CN113736055A - 一种抗菌聚氨酯弹性体及其制备方法 - Google Patents
一种抗菌聚氨酯弹性体及其制备方法 Download PDFInfo
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- CN113736055A CN113736055A CN202010463981.9A CN202010463981A CN113736055A CN 113736055 A CN113736055 A CN 113736055A CN 202010463981 A CN202010463981 A CN 202010463981A CN 113736055 A CN113736055 A CN 113736055A
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- polyurethane elastomer
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- antibacterial
- mixing
- agent
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Classifications
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Abstract
本发明属于高分子复合功能材料技术领域,涉及一种抗菌聚氨酯弹性体及其制备方法。制备所述的抗菌聚氨酯弹性体的原料按质量配比包含:聚醚多元醇或聚酯多元醇100份,异氰酸酯32‑62份,水1‑4.5份,平均粒度为25‑350nm的无机纳米抗菌剂0.3‑2.5份。利用本发明的抗菌聚氨酯弹性体及其制备方法,能够更好的制备抗菌聚氨酯弹性体,制备所得聚氨酯弹性体能够达到更好、更持久、更均匀的抗菌效果,同时降低成本和减少对环境、人体的危害。
Description
技术领域
本发明属于高分子复合功能材料技术领域,涉及一种抗菌聚氨酯弹性体及其制备方法。
背景技术
聚氨酯弹性体,在我国称为聚氨酯(PU),在国际上称为Polyurethane,是高分子结构的主链上含有很多的“氨基甲酸酯”结构(-NHCOO-)的聚合物。
聚氨酯弹性体的应用领域极为广泛,如应用在汽车业(密封圈、轴套、皮革、封条、装饰板等)、建筑业(混凝土模、门密封、喷沙管等)、涂层织物(输送带、同步带等)、电子工业(封装、绝缘体、线路板、电子板涂层等)、食品业(滑道内衬、谷类储存、输送带等)、矿业(铲斗内衬、刮片、泵衬、筛网等)、鞋业(鞋底、底部模制隔膜、缓冲内底等)、体育运动(球场、跑道、哑铃、汽艇等)、涂料(内外墙涂料、彩钢板、家用涂料等)、胶粘剂(胶带、高速公路缝胶等)、纺织行业(地垫、沙发、胸围内衣、化妆棉、床垫等)。
制备聚氨酯弹性体的主要基础原料是异氰酸酯和含有活泼氢的化合物。含有活泼氢的化学物主要是含有两个以上末端羟基的聚酯多元醇或聚醚多元醇等。异氰酸酯和含有活泼氢的化合物在一定条件下发生亲核加成反应,生成含有“氨基甲酸酯”结构(-NHCOO-)的聚合物。选用不同的异氰酸酯、不同的活泼氢化合物,同时添加不同的助剂(例如:增塑剂、抗静电剂、脱模剂、加填剂、发泡剂、泡沫稳定剂等),借助催化剂的作用,从而得到各种化学性质、物理性质不同、应用领域不同的聚氨酯弹性体。
聚氨酯弹性体可分为聚酯类聚氨酯弹性体和聚醚类聚氨酯弹性体,聚酯类聚氨酯弹性体在湿热的条件下,易于细菌和霉菌的生长,使得其物理性质急剧下降;聚醚类聚氨酯弹性体虽具有微弱的防霉抗菌能力,一旦温度和湿度适宜,细菌和霉菌同样快速生长繁殖。尤其是多孔性的聚氨酯弹性体更容易面临细菌滋生的问题,因此纺织品中的鞋垫、床垫、沙发垫、地垫、文胸内衣类直接与人体接触的产品容易细菌过度繁殖,这不但降低了产品的性能,还会产生异味,在一定程度上直接威胁人体健康。
由此可见,开发高效抗菌的聚氨酯弹性体具有重大意义。将抗菌剂与聚氨酯弹性体结合在一起,使得聚氨酯弹性体具有抑制细菌生长繁殖的能力,或者杀灭细菌使其失去生理活性的能力,这样的聚氨酯弹性体即为抗菌聚氨酯弹性体。
关于抗菌聚氨酯弹性体,现有技术有一些报道。
例如中国专利申请CN200610166477.2公开了光触媒抗菌海绵及其枕、垫制品,该光触媒抗菌海绵由下列组份依传统工艺制造而成:晶型为锐钛矿型的TiO2光触媒材料,孔目数1200目以上,添加量为聚醚多元醇的1-8%;聚醚多元醇,其中一种平均分子量400-1500,羟值100-350,另一种平均分子量1500-5000,羟值35-80,配比为1.5-1:1;异氰酸酯,商品名为TDI80/20,指数为85-115;胺类催化剂,三乙烯二胺、五乙烯四胺或己二胺,添加量为聚醚多元醇的0.5-2%;辛酸亚锡催化剂,用量为聚醚多元醇的0.1-1.5%;泡沫稳定剂商品名L580、Y8002或8123,添加量为1-2%;发泡剂,水添加量为聚醚多元醇的1-3%。
又如中国专利申请CN200710008623.3公开了一种纳米抗菌海绵及其加工工艺,其由下列主要原料制成:聚醚多元醇90~110重量份、纳米抗菌剂3-5重量份、外发泡剂8-12重量份、水4-6重量份、泡沫稳定剂1.25-1.7重量份、催化剂0.4-0.60重量份、甲苯二异氰酸酯56-68重量份加工而成。制备工艺是按重量比称取各称取各原料,首先在100份的聚醚多元醇原料中加入3-5份的纳米抗菌剂,使其充分分散在聚醚中,然后依次加入8~12份的外发泡剂、4-6份水、1.25-1.75份泡沫稳定剂、0.4-0.6份催化剂,搅拌使其混合均匀,然后加入56-68份甲苯二异氰酸酯,在转速为3600转/分钟的高速搅拌下搅拌3-5秒后将原料倒入事先准备好的箱体内(圆柱形或长方形)即开始发泡,发泡过程为60-140秒,15-20分钟后即从箱体里移出,可得抗菌海绵,根据需要加工成各种规格形状的海绵鞋用衬料备用,该海绵内的纳米抗菌材料会均匀地分布在海绵体内,由于纳米材料具有缓释作用,可以长久地保持抗菌防臭功能。
又如中国专利申请CN201710982208.1公开了一种抗菌海绵及其制备方法,该制备方法包括:将魔芋粉、抗菌填料、发泡剂、润湿剂及凝胶剂加入到沸水中进行搅拌制得料液M1;将所述料液M1转入海绵型胚中、室温下静置后热处理制得料胚;将所述料胚扎出多个均匀的孔后冷冻,最后真空冷冻干燥即制得所述抗菌海绵;其中,所述抗菌填料由茶叶、石灰水、竹叶、桉树叶、白芷、栀子、厚朴、黄柏、苏木、麦冬、大青叶、薄荷、五味子、姜黄醇、柠檬醛和二氢姜黄酮混合制备得到。
又如中国专利申请CN201910439373.1公开了一种抗菌海绵及其制备方法,所述抗菌海绵由甲组分和乙组分制得;所述甲组分包括如下重量份组分:PE6800 0.2-1份、PE62001-2份、聚醚硅油活性剂0.1-0.5份、1000NI 1-2份、纳米银粉末0.5-1份、硅灰石粉35-50份和水45-55份;所述乙组分为亲水性聚氨酯预聚物45-55份。
又如中国专利申请CN201910686248.0公开了一种抗菌海绵及其制备方法,该抗菌海绵包括如下重量份的组分:软泡聚醚多元醇95-105份、甲苯二异氰酸酯44.5-46.3份、抗菌剂1.5-3份、水2.5-3.5份、有机硅表面活性剂0.8-1.4份、催化剂0.2-0.36份;其中,所述抗菌剂为VANQUISH 100。
但上述现有技术的抗菌聚氨酯弹性体存在的问题包括:抗菌效果有限、有效抗菌时间短、抗菌剂添加量高、抗菌剂价格高或有害。
发明内容
本发明的首要目的是提供一种抗菌聚氨酯弹性体,以能够以更少的抗菌剂添加量使聚氨酯弹性体达到更好、更持久、更均匀的抗菌效果,同时降低成本和减少对环境、人体的危害。
为实现此目的,在基础的实施方案中,本发明提供一种抗菌聚氨酯弹性体,制备所述的抗菌聚氨酯弹性体的原料按质量配比包含:聚醚多元醇或聚酯多元醇100份,异氰酸酯32-62份,水1-4.5份,平均粒度为25-350nm的无机纳米抗菌剂0.3-2.5份。
在一种优选的实施方案中,本发明提供一种抗菌聚氨酯弹性体,其中制备所述的抗菌聚氨酯弹性体的原料按质量配比包含:聚醚多元醇或聚酯多元醇100份,异氰酸酯32-62份,水2-4份,平均粒度为30-100nm的无机纳米抗菌剂0.5-1.7份。
在一种优选的实施方案中,本发明提供一种抗菌聚氨酯弹性体,其中:
所述的聚醚多元醇或聚酯多元醇选自二羟基聚醚多元醇、三羟基聚醚多元醇、聚己二酸乙二醇酯中的一种或几种,平均相对分子质量为1000-6500;
所述的异氰酸酯选自甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、多亚甲基多苯基多异氰酸酯中的一种或几种;
所述的无机纳米抗菌剂选自CuO、ZnO、TiO2、SiO2、WO3中的一种或几种。
在一种优选的实施方案中,本发明提供一种抗菌聚氨酯弹性体,其中制备所述的抗菌聚氨酯弹性体的原料按质量配比还包含催化剂0.1-2.0份(优选催化剂0.4-1.5份)和/或发泡剂5-15份(优选发泡剂8-12份),
所述的催化剂选自三乙烯二胺、五乙烯四胺、已二胺、辛酸亚锡中的一种或几种;
所述的发泡剂选自二氯甲烷、一氟三氯甲烷、戊烷、环戊烷中的一种或几种。
在一种优选的实施方案中,本发明提供一种抗菌聚氨酯弹性体,其中所述的无机纳米抗菌剂是经过表面改性剂、偶联剂和/或表面活性剂表面疏水性处理过的无机纳米抗菌剂(例如:利用硅烷偶联剂KH570改性后的无机抗菌剂,KH570的添加量为无机抗菌剂绝干质量的0.5-20%,优选0.5-3%),或是经离子交换、浸渍负载、部分包裹覆盖和/或机械混合“复合叠加”处理过的无机纳米抗菌剂(例如:利用TiO2表面的可以离子交换的基团与银等离子交换,得到Ag/TiO2复合抗菌剂;再例如:将SiO2与ZnO抗菌剂结合,使用涂层技术将ZnO表面部分包裹形成更稳定的具有复合结构的抗菌剂;再例如:利用十八烷基磺酸钠等表面活性剂处理的、提升纳米粒子表面亲水能力的ZnO抗菌剂)。
在一种优选的实施方案中,本发明提供一种抗菌聚氨酯弹性体,其中制备所述的抗菌聚氨酯弹性体的原料按质量配比还包含0.1-2.5份(优选0.5-1.5份)的泡沫稳定剂(例如:迈图高新材料集团(原美国GE有机硅)供应的Niax品牌的一系列泡沫稳定剂、AirProducts公司的DC198等牌号的泡沫稳定剂、德国BYK化学公司的泡沫稳定剂)。
本发明的第二个目的是提供上述抗菌聚氨酯弹性体的制备方法,以能够更好的制备上述抗菌聚氨酯弹性体,制备所得聚氨酯弹性体能够达到更好、更持久、更均匀的抗菌效果,同时降低成本和减少对环境、人体的危害。
实现此目的,在基础的实施方案中,本发明提供上述抗菌聚氨酯弹性体的制备方法,所述的制备方法包括如下步骤:
(1)取全部或部分所述的聚醚多元醇或聚酯多元醇,加入所述的无机纳米抗菌剂后先搅拌混合,再超声分散混合得分散液(通过机械搅拌得到的预混合液中,无机抗菌剂粉体可以以较小团聚体形式分散在聚醚多元醇或聚酯多元醇中;超声分散的过程,将较小团聚的无机抗菌剂分散成单个的纳米粒子,从而使得所添加的无机抗菌剂在聚醚多元醇或聚酯多元醇中均匀的分散);
(2)在分散液中加入除异氰酸酯外的剩余的原料,进一步搅拌混合后加入异氰酸酯,继续搅拌混合得混合发泡液(该步骤无需特殊设备,所需要的高速搅拌设备即为聚氨酯弹性体生产过程常用的设备,是聚氨酯弹性体生产人员和技术人员常用的混合设备);
(3)将混合发泡液制备成聚氨酯弹性体。
在一种优选的实施方案中,本发明提供上述抗菌聚氨酯弹性体的制备方法,其中步骤(1)中,
所述的搅拌混合的搅拌转速为30-5000转/分钟(优选60-300转/分钟),时间为5-20分钟;
所述的超声分散混合的温度为20-60℃(优选40-50℃),功率为200-3000W,时间为5-100分钟(优选30-60分钟)。
在一种优选的实施方案中,本发明提供上述抗菌聚氨酯弹性体的制备方法,其中步骤(2)中,
所述的进一步搅拌混合的搅拌转速为3000-6000转/分钟,时间为1-120分钟;
所述的继续搅拌混合的搅拌转速为3000-6000转/分钟,时间为3-5秒。
在一种优选的实施方案中,本发明提供上述抗菌聚氨酯弹性体的制备方法,其中步骤(3)中,所述的混合发泡液转移至混合头后,经过输送工段、发泡工段、切割工段、后熟化工段和产品的后加工工段加工成聚氨酯弹性体(可参考化学工业出版社出版的《聚氨酯材料手册》第二版,徐培林、张淑琴主编)。
本发明的有益效果在于,利用本发明的抗菌聚氨酯弹性体及其制备方法,能够更好的制备抗菌聚氨酯弹性体,制备所得聚氨酯弹性体能够达到更好、更持久、更均匀的抗菌效果,同时降低成本和减少对环境、人体的危害。
本发明选择安全性高的无机抗菌剂ZnO、TiO2等。含银的抗菌剂虽然抗菌效果好,但是价格高,随着时间的延长易变色,且在生物体内累积后具有一定的潜在的安全风险,对自然环境如土壤和水体也有可能造成污染。
本发明的无机抗菌剂的平均粒径大小为25-350nm,优选30-100nm;相对于100份的聚醚多元醇或聚酯多元醇,无机抗菌剂的加入量为0.3-2.5份,优选0.5-1.7份。因此最终得到的产品中,无机抗菌剂的绝干质量比在1.0%以下,为0.35-0.83%。
本发明的无机抗菌剂可更均匀地分散。众所周知,无机抗菌剂为纳米粒子时极易团聚形成大的颗粒,这种团聚既造成抗菌性能下降又造成抗菌剂的浪费;同时,由于团聚颗粒过大还有可能造成聚氨酯弹性体产品性能下降。因此,纳米无机抗菌剂要想发挥高效的抗菌性,首先必须解决纳米粒子的稳定性和分散性。本发明采用高速机械搅拌和超声分散的技术,使得无机纳米抗菌剂在聚醚多元醇或聚酯多元醇中均匀的分散,因此最终得到的产品中无机抗菌剂的分散更均匀,具有高效的抗菌效果。
具体实施方式
以下结合实施例对本发明的具体实施方式作出进一步的说明。
实施例1:抗菌聚氨酯弹性体的制备(一)
(1)准确称取所需的所有原料:聚醚多元醇(为平均相对分子质量1000的二羟基聚醚多元醇)100g,异氰酸酯(为甲苯二异氰酸酯)32g,催化剂(为三乙烯二胺)0.4g,泡沫稳定剂(为迈图高新材料集团的泡沫稳定剂NiaxL-533)0.5g,外发泡剂(为二氯甲烷)8g,水2g,无机抗菌剂0.5g。无机抗菌剂为未经任何表面改性的纳米ZnO,平均粒径30nm。
(2)无机抗菌剂的分散液制备:取聚醚多元醇2g,加入无机抗菌剂0.5g。在搅拌器内30转/分钟搅拌20分钟,使之形成预混合液,然后利用超声波分散器将预混合液进一步分散,超声分散条件为:温度60℃,功率200W,时间100分钟。经过机械搅拌和超声分散以后得到的混合液即为无机抗菌剂的分散液。
(3)混合发泡液的制备:由第(2)步得到的无机抗菌剂的分散液加入剩下的聚醚多元醇98g,然后依次加入外发泡剂、水、泡沫稳定剂、催化剂,立即3000转/分钟高速搅拌120分钟混合均匀。混合均匀后加入异氰酸酯,继续3000转/分钟高速搅拌5秒使其混合均匀,即可得到混合发泡液。
(4)聚氨酯弹性体的发泡及后续工艺:由第(3)步得到的混合发泡液立即转移至混合头,经输送工段、发泡工段、切割工段、后熟化工段和产品的后加工工段得到抗菌聚氨酯弹性体。
实施例2:抗菌聚氨酯弹性体的制备(二)
(1)准确称取所需的所有原料:聚醚多元醇(为平均相对分子质量3000的三羟基聚醚多元醇)100g,异氰酸酯(为二苯基甲烷二异氰酸酯)62g,催化剂(为五乙烯四胺)1.5g,泡沫稳定剂(为Air Products公司的DC198泡沫稳定剂)1.5g,外发泡剂(为戊烷)12g,水4g,无机抗菌剂1.7g。无机抗菌剂为未经任何表面改性的纳米CuO,平均粒径100nm。
(2)无机抗菌剂的分散液制备:取聚醚多元醇10g,加入无机抗菌剂1.7g。在搅拌器内5000转/分钟搅拌5分钟,使之形成预混合液,然后利用超声波分散器将预混合液进一步分散,超声分散条件为:温度20℃,功率3000W,时间5分钟。经过机械搅拌和超声分散以后得到的混合液即为无机抗菌剂的分散液。
(3)混合发泡液的制备:由第(2)步得到的无机抗菌剂的分散液加入剩下的聚醚多元醇90g,然后依次加入外发泡剂、水、泡沫稳定剂、催化剂,立即6000转/分钟高速搅拌1分钟混合均匀。混合均匀后加入异氰酸酯,继续6000转/分钟高速搅拌3秒使其混合均匀,即可得到混合发泡液。
(4)聚氨酯弹性体的发泡及后续工艺:由第(3)步得到的混合发泡液立即转移至混合头,经输送工段、发泡工段、切割工段、后熟化工段和产品的后加工工段得到抗菌聚氨酯弹性体。
实施例3:抗菌聚氨酯弹性体的制备(三)
(1)准确称取所需的所有原料:聚酯多元醇(为平均相对分子质量6500的聚己二酸乙二醇酯)100g,异氰酸酯(为多亚甲基多苯基多异氰酸酯)50g,催化剂(为辛酸亚锡)1.0g,泡沫稳定剂(为德国BYK化学公司的泡沫稳定剂SILBYK-9231)1.0g,外发泡剂(为环戊烷)10g,水3g,无机抗菌剂1.1g。无机抗菌剂为经KH570表面改性的纳米TiO2,KH570的添加量为绝干纳米TiO2质量的3%,纳米TiO2平均粒径70nm。
(2)无机抗菌剂的分散液制备:取聚酯多元醇5g,加入无机抗菌剂1.1g。在搅拌器内1000转/分钟搅拌10分钟,使之形成预混合液,然后利用超声波分散器将预混合液进一步分散,超声分散条件为:温度40℃,功率1500W,时间45分钟。经过机械搅拌和超声分散以后得到的混合液即为无机抗菌剂的分散液。
(3)混合发泡液的制备:由第(2)步得到的无机抗菌剂的分散液加入剩下的聚酯多元醇95g,然后依次加入外发泡剂、水、泡沫稳定剂、催化剂,立即4500转/分钟高速搅拌60分钟混合均匀。混合均匀后加入异氰酸酯,继续4500转/分钟高速搅拌4秒使其混合均匀,即可得到混合发泡液。
(4)聚氨酯弹性体的发泡及后续工艺:由第(3)步得到的混合发泡液立即转移至混合头,经输送工段、发泡工段、切割工段、后熟化工段和产品的后加工工段得到抗菌聚氨酯弹性体。
实施例4:抗菌聚氨酯弹性体的检测
将实施例1-3得到的聚氨酯弹性体按照GB/T 20944.3-2008规定的震荡法测试聚氨酯弹性体对大肠杆菌和金黄色葡萄球菌的抗菌率,结果如下表1所示。
表1实施例1-3得到的聚氨酯弹性体的抗菌率测试结果
将实施例1-3得到的聚氨酯弹性体各取0.5kg,在普通家用洗衣机内,各按照标准流程洗涤10次后,再按照GB/T 20944.3-2008规定的震荡法测试聚氨酯弹性体对大肠杆菌和金黄色葡萄球菌的抗菌率,结果如下表2所示。
表2实施例1-3得到的聚氨酯弹性体洗涤10次后的抗菌率测试结果
表2结果表明,经过10次洗涤,抗菌聚氨酯弹性体仍具有良好的抗菌效果。
Claims (10)
1.一种抗菌聚氨酯弹性体,其特征在于,制备所述的抗菌聚氨酯弹性体的原料按质量配比包含:聚醚多元醇或聚酯多元醇100份,异氰酸酯32-62份,水1-4.5份,平均粒度为25-350nm的无机纳米抗菌剂0.3-2.5份。
2.根据权利要求1所述的抗菌聚氨酯弹性体,其特征在于,制备所述的抗菌聚氨酯弹性体的原料按质量配比包含:聚醚多元醇或聚酯多元醇100份,异氰酸酯32-62份,水2-4份,平均粒度为30-100nm的无机纳米抗菌剂0.5-1.7份。
3.根据权利要求1或2所述的抗菌聚氨酯弹性体,其特征在于:
所述的聚醚多元醇或聚酯多元醇选自二羟基聚醚多元醇、三羟基聚醚多元醇、聚己二酸乙二醇酯中的一种或几种,平均相对分子质量为1000-6500;
所述的异氰酸酯选自甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、多亚甲基多苯基多异氰酸酯中的一种或几种;
所述的无机纳米抗菌剂选自CuO、ZnO、TiO2、SiO2、WO3中的一种或几种。
4.根据权利要求1或2所述的抗菌聚氨酯弹性体,其特征在于:制备所述的抗菌聚氨酯弹性体的原料按质量配比还包含催化剂0.1-2.0份和/或发泡剂5-15份,
所述的催化剂选自三乙烯二胺、五乙烯四胺、已二胺、辛酸亚锡中的一种或几种;
所述的发泡剂选自二氯甲烷、一氟三氯甲烷、戊烷、环戊烷中的一种或几种。
5.根据权利要求1或2所述的抗菌聚氨酯弹性体,其特征在于:所述的无机纳米抗菌剂是经过表面改性剂、偶联剂和/或表面活性剂表面疏水性处理过的无机纳米抗菌剂,或是经离子交换、浸渍负载、部分包裹覆盖和/或机械混合“复合叠加”处理过的无机纳米抗菌剂。
6.根据权利要求1或2所述的抗菌聚氨酯弹性体,其特征在于:制备所述的抗菌聚氨酯弹性体的原料按质量配比还包含0.1-2.5份的泡沫稳定剂。
7.一种根据权利要求1-6之一所述的抗菌聚氨酯弹性体的制备方法,其特征在于,所述的制备方法包括如下步骤:
(1)取全部或部分所述的聚醚多元醇或聚酯多元醇,加入所述的无机纳米抗菌剂后先搅拌混合,再超声分散混合得分散液;
(2)在分散液中加入除异氰酸酯外的剩余的原料,进一步搅拌混合后加入异氰酸酯,继续搅拌混合得混合发泡液;
(3)将混合发泡液制备成聚氨酯弹性体。
8.根据权利要求7所述的制备方法,其特征在于:步骤(1)中,
所述的搅拌混合的搅拌转速为30-5000转/分钟,时间为5-20分钟;
所述的超声分散混合的温度为20-60℃,功率为200-3000W,时间为5-100分钟。
9.根据权利要求7所述的制备方法,其特征在于:步骤(2)中,
所述的进一步搅拌混合的搅拌转速为3000-6000转/分钟,时间为1-120分钟;
所述的继续搅拌混合的搅拌转速为3000-6000转/分钟,时间为3-5秒。
10.根据权利要求7所述的制备方法,其特征在于:步骤(3)中,所述的混合发泡液转移至混合头后,经过输送工段、发泡工段、切割工段、后熟化工段和产品的后加工工段加工成聚氨酯弹性体。
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