CN116035924B - 一种适用于喷雾的水包油乳液及其制备方法、喷雾 - Google Patents
一种适用于喷雾的水包油乳液及其制备方法、喷雾 Download PDFInfo
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- CN116035924B CN116035924B CN202310208007.1A CN202310208007A CN116035924B CN 116035924 B CN116035924 B CN 116035924B CN 202310208007 A CN202310208007 A CN 202310208007A CN 116035924 B CN116035924 B CN 116035924B
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Abstract
本发明属于日化新材料领域,公开了一种适用于喷雾的水包油乳液,所述乳液的乳化剂由2‑10wt%聚甘油‑6硬脂酸酯和聚甘油‑6山嵛酸酯、1‑5.0wt%甘油硬脂酸酯和PEG‑100硬脂酸酯、1‑3.0wt%甘油硬脂酸酯组成;所述水包油乳液经过高压均质处理后得到。乳液能够形成低粘稳定的O/W乳化体,HLB值高,兼容性强,对高极性的化学防晒剂具有很好乳化稳定能力。同时,本发明还公开了上述乳液的制备方法,以及一种喷雾。
Description
技术领域
本发明涉及日化新材料领域,具体为一种适用于喷雾的水包油乳液及其制备方法、喷雾。
背景技术
CN1549699A公开了一种可喷雾的低粘度水包油(O/W)乳液,它们能够通过使用含有双结构表面活性剂的疏水相和含有双结构表面活性剂的亲水相,由至少两相,在加入固体颗粒、起泡表面活性剂或防汗剂的条件下制备;其中,其可通过混合下述组分而制备:一种亲水相,其含有:一种或多种双结构表面活性剂化合物和一种有弱起泡特性的洗涤剂组分,其中使用的双结构表面活性剂化合物(a.1)与洗涤剂组分(a.2)的重量比为1∶100~10∶1重量份,优选1∶10~4∶1重量份,特别优选为1∶2~2∶1重量份,其中组分(a.1)和(a.2)以(a.1)和(a.2)的总和形式优选使用0.05~5.0wt%,特别优选为0.5~3.0wt%,1~15wt%的水,特别优选2~10wt%,与一种疏水相,其含有:一种或多种双结构表面活性剂化合物和一种或多种具有HLB值低于6的助两亲物,双结构表面活性剂化合物(b.1)与助两亲物(b.2)的重量比为1∶100~3∶1重量份,优选1∶20~1∶2重量份,特别优选1∶10~1∶5重量份,其中组分(b.1)和(b.2)以(b.1)和(b.2)的总和形式优选使用0.1~8.0wt%,特别优选为0.5~4.0wt%,1~50wt%,优选10~40wt%的疏水组分和,非必要的0.01~10wt%,优选0.5~3wt%一种或多种非离子表面活性剂。
本领域技术人员可达成的共识为:作为喷雾的活性成分,其粘度必须较低,作为一款水包油体系,其主要用于形成包裹油相活性成分的微胶囊,所以得到一种稳定的、粘度低的水包油体系是形成喷雾的必要条件。
在上述方案中,其主要实现方式选择了疏水组分如甘油硬脂酸酯、二十二烷醇、甘油硬脂酸酯柠檬酸酯,同时选择了双结构表面活性剂;
CN114555036A公开了一种包含水包油乳液的不含铝和/或锆盐的止汗剂组合物,该组合物包含油相和非离子乳化剂,该非离子乳化剂具有10或更低的HLB值和高于37℃的熔点;其中所述组合物包含至少4重量%的所述非离子乳化剂;其中所述油相包含熔点大于37℃的亲脂性材料;
其说明书记载:优选地,乳化剂是选自以下的非离子乳化剂:硬脂醇聚醚-2、鲸蜡醇聚醚-2、聚甘油-2-硬脂酸酯、聚甘油-2-二硬脂酸酯、聚甘油-3-二硬脂酸酯、脱水山梨醇棕榈酸酯、甘油硬脂酸酯、乙二醇硬脂酸酯、蔗糖聚硬脂酸酯、棕榈酸鲸腊酯、脱水山梨醇三硬脂酸酯、脱水山梨醇单棕榈酸酯、二甘醇单硬脂酸酯、甘油单硬脂酸酯、脱水山梨醇单硬脂酸酯、PEG-8蜂蜡、山梨醇聚醚-20蜂蜡、PEG-2硬脂酸酯、甘油肉豆蔻酸酯、甘油油酸酯、甘油硬脂酸酯;
为了稳定乳液,优选的是根据本发明的止汗剂组合物进一步包含更亲水的乳化剂,该更亲水的乳化剂选自HLB高于11、优选高于12的阴离子乳化剂、阳离子乳化剂、两性乳化剂、非离子乳化剂。
优选的是这种更亲水的乳化剂是选自以下的非离子乳化剂:硬脂醇聚醚-20、硬脂醇聚醚-21、鲸蜡硬脂醇聚醚-20、吐温80、鲸蜡醇聚醚-20、PEG-40硬脂酸酯、PEG-80脱水山梨醇月桂酸酯、异鲸蜡醇聚醚-20、异硬脂醇聚醚-20、月桂醇聚醚-23、油醇聚醚-10、油醇聚醚-20、PEG-100硬脂酸酯、PEG-20甲基葡糖倍半硬脂酸酯、PEG-60杏仁甘油酯、PEG-8月桂酸酯、聚山梨醇酯20、聚山梨醇酯60、聚山梨醇酯80、聚甘油-10硬脂酸酯、聚甘油-10单棕榈酸酯。
在针对于喷雾型的高极性的化学防晒剂的研发过程中,发现要形成较大面积大喷雾范围、在喷雾过程中体系稳定是比较难的。
所以,本案解决的技术问题是:如何开发出一种能够维持高极性的化学防晒剂稳定性的乳化剂组合。
发明内容
本发明的目的在于提供一种适用于喷雾的水包油乳液,该乳液能够形成低粘稳定的O/W乳化体(乳液或喷剂),HLB值高,兼容性强,对高极性的化学防晒剂具有很好乳化稳定能力。
同时,本发明还公开了一种上述乳液的制备方法,以及一种喷雾。
为实现上述目的,本发明提供如下技术方案:一种适用于喷雾的水包油乳液,所述乳液的乳化剂由2-10wt%聚甘油-6硬脂酸酯和聚甘油-6山嵛酸酯、1-5.0wt%甘油硬脂酸酯和PEG-100 硬脂酸酯、1-3.0wt%甘油硬脂酸酯组成;
所述水包油乳液经过高压均质处理后得到。
在一些实施案例中,所述聚甘油-6硬脂酸酯的用量为2wt%、3wt%、4wt%、5wt%、6wt%、7wt%、8wt%、9wt%或10wt%;
甘油硬脂酸酯和PEG-100 硬脂酸酯的用量为1wt%、2wt%、3wt%、4wt%或5wt%;
甘油硬脂酸酯的用量为1wt%、1.5wt%、2wt%、2.5wt%或3wt%;
在上述的适用于喷雾的水包油乳液中,所述乳液的乳化剂由2-5wt%聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯、1-2wt%甘油硬脂酸酯和PEG-100 硬脂酸酯、1-1.5wt%甘油硬脂酸酯组成。
在上述的适用于喷雾的水包油乳液中,还包括增稠剂,所述增稠剂为高分子增稠剂;所述增稠剂的用量相当于水包油乳液的0.01-1.0wt%;
在一些实施案例中,所述增稠剂的用量相当于水包油乳液的0.01wt%、0.1wt%、0.5wt%、1wt%、2wt%、3wt%、4wt%、5wt%、6wt%、7wt%、8wt%、9wt%或10wt%。
所述高分子增稠剂为黄原胶和/或丙烯酸酯类/C10-30 烷醇丙烯酸酯交联聚合物;
需要说明的是:丙烯酸酯类/C10-30 烷醇丙烯酸酯交联聚合物由路博润先进材料公司提供,英文商品名为:PEMULEN TR-1 POLYMER;中文商品名为:丙烯酸酯类/C10-30 烷醇丙烯酸酯交联聚合物;
在上述的适用于喷雾的水包油乳液中,所述水包油乳液为防晒剂、润肤剂、保湿剂、乳化剂中的一种。
在上述的适用于喷雾的水包油乳液中,所述水包油乳液为防晒乳液;所述水包油乳液中含有防晒剂和余量去离子水。
在上述的适用于喷雾的水包油乳液中,所述防晒剂为甲氧基肉桂酸乙基己酯、水杨酸乙基己酯、二乙氨羟苯甲酰基苯甲酸己酯、乙基己基三嗪酮、双-乙基己氧苯酚甲氧苯基三嗪、苯基苯并咪唑磺酸、PARSOL® Max中的一种或多种。
在上述的适用于喷雾的水包油乳液中,所述水包油乳液中还含有润肤剂、保湿剂、防腐剂、增稠剂、中和剂中的一种或多种。
同时,本发明还公开了一种如上任一所述的水包油乳液的制备方法,包括如下步骤:
步骤1:将含乳化剂的油相加入到水相中,得到大粒径水包油乳液;
步骤2:将大粒径水包油乳液采用高压均质机均质至少一次,即可。
在上述的水包油乳液的制备方法中,高压均质3次,压力700-800bar。
最后,本发明还公开了一种喷雾,所述喷雾由如上任一所述的水包油乳液以及推进剂组成,所述水包油乳液、推进剂相互混合;
或,所述喷雾由如上任一所述的水包油乳液和压缩气体组成,所述压缩气体和水包油乳液通过内囊袋隔离分隔。
与现有技术相比,本发明的有益效果是:
通过选用EVONIK的TEGO® Care PBS 6(聚甘油-6硬脂酸酯和聚甘油-6山嵛酸酯),为聚甘油-6经与硬脂酸、山嵛酸酯化制得,与甘油硬脂酸酯和PEG-100 硬脂酸酯、甘油硬脂酸酯进行合理搭配,可制得低粘稳定的O/W乳化体(乳液或喷剂),HLB值高,兼容性强,对高极性的化学防晒剂具有很好乳化稳定能力。
通过高压均质,可以将常规大粒径的“粗乳液”,经高压分散为粒径在100-200nm之间的细粒径“纳米微乳液”(胶体),同时体系中加入高分子聚合物为增稠稳定剂,高分子会在胶粒表面形成高分子吸附层,增加胶粒间静电斥力势能,减少粒子间的引力势能,带有高分子吸附层的胶粒接近时,吸附层的重叠会产生一种新的斥力势能阻止粒子聚集,起到“空间稳定作用”,保持胶体的动力学稳定。
通过高压均质制得的纳米微乳,粒径小,覆盖的表面积更大,闭合效应增加,防护效果更好,同时采用UVB+UVA全波段复配防晒组合,协同增效,具有“吸收、反射、散射”多重防护效果,协助贡献高SPF指数。
附图说明
图1是实施例1的粒径分布测试结果;
图2是实施例1的喷雾效果图;
其中,(a)为实施例1的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图3是实施例2的粒径分布测试结果;
图4是实施例2的喷雾效果图;
其中,(a)为实施例2的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图5是实施例3的粒径分布测试结果;
图6是实施例3的喷雾效果图;
其中,(a)为实施例3的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图7是实施例4的粒径分布测试结果;
图8是实施例4的喷雾效果图;
其中,(a)为实施例4的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图9是实施例5的粒径分布测试结果;
图10是实施例5的喷雾效果图;
其中,(a)为实施例5的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图11是实施例6的粒径分布测试结果;
图12是实施例6的喷雾效果图;
其中,(a)为实施例6的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图13是对比例1的粒径分布测试结果;
图14是对比例1的喷雾效果图;
其中,(a)为对比例1的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图15是对比例2的粒径分布测试结果;
图16是对比例2的喷雾效果图;
其中,(a)为对比例2的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图17是对比例3的粒径分布测试结果;
图18是对比例3的喷雾效果图;
其中,(a)为对比例3的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图19是对比例4的粒径分布测试结果;
图20是对比例4的喷雾效果图;
其中,(a)为对比例4的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图21是对比例5的粒径分布测试结果;
图22是对比例5的喷雾效果图;
其中,(a)为对比例5的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图23是对比例6的粒径分布测试结果;
图24是对比例6的喷雾效果图;
其中,(a)为对比例6的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图25是对比例7的粒径分布测试结果;
图26是对比例7的喷雾效果图;
其中,(a)为对比例7的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图;
图27是对比例8的粒径分布测试结果;
图28是对比例8的喷雾效果图;
其中,(a)为对比例8的喷雾效果图;(b)为作为平行对比的去离子水的喷雾效果图。
具体实施方式
基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
在进行阐述本发明的方案之前,先阐述关键原料的来源:
聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯:其主要占比为50.0 - 60.0%的聚甘油-6 硬脂酸酯和40.0 - 50.0%的聚甘油-6 山嵛酸酯,由供应商德国赢创德固赛(中国)投资有限公司Evonik提供。
甘油硬脂酸酯和PEG-100 硬脂酸酯:其主要占比为40.0 - 50.0%的甘油硬脂酸酯和50.0 - 60.0%的PEG-100 硬脂酸酯,由供应商禾大化学品(上海)有限公司提供。
PARSOL® Max:主要成分为亚甲基双-苯并三唑基四甲基丁基酚、水、癸基葡糖苷、丙二醇、黄原胶,由供应商荷兰帝斯曼DSM提供。
实施例
一种高SPF值二元防晒喷雾的制备方法,其步骤如下:
(一)、制备常规大粒径O/W防晒乳液
(1)预先溶解氢氧化钠,用于调节pH值,备用;
(2)预先取一定量的去离子水,加入苯基苯并咪唑磺酸、三乙醇胺,混合搅拌至完全溶解透明无颗粒,水溶液pH值:6.5-7.5(直测),备用;
(3)预先取一定量的去离子水,预先分散PARSOL® Max,混合搅拌至呈分散均匀的乳白色水溶液,备用;
(4)预先取适量丁二醇分散黄原胶,混合搅拌至分散均匀,备用;
(5)水锅投料,将去离子水、甘油、丁二醇、羟苯甲酯,依次投入水锅中,加热搅拌至80-85℃,至完全溶解透明无颗粒,保温20min,再将水相抽入乳化锅中,预留少量的水相,待用;
(6)乳化锅保持加热80-85℃,开启乳化锅中的均质和搅拌,依次加入丙烯酸酯类/C10-30 烷醇丙烯酸酯交联聚合物、预分散好的黄原胶(4),均质分撒均匀,料体呈透明无色,保温备用;
(7)油锅投料,将聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯、甘油硬脂酸酯和PEG-100 硬脂酸酯、甘油硬脂酸酯、甲氧基肉桂酸乙基己酯,水杨酸乙基己酯,二乙氨羟苯甲酰基苯甲酸己酯,乙基己基三嗪酮,双-乙基己氧苯酚甲氧苯基三嗪、己二酸二丁酯、碳酸二辛酯、氢化蓖麻油,等各组分原料依次投入油锅中,加热搅拌至80-85℃,至完全溶解呈透明黄色无颗粒油液,备用;
(8)乳化:乳化锅开启真空,均质搅拌,将油相一次性抽入乳化锅中,并将(5)中剩余少量的水相抽入乳化锅中,混合搅拌2-3min,真空均质乳化3000-5000r/min,均质时间3-5min,停止均质,保温搅拌10min;
(9)通冷却循环水冷却,降温至60-65℃时,放掉真空,依次加入预配置(2)、(3),混合搅拌均匀;
(10)继续降温至45-50℃,依次加入预配置氢氧化钠溶液(1),调节料体pH值(10%水溶液):7.0-7.5,再依次加入防腐剂苯氧乙醇和乙基己基甘油,混合搅拌均匀;
(11)降温至38℃,停止搅拌,取料检验,检验合格,过滤出料。
(二)、高压均质制作细粒径O/W防晒纳米微乳
(1)开机清洗高压均质机,调试设备,设定参数;
(2)将上述所制得的常规大粒径O/W防晒乳液倒入进料桶中,先打开低压阀至50bar,再打开高压阀至700-800bar,料体循环高压均质3次,在出料口处收集料体;
(3)通过粒径仪进行料体粒径测试,确定料体的纳米粒径范围。
(三)灌装二元喷雾。
实施例1-6
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考下表1;
表1 配方表
需要说明的是,上表中“添加至配方总重为100重量份”是指:添加去离子水直至体系总重量为100重量份。
对比例1
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯由聚甘油-2-硬脂酸酯替代。
对比例2
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯由聚甘油-3-二硬脂酸酯替代。
对比例3
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯由聚甘油-10硬脂酸酯替代。
对比例4
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的甘油硬脂酸酯和PEG-100 硬脂酸酯由PEG-20甲基葡糖倍半硬脂酸酯替代。
对比例5
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的甘油硬脂酸酯和PEG-100 硬脂酸酯由PEG-40硬脂酸酯替代。
对比例6
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的甘油硬脂酸酯和PEG-100 硬脂酸酯由蔗糖聚硬脂酸酯替代。
对比例7
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的甘油硬脂酸酯由甘油肉豆蔻酸酯替代。
对比例8
一种高SPF值二元防晒喷雾,其制备方法参考上述实施例,配方参考实施例4,不同的是:
乳化剂中的甘油硬脂酸酯由二甘醇单硬脂酸酯替代。
粒径测定方法:
以去离子水为分散介质,在50ml烧杯中,取25ml分散介质,加入10ml被测样品;
采用超声机将其分散均匀,待充分分散后,观察其乳液浓度,是否呈现轻微的云雾状或浑浊,如果不是可采用稀释或添加样品的方式使其达到该效果;
取已分散好的样品乳液,加到清洗干净的样品池中,并盖上样品池盖测试;
通过粒径仪测试获得“测试结果及粒径分布”等数据结果,同时进行平行实验测试,获得“平均粒径”。
喷雾效果测试:
将试样灌装到喷雾瓶中,并置于离测试纸10-15cm处,按压泵头,测量试纸上喷雾面积,并在相同条件下以去离子水作为空白对照,若样品喷雾面积与空白对照的比值>50%,即视作样品具有良好的雾化喷雾效果。
稳定性测试:GB/T 29665-2013 护肤乳液(O/W型)。
测试结果参考表2;
表2 测试结果
结果分析:
1、从测试结果中看,实施例1、实施例2由于整体乳化剂的用量偏低,存在不足以稳定乳化高极性高含量的化学防晒剂,进而在耐热耐寒及离心时出现“出油、分层”等现象;
2、实施例3、实施例4、实施例5、实施例6,制得的乳液粒径均匀且在100-200nm范围内,料体细腻,整体稳定性好,喷雾效果优异,其中以实施例4效果为最好,分散指数:PI=0.0940,平均粒径分布细,稳定性高,雾化效果好;
3、对比例主要通过更换同类型的不同乳化剂来验证该乳化剂组合对整个配方稳定性,所制得乳液粒径大小、喷雾效果的影响。对比例1、对比例2,一方面是由于乳化剂用量偏低,另一方面是更换的聚甘油-2-硬脂酸酯、聚甘油-3-二硬脂酸酯对高极性的防晒剂未能很好地乳化稳定。同理,对比例3的聚甘油-10硬脂酸酯,虽然乳化剂用量高,但是乳化剂本身对防晒剂的乳化稳定能力差,导致不稳定分层,乳液粒径整体偏大,经时粘度变化大,进而影响喷雾效果;
4、对比例4、对比例5、对比例6,为保留主乳化剂聚甘油-6 硬脂酸酯和聚甘油-6山嵛酸酯的前提下,更换助乳化剂进行对比测试,从测试结果来看,主乳化剂不变的情况下,对配方整体的稳定性影响不大,但助乳化剂对乳液乳化效果有区别,制得乳液粒径大小差异明显;
5、对比例7、对比例8主要对比的是实施例4,不同的是更换同类型的助乳化剂,但从测试结果来看,虽然对比例7、对比例8所制得的乳液稳定性无异常且喷雾效果相对不错,但其乳液粒径较实施例4大很多,具有后续增大的趋势,存在粒径变大,雾化效果变差的风险。
Claims (7)
1.一种适用于喷雾的水包油防晒乳液,其特征在于,所述水包油防晒乳液中含有防晒剂、乳化剂和去离子水;
所述水包油防晒乳液的乳化剂由2-5wt%聚甘油-6 硬脂酸酯和聚甘油-6 山嵛酸酯、1-2wt%甘油硬脂酸酯和PEG-100 硬脂酸酯、1-1.5wt%甘油硬脂酸酯组成;
所述水包油防晒乳液经过高压均质处理后得到。
2.根据权利要求1所述的适用于喷雾的水包油防晒乳液,其特征在于,还包括增稠剂,所述增稠剂为高分子增稠剂;所述增稠剂的用量相当于水包油防晒乳液的0.01-1.0wt%;
所述高分子增稠剂为黄原胶和/或丙烯酸酯类/C10-30 烷醇丙烯酸酯交联聚合物。
3.根据权利要求1所述的适用于喷雾的水包油防晒乳液,其特征在于,所述防晒剂为甲氧基肉桂酸乙基己酯、水杨酸乙基己酯、二乙氨羟苯甲酰基苯甲酸己酯、乙基己基三嗪酮、双-乙基己氧苯酚甲氧苯基三嗪、苯基苯并咪唑磺酸、PARSOL® Max中的一种或多种。
4.根据权利要求3所述的适用于喷雾的水包油防晒乳液,其特征在于,所述水包油防晒乳液中还含有润肤剂、保湿剂、防腐剂、增稠剂、中和剂中的一种或多种。
5.一种如权利要求1-4任一所述的水包油防晒乳液的制备方法,其特征在于,包括如下步骤:
步骤1:将含乳化剂的油相加入到水相中,得到大粒径水包油乳液;
步骤2:将大粒径水包油乳液采用高压均质机均质至少一次,即可。
6.根据权利要求5所述的水包油防晒乳液的制备方法,其特征在于,高压均质3次,压力700-800bar。
7.一种喷雾,其特征在于,所述喷雾由如权利要求1-4任一所述的水包油防晒乳液以及推进剂组成,所述水包油防晒乳液、推进剂相互混合;
或,所述喷雾由如权利要求1-4任一所述的水包油防晒乳液和压缩气体组成,所述压缩气体和水包油防晒乳液通过内囊袋隔离分隔。
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