEMISTRY》", 31 August 2021, 东华大学出版社, pages: 75 * |
张锦: "《石墨烯表征技术》", 31 October 2021, 华东理工大学出版社, pages: 38 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN1318683C (zh) | 一种导电纤维的制备方法及其制品 | |
CN101403189B (zh) | 一种自组装多功能聚苯胺/纯棉复合导电织物的制备方法 | |
CN108330684A (zh) | 一种多功能棉织物及其制备方法 | |
CN107956110B (zh) | 一种还原氧化石墨烯/聚丙烯腈复合纤维及其制备方法 | |
CN112480581B (zh) | 改性聚乙烯醇/纳米金属复合的柔性拉伸应变传感材料制备方法 | |
CN101613943B (zh) | 一种层层自组装聚苯胺/尼龙复合导电织物的制备方法 | |
CN102444023A (zh) | 聚苯胺复合纳米银导电纤维制备方法 | |
CN108625158A (zh) | 一种抗静电石墨烯涂层织物及其制备方法 | |
CN102002858B (zh) | 一种导电纤维素纤维及其制备方法 | |
CN114875678A (zh) | 多功能导电纱线及其制备方法 | |
CN108389729B (zh) | 一种石墨烯织物电极或纱线电极的制备方法及在超级电容器中的应用 | |
CN101168923A (zh) | 导电织物纤维的制备方法 | |
CN102011313A (zh) | 一种聚吡咯/纳米铂复合导电纤维及其制备方法 | |
CN113005781B (zh) | 一种基于级联催化接枝聚合的导电织物加工方法 | |
CN116180296A (zh) | 一种抗菌面料及其制备方法 | |
CN111139637B (zh) | 一种涂覆织物基材及其制备方法与使用方法 | |
CN115874304A (zh) | 一种抗静电的纺织面料的制备方法 | |
CN114381932A (zh) | 一种轻质防静电面料及其制备方法 | |
CN110656391B (zh) | 一种复合导电面料及其制造方法 | |
CN108060586B (zh) | 一种高导电性的击剑服 | |
KR102264311B1 (ko) | 전도성 및 산화방지성이 우수한 섬유의 제조방법 | |
CN112962316A (zh) | 一种导电安全面料及其制备方法 | |
TW202033860A (zh) | 導電紗線的製造方法 | |
CN110230137A (zh) | 一种有机碳黑导电纱线及其制备工艺 | |
CN115305718B (zh) | 一种高电阻柔性非织造材料及其生产工艺 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |