CN114437286A - 一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料及其制备方法 - Google Patents
一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料及其制备方法 Download PDFInfo
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 132
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 66
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 45
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000009987 spinning Methods 0.000 title claims abstract description 15
- 238000004513 sizing Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 25
- 239000003999 initiator Substances 0.000 claims abstract description 19
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 15
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims abstract description 14
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 9
- -1 polyoxyethylene methyl ether Polymers 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
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- 238000003756 stirring Methods 0.000 claims description 6
- JUEDJIRGERJMGO-UHFFFAOYSA-N C(C)(C)[Na].C(C=C)(=O)N Chemical compound C(C)(C)[Na].C(C=C)(=O)N JUEDJIRGERJMGO-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
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- 238000007664 blowing Methods 0.000 claims description 2
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
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- 238000005303 weighing Methods 0.000 description 6
- 239000004753 textile Substances 0.000 description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical group [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000001632 sodium acetate Substances 0.000 description 4
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- 229920000742 Cotton Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical class COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 238000007605 air drying Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- KIZFHUJKFSNWKO-UHFFFAOYSA-M calcium monohydroxide Chemical compound [Ca]O KIZFHUJKFSNWKO-UHFFFAOYSA-M 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
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- 229920001519 homopolymer Polymers 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical group [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1803—C3-(meth)acrylate, e.g. (iso)propyl (meth)acrylate
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- 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
- D06M11/76—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 oxides or carbonates
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- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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Abstract
本发明公开了一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料及其制备方法,其各原料按重量份的组成为:改性纳米碳酸钙1~3份,丙烯酰胺5~9份,丙烯酸丙酯23~27份,丙烯酸丁酯15~19份,甲基丙烯酸乙酯3~7份,引发剂1~2份,反应型乳化剂0.5~1.5份,pH调节剂3~6份,去离子水30~40份。本发明提供的浆料上浆性能优异,具有较高的渗透和披覆能力。
Description
技术领域
本发明涉及高分子乳液聚合技术领域,特别涉及一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料及其制备方法。
背景技术
当今纺织领域,淀粉、PVA、丙烯酸类浆料是三大类主用浆料,各自对织造做出了应有的贡献。淀粉浆料具有资源广泛、价格低廉、对亲水性纤维黏附性好、生物降解性好的特点,但是其浆膜脆硬,上浆性能不能满足要求,特别是对疏水性纤维的粘附性不够。PVA浆料尽管性能不是十分完美,但是成膜强韧、浆料性能较好,是涤棉上浆的主用浆料之一。但是PVA浆料使用上有一个环境保护的问题,它不易分解,长期沉积会引起生态破坏。随着人类环境保护意识增强、发展经济可持续化情况下,PVA浆料在很多国家被禁止使用,国内己出现了少用、不用PVA浆料的观点。丙烯酸类浆料是三大浆料之一,单独使用在喷水织机上已独领风骚,丙烯酸类浆料对环境友好,易被微生物降解,废水处理容易,回收方便。丙烯酸类浆料是丙烯酸类单体的均聚物、共聚物或共混物用作浆料时总称。制造丙烯酸类浆料最基本的单体是丙烯酸、甲基丙烯酸,它们的衍生物丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酰胺和丙烯腈都是丙烯酸类浆料的生产原料。
随着对纺织服装在外观、功能和时尚方面的需求不断提高,在过去很长一段时间里,许多纳米结构和纳米材料,包括纳米颗粒、碳纳米管、纳米电子元件等被逐渐运用于纤维纺织加工中。碳酸钙是一种重要的无机化工产品,是目前用途最广泛的无机填料之一。纳米碳酸钙由于粒径不同而适用于不同的领域,如在橡胶、塑料、造纸、纺织、油墨等行业有着广泛的应用。专利200910053522.7公布了一种有机蒙脱土/丙烯酸类浆料,浆料中加入有机蒙脱土纳米材料提高粘附力,并且工艺简单成本低,适合工业化生产,但是该方法使用了大量的丙烯酸酯类单体,包括软性单体丙烯酸丁酯等,导致浆膜柔软但缺乏坚韧度无法达到理想的上浆环境。专利200610069725.1公布了一种无污染的绿色纳米浆料及生产方法,依靠丙烯酰胺和甲基丙烯酸酯两种单体在淀粉体系中反应,制备出网状复合体,提高纱支的拉伸强力;该方法虽然一定程度上改善了浆膜柔而不坚的问题,但是浆膜吸湿再粘严重,也影响上浆效果。专利201910287474.1公布了一种用于纺织的新型合成丙烯酸乳液及其制备方法,通过添加MgAl-SDS-LDH,使得聚合物分子与片状无机添加剂之间的结合位点更多,形成更加致密的结构,提升了膜的强韧性,通过LDH片层与聚合物分子之间的相互作用,降低了体系的吸湿再粘,但是该方法的乳液粘度还是稍微偏高,影响上浆效率。
发明内容
基于上述现有技术所存在的问题,本发明的目的在于提供一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料及其制备方法,使其能够稳定的工业化生产,满足对纺织上浆的要求,从而完全取代PVA,解决涤棉经纱上浆不用PVA难织造的问题。
为了达到上述目的,本发明采用如下技术方案:
一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特点在于:所述改性纳米碳酸钙/丙烯酸类浆料的各原料按重量份的组成为:改性纳米碳酸钙1~3份,丙烯酰胺5~9份,丙烯酸丙酯23~27份,丙烯酸丁酯15~19份,甲基丙烯酸乙酯3~7份,引发剂1~2份,反应型乳化剂0.5~1.5份,pH调节剂3~6份,去离子水30~40份。
优选的,所述的改性纳米碳酸钙为磷酸酯改性纳米碳酸钙,其制备方法为:将磷酸酯、纳米碳酸钙和水加入三口烧瓶中,再放入适量玻璃珠,在恒温水浴振荡器上,80℃恒温震荡0.5h,趁热过滤,50℃鼓风干燥48h,研磨后过70目筛,即得磷酸酯改性纳米碳酸钙。其中,磷酸酯、纳米碳酸钙和水的用量比为5g:10g:150mL。
优选的,所述的引发剂为过硫酸铵、过氧化氢和过硫酸钾中的至少一种。
优选的,所述的反应型乳化剂为聚氧乙烯基甲基醚、丙烯酰胺基异丙基磺酸钠和含双键的醇醚磺基琥珀酸酯钠盐中的至少一种。
本发明所述的应用于纺织的改性纳米碳酸钙/丙烯酸类浆料的制备方法,包括如下步骤:
(1)在三口烧瓶中加入改性纳米碳酸钙1~3份、反应型乳化剂0.1~0.5份、引发剂1~2份、去离子水30~40份混合均匀,得分散液备用;
(2)将丙烯酰胺5~9份、丙烯酸丙酯23~27份、丙烯酸丁酯15~19份、甲基丙烯酸乙酯3~7份及剩余反应型乳化剂加入预乳化瓶中,得预乳化液备用;
(3)将步骤1中的三口烧瓶恒温为75~85℃,将步骤2中的预乳化液逐步滴加至三口烧瓶中,滴加时间为4~6小时;
(4)滴加完成后降温至35~45℃,加入pH调节剂3~6份调节乳液pH,搅拌均匀,降温至常温过滤,即得改性纳米碳酸钙/丙烯酸类浆料。
本发明改性纳米碳酸钙/丙烯酸类浆料的关键在于:
1、丙烯酸及丙烯酸酯共聚技术
本发明中乳液聚合机理是丙烯酸及丙烯酸酯类单体的自由基反应,整个过程以水为反应介质,反应生成的聚合物颗粒以几微米的粒径均匀分散在水中而形成白色乳液状。
2、纳米碳酸钙改性技术
磷酸酯改性碳酸钙主要是通过磷酸酯与Ca2+形成磷酸酯钙和磷酸酯氢钙沉积、包覆在碳酸钙颗粒表面。
碱性环境中CO3 2-微乎其微,碳酸钙晶体表面吸附的Ca2+或羟基钙离子增多,改性过程又产生了沉淀和水,因而有利于平衡往右边移动,显然,弱碱环境更有利于磷酸酯改性碳酸钙反应过程的进行。
本发明针对涤棉经纱上浆存在的各种问题,对合成的丙烯酸类浆料分子进行设计,主要考虑一下几个方面:
1、为了兼顾水溶及退浆性能,选择带有—COOH(—COONH—O)基团的单体,而不选用急性强的;
2、为了调节乳液的粘附性及成膜性,选择带有—COOR基团的单体;
3、为了调节乳液的柔顺性,选择软单体;
综上所述,本发明选用丙烯酰胺、丙烯酸丙酯、丙烯酸丁酯和甲基丙烯酸乙酯复配作为反应单体。
本发明的有益效果体现在:
1、本发明提供的浆料上浆性能优异,具有较高的渗透和披覆能力;
2、本发明提供的制备方法简单,适用于工业化生产,设备简单,生产稳定且安全环保;
3、本发明采用改性纳米碳酸钙与浆料一起聚合,有效地提高了浆料的玻璃化温度,同时提高了浆料的粘着力和耐磨性。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
具体的,本实施例改性纳米碳酸钙的制备步骤如下:
在250mL的三口烧瓶中,加入5g磷酸酯、10g纳米碳酸钙和150mL水,再放入几颗小玻璃珠,在恒温水浴振荡器上,80℃恒温震荡0.5h,趁热过滤,50℃鼓风干燥48h,研磨后过70目筛,即得改性纳米碳酸钙。
实施例1
本实施例改性纳米碳酸钙/丙烯酸类浆料的各原料按重量份的构成为:改性纳米碳酸钙1份,丙烯酰胺5份,丙烯酸丙酯23份,丙烯酸丁酯15份,甲基丙烯酸乙酯3份,引发剂1份,反应型乳化剂0.5份,pH调节剂3份,去离子水30份。
具体的,本实施例所用各原料为:引发剂为过硫酸铵;反应型乳化剂为聚氧乙烯基甲基醚;pH调节剂为醋酸钠。
本实施例改性纳米碳酸钙/丙烯酸类浆料的制备方法为:
(1)在三口烧瓶中加入改性纳米碳酸钙1份、反应型乳化剂0.2份、引发剂1份、去离子水30份混合均匀,得分散液备用;
(2)将丙烯酰胺5份、丙烯酸丙酯23份、丙烯酸丁酯15份、甲基丙烯酸乙酯3份、反应型乳化剂0.3份加入预乳化瓶中,得预乳化液备用;
(3)将步骤1中的三口烧瓶恒温为75℃,将步骤2中的预乳化液逐步滴加至三口烧瓶中,滴加时间为4小时;
(4)滴加完成后降温至35℃,加入pH调节剂3份调节乳液pH,搅拌均匀,降温至常温过滤,即得改性纳米碳酸钙/丙烯酸类浆料。
检测步骤(4)所获得成品乳液的固含量、粘度、粘附力、吸湿率及上浆率,其结果如表1所示。
实施例2
本实施例改性纳米碳酸钙/丙烯酸类浆料的各原料按重量份的构成为:改性纳米碳酸钙3份,丙烯酰胺9份,丙烯酸丙酯27份,丙烯酸丁酯19份,甲基丙烯酸乙酯7份,引发剂2份,反应型乳化剂1.5份,pH调节剂6份,去离子水40份。
具体的,本实施例所用各原料为:引发剂为过硫酸铵;反应型乳化剂为丙烯酰胺基异丙基磺酸钠;pH调节剂为醋酸钠。
本实施例改性纳米碳酸钙/丙烯酸类浆料的制备方法为:
(1)在三口烧瓶中加入改性纳米碳酸钙3份、反应型乳化剂0.5份、引发剂2份、去离子水40份混合均匀,得分散液备用;
(2)将丙烯酰胺9份、丙烯酸丙酯27份、丙烯酸丁酯19份、甲基丙烯酸乙酯7份、反应型乳化剂1份加入预乳化瓶中,得预乳化液备用;
(3)将步骤1中的三口烧瓶恒温为85℃,将步骤2中的预乳化液逐步滴加至三口烧瓶中,滴加时间为6小时;
(4)滴加完成后降温至45℃,加入pH调节剂6份调节乳液pH,搅拌均匀,降温至常温过滤,即得改性纳米碳酸钙/丙烯酸类浆料。
检测步骤(4)所获得成品乳液的固含量、粘度、粘附力、吸湿率及上浆率,其结果如表1所示。
实施例3
本实施例改性纳米碳酸钙/丙烯酸类浆料的各原料按重量份的构成为:改性纳米碳酸钙2份,丙烯酰胺7份,丙烯酸丙酯24份,丙烯酸丁酯16份,甲基丙烯酸乙酯5份,引发剂1份,反应型乳化剂1份,pH调节剂5份,去离子水40份。
具体的,本实施例所用各原料为:引发剂为过硫酸铵;反应型乳化剂为丙烯酰胺基异丙基磺酸钠;pH调节剂为醋酸钠。
本实施例改性纳米碳酸钙/丙烯酸类浆料的制备方法为:
(1)在三口烧瓶中加入改性纳米碳酸钙2份、反应型乳化剂0.5份、引发剂1份、去离子水40份混合均匀,得分散液备用;
(2)将丙烯酰胺7份、丙烯酸丙酯24份、丙烯酸丁酯16份、甲基丙烯酸乙酯5份、反应型乳化剂0.5份加入预乳化瓶中,得预乳化液备用;
(3)将步骤1中的三口烧瓶恒温为80℃,将步骤2中的预乳化液逐步滴加至三口烧瓶中,滴加时间为4小时;
(4)滴加完成后降温至40℃,加入pH调节剂5份调节乳液pH,搅拌均匀,降温至常温过滤,即得改性纳米碳酸钙/丙烯酸类浆料。
检测步骤(4)所获得成品乳液的固含量、粘度、粘附力、吸湿率及上浆率,其结果如表1所示。
实施例4
本实施例改性纳米碳酸钙/丙烯酸类浆料的各原料按重量份的构成为:改性纳米碳酸钙1份,丙烯酰胺5份,丙烯酸丙酯27份,丙烯酸丁酯19份,甲基丙烯酸乙酯3份,引发剂2份,反应型乳化剂1.5份,pH调节剂6份,去离子水40份。
具体的,本实施例所用各原料为:引发剂为过硫酸铵;反应型乳化剂为聚氧乙烯基甲基醚;pH调节剂为醋酸钠。
本实施例改性纳米碳酸钙/丙烯酸类浆料的制备方法为:
(1)在三口烧瓶中加入改性纳米碳酸钙1份、反应型乳化剂0.5份、引发剂2份、去离子水40份混合均匀,得分散液备用;
(2)将丙烯酰胺5份、丙烯酸丙酯27份、丙烯酸丁酯19份、甲基丙烯酸乙酯3份、反应型乳化剂1份加入预乳化瓶中,得预乳化液备用;
(3)将步骤1中的三口烧瓶恒温为80℃,将步骤2中的预乳化液逐步滴加至三口烧瓶中,滴加时间为5小时;
(4)滴加完成后降温至40℃,加入pH调节剂6份调节乳液pH,搅拌均匀,降温至常温过滤,即得改性纳米碳酸钙/丙烯酸类浆料。
检测步骤(4)所获得成品乳液的固含量、粘度、粘附力、吸湿率及上浆率,其结果如表1所示。
检测条件说明:
1、固含量的检测方法
准确称取1g乳液,均匀涂于瓶底或锡纸上,放入干燥箱,105℃恒温烘12小时,取出放入干燥器中,凉至室温,称重。按以下的公式计算固含量:固含量=干燥后称重÷干燥前称重×100%。
2、粘度的检测方法
将浆液配置成质量分数为4%的溶液,在30℃下用NDJ-79型旋转粘度计测量浆液粘度。
3、粘附力的检测方法
配制1500mL含固率为1%的浆液在温度95℃以上的条件下充分调浆后倒入浆槽中并保持90℃以上的温度将绕在架子上的粗纱浸入浆液5分钟取出悬挂自然晾干。在20℃RH65%的环境中平衡24小时后,用粘附力测试仪XL-1B测定拉伸强度得到粘附力数据。测试条件为:夹距100mm,拉伸速度100mm/min,最大负载200N,样本容量为30,温度T=20℃相对湿度RH=65%。
4、吸湿率的检测方法
将含固率6%的浆液倒入铺有聚乙烯膜的盘中自然晾干,然后剪下一块烘干(105℃)12小时至恒重,称重,得到干膜重。然后放入20℃RH95%的恒湿器中平衡72小时,取出时称重得到湿膜重。用下列公式计算吸湿率:吸湿率=(湿膜重-干膜重)÷干膜重×100%。
5、上浆率的检测方法
烘干浆粗纱至恒重,称量粗纱,得到浆纱前的粗纱重量,待粘附力测定后,将该粗纱烘干至恒重,称重得到浆纱后的粗纱重量,随后放入95℃、2%NaOH的溶液中浸20分钟,取出用热水洗涤,再用冷水清洗,然后烘干至恒重并称重得退浆后重量。用下列公式计算上浆率:上浆率=(浆纱后粗砂干重-浆纱前粗砂干重)÷浆纱前粗砂干重×100%。
表1、各实施例检测结果
固含量/% | 粘度/mPa·s | 粘附力/N | 吸湿率/% | 上浆率/% | |
实施例1 | 58 | 5 | 88 | 11 | 14 |
实施例2 | 56 | 6 | 90 | 14 | 16 |
实施例3 | 53 | 5 | 89 | 12 | 16 |
实施例4 | 52 | 4 | 85 | 6 | 13 |
以上所述仅为本发明的示例性实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特征在于:所述改性纳米碳酸钙/丙烯酸类浆料的各原料按重量份的组成为:改性纳米碳酸钙1~3份,丙烯酰胺5~9份,丙烯酸丙酯23~27份,丙烯酸丁酯15~19份,甲基丙烯酸乙酯3~7份,引发剂1~2份,反应型乳化剂0.5~1.5份,pH调节剂3~6份,去离子水30~40份。
2.根据权利要求1所述的一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特征在于:所述的改性纳米碳酸钙为磷酸酯改性纳米碳酸钙。
3.根据权利要求2所述的一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特征在于:所述的磷酸酯改性纳米碳酸钙的制备方法为:将磷酸酯、纳米碳酸钙和水加入三口烧瓶中,再放入适量玻璃珠,在恒温水浴振荡器上,80℃恒温震荡0.5h,趁热过滤,50℃鼓风干燥48h,研磨后过70目筛,即得磷酸酯改性纳米碳酸钙。
4.根据权利要求3所述的一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特征在于:磷酸酯、纳米碳酸钙和水的用量比为5g:10g:150mL。
5.根据权利要求1所述的一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特征在于:所述的引发剂为过硫酸铵、过氧化氢和过硫酸钾中的至少一种。
6.根据权利要求1所述的一种应用于纺织的改性纳米碳酸钙/丙烯酸类浆料,其特征在于:所述的反应型乳化剂为聚氧乙烯基甲基醚、丙烯酰胺基异丙基磺酸钠和含双键的醇醚磺基琥珀酸酯钠盐中的至少一种。
7.一种权利要求1~6中任意一项所述的应用于纺织的改性纳米碳酸钙/丙烯酸类浆料的制备方法,其特征在于,包括如下步骤:
(1)在三口烧瓶中加入改性纳米碳酸钙1~3份、反应型乳化剂0.1~0.5份、引发剂1~2份、去离子水30~40份混合均匀,得分散液备用;
(2)将丙烯酰胺5~9份、丙烯酸丙酯23~27份、丙烯酸丁酯15~19份、甲基丙烯酸乙酯3~7份及剩余反应型乳化剂加入预乳化瓶中,得预乳化液备用;
(3)将步骤1中的三口烧瓶恒温为75~85℃,将步骤2中的预乳化液逐步滴加至三口烧瓶中,滴加时间为4~6小时;
(4)滴加完成后降温至35~45℃,加入pH调节剂3~6份调节乳液pH,搅拌均匀,降温至常温过滤,即得改性纳米碳酸钙/丙烯酸类浆料。
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