CN116874737A - 慢回弹低温感降噪耳塞用组合料及其制备方法 - Google Patents
慢回弹低温感降噪耳塞用组合料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种慢回弹低温感降噪耳塞用组合料、制备方法及其应用,主要解决聚氨酯降噪耳塞硬度偏高、低温变硬、水洗后拉伸撕裂变差的技术问题。本发明通过采用慢回弹低温感降噪耳塞用组合料及其制备方法,由A、B组分构成。以重量份数计,包括以下组分:A组分:聚醚多元醇a:30~60份,聚醚多元醇b:25~60份,聚合物多元醇c:5~15份,水:0.8~2.3份,反应型催化剂:0.5~1.5份,泡沫稳定剂:0.5~1.5份,交联剂:0.5~2份,扩链剂:1~3份,开孔剂:1~5份,抗菌剂:1~3份;B组分:改性异氰酸酯:20~60份,聚醚多元醇d:5~30份;A组分与B组分的重量份数比为100:(60~80),较好地解决该技术问题,在耳塞制备工业中应用。
Description
技术领域
本发明涉及一种慢回弹低温感降噪耳塞用组合料及其制备方法,属于聚氨酯发泡技术领域。
背景技术
噪声污染已同空气污染、水污染一起,被公认为当代三大污染,引起了人们的极大重视。噪声污染的防治与控制已成为当今全球性的有待解决的一项重大课题。人们寻求通过改进工艺技术、机械结构(控制声源)以及在传播过程中来阻止其传播来降低噪声,但由于受到经济、科技、生产环境等方面的限制,实施难度较大。因此在人耳处,即佩戴降噪耳塞来减少噪声对身体的影响,就变得有效而实用。
目前市面上主流的耳塞大致分为PVC泡沫塑料、硅胶类、慢回弹聚氨酯海绵三类,而慢回弹聚氨酯海绵具有轻质,柔软的特性,并且它的高粘弹性能使得它在吸隔声方面得到广泛的应用。但是目前市面上的慢回弹聚氨酯海绵的回弹时间大约都在10秒左右,且低温时,慢回弹海绵容易变硬,给使用佩戴带来了不舒适感。
中国专利CN 110872371A公开了一种采用Z15吸音粒子慢回弹海绵耳塞的制备方法,该发明开发了一种具有高回弹且回弹慢的聚氨酯软质海绵隔音耳塞,在保持隔音效果稳定的基础上,增加其超柔软、手感好、不易撕裂、佩戴时的舒适度的效果,杜绝了传统耳塞佩戴一段时间后容易开裂、变硬起粉等现象。该发明中存在表述不明确等问题,其主要目的就是改善拉伸撕裂变硬起粉等问题,但全文未公开制备的耳塞的具体物理性能数据,且该项发明中所用助剂含有有机锡催化剂,二氯甲烷发泡剂,长期佩戴会引起耳朵不适甚至引发炎症。
中国专利CN 112794970A公开了一种具有微胀气感超柔软的降噪耳塞及其制备方法,该发明中制备的降噪耳塞密度高达550kg/m3,配方中依旧大量使用到低分子量、高羟值聚醚,使得耳塞在25℃下邵F表面硬度达到55,且慢回弹时间相对较短,这些都会影响到用户的佩戴体验以及生理健康。其一,过高的密度是会一定程度上提高隔音性能,但这势必也会造成过高的硬度,这会加剧其高温感效应。同时,叠加较快的回复时间,这会使人们佩戴耳塞时,很容易产生肿胀和压迫感。其二,人体中耳朵里的细菌非常多,耳朵容纳细菌的程度远高于其他部位。据研究发现,佩戴耳塞1小时,细菌数量将会达到原来的700倍,极不利于耳朵的健康,这是因为戴上耳塞后,耳朵内的空气难以流通,耳朵内温度也急剧升高,更容易滋生细菌,所以开发一款相对透气的、且兼具除螨杀菌的耳塞显得尤为重要,该发明中尚未提及。
发明内容
本发明所要解决的技术问题之一是,现有技术中存在聚氨酯降噪耳塞硬度偏高、低温变硬、水洗后拉伸撕裂变差的技术问题,提供一种新的慢回弹低温感降噪耳塞用组合料,该组合料制备得到的慢回弹低温感降噪耳塞具有柔软、温感弱、回复时间长以及高撕裂拉伸的优点。本发明所要解决的技术问题之二是,提供一种与解决问题之一相对应的慢回弹低温感降噪耳塞的制备方法。
为解决上述技术问题之一,本发明采用的技术方案如下:一种慢回弹低温感降噪耳塞用组合料,以重量份数计,包括以下组分:A组分:聚醚多元醇a:30~60份,聚醚多元醇b:25~60份,聚合物多元醇c:5~15份,水:0.8~2.3份,反应型催化剂:0.5~1.5份,泡沫稳定剂:0.5~1.5份,交联剂:0.5~2份,扩链剂:1~3份,开孔剂:1~5份,抗菌剂:1~3份;B组分:改性异氰酸酯:20~60份,聚醚多元醇d:5~30份;A组分与B组分的重量份数比为100:60~80;其中,聚醚多元醇a为丙三醇、三羟甲基丙烷、乙醇胺或山梨醇中的至少一种作为起始剂,分子量为4000~8000的环氧乙烷-环氧丙烷共聚的聚醚多元醇,其EO含量≥70%,不饱和度为0.01~0.2mmol/g,官能度2~4;聚醚多元醇b为丙三醇、季戊四醇、木糖醇、山梨醇或蔗糖中的至少一种为起始剂,分子量为1000~2500的聚醚多元醇,不饱和度为0.01~0.2mmol/g,官能度为2~4;聚合物多元醇c的官能度为2~4,粘度为2500~3500mpa·s,固含量为26%~30%;所述的泡沫稳定剂为聚硅氧烷-氧化烯烃嵌段或接枝共聚物;所述的交联剂为含有两个官能团以上的小分子多元醇和多元胺类化合物;所述的扩链剂为含有两个官能团的非胺类小分子醇类化合物;所述的开孔剂为聚氧化烯烃-聚硅氧烷型共聚物;所述的抗菌剂为季铵盐类反应型抗菌剂;所述的异氰酸酯选自甲苯二异氰酸酯、粗MDI或碳化二亚胺改性异氰酸酯中的至少一种;所述的聚醚多元醇d为选自聚酯多元醇、聚氧化丙烯多元醇、聚四氢呋喃多元醇或其他烯烃多元醇中的至少一种,官能度不小于2,分子量为1000~3000。
上述技术方案中,优选地,所述的B组分还包括储存稳定剂,储存稳定剂的重量份数为20-40×10-6;所述的储存稳定剂选自磷酸或苯甲酰氯中的一种。
上述技术方案中,优选地,所述的反应型催化剂选自发泡型叔胺类催化剂、凝胶叔胺型催化剂或平衡叔胺型催化剂中的至少一种;所述的泡沫稳定剂选自B-8002或L-580中的至少一种;所述的交联剂为二乙醇胺或三乙醇胺中的至少一种;所述的扩链剂选自1,4丁二醇、乙二醇、二甘醇或新戊二醇中的至少一种;所述的开孔剂选自CHE-350D或SKC-1900中的至少一种;所述的抗菌剂为银离子抗菌剂或季铵盐类的反应型抗菌剂中的至少一种;所述的异氰酸酯选自MDI-LL、BASF-103C或MDI-100L中的一种;所述的聚醚多元醇d为聚四氢呋喃醚。
上述技术方案中,优选地,所述的发泡型叔胺类催化剂选自二甲氨基乙氧基乙醇、三甲基羟乙基乙二胺或N,N,N'-三甲基-N'-羟乙基双氨乙基醚中的至少一种;凝胶叔胺型催化剂选自N,N-双(二甲胺丙基)异丙醇胺或N-(二甲氨基丙基)二异丙醇胺;平衡叔胺型催化剂为二甲基乙醇胺。
为解决上述技术问题之二,本发明采用的技术方案如下:
一种前述的慢回弹低温感降噪耳塞的制备方法,其特征在于,包括以下步骤:
(1)A组分的制备:
以重量份数计,分别称取聚醚多元醇a:30~60份,聚醚多元醇b:25~60份,聚合物多元醇c:5~15份,水:0.8~2.3份,反应型催化剂:0.5~1.5份,泡沫稳定剂:0.5~1.5份,交联剂:0.5~2份,扩链剂:1~3份,开孔剂:1~5份,抗菌剂:1~3份,并依次加入容器中,充分搅拌混合,得到组分A;
(2)B组分的制备:
以重量份数计,称取聚醚多元醇d:5~30份,加入反应釜中,搅拌升温至100~110℃,真空条件下脱水脱气2~3小时,降温至40℃~45℃,加入改性异氰酸酯:20~60份,储存稳定剂20-40×10-6份,再升温至80~85℃反应2~3h,检测NCO含量在18%~24%时,得到B组分;
(3)慢回弹低温感降噪耳塞的制备方法:
a)将模具温度升至40~60℃,并在模具内表面均匀喷涂脱模剂;
b)等待2~3min,待脱模剂在模具表面固化成膜;
c)将制备好的组分A和组分B按100:60~80比例混合,在2000~5000rpm的转速下,充分搅拌3~5S后,快速注入模具并合模锁紧;
d)保模6~10分钟,然后开模,取出制品后,常温下熟化2~4天,即得到慢回弹低温感降噪耳塞。
上述技术方案中,优选地,所述的脱模剂为水溶性脱模剂。
上述技术方案中,优选地,所述的脱模剂为3011B。
本发明提供的一种慢回弹低温感降噪耳塞用组合料,将以多元醇为主的组分A以及自制预聚改性异氰酸酯组分B相结合发泡制成一种慢回弹低温感降噪耳塞,本发明通过采用低温感聚醚完全替代传统的慢回弹聚醚,在获得更加优异的慢回弹效果(回复时间可达20秒)的同时,也极大地改善了低温变硬的问题;其次对异氰酸酯进行预聚改性,有效提高了聚氨酯降噪耳塞的拉伸撕裂性能,使之能反复清洗;然后通过引入反应型阳离子季铵氯化物抗菌剂,可以有效杀死细菌,改善由于长时间佩戴耳塞导致的过敏炎症,同时也可以避免传统银离子抗菌剂由于长期清洗,迁移至表面,最终被洗脱的状况。通过本发明的组合料制备得到的慢回弹低温感降噪耳塞的拉伸强度≧200kpa,断裂伸长率≧120%,撕裂强度≧4.0取得了较好的技术效果。
具体实施方式
表1原料清单–助剂
表2原料清单–主要原料
【实施例1】
(1)A组分的制备
以重量份数计,分别称取聚醚多元醇a CHK-3602:30份,聚醚多元醇b CHE-5110VE:60份,聚合物多元醇c CHP-H30:10份,水:0.8份,反应型催化剂33LV:0.5份,DMEA:0.2份,泡沫稳定剂B-8002:1份,交联剂DEOA:0.5份,扩链剂EG 1份,BDO 2份,开孔剂SKC-1900:3份,抗菌剂Fresche 4850:1份,并依次加入容器中,充分搅拌混合,得到组分A。
(2)B组分的制备
以重量份数计,称取聚醚多元醇d PTMG-2000:10份,加入反应釜中,搅拌升温至105℃,真空条件下脱水脱气2小时,降温至40℃,加入改性异氰酸酯LL:30份,储存稳定剂苯甲酰氯:20×10-6份,再升温至5℃反应2h,检测NCO含量在21%,得到B组分。
(3)慢回弹低温感降噪耳塞的制备
①将模具温度升至50℃,并在模具内表面均匀喷涂脱模剂;
②等待3min,待脱模剂在模具表面固化成膜;
③将制备好的组分A和组分B按100:60比例混合,在2500rpm的转速下,充分搅拌5S后,快速注入模具并合模锁紧;
④保模7分钟,然后开模,取出制品后,常温下熟化2天,即得到慢回弹低温感降噪耳塞。制备得到慢回弹低温感降噪耳塞的常规物性检测数据如表5。
⑤
【实施例2至实施例7以及比较例1至比较例2】
实施例2至实施例4按照实施例1的各个步骤进行,唯一的区别为反应原料种类、催化剂种类、原料配比、工艺参数不同,具体见表3,制备得到慢回弹低温感降噪耳塞的常规物性检测数据如表5。
实施例5至实施例7以及比较例1至比较例2按照实施例1的各个步骤进行,唯一的区别为反应原料种类、催化剂种类、原料配比、工艺参数不同,具体见表4,制备得到慢回弹低温感降噪耳塞的常规物性检测数据如表5。
表3实施例1至实施例4中各组分的原料重量份数
表4实施例5至实施例7及比较例1至比较例2中各组分的原料重量份数
表5实施例1至7和比较例1至2制备的聚氨酯降噪耳塞的性能检测数据
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备注:其中噪值测试方法参考T/CAIACN 006-2021《无线降噪耳机技术要求和测量方法》。
从实施例1到7中可以看出,本发明提供的聚氨酯慢回弹耳塞的回弹时间均保持在20s之上,远大于市面上常规的慢回弹,给予用户足够的时间去塑形佩戴,操作简单。同时较低的温感和密度也使得耳塞的硬度适中,极大地降低了用户佩戴的肿胀感。比较例1为本发明中A组分和未经改性的异氰酸酯反应制得,可以发现,B组分经预聚改性之后,可以有效地提高耳塞的拉伸撕裂性能(拉伸强度≧200kpa,断裂伸长率≧120%,撕裂强度≧4.0),使之可以多次水洗后依旧可以保持较高的撕裂性能。比较例2则为市面上常规的聚氨酯降噪耳塞的制备路线,其各方面性能较之本发明中所提供的聚氨酯慢回弹耳塞均相对较差。
以上内容对本发明所提供的一种慢回弹低温感降噪耳塞进行了详细介绍。本文中的实施例对本发明的原理及实施方式进行了阐述,以上实施例的介绍只是为了理解本发明的核心思想,但本发明的保护范围不限于此,任何熟悉本领域的技术人员在不脱离本发明原理的前提下,对本发明的修改都应当落入权利要求的保护范围内。
Claims (7)
1.一种慢回弹低温感降噪耳塞用组合料,以重量份数计,包括以下组分:A组分:聚醚多元醇a:30~60份,聚醚多元醇b:25~60份,聚合物多元醇c:5~15份,水:0.8~2.3份,反应型催化剂:0.5~1.5份,泡沫稳定剂:0.5~1.5份,交联剂:0.5~2份,扩链剂:1~3份,开孔剂:1~5份,抗菌剂:1~3份;B组分:改性异氰酸酯:20~60份,聚醚多元醇d:5~30份;A组分与B组分的重量份数比为100:60~80;其中,聚醚多元醇a为丙三醇、三羟甲基丙烷、乙醇胺或山梨醇中的至少一种作为起始剂,分子量为4000~8000的环氧乙烷-环氧丙烷共聚的聚醚多元醇,其EO含量≥70%,不饱和度为0.01~0.2mmol/g,官能度2~4;聚醚多元醇b为丙三醇、季戊四醇、木糖醇、山梨醇或蔗糖中的至少一种为起始剂,分子量为1000~2500的聚醚多元醇,不饱和度为0.01~0.2mmol/g,官能度为2~4;聚合物多元醇c的官能度为2~4,粘度为2500~3500mpa·s,固含量为26%~30%;所述的泡沫稳定剂为聚硅氧烷-氧化烯烃嵌段或接枝共聚物;所述的交联剂为含有两个官能团以上的小分子多元醇和多元胺类化合物;所述的扩链剂为含有两个官能团的非胺类小分子醇类化合物;所述的开孔剂为聚氧化烯烃-聚硅氧烷型共聚物;所述的抗菌剂为季铵盐类反应型抗菌剂;所述的异氰酸酯选自甲苯二异氰酸酯、粗MDI或碳化二亚胺改性异氰酸酯中的至少一种;所述的聚醚多元醇d为选自聚酯多元醇、聚氧化丙烯多元醇、聚四氢呋喃多元醇或其他烯烃多元醇中的至少一种,官能度不小于2,分子量为1000~3000。
2.根据权利要求1所述的慢回弹低温感降噪耳塞用组合料,其特征在于,所述的B组分还包括储存稳定剂,储存稳定剂的重量份数为20-40×10-6;所述的储存稳定剂选自磷酸或苯甲酰氯中的一种。
3.根据权利要求1所述的慢回弹低温感降噪耳塞用组合料,其特征在于,所述的反应型催化剂选自发泡型叔胺类催化剂、凝胶叔胺型催化剂或平衡叔胺型催化剂中的至少一种;所述的泡沫稳定剂选自B-8002或L-580中的至少一种;所述的交联剂为二乙醇胺或三乙醇胺中的至少一种;所述的扩链剂选自1,4丁二醇、乙二醇、二甘醇或新戊二醇中的至少一种;所述的开孔剂选自CHE-350D或SKC-1900中的至少一种;所述的抗菌剂为银离子抗菌剂或季铵盐类的反应型抗菌剂中的至少一种;所述的异氰酸酯选自MDI-LL、BASF-103C或MDI-100L中的一种;所述的聚醚多元醇d为聚四氢呋喃醚。
4.根据权利要求3所述的慢回弹低温感降噪耳塞用组合料,其特征在于,所述的发泡型叔胺类催化剂选自二甲氨基乙氧基乙醇、三甲基羟乙基乙二胺或N,N,N'-三甲基-N'-羟乙基双氨乙基醚中的至少一种;凝胶叔胺型催化剂选自N,N-双(二甲胺丙基)异丙醇胺或N-(二甲氨基丙基)二异丙醇胺;平衡叔胺型催化剂为二甲基乙醇胺。
5.一种权利要求1所述的慢回弹低温感降噪耳塞的制备方法,其特征在于,包括以下步骤:
(1)A组分的制备:
以重量份数计,分别称取聚醚多元醇a:30~60份,聚醚多元醇b:25~60份,聚合物多元醇c:5~15份,水:0.8~2.3份,反应型催化剂:0.5~1.5份,泡沫稳定剂:0.5~1.5份,交联剂:0.5~2份,扩链剂:1~3份,开孔剂:1~5份,抗菌剂:1~3份,并依次加入容器中,充分搅拌混合,得到组分A;
(2)B组分的制备:
以重量份数计,称取聚醚多元醇d:5~30份,加入反应釜中,搅拌升温至100~110℃,真空条件下脱水脱气2~3小时,降温至40℃~45℃,加入改性异氰酸酯:20~60份,储存稳定剂20-40×10-6份,再升温至80~85℃反应2~3h,检测NCO含量在18%~24%时,得到B组分;
(3)慢回弹低温感降噪耳塞的制备方法:
a)将模具温度升至40~60℃,并在模具内表面均匀喷涂脱模剂;
b)等待2~3min,待脱模剂在模具表面固化成膜;
c)将制备好的组分A和组分B按100:60~80比例混合,在2000~5000rpm的转速下,充分搅拌3~5S后,快速注入模具并合模锁紧;
d)保模6~10分钟,然后开模,取出制品后,常温下熟化2~4天,即得到慢回弹低温感降噪耳塞。
6.根据权利要求5所述的慢回弹低温感降噪耳塞的制备方法,其特征在于,所述的脱模剂为水溶性脱模剂。
7.根据权利要求6所述的慢回弹低温感降噪耳塞的制备方法,其特征在于,所述的脱模剂为3011B。
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