CN116731607A - (TiZnCe)O2-X/PDMS涂层及其制备与应用 - Google Patents
(TiZnCe)O2-X/PDMS涂层及其制备与应用 Download PDFInfo
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- CN116731607A CN116731607A CN202310702365.8A CN202310702365A CN116731607A CN 116731607 A CN116731607 A CN 116731607A CN 202310702365 A CN202310702365 A CN 202310702365A CN 116731607 A CN116731607 A CN 116731607A
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- tiznce
- pdms
- coating
- cerium
- titanium
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- 238000000576 coating method Methods 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 235000013870 dimethyl polysiloxane Nutrition 0.000 title claims abstract 21
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 title claims abstract 21
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 13
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- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 claims description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 claims description 6
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 claims description 6
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- PYPNFSVOZBISQN-LNTINUHCSA-K cerium acetylacetonate Chemical compound [Ce+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O PYPNFSVOZBISQN-LNTINUHCSA-K 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 4
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
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- 239000011592 zinc chloride Substances 0.000 claims description 4
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- INNSZZHSFSFSGS-UHFFFAOYSA-N acetic acid;titanium Chemical compound [Ti].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O INNSZZHSFSFSGS-UHFFFAOYSA-N 0.000 claims description 3
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- ZEDZJUDTPVFRNB-UHFFFAOYSA-K cerium(3+);triiodide Chemical compound I[Ce](I)I ZEDZJUDTPVFRNB-UHFFFAOYSA-K 0.000 claims description 3
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Classifications
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- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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Abstract
本发明涉及表面涂层技术领域,尤其是涉及(TiZnCe)O2‑X/PDMS涂层及其制备与应用。本发明首先将钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀后反应,反应后后处理得到氧化物前驱体;然后将氧化物前驱体进行热处理,得到(TiZnCe)O2‑X粉体;进一步将(TiZnCe)O2‑X粉体与、PDMS和固化剂混匀,得到(TiZnCe)O2‑X/PDMS粉体涂层;最后通过压缩空气喷涂方法在基体上喷涂上述粉体涂层,后处理得到(TiZnCe)O2‑X/PDMS涂层;其中,X为0~2,且X不为2。本发明的(TiZnCe)O2‑X/PDMS涂层可进一步应用于硅酮橡胶手套,得到压力修复手套,并用于患者创面愈合压力治疗。
Description
技术领域
本发明涉及表面涂层技术领域,尤其是涉及(TiZnCe)O2-X/PDMS涂层及其制备与应用。
背景技术
遗传性大疱性表皮松解症(Epidermolysis bullosa,EB)是一种由基因缺陷引起,以轻微摩擦或外伤后皮肤、粘膜水疱或大疱形成为特征的严重的遗传性皮肤病。其中,隐性遗传(RDEB)亚型因VII型胶原基因(COL7A1)突变,导致功能性VII型胶原(C7)缺乏,导致严重的全身症状。患者的手足部因日常生活中的活动和摩擦反复起疱、溃疡和愈合,出现严重的并指畸形伴随反复皮肤创伤及瘢痕形成,使得关节长期屈曲并挛缩,导致活动功能障碍,使患者丧失最基本的生活自理能力。Fromy等调查了手指受逐渐增加的压力作用时健康人的皮肤血流量的变化情况,发现在低压力(约2.67kPa)下手指皮肤血流量明显增加,当压力增大到“毛细血管关闭”(约4.27kPa)时手指皮肤血流量减少。
目前市场上的压力手套或压力袜产品按其压力范围主要分为3种:压力在2.40~2.67kPa之间,用于保健的低压手套;压力在2.67~4.00kPa之间,用于治疗水肿或轻度静脉曲张的中压手套;压力在4.00~5.33kPa之间,用于治疗患有严重静脉疾病患者的高压手套。现有的分指硅胶压力手套产品给予瘢痕持续的压力和保湿保软的作用,以达到延缓手指关节挛缩,防止并指复发,但临床使用中存在舒适度差,患者依从性低的问题。
聚二甲基硅氧烷(Polydimethylsiloxane,PDMS)是一种疏水类的线性高分子有机硅材料。具有低表面张力,易于铺展、良好的生物相容性,适宜的黏度的结合赋予个人护理制品润滑、低黏度赋予皮肤干爽的感觉。尤其是PDMS材料优异的弹性及回弹性,耐温耐候性能突出,透光性能以及优异的透气性能,是传统聚酯薄膜透气性的50倍以上。PDMS薄膜系列产品在医疗器械,柔性电子,光学以及透气功能型应用中均具备良好的应用前景。
事实上TiO2和ZnO光催材料因其广谱抑菌性一直被广泛研究,但是由于和ZnO薄膜的抗菌性存在不确定性其经常与其他物质混合来优化其抗菌作用。根据光催化反应的基本理论,TiO2和ZnO需要在光照条件下才能起到良好的杀灭效果。已有的报道和专利表明,通过二元掺杂金属离子可实现在弱光和无光条件下TiO2和ZnO材料的抗菌和皮肤修复,但是性能稳定性还有待进一步提高。关于CeOx纳米粒子的生物亲和性的研究,M.Sendra团队提出纳米粒子和细胞壁的电荷量会影响细胞多样性。团队通过在海藻培养皿中分别加入正负电位的CeOx来探究Zeta电位对细胞分化的影响。研究发现,正Zeta电位的CeOx纳米颗粒可以增加细胞多样性,在细胞复杂性达到一定范围内时,CeOx不会引起毒性;当复杂性高达一定程度后CeOx增加了活性氧和毒性的产生。Martin T.Matter团队验证了CeOx纳米粒子的抗菌性,并且证明了其抑制细胞在材料表面生长的效果。纳米粒子形成与细菌相似大小和表面电荷的超结构,因在TiO2中添加CeOx后,最先因为掺杂引入的Ce离子半径均超过Ti的离子半径,这类掺杂会促使TiO2的晶格胀大,会造成二氧化钛产生晶格畸变,少许晶格畸变可产生电子陷阱,进而利于空穴的分离出来转移,提高其催化反应工作能力;次之因为引入残渣电子能级,促使掺杂TiO2的禁带宽度缩小,提高了跃迁全过程中对可见光的使用率。
此外二氧化钛TiO2是一种无机物,具有无毒、最佳的不透明性、最佳白度和光亮度,广泛应用于涂料、化妆品等工业。纳米二氧化钛可使玻璃表面附着的水滴迅速扩散成均匀的水膜,表面不会产生会发生光散射的雾,可维持高度的透明性,用纳米二氧化钛制成的防雾薄膜具有良好的耐磨损、耐擦伤、耐溶剂性。氧化铈CeOx稀土元素的盐能降低凝血酶原的含量,使其失活,并抑制凝血活素的生成,使纤维蛋白原沉淀,催化分解磷酸化合物,氧化铈也用在化妆品中起到抗紫外线作用。
发明内容
为了解决上述问题,本发明的目的是提供(TiZnCe)O2-X/PDMS涂层及其制备与应用。本发明首先将钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀后反应,反应后后处理得到氧化物前驱体;然后将氧化物前驱体进行热处理,得到(TiZnCe)O2-X粉体;进一步将(TiZnCe)O2-X粉体与、PDMS和固化剂混匀,得到(TiZnCe)O2-X/PDMS粉体涂层;最后通过压缩空气喷涂方法在基体上喷涂上述粉体涂层,后处理得到(TiZnCe)O2-X/PDMS涂层;其中,X为0~2,且X不为2。本发明的(TiZnCe)O2-X/PDMS涂层可进一步应用于硅酮橡胶手套,得到压力修复手套,并用于患者创面愈合压力治疗。
本发明的目的可以通过以下技术方案来实现:
本发明的第一个目的是提供一种(TiZnCe)O2-X/PDMS涂层的制备方法,包括以下步骤:
(S1)将钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀后反应,反应后后处理得到氧化物前驱体;
(S2)将步骤(S1)制备得到的氧化物前驱体进行热处理,得到(TiZnCe)O2-X粉体;
(S3)将步骤(S2)制备得到的(TiZnCe)O2-X粉体与、PDMS和固化剂混匀,得到(TiZnCe)O2-X/PDMS粉体涂层;
(S4)通过压缩空气喷涂方法在基体上喷涂步骤(S3)制备得到的(TiZnCe)O2-X/PDMS粉体涂层,后处理得到(TiZnCe)O2-X/PDMS涂层;
其中,X为0~2,且X不为2。
在本发明的一个实施方式中,步骤(S1)中,所述钛金属盐选自异丙醇钛、乙酰丙酮钛、乙酸钛、芳香族钛、氯化钛、溴化钛或碘化钛中的一种;
所述锌金属盐选自异丙醇锌、乙酰丙酮锌、乙酸锌、芳香族锌、氯化锌、溴化锌或碘化锌中的一种;
所述铈金属盐选自异丙醇铈、乙酰丙酮铈、乙酸铈、芳香族铈、氯化铈、溴化铈或碘化铈中的一种。
在本发明的一个实施方式中,步骤(S1)中,钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀时可以适当升温(低于60℃)以加速溶解。
在本发明的一个实施方式中,步骤(S1)中,反应过程中,升温速率为5℃/min,反应温度为200℃~300℃,反应温度下时间维持40min~60min。
在本发明的一个实施方式中,步骤(S1)中,所述后处理为保温处理后依次进行离心、洗涤后干燥;
保温过程中,温度为200℃~300℃,时间为24h~96h,然后以5℃/min的降温速率随炉冷却至室温;
离心、洗涤次数为3次以上;
离心过程中,转速为10000rpm以上,离心时间为5min~20min;
洗涤过程中,使用有机溶剂进行洗涤;所述有机溶剂选自乙醇、异丙醇、***或三氯甲烷中的一种,优选地,有机溶剂选自***或三氯甲烷;
干燥过程中,温度为60℃~120℃。
在本发明的一个实施方式中,步骤(S2)中,热处理过程处于氩气气氛下,氩气流速为0.05L/min~1L/min,优选地,氩气流速为0.2L/min;
热处理过程中,温度为220℃~350℃,时间为2h~10h。
在本发明的一个实施方式中,(TiZnCe)O2-X粉体的粒径为3nm~15nm。
在本发明的一个实施方式中,步骤(S3)中,(TiZnCe)O2-X/PDMS粉体涂层中还含有SYLGARD-84二甲基硅烷或道康宁DC-732W中的一种;
(TiZnCe)O2-X粉体、PDMS、SYLGARD-84二甲基硅烷或道康宁DC-732W、化剂的质量百分比为1%~9%:0.5%~1%:0.5%~1%:89%~98%。
在本发明的一个实施方式中,步骤(S4)中,压缩空气喷涂过程中,喷涂压力为0.1MPa~0.25MPa,涂层厚度为10μm~50μm。
在本发明的一个实施方式中,步骤(S4)中,所述后处理为固化干燥处理;
固化干燥过程处于紫外状态,温度为10℃~30℃,湿度为40%~70%,时间为30min~90min。
本发明的第二个目的是提供一种通过上述方法制备得到的(TiZnCe)O2-X/PDMS涂层。
本发明的第三个目的是提供一种含有毛刷状的(TiZnCe)O2-X/PDMS涂层的手套。
本发明的第四个目的是提供一种含有毛刷状的(TiZnCe)O2-X/PDMS涂层的手套在患者创面愈合压力治疗中的应用。
与现有技术相比,本发明具有以下有益效果:
本发明提供了(TiZnCe)O2-X/PDMS涂层及其制备方法,其中,X为0~2,且X不为2;利用本发明制备方法得到的(TiZnCe)O2-X/PDMS涂层可与微米模印技术相结合应用于硅酮橡胶手套,得到含有毛刷状的(TiZnCe)O1.98/PDMS涂层的手套,并作为压力修复手套,进一步用于患者创面愈合压力治疗。
附图说明
图1为实施例2中含有毛刷状的(TiZnCe)O1.98/PDMS涂层的单手指的结构示意图;
图中标号:1、硅酮橡胶手套单个手指;2、毛刷状凸起;3、(TiZnCe)O1.98/PDMS涂层。
具体实施方式
本发明提供一种(TiZnCe)O2-X/PDMS涂层的制备方法,包括以下步骤:
(S1)将钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀后反应,反应后后处理得到氧化物前驱体;
(S2)将步骤(S1)制备得到的氧化物前驱体进行热处理,得到(TiZnCe)O2-X粉体;
(S3)将步骤(S2)制备得到的(TiZnCe)O2-X粉体与、PDMS和固化剂混匀,得到(TiZnCe)O2-X/PDMS粉体涂层;
(S4)通过压缩空气喷涂方法在基体上喷涂步骤(S3)制备得到的(TiZnCe)O2-X/PDMS粉体涂层,后处理得到(TiZnCe)O2-X/PDMS涂层;
其中,X为0~2,且X不为2。
在本发明的一个实施方式中,步骤(S1)中,所述钛金属盐选自异丙醇钛、乙酰丙酮钛、乙酸钛、芳香族钛、氯化钛、溴化钛或碘化钛中的一种;
所述锌金属盐选自异丙醇锌、乙酰丙酮锌、乙酸锌、芳香族锌、氯化锌、溴化锌或碘化锌中的一种;
所述铈金属盐选自异丙醇铈、乙酰丙酮铈、乙酸铈、芳香族铈、氯化铈、溴化铈或碘化铈中的一种。
在本发明的一个实施方式中,步骤(S1)中,钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀时可以适当升温(低于60℃)以加速溶解。
在本发明的一个实施方式中,步骤(S1)中,反应过程中,升温速率为5℃/min,反应温度为200℃~300℃,反应温度下时间维持40min~60min。
在本发明的一个实施方式中,步骤(S1)中,所述后处理为保温处理后依次进行离心、洗涤后干燥;
保温过程中,温度为200℃~300℃,时间为24h~96h,然后以5℃/min的降温速率随炉冷却至室温;
离心、洗涤次数为3次以上;
离心过程中,转速为10000rpm以上,离心时间为5min~20min;
洗涤过程中,使用有机溶剂进行洗涤;所述有机溶剂选自乙醇、异丙醇、***或三氯甲烷中的一种,优选地,有机溶剂选自***或三氯甲烷;
干燥过程中,温度为60℃~120℃。
在本发明的一个实施方式中,步骤(S2)中,热处理过程处于氩气气氛下,氩气流速为0.05L/min~1L/min,优选地,氩气流速为0.2L/min;
热处理过程中,温度为220℃~350℃,时间为2h~10h。
在本发明的一个实施方式中,(TiZnCe)O2-X粉体的粒径为3nm~15nm。
在本发明的一个实施方式中,步骤(S3)中,(TiZnCe)O2-X/PDMS粉体涂层中还含有SYLGARD-84二甲基硅烷或道康宁DC-732W中的一种;
(TiZnCe)O2-X粉体、PDMS、SYLGARD-84二甲基硅烷或道康宁DC-732W、化剂的质量百分比为1%~9%:0.5%~1%:0.5%~1%:89%~98%。
在本发明的一个实施方式中,步骤(S4)中,压缩空气喷涂过程中,喷涂压力为0.1MPa~0.25MPa,涂层厚度为10μm~50μm。
在本发明的一个实施方式中,步骤(S4)中,所述后处理为固化干燥处理;
固化干燥过程处于紫外状态,温度为10℃~30℃,湿度为40%~70%,时间为30min~90min。
本发明提供一种通过上述方法制备得到的(TiZnCe)O2-X/PDMS涂层。
本发明提供一种含有毛刷状的(TiZnCe)O2-X/PDMS涂层的手套。
本发明提供一种含有毛刷状的(TiZnCe)O2-X/PDMS涂层的手套在患者创面愈合压力治疗中的应用。
下面结合附图和具体实施例对本发明进行详细说明。
下述实施例中,若无特殊说明,所用试剂均为市售试剂,所用检测手段及方法均为本领域常规检测手段及方法。
实施例1
本实施例提供一种(TiZnCe)O1.98/PDMS涂层及其制备方法。
(S1)将乙酰丙酮钛(0.26g)、氯化锌(0.14g)、乙酸铈(0.32g)与25mL苯甲醇置于聚四氟乙烯反应釜混和,45℃下加热以加速混匀;然后将该聚四氟乙烯反应釜密封好,置于高温干燥箱中,250℃(升温速率为5℃/min)反应50min,然后保温48h,最后以5℃/min的降温速率随炉冷却至室温,得到溶胶-凝胶产物;取出溶胶-凝胶产物,置于50mL离心管中,加入***进行洗涤操作,然后置于离心机中进行10000rpm离心20min,离心结束后倒去洗涤废液,洗涤离心过程重复4次;然后将终产物置于80℃干燥箱中干燥,得到氧化物前驱体;
(S2)将步骤(S1)得到的氧化物前驱体置于非氧气炉进行热处理,炉中氩气流速为0.2L/min,300℃保温6h,得到粒径为3nm的(TiZnCe)O1.98粉体;
(S3)将步骤(S2)得到的(TiZnCe)O1.98粉体(4.5wt%)与PDMS(0.5wt%)、道康宁DC-732W(0.8wt%)、正硅酸乙酯(94.2wt%)混匀,得到(TiZnCe)O1.98/PDMS粉体涂层;
(S4)将步骤(S3)得到的(TiZnCe)O1.98/PDMS粉体涂层利用压缩空气喷涂方法喷涂在聚碳酸酯上,并控制喷涂压力为0.2MPa,喷涂厚度为35μm;喷涂结束后将其置于无菌操作箱中进行固化干燥处理,开启无菌操作相中200W紫外灯,控制温度为20℃,湿度为50%,固化干燥60min,得到(TiZnCe)O1.98/PDMS涂层。
实施例2
本实施例提供一种含有毛刷状的(TiZnCe)O1.98/PDMS涂层及其制备方法。
本实施例步骤(S1)、(S2)、(S3)与实施例1均相同;
(S4)利用微米模印技术制备硅酮橡胶手套包括以下步骤:
用柔软的沙泥做成一个平整的模子,将测试者的手放入,挤压后成印模,然后用手持光学3D扫描仪(Sense)进行扫描,生成手掌印模;然后选择FDM(熔融挤压成型)打印机利用树脂材料打印手掌印模;打印结束后,将手套支撑材料(聚氨酯纤维)和丝网(孔径为1mm的铜网)覆盖于手掌模印外,最后将PDMS涂覆在其表面,控制厚度为5mm;将整体置于无菌操作箱中进行固化干燥处理,开启无菌操作箱中200W紫外灯,控制温度为20℃,湿度为50%,固化干燥60min,得到硅酮橡胶手套;
(S5)去除手掌印模和手套支撑材料后将步骤(S3)得到的(TiZnCe)O1.98/PDMS粉体涂层利用压缩空气喷涂方法喷涂在硅酮橡胶手套内侧,并控制喷涂厚度为35μm;喷涂结束后将其置于无菌操作箱中进行固化干燥处理,开启无菌操作箱中200W紫外灯,控制温度为20℃,湿度为50%,固化干燥60min,取出丝网后得到含有毛刷状的(TiZnCe)O1.98/PDMS涂层的手套(也可称为“压力修复手套”,其中含有毛刷状的(TiZnCe)O1.98/PDMS涂层的单手指的结构示意图如图1所示,硅酮橡胶手套单个手指1内侧含有毛刷状凸起2,(TiZnCe)O1.98/PDMS涂层3包覆于毛刷状凸起2外表面)。
本实施例制备得到的含有毛刷状的(TiZnCe)O1.98/PDMS涂层的手套可进一步应用于患者创面愈合压力治疗中。
实施例3
本实施例提供一种(TiZnCe)O1.97/PDMS涂层及其制备方法。
(S1)将异丙醇钛(0.28g)、乙酸锌(0.18g)、氯化铈(0.35g)与30mL苯甲醇置于聚四氟乙烯反应釜混和,50℃下加热以加速混匀;然后将该聚四氟乙烯反应釜密封好,置于高温干燥箱中,300℃(升温速率为5℃/min)反应40min,然后保温24h,最后以5℃/min的降温速率随炉冷却至室温,得到溶胶-凝胶产物;取出溶胶-凝胶产物,置于50mL离心管中,加入三氯甲烷进行洗涤操作,然后置于离心机中进行12000rpm离心10min,离心结束后倒去洗涤废液,洗涤离心过程重复5次;然后将终产物置于1200℃干燥箱中干燥,得到氧化物前驱体;
(S2)将步骤(S1)得到的氧化物前驱体置于非氧气炉进行热处理,炉中氩气流速为1L/min,350℃保温2h,得到粒径为10nm的(TiZnCe)O1.97粉体;
(S3)将步骤(S2)得到的(TiZnCe)O1.97粉体(9wt%)与PDMS(1wt%)、SYLGARD-84二甲基硅烷(1wt%)、正硅酸四甲酯(89wt%)混匀,得到(TiZnCe)O1.97/PDMS粉体涂层;
(S4)将步骤(S3)得到的(TiZnCe)O1.97/PDMS粉体涂层利用压缩空气喷涂方法喷涂在玻璃板上,并控制喷涂压力为0.1MPa,喷涂厚度为10μm;喷涂结束后将其置于无菌操作箱中进行固化干燥处理,开启无菌操作相中200W紫外灯,控制温度为30℃,湿度为70%,固化干燥90min,得到(TiZnCe)O1.97/PDMS涂层。
实施例4
本实施例提供一种(TiZnCe)O1.99/PDMS涂层及其制备方法。
(S1)将氯化钛(0.38g)、乙酰丙酮锌(0.53g)、乙酰丙酮铈(0.87g)与50mL苯甲醇置于聚四氟乙烯反应釜混和,55℃下加热以加速混匀;然后将该聚四氟乙烯反应釜密封好,置于高温干燥箱中,200℃(升温速率为5℃/min)反应60min,然后保温96h,最后以5℃/min的降温速率随炉冷却至室温,得到溶胶-凝胶产物;取出溶胶-凝胶产物,置于50mL离心管中,加入乙醇进行洗涤操作,然后置于离心机中进行15000rpm离心5min,离心结束后倒去洗涤废液,洗涤离心过程重复3次;然后将终产物置于60℃干燥箱中干燥,得到氧化物前驱体;
(S2)将步骤(S1)得到的氧化物前驱体置于非氧气炉进行热处理,炉中氩气流速为0.05L/min,220℃保温10h,得到粒径为15nm的(TiZnCe)O1.99粉体;
(S3)将步骤(S2)得到的(TiZnCe)O1.99粉体(1wt%)与PDMS(0.5wt%)、SYLGARD-84二甲基硅烷(0.5wt%)、正硅酸四丁酯(98wt%)混匀,得到(TiZnCe)O1.99/PDMS粉体涂层;
(S4)将步骤(S3)得到的(TiZnCe)O1.99/PDMS粉体涂层利用压缩空气喷涂方法喷涂在聚碳酸酯上,并控制喷涂压力为0.25MPa,喷涂厚度为50μm;喷涂结束后将其置于无菌操作箱中进行固化干燥处理,开启无菌操作相中200W紫外灯,控制温度为10℃,湿度为40%,固化干燥30min,得到(TiZnCe)O1.99/PDMS涂层。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于上述实施例,本领域技术人员根据本发明的解释,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (10)
1.一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,包括以下步骤:
(S1)将钛金属盐、锌金属盐、铈金属盐与苯甲醇混匀后反应,反应后后处理得到氧化物前驱体;
(S2)将步骤(S1)制备得到的氧化物前驱体进行热处理,得到(TiZnCe)O2-X粉体;
(S3)将步骤(S2)制备得到的(TiZnCe)O2-X粉体与、PDMS和固化剂混匀,得到(TiZnCe)O2-X/PDMS粉体涂层;
(S4)通过压缩空气喷涂方法在基体上喷涂步骤(S3)制备得到的(TiZnCe)O2-X/PDMS粉体涂层,后处理得到(TiZnCe)O2-X/PDMS涂层;
其中,X为0~2,且X不为2。
2.根据权利要求1所述的一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,步骤(S1)中,所述钛金属盐选自异丙醇钛、乙酰丙酮钛、乙酸钛、芳香族钛、氯化钛、溴化钛或碘化钛中的一种;
所述锌金属盐选自异丙醇锌、乙酰丙酮锌、乙酸锌、芳香族锌、氯化锌、溴化锌或碘化锌中的一种;
所述铈金属盐选自异丙醇铈、乙酰丙酮铈、乙酸铈、芳香族铈、氯化铈、溴化铈或碘化铈中的一种。
3.根据权利要求1所述的一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,步骤(S1)中,反应过程中,温度为200℃~300℃,时间为40min~60min;
所述后处理为保温处理后依次进行离心、洗涤后干燥。
4.根据权利要求1所述的一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,步骤(S2)中,热处理过程处于氩气气氛下,温度为220℃~350℃,时间为2h~10h。
5.根据权利要求1所述的一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,步骤(S3)中,(TiZnCe)O2-X/PDMS粉体涂层中还含有SYLGARD-84二甲基硅烷或道康宁DC-732W中的一种;
(TiZnCe)O2-X粉体、PDMS、SYLGARD-84二甲基硅烷或道康宁DC-732W、化剂的质量百分比为1%~9%:0.5%~1%:0.5%~1%:89%~98%。
6.根据权利要求1所述的一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,步骤(S4)中,压缩空气喷涂过程中,喷涂压力为0.1MPa~0.25MPa,涂层厚度为10μm~50μm。
7.根据权利要求1所述的一种(TiZnCe)O2-X/PDMS涂层的制备方法,其特征在于,步骤(S4)中,所述后处理为固化干燥处理;
固化干燥过程处于紫外状态,温度为10℃~30℃,湿度为40%~70%,时间为30min~90min。
8.一种通过权利要求1-7任一所述方法制备得到的(TiZnCe)O2-X/PDMS涂层。
9.一种含有毛刷状的权利要求8所述的(TiZnCe)O2-X/PDMS涂层的手套。
10.一种如权利要求9所述的含有毛刷状的(TiZnCe)O2-X/PDMS涂层的手套在患者创面愈合压力治疗中的应用。
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