CN107858827A - 一种抑菌防雾霾纱窗材料的制备方法 - Google Patents
一种抑菌防雾霾纱窗材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种抑菌防雾霾纱窗材料的制备方法,属于纱窗制备技术领域。本发明以乌拉草为原料经酸浸、水浴加热条件下碱煮、过滤得到碱煮纤维,将壳聚糖用醋酸酸化,与环氧氯丙烷加热反应后,将乌拉草纤维、改性壳聚糖、硅烷偶联剂混合置于梳理机中梳理得到棉纱,棉纱经压制成型、浸胶处理、干燥得到抑菌防雾霾纱窗材料,因表面带有电荷就会吸附相反的电荷而形成扩散双电层,当颗粒彼此接近时,因各具同性电荷而相斥,使微小颗粒物在通过棉纱时由于静电效应被牢牢吸附在棉纱的孔隙中,在酸性条件下将环氧丙基接枝到壳聚糖的氨基上,得到改性壳聚糖,其抗菌活性就会越高,抑制细菌的生长,从而使纱窗材料具有较好的抑菌效果,应用前景广阔。
Description
技术领域
本发明公开了一种抑菌防雾霾纱窗材料的制备方法,属于纱窗制备技术领域。
背景技术
纱窗是挡住蚊蝇虫的网状中间成方格有孔的网。隐形纱窗(卷帘纱窗)是市面上比较流行的纱窗,一般隐形纱窗可自行调整纱盒内弹簧力量,有的纱盒可拆下来加力减力,有的还可自动除浮尘。夏天来了,蚊虫让人头痛不已,只要有一只蚊子在家里,一晚上你就别想睡安稳觉了。除了蚊香、花露水等“亡羊补牢”的招数之外,纱窗便是大家用来防蚊的主要手段了。现在的纱窗也比以前的固定纱窗多了更多的花样,出了隐形纱窗卷帘纱窗和折叠纱窗等,不再像以前那样费力地将纱窗拆上拆下了。 不过也有人对老式纱窗情有独钟,认为坚固耐用。
日前,专业调查机构InsightCN通过其网络调查平台对1000人进行了有关纱窗的调查。调查结果显示,有86.7%的人使用纱窗,而接受调查的1000人中,88.4%住在10楼以下,可见纱窗与楼层的关系密不可分。而其中,仍有34.1%的家庭使用的是老式的固定纱窗。不过,有近半的被调查者打算换新纱窗,另有42.2%的家庭打算近几年内更换,只有一成的调查者没有考虑过调换纱窗,可见,纱窗的市场潜力挺大,另一方面也可看出,纱窗的使用寿命不长,不少家庭需要定期更换,产品的质量层次不齐。
随着工业技术的发展,使得大气污染越来越严重,人们生活的空气质量也严重下降,从而人们的生活也受到了严重影响,尤其是雾霾天气的出现。而空气中悬浮颗粒物的不断增多是雾霾天气出现的罪魁祸首。在空气质量还不能快速提高的基础上,提高室内空气质量变得尤为必要。而室内外空气的交换要通过窗户来实现,对于一些室内的空气净化设备,并不能从源头上解决空气的净化问题,难以满足大多数用户的需求。现在的纱窗还普遍存在孔隙易产生细菌的缺陷,对人们的健康造成一定的伤害。因此,发明一种既能够防止雾霾又有抑菌效果的纱窗材料对纱窗制备技术领域具有积极意义。
发明内容
本发明主要解决的技术问题,针对纱窗材料在雾霾天气下易透过微小颗粒物、纱窗孔隙易滋生细菌的缺陷,提供了一种抑菌防雾霾纱窗材料的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种抑菌防雾霾纱窗材料的制备方法,其特征在于具体制备步骤为:
(1)取100~120g乌拉草放入400~450mL硫酸溶液中浸泡,取出酸浸处理的乌拉草,将酸浸处理的乌拉草置于水浴锅中,加热升温,向水浴锅中加入100~120mL氢氧化钠溶液、50~60mL多聚磷酸钠溶液、30~40mL硅酸钠溶液,蒸煮后,过滤,去除滤液得到碱煮纤维;
(2)将上述碱煮纤维用150~180mL盐酸浸泡后,取出浸泡后的碱煮纤维,放入超声机中超声处理后,用水冲洗,置于烘箱中,加热升温,干燥,得到乌拉草纤维;
(3)按重量份数计,取15~20份壳聚糖溶于30~40份醋酸溶液中,搅拌后,得到酸化壳聚糖溶液,向酸化壳聚糖溶液中加入5~8份环氧氯丙烷,加热升温,反应,得到反应产物;
(4)将上述反应产物用蒸馏水透析,得到透析后的反应产物,将透析后的反应产物置于旋转蒸发仪中,旋蒸,得到旋蒸产物,冷冻干燥得到改性壳聚糖;
(5)将60~70mL无水乙醇置于带有搅拌器和滴液漏斗的三口烧瓶中,用滴液漏斗向三口烧瓶中加入18~20mL钛酸四丁酯,同时启动搅拌器,开始搅拌,待钛酸四丁酯滴加完毕后向三口烧瓶中加入4~6mL三乙醇胺搅拌混合,得到均匀的溶液,将1~2mL水、8~10mL无水乙醇、2~4mL质量分数为20%的盐酸混合,倒入上述三口烧瓶中,继续搅拌混合,再静置陈化,得到二氧化钛溶胶;
(6)按重量份数计,将60~70份乌拉草纤维、20~30份改性壳聚糖、5~7份KH-550硅烷偶联剂混合,放入梳理机中梳理,得到棉网,将棉网放入热压机中热压定型,得到成型棉纱,将成型棉纱放入70~80份二氧化钛溶胶中浸泡后,取出放入烘箱中,干燥,得到抑菌防雾霾纱窗材料。
步骤(1)所述的硫酸溶液的质量分数为30%,控制浸泡温度为50~55℃,浸泡处理时间为1~2h,加热升温后温度为90~100℃,氢氧化钠溶液的质量分数为40%,多聚磷酸钠溶液的质量分数为4%,硅酸钠溶液的质量分数为6%,蒸煮时间为2~3h。
步骤(2)所述的盐酸的质量分数为10%,盐酸浸泡时间为8~10min,超声频率为25~30kHz,超声处理时间为10~15min,加热升温后温度为100~110℃,干燥时间为10~12h。
步骤(3)所述的醋酸溶液的质量分数为2%,搅拌时间为30~35min,加热升温后温度为60~65℃,反应时间为20~24h。
步骤(4)所述的控制截留分子量为8000~10000D,旋蒸转速为80~90r/min,旋蒸时间为20~25min,冷冻干燥温度为 -30~-20℃,冷冻干燥时间为30~35min。
步骤(5)所述的滴液漏斗的滴加速率为2~3mL/min,搅拌器转速为200~300r/min,搅拌混合时间为1~2h,盐酸的质量分数为20%,继续搅拌混合时间为2~3h,静置陈化时间为20~24h。
步骤(6)所述的得到的棉网厚度为2~3mm,控制热压温度为150~160℃,热压压力为1.2~1.4MPa,浸泡时间为45~50min,烘箱设定温度为70~75℃,干燥时间为9~10h。
本发明的有益效果是:
(1)本发明以乌拉草为原料经酸浸、水浴加热条件下碱煮、过滤得到碱煮纤维,将碱煮纤维用盐酸浸泡中和、超声处理、洗涤干燥得到乌拉草纤维,将壳聚糖用醋酸酸化,与环氧氯丙烷加热反应后,经蒸馏水透析、旋蒸、冷冻干燥得到改性壳聚糖,用无水乙醇、钛酸四丁酯共混酸化得到二氧化钛溶胶,将乌拉草纤维、改性壳聚糖、硅烷偶联剂混合置于梳理机中梳理得到棉纱,棉纱经压制成型、浸胶处理、干燥得到抑菌防雾霾纱窗材料,乌拉草纤维制备得到棉纱浸泡二氧化钛后,二氧化钛颗粒在液态,尤其是极性的介质中,因表面带有电荷就会吸附相反的电荷而形成扩散双电层,使颗粒有效直径增加,当颗粒彼此接近时,因各具同性电荷而相斥,有利于分散体系的稳定,纤维表面带负电荷会使作为包覆膜的二氧化钛带正电,从而使微小颗粒物在通过棉纱时由于静电效应被牢牢吸附在棉纱的孔隙中,使纱窗防止雾霾天气对室内人体健康造成危害;
(2)本发明在酸性条件下将环氧丙基接枝到壳聚糖的氨基上,得到改性壳聚糖,改性后的壳聚糖的脱乙酰度提高,其抗菌活性就会越高,氨基量的增加使壳聚糖的正电荷增多,从而提高与细菌负电胞体的接触,干扰其生长,另外壳聚糖使细菌的细胞壁先从细胞膜上分离,再破坏了细胞膜,致使胞内的酶和核酸泄漏,同时在壳聚糖酸性溶液中氨基正离子,大分子量的壳聚糖与细菌细胞结合,破坏细胞膜结构导致钾离子和ATP的渗透,抑制细菌的生长,乌拉草中含有四羟基黄酮类物质木犀草素,可作用于细菌细胞壁和原生质膜,使其结构发生变化,使细胞壁破裂或缺失,胞内容物流出从而影响膜的通透性,细胞出现空腔,结构和功能被破坏,阻止营养物质向细胞内运输,细胞质壁分离, 导致内容物外泄而使细菌死亡,二氧化钛胶膜在光催化下易产生负氧离子净化空气,从而使纱窗材料具有较好的抑菌效果,应用前景广阔。
具体实施方式
取100~120g乌拉草放入400~450mL质量分数为30%的硫酸溶液中浸泡,控制浸泡温度为50~55℃,浸泡处理时间为1~2h,取出酸浸处理的乌拉草,将酸浸处理的乌拉草置于水浴锅中,加热升温至90~100℃,向水浴锅中加入100~120mL质量分数为40%的氢氧化钠溶液、50~60mL质量分数为4%的多聚磷酸钠溶液、30~40mL质量分数为6%的硅酸钠溶液,蒸煮2~3h后,过滤,去除滤液得到碱煮纤维;将上述碱煮纤维用150~180mL质量分数为10%的盐酸浸泡8~10min后,取出浸泡后的碱煮纤维,放入超声机中以25~30kHz的频率超声处理10~15min后,用水冲洗,置于烘箱中,加热升温至100~110℃,干燥10~12h,得到乌拉草纤维;按重量份数计,取15~20份壳聚糖溶于30~40份质量分数为2%的醋酸溶液中,搅拌30~35min后,得到酸化壳聚糖溶液,向酸化壳聚糖溶液中加入5~8份环氧氯丙烷,加热升温至60~65℃,反应20~24h,得到反应产物;将上述反应产物用蒸馏水透析,控制截留分子量为8000~10000D,得到透析后的反应产物,将透析后的反应产物置于旋转蒸发仪中,以80~90r/min转速旋蒸20~25min,得到旋蒸产物,在-30~-20℃下冷冻干燥30~35min得到改性壳聚糖;将60~70mL无水乙醇置于带有搅拌器和滴液漏斗的三口烧瓶中,用滴液漏斗以2~3mL/min的滴加速率向三口烧瓶中加入18~20mL钛酸四丁酯,同时启动搅拌器,以200~300r/min的转速开始搅拌,待钛酸四丁酯滴加完毕后向三口烧瓶中加入4~6mL三乙醇胺搅拌混合1~2h,得到均匀的溶液,将1~2mL水、8~10mL无水乙醇、2~4mL质量分数为20%的盐酸混合,倒入上述三口烧瓶中,继续搅拌混合2~3h,再静置陈化20~24h,得到二氧化钛溶胶;按重量份数计,将60~70份乌拉草纤维、20~30份改性壳聚糖、5~7份KH-550硅烷偶联剂混合,放入梳理机中梳理,得到厚度为2~3mm的棉网,将棉网放入热压机中热压定型,控制热压温度为150~160℃,热压压力为1.2~1.4MPa,得到成型棉纱,将成型棉纱放入70~80份二氧化钛溶胶中浸泡45~50min后,取出放入设定温度为70~75℃的烘箱中,干燥9~10h,得到抑菌防雾霾纱窗材料。
实例1
取100g乌拉草放入400mL质量分数为30%的硫酸溶液中浸泡,控制浸泡温度为50℃,浸泡处理时间为1h,取出酸浸处理的乌拉草,将酸浸处理的乌拉草置于水浴锅中,加热升温至90℃,向水浴锅中加入100mL质量分数为40%的氢氧化钠溶液、50mL质量分数为4%的多聚磷酸钠溶液、30mL质量分数为6%的硅酸钠溶液,蒸煮2h后,过滤,去除滤液得到碱煮纤维;将上述碱煮纤维用150mL质量分数为10%的盐酸浸泡8min后,取出浸泡后的碱煮纤维,放入超声机中以25kHz的频率超声处理10min后,用水冲洗,置于烘箱中,加热升温至100℃,干燥10h,得到乌拉草纤维;按重量份数计,取15份壳聚糖溶于30份质量分数为2%的醋酸溶液中,搅拌30min后,得到酸化壳聚糖溶液,向酸化壳聚糖溶液中加入5份环氧氯丙烷,加热升温至60℃,反应20h,得到反应产物;将上述反应产物用蒸馏水透析,控制截留分子量为8000D,得到透析后的反应产物,将透析后的反应产物置于旋转蒸发仪中,以80r/min转速旋蒸20min,得到旋蒸产物,在-30℃下冷冻干燥30min得到改性壳聚糖;将60mL无水乙醇置于带有搅拌器和滴液漏斗的三口烧瓶中,用滴液漏斗以2mL/min的滴加速率向三口烧瓶中加入18mL钛酸四丁酯,同时启动搅拌器,以200r/min的转速开始搅拌,待钛酸四丁酯滴加完毕后向三口烧瓶中加入4mL三乙醇胺搅拌混合1h,得到均匀的溶液,将1mL水、8mL无水乙醇、2mL质量分数为20%的盐酸混合,倒入上述三口烧瓶中,继续搅拌混合2h,再静置陈化20h,得到二氧化钛溶胶;按重量份数计,将60份乌拉草纤维、20份改性壳聚糖、5份KH-550硅烷偶联剂混合,放入梳理机中梳理,得到厚度为2mm的棉网,将棉网放入热压机中热压定型,控制热压温度为150℃,热压压力为1.2MPa,得到成型棉纱,将成型棉纱放入70份二氧化钛溶胶中浸泡45min后,取出放入设定温度为70℃的烘箱中,干燥9h,得到抑菌防雾霾纱窗材料。
实例2
取110g乌拉草放入420mL质量分数为30%的硫酸溶液中浸泡,控制浸泡温度为52℃,浸泡处理时间为1.5h,取出酸浸处理的乌拉草,将酸浸处理的乌拉草置于水浴锅中,加热升温至95℃,向水浴锅中加入110mL质量分数为40%的氢氧化钠溶液、55mL质量分数为4%的多聚磷酸钠溶液、35mL质量分数为6%的硅酸钠溶液,蒸煮2.5h后,过滤,去除滤液得到碱煮纤维;将上述碱煮纤维用165mL质量分数为10%的盐酸浸泡9min后,取出浸泡后的碱煮纤维,放入超声机中以27kHz的频率超声处理12min后,用水冲洗,置于烘箱中,加热升温至105℃,干燥11h,得到乌拉草纤维;按重量份数计,取17份壳聚糖溶于35份质量分数为2%的醋酸溶液中,搅拌32min后,得到酸化壳聚糖溶液,向酸化壳聚糖溶液中加入7份环氧氯丙烷,加热升温至62℃,反应22h,得到反应产物;将上述反应产物用蒸馏水透析,控制截留分子量为9000D,得到透析后的反应产物,将透析后的反应产物置于旋转蒸发仪中,以85r/min转速旋蒸22min,得到旋蒸产物,在-25℃下冷冻干燥32min得到改性壳聚糖;将65mL无水乙醇置于带有搅拌器和滴液漏斗的三口烧瓶中,用滴液漏斗以2mL/min的滴加速率向三口烧瓶中加入19mL钛酸四丁酯,同时启动搅拌器,以250r/min的转速开始搅拌,待钛酸四丁酯滴加完毕后向三口烧瓶中加入5mL三乙醇胺搅拌混合1.5h,得到均匀的溶液,将2mL水、9mL无水乙醇、3mL质量分数为20%的盐酸混合,倒入上述三口烧瓶中,继续搅拌混合2.5h,再静置陈化22h,得到二氧化钛溶胶;按重量份数计,将65份乌拉草纤维、25份改性壳聚糖、6份KH-550硅烷偶联剂混合,放入梳理机中梳理,得到厚度为2mm的棉网,将棉网放入热压机中热压定型,控制热压温度为155℃,热压压力为1.3MPa,得到成型棉纱,将成型棉纱放入75份二氧化钛溶胶中浸泡47min后,取出放入设定温度为72℃的烘箱中,干燥9.5h,得到抑菌防雾霾纱窗材料。
实例3
取120g乌拉草放入450mL质量分数为30%的硫酸溶液中浸泡,控制浸泡温度为55℃,浸泡处理时间为2h,取出酸浸处理的乌拉草,将酸浸处理的乌拉草置于水浴锅中,加热升温至100℃,向水浴锅中加入120mL质量分数为40%的氢氧化钠溶液、60mL质量分数为4%的多聚磷酸钠溶液、40mL质量分数为6%的硅酸钠溶液,蒸煮3h后,过滤,去除滤液得到碱煮纤维;将上述碱煮纤维用180mL质量分数为10%的盐酸浸泡10min后,取出浸泡后的碱煮纤维,放入超声机中以30kHz的频率超声处理15min后,用水冲洗,置于烘箱中,加热升温至110℃,干燥12h,得到乌拉草纤维;按重量份数计,取20份壳聚糖溶于40份质量分数为2%的醋酸溶液中,搅拌35min后,得到酸化壳聚糖溶液,向酸化壳聚糖溶液中加入8份环氧氯丙烷,加热升温至65℃,反应24h,得到反应产物;将上述反应产物用蒸馏水透析,控制截留分子量为10000D,得到透析后的反应产物,将透析后的反应产物置于旋转蒸发仪中,以90r/min转速旋蒸25min,得到旋蒸产物,在-20℃下冷冻干燥35min得到改性壳聚糖;将70mL无水乙醇置于带有搅拌器和滴液漏斗的三口烧瓶中,用滴液漏斗以3mL/min的滴加速率向三口烧瓶中加入20mL钛酸四丁酯,同时启动搅拌器,以300r/min的转速开始搅拌,待钛酸四丁酯滴加完毕后向三口烧瓶中加入6mL三乙醇胺搅拌混合2h,得到均匀的溶液,将2mL水、10mL无水乙醇、4mL质量分数为20%的盐酸混合,倒入上述三口烧瓶中,继续搅拌混合3h,再静置陈化24h,得到二氧化钛溶胶;按重量份数计,将70份乌拉草纤维、30份改性壳聚糖、7份KH-550硅烷偶联剂混合,放入梳理机中梳理,得到厚度为3mm的棉网,将棉网放入热压机中热压定型,控制热压温度为160℃,热压压力为1.4MPa,得到成型棉纱,将成型棉纱放入80份二氧化钛溶胶中浸泡50min后,取出放入设定温度为75℃的烘箱中,干燥10h,得到抑菌防雾霾纱窗材料。
对比例
以北京某公司生产的抑菌防雾霾纱窗材料作为对比例 对本发明制得的抑菌防雾霾纱窗材料和对比例中的抑菌防雾霾纱窗材料进行性能检测,检测结果如表1所示:
1、测试方法:
大肠杆菌平均菌数测试按JC/T897-2002的规定进行抑菌性能检测;
金黄色葡萄球菌平均菌数测试按JC/T897-2002的规定进行抑菌性能检测;
白色念球菌抑菌率的测试按GB/T20944.2-2007的规定进行性能检测;
防雾霾试验:在严重雾霾天气时,在当天6:00启用防雾霾模式,对窗户分别安装实例1~3和对比例中的纱窗,在当天的20:00分别对安装了实例1~3纱窗的室内、安装了对比例纱窗的室内和室外进行检测,结果表2所示。
表1
表2
根据上述中数据可知本发明制得的抑菌防雾霾纱窗材料的抑菌效果好,达到99.99%,防雾霾效果好,PM2.5控制在20μg/m3以下,PM10在30μg/m3以下,二氧化硫和一氧化氮以及臭氧的含量都得到了明显的控制,具有广阔的应用前景。
Claims (7)
1.一种抑菌防雾霾纱窗材料的制备方法,其特征在于具体制备步骤为:
(1)取100~120g乌拉草放入400~450mL硫酸溶液中浸泡,取出酸浸处理的乌拉草,将酸浸处理的乌拉草置于水浴锅中,加热升温,向水浴锅中加入100~120mL氢氧化钠溶液、50~60mL多聚磷酸钠溶液、30~40mL硅酸钠溶液,蒸煮后,过滤,去除滤液得到碱煮纤维;
(2)将上述碱煮纤维用150~180mL盐酸浸泡后,取出浸泡后的碱煮纤维,放入超声机中超声处理后,用水冲洗,置于烘箱中,加热升温,干燥,得到乌拉草纤维;
(3)按重量份数计,取15~20份壳聚糖溶于30~40份醋酸溶液中,搅拌后,得到酸化壳聚糖溶液,向酸化壳聚糖溶液中加入5~8份环氧氯丙烷,加热升温,反应,得到反应产物;
(4)将上述反应产物用蒸馏水透析,得到透析后的反应产物,将透析后的反应产物置于旋转蒸发仪中,旋蒸,得到旋蒸产物,冷冻干燥得到改性壳聚糖;
(5)将60~70mL无水乙醇置于带有搅拌器和滴液漏斗的三口烧瓶中,用滴液漏斗向三口烧瓶中加入18~20mL钛酸四丁酯,同时启动搅拌器,开始搅拌,待钛酸四丁酯滴加完毕后向三口烧瓶中加入4~6mL三乙醇胺搅拌混合,得到均匀的溶液,将1~2mL水、8~10mL无水乙醇、2~4mL质量分数为20%的盐酸混合,倒入上述三口烧瓶中,继续搅拌混合,再静置陈化,得到二氧化钛溶胶;
(6)按重量份数计,将60~70份乌拉草纤维、20~30份改性壳聚糖、5~7份KH-550硅烷偶联剂混合,放入梳理机中梳理,得到棉网,将棉网放入热压机中热压定型,得到成型棉纱,将成型棉纱放入70~80份二氧化钛溶胶中浸泡后,取出放入烘箱中,干燥,得到抑菌防雾霾纱窗材料。
2.根据权利要求1所述的一种抑菌防雾霾纱窗材料的制备方法,其特征在于:
步骤(1)所述的硫酸溶液的质量分数为30%,控制浸泡温度为50~55℃,浸泡处理时间为1~2h,加热升温后温度为90~100℃,氢氧化钠溶液的质量分数为40%,多聚磷酸钠溶液的质量分数为4%,硅酸钠溶液的质量分数为6%,蒸煮时间为2~3h。
3.根据权利要求1所述的一种抑菌防雾霾纱窗材料的制备方法,其特征在于:
步骤(2)所述的盐酸的质量分数为10%,盐酸浸泡时间为8~10min,超声频率为25~30kHz,超声处理时间为10~15min,加热升温后温度为100~110℃,干燥时间为10~12h。
4.根据权利要求1所述的一种抑菌防雾霾纱窗材料的制备方法,其特征在于:
步骤(3)所述的醋酸溶液的质量分数为2%,搅拌时间为30~35min,加热升温后温度为60~65℃,反应时间为20~24h。
5.根据权利要求1所述的一种抑菌防雾霾纱窗材料的制备方法,其特征在于:
步骤(4)所述的控制截留分子量为8000~10000D,旋蒸转速为80~90r/min,旋蒸时间为20~25min,冷冻干燥温度为 -30~-20℃,冷冻干燥时间为30~35min。
6.根据权利要求1所述的一种抑菌防雾霾纱窗材料的制备方法,其特征在于:
步骤(5)所述的滴液漏斗的滴加速率为2~3mL/min,搅拌器转速为200~300r/min,搅拌混合时间为1~2h,盐酸的质量分数为20%,继续搅拌混合时间为2~3h,静置陈化时间为20~24h。
7.根据权利要求1所述的一种抑菌防雾霾纱窗材料的制备方法,其特征在于:
步骤(6)所述的得到的棉网厚度为2~3mm,控制热压温度为150~160℃,热压压力为1.2~1.4MPa,浸泡时间为45~50min,烘箱设定温度为70~75℃,干燥时间为9~10h。
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