CN116926707A - 聚合原料含弱亲水性单体的具抗菌功能的无纺布材料、其制备方法及其制得的制品 - Google Patents
聚合原料含弱亲水性单体的具抗菌功能的无纺布材料、其制备方法及其制得的制品 Download PDFInfo
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- CN116926707A CN116926707A CN202210371478.XA CN202210371478A CN116926707A CN 116926707 A CN116926707 A CN 116926707A CN 202210371478 A CN202210371478 A CN 202210371478A CN 116926707 A CN116926707 A CN 116926707A
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- master batch
- monomer
- woven fabric
- spinning
- mixture
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 54
- 239000000178 monomer Substances 0.000 title claims abstract description 51
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 10
- 239000002994 raw material Substances 0.000 title claims abstract description 7
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- 239000000203 mixture Substances 0.000 claims abstract description 43
- 238000009987 spinning Methods 0.000 claims abstract description 41
- 238000002156 mixing Methods 0.000 claims abstract description 36
- -1 polypropylene Polymers 0.000 claims abstract description 34
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000004743 Polypropylene Substances 0.000 claims abstract description 24
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- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 239000004744 fabric Substances 0.000 claims description 17
- 238000010894 electron beam technology Methods 0.000 claims description 13
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 11
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- 230000002140 halogenating effect Effects 0.000 claims description 11
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 11
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 8
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
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- 239000004750 melt-blown nonwoven Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 claims description 6
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
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- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
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- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 claims description 3
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 3
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 3
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- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 3
- XVDWMONETMNKBK-UHFFFAOYSA-N calcium;dihypobromite Chemical compound [Ca+2].Br[O-].Br[O-] XVDWMONETMNKBK-UHFFFAOYSA-N 0.000 claims description 3
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 claims description 3
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- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
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- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical group BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004132 cross linking Methods 0.000 claims description 2
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- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 claims description 2
- ORQYPOUSZINNCB-UHFFFAOYSA-N potassium;hypobromite Chemical compound [K+].Br[O-] ORQYPOUSZINNCB-UHFFFAOYSA-N 0.000 claims description 2
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 claims description 2
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 2
- CRWJEUDFKNYSBX-UHFFFAOYSA-N sodium;hypobromite Chemical compound [Na+].Br[O-] CRWJEUDFKNYSBX-UHFFFAOYSA-N 0.000 claims description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 5
- 230000026030 halogenation Effects 0.000 abstract description 2
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
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Classifications
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- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
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- A61L15/24—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
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- A61L15/42—Use of materials characterised by their function or physical properties
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
- C08F226/04—Diallylamine
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F8/20—Halogenation
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- D01F1/103—Agents inhibiting growth of microorganisms
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- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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- D04H1/4291—Olefin series
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
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Abstract
本发明提供了一种聚合原料含弱亲水性单体的具抗菌功能的无纺布材料、其制备方法、及其制得的口罩。该方法包括以下步骤:A、制备母粒料:在混合器中,依次加入聚丙烯颗粒料、二烯丙基胺、第二单体,搅拌混合均匀后得母粒混合料,第二单体为弱亲水性单体;然后经过辐照、抽提、卤化;B、混料:将母粒卤化料、聚丙烯颗粒料及助剂加入混合器中,进行搅拌混合均匀后得纺丝混合料;C、挤压熔融;D、纺丝;E、后处理及成网;F、卷绕及整理得成品无纺布。应用本发明的抗菌无纺布制成的制品抑菌灭菌效果良好且安全环保。
Description
技术领域
本发明属于抗菌材料技术领域,尤其涉及是无纺布抗菌材料。
背景技术
目前,口罩已成为阻隔颗粒状尘埃及细菌、保护易感人群、进行有效个体防护的重要物品。现有市场中存在的防护口罩,它们大多是采用聚丙烯熔喷非织造布作为过滤层,依靠阻挡截留、静电吸附等作用对尘埃和细菌进行阻隔,进而对人们起到有效的防护作用。但据有关研究显示,滞留在口罩过滤层的细菌和病毒还可以继续繁殖生长,对人体造成二次侵害。为了防止这些病原微生物对人体再次造成伤害,研制一款具有抗菌性能的口罩就很有必要。
从实现工业化的可行性、环保性及经济性等多方面因素的考虑,聚丙烯是口罩的优选原材料。这些由超细的聚丙烯熔喷布制成的口罩,展现了优异的过滤效率,但不能实现对有害微生物、病毒的杀灭作用。聚丙烯纤维表面没有活性的基团,很难通过化学的方法将抗菌功能基团接上去实现抗菌性能。在现有的技术方案中,只能是利用无机抗菌剂通过共混纺丝的方法来实现纤维的抗菌。由于无机抗菌剂颗粒易堵塞喷丝孔造成断丝,生产故障较多,难以适应工业化生产。因此,该法生产的抗菌口罩很少在市场上出现;另一方面,由于无机抗菌剂杀菌速率慢,对拦截的有害细菌、病毒很难实现有效的即时杀灭;同时,无机抗菌剂也属溶出型抗菌剂,被释放溶出来的无机抗菌剂,在杀灭细菌的同时,也有被吸入体内,有对人的健康造成负面影响的风险。
因此,研究制备安全高效的适于制作抗菌口罩的材料,对保护人们的身体健康,特别是在新冠病毒肆虐期间,就具有极其重要的现实意义。
发明内容
针对现有抗菌功能口罩制备材料的不足,本发明提出了以下技术方案:
一种聚合原料含弱亲水性单体的具抗菌功能的无纺布材料,其包括以下步骤:
A、制备母粒料:
A.1、混合:
在混合器中,依次加入聚丙烯颗粒料、二烯丙基胺、第二单体,搅拌混合均匀后得母粒混合料,其中,二烯丙基胺的添加量为聚丙烯颗粒料质量分数的 0.3%~7.5%,第二单体的添加量为二烯丙基胺质量分数的100~250%,第二单体为弱亲水性单体,选自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、醋酸乙烯酯、马来酸二甲酯、马来酸二甲酯、马来酸二胺中的一种或两种以上的混合;
A.2、辐照:
用电子束加速器对母粒混合料在低氧氛围下进行辐照处理得母粒辐照料;
A.3、抽提:
将母粒辐照料及夹带剂一起置于超临界萃取装置的萃取釜中,用超临界状态下的CO2萃取,将未反应的单体溶解,并经分离釜分离出来以脱除去未反应的残余单体得母粒抽提料,夹带剂为对残余单体有较好相溶性的溶剂,选自乙醇、甲醇中的一种或两种的混合,优选乙醇,夹带剂的用量为CO2质量分数的 5.0%~40.0%;
A.4、卤化:
将母粒抽提料浸渍于pH值为6.5~7.5、质量百分浓度为0.1~10.0%的次卤酸盐水溶液中,于常温进行卤化反应30~80分钟后,取出脱水并于40~70℃温度下直至烘干,得含有如通式(I)所示结构的N-卤二烯丙基胺的共聚物的母粒卤化料,通式(I)所示结构的N-卤二烯丙基胺的共聚物中包含N-卤二烯丙基胺结构单元和第二官能团结构单元;N-卤二烯丙基胺结构单元是五元含氮杂环卤胺化合物或六元含氮杂环卤胺化合物或它们的混合,N-卤二烯丙基胺结构单元是由前驱体二烯丙基胺聚合再经卤化反应后转化而成;第二官能团结构单元是通过前驱体第二单体聚合反应后转化而成,第二单体为弱亲水性单体;
式(I)中,X表示卤素原子氯或溴,优选氯原子;n表示聚合度;
B、混料:
将母粒卤化料、聚丙烯颗粒料及助剂加入混合器中,进行搅拌混合均匀后得纺丝混合料,母粒卤化料、聚丙烯颗粒料按30:70~50:50的质量份数混合,其助剂的添加量为混合料质量分数的0.0~5.0%
C、挤压熔融:
将纺丝混合料喂入到螺杆挤压机中,并在挤压机中继续混合、加温、挤压,直至它们从固态转变为熔融状态;
D、纺丝:
然后,将熔融状态的纺丝混合料过滤后泵送到喷丝装置,进入喷丝头进行纺丝;
E、后处理及成网:
将喷丝装置挤出的细丝流经牵伸后形成的细丝,再经过熔喷无纺布法,使纤网变成无纺布;
F、卷绕及整理
将制成的无纺布卷绕成布,进行定幅、定长、分切、整理,再卷绕得成品无纺布。
二烯丙基胺的添加量优选为聚丙烯颗粒料质量分数的1.4%~2.1%。
第二单体的添加量优选为二烯丙基胺质量分数的150%~230%,更优选 150%~200%。
步骤A.1制备母粒混合料时,在第二单体加入后还加入具交联性的单体或齐聚物,其选自二异丙烯基苯、二乙烯基苯、三烯丙基胺、亚甲基双丙烯酰胺、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、二乙二醇二丙烯酸酯,三乙二醇二丙烯酸酯,1,4-丁二醇二丙烯酸酯,三羟甲基丙烷三丙烯酸酯,季戊四醇三丙烯酸酯中的一种或两种以上的混合。
优选的,步骤A.3中的夹带剂优选乙醇。
优选的,步骤B中助剂添加量优选0.01%~2.0%。
具体来说,所述的电子束加速器为高能电子束加速器,包括高压加速器、感应加速器、谐振加速器。
具体来说,所述的辐照处理是指用电子束加速器对母粒料按10~150kGy的剂量进行辐射,优选20~60kGy的剂量。
具体来说,所述的次卤酸盐选自次氯酸钠、次氯酸钾、次氯酸钙、次溴酸钠、次溴酸钾、次溴酸钙中的一种,优选次氯酸钠、次氯酸钙。
作为可选方式,在不损害本发明效果的前题下,在A.1混合步骤中,在混合器中,依次加入聚丙烯颗粒料、二烯丙基胺、第二单体的同时,还可加入交联剂单体或齐聚物,其交联剂单体或齐聚物的添加量为共聚单体质量分数的 0.01~30.0%,优选在1.0%~20.0%,更优选1.0%~10.0%。
所述的交联剂单体或齐聚物为具2个或2个以上乙烯基的单体或齐聚物,包括二异丙烯基苯、二乙烯基苯、三烯丙基胺、亚甲基双丙烯酰胺、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、二乙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、1,4- 丁二醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、季戊四醇三丙烯酸酯等,选自它们中的一种或两种以上的混合物,优选二乙烯基苯。
作为优选方式,在不损害本发明效果的前题下,为使卤化反应的顺利进行,在A.4卤化步骤中,在次卤酸盐水溶液中,还可添加入界面相容剂,其添加量为次卤酸盐水溶液质量百分数的1~10%,优选1~5%。
所述的界面相容剂为固体与液体相接触构成界面时,两者之间产生的物理和化学的相容性,包括甲醇、乙醇、丙醇、异丙醇、丁醇、苯酚、乙酸乙酯、四氢呋喃、甲乙酮等,选自它们中的一种或两种以上的混合,优选乙醇、丙醇。
本发明的第二个目的在于提供具抗菌功能的无纺布及无纺布制品,为了实现以上目的,本发明应用了如上任一所述的无纺布,制成口罩。
除了口罩外,本发明的材料还可以制成过滤材料、湿面巾、柔巾卷、面膜、美容用品、絮片、伤口敷料、失禁产品等。
本发明具抗菌功能的无纺布,在如通式(I)所示的N-卤二烯丙基胺系共聚物中,N-卤二烯丙基胺的结构单元是由二烯丙基胺聚合分别生成五元含氮杂环胺和六元含氮杂环胺的混合物,再经卤化转化而成五元含氮杂环或六元含氮杂环 N-X键的卤胺化合物,极性稍高的N-卤二烯丙基胺系共聚物与极性低的聚烯烃基体材料,熔融共混纺丝时,在迁移效应作用下,在丝纤维的表面富集了更多N- 卤二烯丙基胺系共聚物,当丝纤维接触细菌时,结构中氧化性卤能够释放出来,破坏细菌的细胞膜,使细菌细胞中蛋白质结构受到氧化,从而抑制细菌的繁殖或者使细菌失活,起到杀菌作用,具稳定性强、杀菌广谱高效、毒性低等特点。
上述具抗菌功能的无纺布材料的制备方法中,由于抗菌剂的前驱体是共聚物中的二烯丙基胺结构单元,但由于二烯丙基胺聚合在进行自由基链增长反应时,同时也存在自由基链转移反应,而不能形成分子质量较大的长链聚合物,为了得到更高分子质量的聚合物,通常是采用与其它单体共聚以减少链转移反应的发生。为了在共聚物中得到主要成份为二烯丙基胺结构单元,本发明采用了添加第二单体,与二烯丙基胺进行共聚,其第二单体选用了弱亲水性单体,可以降低二烯丙基胺的自由基链转移反应,使得能形成分子质量较大的共聚物,当其用于弱极性液体作过滤材料时,无纺布材料更具亲润性,以达到工程更优化的目的。
高能辐射是一种均匀、高效和易控的引发方式,高能射线可实现对固体有机物表面的接枝,及单体的聚合固化,与其他化学方法相比,在成本方面有其极大的竞争优势。因此,在本发明中,在母粒料制备的过程中,二烯丙基胺的聚合选择了高能辐射的方式。由于电子加速器产生的高能电子束,其辐照强度大,因此,射线发生器的射线源,优选高能电子束加速器。
经辐照后的母粒料,通过用超临界CO2流体萃取,并分离脱除去未反应的残余单体,达到使用更加安全卫生的目的。
本发明所选原料廉价易得,生产成本低,通过辐射的方法,将卤胺化合物混入到聚丙烯基体中进行共混纺丝并制备无纺布,后再制作成口罩,作为具抗菌功能的口罩,其丝纤维作为无纺布的同时,也作为抑菌、灭菌等抗菌功能化合物的载体支撑物,人们在使用口罩,达到抑菌、灭菌等抗菌目的过程中,抗菌剂就不会以小分子的形式散落到环境中,造成对环境的二次污染,可实现安全、环保的抗菌目的。
应用本发明的抗菌无纺布制成的制品有包括口罩、过滤材料、湿面巾、柔巾卷、面膜、美容用品、絮片等。
具体实施方式
本发明通过下面的实施例进行进一步的阐述,但实施例并不限制本发明的范围。
实施例1
本例是一种具抗菌功能的无纺布材料的制备方法,其包括以下步骤:
A、制备母粒料:
A.1、混合:
在装有搅拌装置的1.0M3混合器中,依次加入熔融指数1300g/10min的聚丙烯粒料300kg,二烯丙基胺4.2kg,丙烯酸甲酯4.0kg,丙烯酸乙酯4.0kg,搅拌20~30min混合均匀后得母粒混合料。
A.2、辐照:
接着,将上述母粒混合料分装入具密封功能30cm*40cm的耐压塑料袋中,抽真空,相对压力为-0.07~-0.08MPa。并按注0.05MPa工业用氮气-再抽真空重复 5次后再密封,压平后并置于5Mev的高能电子束加速器辐照装置的输送带上,按25kGy的剂量进行辐照处理得母粒辐照料。
A.3、抽提:
然后,将上述经辐照处理后的母粒辐照料及20kg的乙醇一起置于0.5M3的萃取釜中,密封并充满液态CO2后,调整工艺使之在40℃、8.5Mpa的超临界状态下进行抽提,将未反应的单体溶解,萃取40分钟后缷压,分离并脱除去未反应的残余单体从而得到母粒抽提料。
所述的超临界萃取装置是一种利用超临界流体萃取技术来进行萃取操作的设备,实现从辐照后的固体辐照料中萃取、分离残余未聚合单休的装置,其过程的主要设备是由高压萃取釜、分离釜、换热器、高压泵(压缩机)、储罐以及连接这些设备的管道、阀门和接头等构成,萃取时间为0.5~1.0小时。
A.4、卤化:
用水调节次氯酸钠的质量百分浓度为2.0%,用稀盐酸调pH值为7~7.5后,再添加乙醇混合均匀得卤化液,其乙醇添加量为次氯酸钠水溶液质量的1.5%。
再将上述经抽提处理的母粒抽提料,浸渍于上述卤化液中,于常温下卤化反应50min,取出脱水并于60~65℃温度下直至烘干,得到母粒卤化料。
B、混料:
将上述母粒卤化料、熔融指数为1300g/10min的聚丙烯粒料、按40:60的比例,加入到混料斗中,在混料斗中进行搅拌混合均匀后得纺丝混合料。
所述的助剂为使工艺过程更顺畅,产品性能更佳的一种添加剂,包括分散剂、相溶剂、增强剂、色母粒等,选自它们中的一种或两种以上的混合。
C、挤压熔融:
接着将上述纺丝混合料喂入到螺杆挤压机中,调节螺杆挤压机的温度为 230~245℃,并在挤压机中继续混合、挤压,直至它们从固态转变为熔融状态。
D、纺丝:
然后,将上述经挤压熔融后的熔体在经过过滤组件的过滤后,控制熔体的压力为6~7MPa,通过用计量泵泵送到喷丝装置,进入喷丝头进行纺丝。
E、后处理及成网
利用高速热空气对模头喷丝孔挤出的聚合物熔体细流进行牵伸,由此形成超细纤维并凝聚在凝网帘或滚筒上,并依靠自身粘合而成25g/m2的非织造布。
F、卷绕及整理
最后将制成的25g/m2非织造无纺布,卷绕成布,并按需求重新分切成 70cm~180cm宽、卷绕直径为600~800mm的成品熔喷无纺布。
实施例2
本例是一种具抗菌功能的无纺布材料制备方法的另一实施例,其包括以下步骤:
A、制备母粒料:
A.1、混合:
在装有搅拌装置1.0M3的混合器中,依次加入熔融指数为1300g/10min的聚丙烯粒料300kg、二烯丙基胺4.5kg、丙烯酸甲酯3.5kg、丙烯酸乙酯4.0kg、醋酸乙烯酯0.5kg,搅拌25~30min混合均匀后得母粒混合料。
A.2、辐照:
接着,将上述母粒混合料分装入具密封功能40cm*40cm的耐压塑料袋中,抽真空,相对压力为-0.075~-0.085MPa。并按注0.012MPa工业用氮气-再抽真空重复4次后再密封,压平后并置于5Mev的高能电子束加速器辐照装置的输送带上,按25kGy的剂量进行辐照处理得母粒辐照料。
A.3、抽提:
然后,将上述经辐照处理后的母粒辐照料及30kg的乙醇一起置于0.5M3的萃取釜中,密封并充满液态CO2后,调整工艺使之在40℃、8.6Mpa超临界状态下进行抽提,将未反应的单体溶解,萃取40分钟后缷压,分离并脱除去未反应的残余单体从而得到得母粒抽提料。
A.4、卤化:
用稀盐酸调节次氯酸钠水溶液的pH值为7.3后,用水调节次氯酸钠的质量百分浓度为2.2%,再添加乙醇混合均匀得卤化液,其乙醇添加量为次氯酸钠水溶液质量的1.5%。
再将上述经抽提处理的母粒抽提料,浸渍于上述卤化液中,于常温下进行卤化反应60分钟,取出脱水并于60~63℃下直至烘干,得含母粒卤化料。
B、混料:
将上述母粒卤化料、熔融指数为1300g/10min的聚丙烯粒料、按30:70的比例,加入到混料斗中,在混料斗中进行搅拌混合均匀后得纺丝混合料。
C、挤压熔融:
接着将上述纺丝混合料喂入到螺杆挤压机中,调节螺杆挤压机的温度为 230~240℃,并在挤压机中继续混合、挤压,直至它们从固态转变为熔融状态。
D、纺丝:
然后,将上述经挤压熔融后的熔体在经过过滤组件的过滤后,控制熔体的压力为6.5~7MPa,通过用计量泵泵送到喷丝装置,进入喷丝头进行纺丝。
E、后处理及成网
利用高速热空气对模头喷丝孔挤出的聚合物熔体细流进行牵伸,由此形成超细纤维并凝聚在凝网帘或滚筒上,并依靠自身粘合而成25g/m2的非织造布。
F、卷绕及整理
最后将制成的25g/m2非织造无纺布,卷绕成布,并按需求重新分切成 70cm~180cm宽、卷绕直径为600~800mm的成品熔喷无纺布。
实施例3
本例是一种具抗菌功能熔喷无纺布的制备方法,其包括以下步骤:
A、制备母粒料:
A.1、混合:
在装有搅拌的1.0M3混合器中,依次加入熔融指数1300g/10min的聚丙烯粒料300kg,二烯丙基胺6.5kg,丙烯酸甲酯4.0kg,甲基丙烯酸乙酯3.0kg、马来酸二甲酯0.5kg,马来酸二胺0.5kg,乙二醇二丙烯酸酯0.5kg,搅拌25~30min 混合均匀后得母粒混合料。
A.2、辐照:
接着,将上述母粒混合料分装入具密封功能30cm*40cm的耐压塑料袋中,抽真空,相对压力为-0.07~-0.08MPa。并按注0.02MPa工业用氮气-再抽真空重复 5次后再密封,压平后并置于5Mev的高能电子束加速器辐照装置的输送带上,按22kGy的剂量进行辐照处理得母粒辐照料。
A.3、抽提:
然后,将上述经辐照处理后的母粒辐照料及17kg的乙醇一起置于0.5M3的萃取釜中,密封并充满液态CO2后,调整工艺使之在38℃、8.5Mpa的超临界状态下进行抽提,将未反应的单体溶解,萃取45分钟后缷压,分离并脱除去未反应的残余单体从而得到母粒抽提料。
A.4、卤化:
用水调节次氯酸钠的质量百分浓度为1.5%,用稀盐酸调pH值为7~7.5后,再添加乙醇混合均匀得卤化液,其乙醇添加量为次氯酸钠水溶液质量的1.5%。
再将上述经抽提处理的母粒抽提料,浸渍于上述卤化液中,于常温下卤化反应50min,取出脱水并于60~65℃温度下直至烘干,得到母粒卤化料。
B、混料:
将上述母粒卤化料、熔融指数为1200g/10min的聚丙烯粒料、按32.5:67.5 的比例,加入到混料斗中,在混料斗中进行搅拌混合均匀后得纺丝混合料。
C、挤压熔融:
接着将上述纺丝混合料喂入到螺杆挤压机中,调节螺杆挤压机的温度为 230~245℃,并在挤压机中继续混合、挤压,直至它们从固态转变为熔融状态。
D、纺丝:
然后,将上述经挤压熔融后的熔体在经过过滤组件的过滤后,控制熔体的压力为6~7MPa,通过用计量泵泵送到喷丝装置,进入喷丝头进行纺丝。
E、后处理及成网
利用高速热空气对模头喷丝孔挤出的聚合物熔体细流进行牵伸,由此形成超细纤维并凝聚在凝网帘或滚筒上,并依靠自身粘合而成28g/m2的非织造布。
F、卷绕及整理
最后将制成的25g/m2非织造无纺布,卷绕成布,并按需求重新分切成 70cm~180cm宽、卷绕直径为600~800mm的成品熔喷无纺布。
实施例4
本例为本发明具抗菌功能无纺布抗菌性能测试的实施例。
无纺布抗菌性能测试,根据中华人民共和国纺织行业标准FZ/T 73023-2006 抗菌针织品的检测方法进行测定,其抗菌性能效果见表1。
表1
实施例5
本例是一种具抗菌功能口罩的制备方法。
采用实施例1制作成的抗菌无纺布,作为中间层制作成具抗菌功能的口罩。
实施例6
本例是一种具抗菌功能口罩的制备方法。
采用实施例2制作成的抗菌无纺布,合二层作为中间层;加上纺粘布的里层和面层共四层,制作成具抗菌功能的口罩。
实施例7
本例是一种具抗菌功能过滤布的制备方法。
采用实施例3制作成的抗菌无纺布,作为过滤芯层制作成具抗菌功能的空气清新器的过滤网。
实施例8
本例是一种具抗菌功能餐台布的制备方法。
采用实施例2制作成的抗菌无纺布,制作为餐台具抗菌功能的餐台布。
实施例9
本例是一种具抗菌功能伤口敷料的制备方法。
采用实施例3制作成的抗菌无纺布,制作成具抗菌功能的伤口敷料。
实施例10
本例是一种具抗菌功能失禁产品的制备方法。
采用实施例3制作成的抗菌无纺布,作为贴肤层,制作成具抗菌功能的失禁品。
Claims (10)
1.一种聚合原料含弱亲水性单体的具抗菌功能的无纺布材料的制备方法,其特征在于包括以下步骤:
A、制备母粒料:
A.1、混合:
在混合器中,依次加入聚丙烯颗粒料、二烯丙基胺、第二单体,搅拌混合均匀后得母粒混合料,其中,二烯丙基胺的添加量为聚丙烯颗粒料质量分数的0.3%~7.5%,第二单体的添加量为二烯丙基胺质量分数的100~250%,第二单体为弱亲水性单体,选自丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、醋酸乙烯酯、马来酸二甲酯、马来酸二甲酯、马来酸二胺中的一种或两种以上的混合;
A.2、辐照:
用电子束加速器对母粒混合料在低氧氛围下进行辐照处理得母粒辐照料;
A.3、抽提:
将母粒辐照料及夹带剂一起置于超临界萃取装置的萃取釜中,用超临界状态下的CO2萃取,将未反应的单体溶解,并经分离釜分离出来以脱除去未反应的残余单体得母粒抽提料,夹带剂为对残余单体有较好相溶性的溶剂,选自乙醇、甲醇中的一种或两种的混合,优选乙醇,夹带剂的用量为CO2质量分数的5.0%~40.0%;
A.4、卤化:
将母粒抽提料浸渍于pH值为6.5~7.5、质量百分浓度为0.1~10.0%的次卤酸盐水溶液中,于常温进行卤化反应30~80分钟后,取出脱水并于40~70℃温度下直至烘干,得含有如通式(I)所示结构的N-卤二烯丙基胺的共聚物的母粒卤化料,通式(I)所示结构的N-卤二烯丙基胺的共聚物中包含N-卤二烯丙基胺结构单元和第二官能团结构单元;N-卤二烯丙基胺结构单元是五元含氮杂环卤胺化合物或六元含氮杂环卤胺化合物或它们的混合,N-卤二烯丙基胺结构单元是由前驱体二烯丙基胺聚合再经卤化反应后转化而成;第二官能团结构单元是通过前驱体第二单体聚合反应后转化而成;
式(I)中,X表示卤素原子氯或溴,优选氯原子;n表示聚合度;
B、混料:
将母粒卤化料、聚丙烯颗粒料及助剂加入混合器中,进行搅拌混合均匀后得纺丝混合料,母粒卤化料、聚丙烯颗粒料按30:70~50:50的质量份数混合,其助剂的添加量为混合料质量分数的0.0~5.0%;
C、挤压熔融:
将纺丝混合料喂入到螺杆挤压机中,并在挤压机中继续混合、加温、挤压,直至它们从固态转变为熔融状态;
D、纺丝:
将熔融状态的纺丝混合料过滤后泵送到喷丝装置,进入喷丝头进行纺丝;
E、后处理及成网:
将喷丝装置挤出的细丝流经牵伸后形成的细丝,再经过熔喷无纺布法,使纤网变成无纺布;
F、卷绕及整理:
将制成的无纺布卷绕成布,进行定幅、定长、分切、整理,再卷绕得成品无纺布。
2.根据权利要求1所述的制备方法,其特征在于:二烯丙基胺的添加量为聚丙烯颗粒料质量分数的1.4%~2.1%。
3.根据权利要求2所述的制备方法,其特征在于:步骤A.1制备母粒混合料时,在加入第二单体后还加入具交联性的单体或齐聚物,其选自二异丙烯基苯、二乙烯基苯、三烯丙基胺、亚甲基双丙烯酰胺、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、二乙二醇二丙烯酸酯,三乙二醇二丙烯酸酯,1,4-丁二醇二丙烯酸酯,三羟甲基丙烷三丙烯酸酯,季戊四醇三丙烯酸酯中的一种或两种以上的混合。
4.根据权利要求1所述的制备方法,其特征在于:步骤A.3中的夹带剂优选乙醇。
5.根据权利要求1所述的制备方法,其特征在于:步骤B中助剂添加量优选0.01%~2.0%。
6.根据权利要求1所述的制备方法,其特征在于:所述的电子束加速器为高能电子束加速器,包括高压加速器、感应加速器、谐振加速器。
7.根据权利要求1所述的制备方法,其特征在于:所述的辐照处理是指用电子束加速器对母粒料按10~150kGy的剂量进行辐射。
8.根据权利要求1所述的制备方法,其特征在于:所述的次卤酸盐选自次氯酸钠、次氯酸钾、次氯酸钙、次溴酸钠、次溴酸钾、次溴酸钙中的一种,优选次氯酸钠、次氯酸钙。
9.由权利要求1~8任一所述的方法所制得的无纺布。
10.一种应用如权利要求9所述的无纺布制得的制品。
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