CN113907952A - 一种不粘敷料及其制备方法 - Google Patents
一种不粘敷料及其制备方法 Download PDFInfo
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- CN113907952A CN113907952A CN202111014416.5A CN202111014416A CN113907952A CN 113907952 A CN113907952 A CN 113907952A CN 202111014416 A CN202111014416 A CN 202111014416A CN 113907952 A CN113907952 A CN 113907952A
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- 238000002360 preparation method Methods 0.000 title claims description 23
- 229920000742 Cotton Polymers 0.000 claims abstract description 43
- 229920001477 hydrophilic polymer Polymers 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 14
- 238000002791 soaking Methods 0.000 claims abstract description 14
- 239000002861 polymer material Substances 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 230000001954 sterilising effect Effects 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 239000004814 polyurethane Substances 0.000 claims abstract description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 3
- 229920002635 polyurethane Polymers 0.000 claims abstract description 3
- 239000004952 Polyamide Substances 0.000 claims description 56
- 229920002647 polyamide Polymers 0.000 claims description 56
- 239000004332 silver Substances 0.000 claims description 42
- 229910052709 silver Inorganic materials 0.000 claims description 42
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 31
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims description 16
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000000178 monomer Substances 0.000 claims description 13
- 125000003277 amino group Chemical group 0.000 claims description 12
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 12
- -1 silver ions Chemical class 0.000 claims description 12
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 11
- 229960001124 trientine Drugs 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 239000008213 purified water Substances 0.000 claims description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 230000000536 complexating effect Effects 0.000 claims description 8
- 229940014800 succinic anhydride Drugs 0.000 claims description 8
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 150000001336 alkenes Chemical class 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
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- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 4
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- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical compound CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 claims description 2
- DSZTYVZOIUIIGA-UHFFFAOYSA-N 1,2-Epoxyhexadecane Chemical compound CCCCCCCCCCCCCCC1CO1 DSZTYVZOIUIIGA-UHFFFAOYSA-N 0.000 claims description 2
- MPGABYXKKCLIRW-UHFFFAOYSA-N 2-decyloxirane Chemical compound CCCCCCCCCCC1CO1 MPGABYXKKCLIRW-UHFFFAOYSA-N 0.000 claims description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 230000003670 easy-to-clean Effects 0.000 abstract description 3
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- MCSINKKTEDDPNK-UHFFFAOYSA-N propyl propionate Chemical compound CCCOC(=O)CC MCSINKKTEDDPNK-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229940059260 amidate Drugs 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- NPUKDXXFDDZOKR-LLVKDONJSA-N etomidate Chemical compound CCOC(=O)C1=CN=CN1[C@H](C)C1=CC=CC=C1 NPUKDXXFDDZOKR-LLVKDONJSA-N 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
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- 206010053615 Thermal burn Diseases 0.000 description 2
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开一种不粘敷料,包括医用棉质基材和亲水防黏连层,所述亲水防黏连层由超亲水高分子材料组成,所述超亲水高分子材料包括聚乙烯吡咯烷酮、聚氨酯、聚乙二醇、聚乙烯吡咯烷酮中的任意一种或多种。该不粘敷料,不仅具有亲水防黏连的作用,而且还能提高医用棉质基材的渗液吸收能力,减少敷料与创面黏连减轻患者换药疼痛,同时伤口上不残留意外物质易清洁。还公开了不粘敷料的制备方法,包括如下步骤:先将超亲水高分子材料溶于溶剂中,得到超亲水高分子溶液;然后将医用棉质基材进行干燥处理后,浸泡于超亲水高分子溶液中;浸泡完成后压榨去掉多余液体,晾干或烘干,灭菌后即得到所述的不粘敷料。操作简单,成本低廉环保,适合工业生产。
Description
技术领域
本发明属于医疗卫生/纳米材料领域,尤其涉及一种不粘敷料及制备方法。
背景技术
医用棉质基材(如医用脱脂棉纱布,外科纱布敷料,脱脂棉无纺布)无毒、无刺激、生物相容性好,广泛应用于医用敷料,然而这种敷料应用于创面,特别大面积烧烫伤创面,这种敷料容易与创面黏连,换药易对患者造成疼痛、对伤口造成二次伤害。
目前为了克服上述问题,通常采用将敷料浸泡于液体石蜡油或医用凡士林(如医用凡士林纱布)等油脂类憎水物的方式以减少创面黏连,但是浸泡这类油性物质,会使敷料吸水性(吸收渗液能力)及吸液速度下降,同时油性物质也容易残留在创面上较难清洁清洗,同时也影响创面愈合的速度。因此,开发一种新型的不粘敷料迫在眉睫。
发明内容
本发明所要解决的技术问题是,克服以上背景技术中提到的不足和缺陷,提供一种亲水防黏连同时提高其渗液吸收能力的不粘敷料及制备方法,减少敷料与创面黏连减轻患者换药疼痛,同时伤口上不残留意外物质易清洁。
为解决上述技术问题,本发明提出的技术方案为:
一种不粘敷料,包括医用棉质基材和亲水防黏连层,所述亲水防黏连层由超亲水高分子材料组成,所述超亲水高分子材料包括聚乙烯吡咯烷酮、聚氨酯、聚乙二醇、聚乙烯吡咯烷酮中的任意一种或多种。
不粘伤口的原理:通过改性处理后的医用棉质基材,纤维表面被接枝或吸附上了一层超吸水亲水超滑的材料,该材料由超亲水高分子材料组成,在干燥状态与常规敷料基材外观手感一致,一旦遇水,吸水后能迅速吸收自身体积百倍及几百倍的水,在医用棉质基材与伤口皮肤界面之间形成一种“微水凝胶”,这种界面具有遇水不粘、在湿润状态下超滑的性质,从而使医用棉质基材与创面不粘,且大大增加了医用棉质基材吸收渗液的能力。且本发明的不粘敷料在创面干燥的情况下换药,只要湿润不粘敷料即可轻松与创面分离而不造成二次伤害,减轻换药时病人的痛苦。同时本发明的不粘敷料改善了传统油性防粘纱布的油腻、不透气、残留油性物质难清洗等问题,给人亲肤、清爽的感受,且生物相容性好。
上述的不粘敷料,优选的,所述医用棉质基材包括纯棉无纺布、医用纱布、脱脂棉纱布或黏胶纤维混纺的无纺布。
优选的,所述医用棉质基材中负载有改性聚酰胺络合银;所述改性聚酰胺络合银主要由银离子与改性聚酰胺的氨基络合而成,所述改性聚酰胺的氨基仅存在于其分子结构的内部。
优选的,所述氨基和银离子的摩尔比为3~50:1(更优选为3:1),所述改性聚酰胺的结构式为:
医用棉质基材以纤维素为主要组分,纤维素中富含的羟基,在水溶液水中会产生电离带一定负电荷。改性聚酰胺中含有的氨基仅存在于分子结构内部,使得银离子包裹于改性聚酰胺内部,多余的氨基在水溶液中质子化后使其表面富含正电荷,与纤维素中的羟基发生静电吸附及产生氢键等作用,使聚酰胺分子在纤维素纱布上有良好的分散均匀性与附着稳定性及确定的比例关系,从而使聚酰胺络合银与纱布紧密结合不脱落,并保持优异的抑菌性能。
实验证明,该改性聚酰胺络合银负载于纱布后,其银离子能够固定微量释放,释放稳定;银离子释放持续时间达7天以上,释放持久;对大肠杆菌、金色葡萄球菌、绿农杆菌、白色念珠菌等抑菌率达99.9%以上,抑菌性能优异;且无刺激、无致敏、无急慢性全身毒性、无遗传毒性,具有良好的生物相容性。
基于一个总的发明构思,本发明还提供一种不粘敷料的制备方法,包括如下步骤:
(1)将所述超亲水高分子材料溶于溶剂中,得到超亲水高分子溶液;
(2)将所述医用棉质基材进行干燥处理后,浸泡于所述超亲水高分子溶液中;
(3)浸泡完成后压榨去掉多余液体,晾干或烘干,灭菌后即得到所述的不粘敷料。
上述的制备方法,优选的,所述溶剂包括二丙酮醇、丁酮、纯化水、酒精中的任意一种或多种,所述超亲水高分子溶液中所含超亲水高分子材料的浓度为0.1-5:100g/mL。
优选的,所述干燥处理为真空烘干,烘干时间为30min~60min,所述浸泡的时间为30min以上。
优选的,在所述医用棉质基材进行干燥处理后先浸泡于改性聚酰胺络合银溶液,然后再浸泡于所述超亲水高分子溶液中;
所述改性聚酰胺络合银溶液的制备方法包括如下步骤:
S1、通过多氨基单体与烯烃类物质发生缩聚反应合成超支化多氨基聚合物,然后通过酸酐类物质或环氧烷类物质对所述超支化多氨基聚合物进行改性,得到改性聚酰胺;
S2、分别将所述改性聚酰胺及硝酸银或醋酸银溶解于纯化水溶液中,将硝酸银或醋酸银溶液缓慢滴加到改性聚酰胺溶液中进行络合反应,加热挥发后,得到改性聚酰胺络合银溶液。
更优选的,所述多氨基单体为二乙烯三胺、三乙烯四胺、四乙烯五胺和五乙烯六胺中的任意一种或几种,所述烯烃类物质为丙烯酸、丙烯酸甲酯、甲基丙烯酸甲酯和丙烯酸乙酯中的任意一种或几种,所述酸酐类物质为丁二酸酐、马来酸酐中的任意一种或几种,所述环氧烷类物质为环氧乙烷、环氧丙烷、1,2-环氧丁烷、环氧十二烷和1,2-环氧十六烷中的任意一种或几种;所述多氨基单体和烯烃类物质的摩尔比为1:1~6,所述超支化多氨基聚合物和酸酐类物质的摩尔比为1:3~200,所述超支化多氨基聚合物和环氧烷类物质的摩尔比为1:3~200。
更优选的,所述缩聚反应的操作包括如下步骤:将多氨基单体在冰水浴冷却到5-10℃,然后滴加烯烃类物质,滴加完毕后常温下反应1-4h生成淡黄色中间体,将中间体放置到旋转蒸发仪上减压真空度0.1-1000Pa,除去未反应单体及其他溶剂,再升温到80-170℃减压反应2-48h,即得到多氨基超支化聚合物;
所述改性的反应条件为:在100-160℃下减压10Pa-105Pa,反应时间为1-24h;
所述络合反应的反应温度为50-100℃,反应时间为5min-60min;所述聚酰胺络合银溶液中,氨基和银离子的摩尔比为3~50:1;
所述加热挥发的加热温度为80-95℃,加热时间为30min-120min。
总的来说,本发明先制备超亲水防粘的亲水防黏连层,用亲水防黏连层,对医用棉质基材(如纯棉无纺布、医用纱布、脱脂棉与黏胶纤维混纺的无纺布)进行表面超亲水改性处理,然后干燥、分切、包装、灭菌即可制的不粘敷料。进一步的若在亲水防黏连层中或者医用棉质基材中增加抑菌成分(如改性聚酰胺络合银)可增加其抗菌的功能。
与现有技术相比,本发明的有益效果为:
1、本发明的不粘敷料,不仅具有亲水防黏连的作用,而且还能提高医用棉质基材的渗液吸收能力,减少敷料与创面黏连减轻患者换药疼痛,同时伤口上不残留意外物质易清洁。
2、本发明的不粘敷料,还可以在亲水防黏连层中或者医用棉质基材中增加抑菌成分(如改性聚酰胺络合银),可进一步增加其抗菌的功能。
3、本发明的制备方法,操作简单,成本低廉环保,适合工业生产。
具体实施方式
为了便于理解本发明,下文将结合说明书和较佳的实施例对本发明做更全面、细致地描述,但本发明的保护范围并不限于以下具体实施例。
除非另有定义,下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的,并不是旨在限制本发明的保护范围。
除非另有特别说明,本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。
实施例1:
一种不粘敷料,由纯棉无纺布和亲水防黏连层组成,亲水防黏连层由PVP(k90)和PU组成。该不粘敷料的制备方法如下:
(1)超亲水高分子溶液的制备:将2g PVP(k90)加入到事先量好的30mL二丙酮醇与10mL丁酮的混合溶剂中搅拌使之溶解得到溶液A,将2g PU加入到事先量好的30mL二丙酮醇与10mL丁酮的混合溶剂中搅拌使之溶解得到溶液B;再把溶解好的A、B两种溶液按2:1体积混合搅匀即配成超亲水高分子溶液;
(2)基材准备及处理:将纯棉无纺布材料,放入真空干燥箱中,真空烘干30min;
(3)基材涂层处理:将处理过的纱布在超亲水高分子溶液中浸润,压榨去掉多余液体,晾干,得到改性后的纱布;
(4)产品、包装、灭菌,即得到不粘敷料。
实施例2:
一种不粘敷料,由普通医用纱布和亲水防黏连层组成,亲水防黏连层由PEGMn4000组成。该不粘敷料的制备方法如下:
(1)超亲水高分子溶液的制备:取2g PEG Mn4000加入500mL纯化水中搅拌1h充分溶解;
(2)基材准备及处理:普通医用纱布材料,放入真空干燥箱中,真空烘干30min,取出纱布,放入等离子清洗机,正反两面等离子处理各3min(可以增加纱布与亲水防黏连层的结合效果);
(3)处理过的纱布置于超亲水高分子溶液中浸没30min后取出,取出100℃烘干,得到改性后的纱布;
(4)产品、包装、灭菌,即得到不粘敷料。
实施例3:
一种不粘敷料,由医用脱脂棉纱布和亲水防黏连层组成,亲水防黏连层由PVP和醋酸氯己定组成。该不粘敷料的制备方法如下:
(1)超亲水高分子溶液的制备:取3g PVP(k90)、0.05g醋酸氯己定溶解于5000mL的酒精中;
(2)基材准备及处理:将医用脱脂棉纱布,放入真空干燥箱中,真空烘干30min;
(3)基材涂层处理:将处理过的纱布在超亲水高分子溶液浸润,压榨去掉多余液体,晾干,得到改性后的纱布;
(4)产品、包装、灭菌,即得到不粘敷料。
实施例4:
一种不粘敷料,由纯棉无纺布和亲水防黏连层组成,亲水防黏连层由PVP(k90)和PU组成,纯棉无纺布中负载有改性聚酰胺络合银。该不粘敷料的制备方法如下:
(1)改性聚酰胺络合银:将三乙烯四胺在冰水浴冷却到5-10℃,然后用漏斗向其缓慢滴加丙烯酸,滴加完毕后常温下反应4h生成淡黄色中间体,将中间体放置到旋转蒸发仪上减压除去未反应单体及其他溶剂,再升温到120℃-140℃减压反应2-4h,得到多氨基超支化聚合物;然后通过丁二酸酐对超支化多氨基聚合物进行改性(具体是在140-150℃继续减压10-100Pa,反应时间为1-4h),使其端氨基酰胺化并转移至分子结构的内部,得到改性聚酰胺;三乙烯四胺和丙烯酸的摩尔比为1:2,超支化多氨基聚合物和丁二酸酐的摩尔比为1:30;分别将改性聚酰胺20g及硝酸银10g溶解于1000mL纯化水溶液中,将硝酸银溶液缓慢滴加到改性聚酰胺溶液中进行络合反应(50℃,200转/min,20min),加热至95℃进行挥发后(30min),进行干燥,得到改性聚酰胺络合银溶液(氨基和银离子的摩尔比为3:1);
(2)超亲水高分子溶液的制备:将2g PVP(k90)加入到事先量好的30mL二丙酮醇与10mL丁酮的混合溶剂中搅拌使之溶解得到溶液A,将2g PU加入到事先量好的30mL二丙酮醇与10mL丁酮的混合溶剂中搅拌使之溶解得到溶液B;再把溶解好的A、B两种溶液按2:1体积混合搅匀即配成超亲水高分子溶液;
(3)基材准备及处理:将纯棉无纺布材料,放入真空干燥箱中,真空烘干30min;
(4)浸染固化:在常温下,将步骤(3)烘干的纯棉无纺布浸染于聚酰胺络合银溶液中2-3s,110℃烘烤干燥,得到载银纱布;
(5)基材涂层处理:在常温下,将载银纱布在超亲水高分子溶液浸润,压榨去掉多余液体,110℃烘烤干燥,得到改性后的纱布;
(6)产品、包装、灭菌,即得到不粘敷料。
实施例5:
一种不粘敷料,由普通医用纱布和亲水防黏连层组成,亲水防黏连层由PEGMn4000组成,普通医用纱布中负载有改性聚酰胺络合银。该不粘敷料的制备方法如下:
(1)改性聚酰胺络合银:将三乙烯四胺在冰水浴冷却到5-10℃,然后用漏斗向其缓慢滴加丙烯酸,滴加完毕后常温下反应4h生成淡黄色中间体,将中间体放置到旋转蒸发仪上减压除去未反应单体及其他溶剂,再升温到120℃-140℃减压反应2-4h,得到多氨基超支化聚合物;然后通过丁二酸酐对超支化多氨基聚合物进行改性(具体是在140-150℃继续减压10-100Pa,反应时间为1-4h),使其端氨基酰胺化并转移至分子结构的内部,得到改性聚酰胺;三乙烯四胺和丙烯酸的摩尔比为1:2,超支化多氨基聚合物和丁二酸酐的摩尔比为1:30;分别将改性聚酰胺20g及硝酸银10g溶解于1000mL纯化水溶液中,将硝酸银溶液缓慢滴加到改性聚酰胺溶液中进行络合反应(50℃,200转/min,20min),加热至95℃进行挥发后(30min),进行干燥,得到改性聚酰胺络合银溶液(氨基和银离子的摩尔比为3:1);
(2)超亲水高分子溶液的制备:取2g PEG Mn4000加入500mL纯化水中搅拌1h充分溶解;
(3)基材准备及处理:普通医用纱布材料,放入真空干燥箱中,真空烘干30min,取出纱布,放入等离子清洗机,正反两面等离子处理各3min;
(4)浸染固化:在常温下,将步骤(3)烘干的普通医用纱布材料浸染于聚酰胺络合银溶液中2-3s,110℃烘烤干燥,得到载银纱布;
(5)基材涂层处理:在常温下,将载银纱布在超亲水高分子溶液浸润,压榨去掉多余液体,110℃烘烤干燥,得到改性后的纱布;
(6)产品、包装、灭菌,即得到不粘敷料。
实施例6:
一种不粘敷料,由医用脱脂棉纱布和亲水防黏连层组成,亲水防黏连层由PVP和醋酸氯己定组成,医用脱脂棉纱布中负载有改性聚酰胺络合银。该不粘敷料的制备方法如下:
(1)改性聚酰胺络合银:将三乙烯四胺在冰水浴冷却到5-10℃,然后用漏斗向其缓慢滴加丙烯酸,滴加完毕后常温下反应4h生成淡黄色中间体,将中间体放置到旋转蒸发仪上减压除去未反应单体及其他溶剂,再升温到120℃-140℃减压反应2-4h,得到多氨基超支化聚合物;然后通过丁二酸酐对超支化多氨基聚合物进行改性(具体是在140-150℃继续减压10-100Pa,反应时间为1-4h),使其端氨基酰胺化并转移至分子结构的内部,得到改性聚酰胺;三乙烯四胺和丙烯酸的摩尔比为1:2,超支化多氨基聚合物和丁二酸酐的摩尔比为1:30;分别将改性聚酰胺20g及硝酸银10g溶解于1000mL纯化水溶液中,将硝酸银溶液缓慢滴加到改性聚酰胺溶液中进行络合反应(50℃,200转/min,20min),加热至95℃进行挥发后(30min),进行干燥,得到改性聚酰胺络合银溶液(氨基和银离子的摩尔比为3:1);
(2)超亲水高分子溶液的制备:超亲水高分子溶液的制备:取3g PVP(k90)、0.05g醋酸氯己定溶解于5000mL的酒精中;
(3)基材准备及处理:将医用脱脂棉纱布,放入真空干燥箱中,真空烘干30min;
(4)浸染固化:在常温下,将步骤(3)烘干的医用脱脂棉纱布浸染于聚酰胺络合银溶液中2-3s,110℃烘烤干燥,得到载银纱布;
(5)基材涂层处理:在常温下,将载银纱布在超亲水高分子溶液浸润,压榨去掉多余液体,110℃烘烤干燥,得到不粘纱布;
(6)产品、包装、灭菌,即得到不粘敷料。
为了进一步证明本发明的不粘敷料的技术效果,进行如下试验:
不粘及促愈合实验对象选择巴马小猪,依据YY1477.2-2016《接触性创面敷料性能评价用标准试验模型第2部分:评价促进创面愈合性能的动物烫伤模型》);液体吸收能力参考YY0471.1-2004《接触性创面试验方法第1部分:液体吸收性》;微生物抑菌试验(对大肠杆菌、金色葡萄球菌、白色念珠菌的抑菌性能结果)按照GB15979-2001《一次性使用卫生用品卫生标准》附录C产品杀菌性能、抑菌性能与稳定性测试方法。得到的试验结果见表1。
表1:实施例1-6中制备得到的产品的不粘情况
Claims (10)
1.一种不粘敷料,其特征在于,包括医用棉质基材和亲水防黏连层,所述亲水防黏连层由超亲水高分子材料组成,所述超亲水高分子材料包括聚乙烯吡咯烷酮、聚氨酯、聚乙二醇、聚乙烯吡咯烷酮中的任意一种或多种。
2.根据权利要求1所述的不粘敷料,其特征在于,所述医用棉质基材包括纯棉无纺布、医用纱布、脱脂棉纱布或黏胶纤维混纺的无纺布。
3.根据权利要求1或2所述的不粘敷料,其特征在于,所述医用棉质基材中负载有改性聚酰胺络合银;所述改性聚酰胺络合银主要由银离子与改性聚酰胺的氨基络合而成,所述改性聚酰胺的氨基仅存在于其分子结构的内部。
5.一种如权利要求1-4中任一项所述的不粘敷料的制备方法,其特征在于,包括如下步骤:
(1)将所述超亲水高分子材料溶于溶剂中,得到超亲水高分子溶液;
(2)将所述医用棉质基材进行干燥处理后,浸泡于所述超亲水高分子溶液中;
(3)浸泡完成后压榨去掉多余液体,晾干或烘干,灭菌后即得到所述的不粘敷料。
6.根据权利要求5所述的制备方法,其特征在于,所述溶剂包括二丙酮醇、丁酮、纯化水、酒精中的任意一种或多种,所述超亲水高分子溶液中所含超亲水高分子材料的浓度为0.1-5:100g/mL。
7.根据权利要求5所述的制备方法,其特征在于,所述干燥处理为真空烘干,烘干时间为30min~60min,所述浸泡的时间为30min以上。
8.根据权利要求5-7中任一项所述的制备方法,其特征在于,在所述医用棉质基材进行干燥处理后先浸泡于改性聚酰胺络合银溶液,干燥后再浸泡于所述超亲水高分子溶液中;
所述改性聚酰胺络合银溶液的制备方法包括如下步骤:
S1、通过多氨基单体与烯烃类物质发生缩聚反应合成超支化多氨基聚合物,然后通过酸酐类物质或环氧烷类物质对所述超支化多氨基聚合物进行改性,得到改性聚酰胺;
S2、分别将所述改性聚酰胺及硝酸银或醋酸银溶解于纯化水溶液中,将硝酸银或醋酸银溶液缓慢滴加到改性聚酰胺溶液中进行络合反应,加热挥发后,得到改性聚酰胺络合银溶液。
9.根据权利要求8所述的制备方法,其特征在于,所述多氨基单体为二乙烯三胺、三乙烯四胺、四乙烯五胺和五乙烯六胺中的任意一种或几种,所述烯烃类物质为丙烯酸、丙烯酸甲酯、甲基丙烯酸甲酯和丙烯酸乙酯中的任意一种或几种,所述酸酐类物质为丁二酸酐、马来酸酐中的任意一种或几种,所述环氧烷类物质为环氧乙烷、环氧丙烷、1,2-环氧丁烷、环氧十二烷和1,2-环氧十六烷中的任意一种或几种;所述多氨基单体和烯烃类物质的摩尔比为1:1~6,所述超支化多氨基聚合物和酸酐类物质的摩尔比为1:3~200,所述超支化多氨基聚合物和环氧烷类物质的摩尔比为1:3~200。
10.根据权利要求8所述的制备方法,其特征在于,所述缩聚反应的操作包括如下步骤:将多氨基单体在冰水浴冷却到5-10℃,然后滴加烯烃类物质,滴加完毕后常温下反应1-4h生成淡黄色中间体,将中间体放置到旋转蒸发仪上减压真空度0.1-1000Pa,除去未反应单体及其他溶剂,再升温到80-170℃减压反应2-48h,即得到多氨基超支化聚合物;
所述改性的反应条件为:在100-160℃下减压10Pa-105Pa,反应时间为1-24h;
所述络合反应的反应温度为50-100℃,反应时间为5min-60min;所述聚酰胺络合银溶液中,氨基和银离子的摩尔比为3~50:1;
所述加热挥发的加热温度为80-95℃,加热时间为30min-120min。
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