CN116253987A - 一种水性聚氨酯乳液、可生物降解手套及其制备方法和应用 - Google Patents
一种水性聚氨酯乳液、可生物降解手套及其制备方法和应用 Download PDFInfo
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- CN116253987A CN116253987A CN202310048567.5A CN202310048567A CN116253987A CN 116253987 A CN116253987 A CN 116253987A CN 202310048567 A CN202310048567 A CN 202310048567A CN 116253987 A CN116253987 A CN 116253987A
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- aqueous polyurethane
- polyurethane emulsion
- sulfur
- prepolymer
- diisocyanate
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- 239000011593 sulfur Substances 0.000 claims abstract description 53
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
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- KVNRLNFWIYMESJ-UHFFFAOYSA-N butyronitrile Chemical compound CCCC#N KVNRLNFWIYMESJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种水性聚氨酯乳液、可生物降解手套及其制备方法和应用。本发明的水性聚氨酯乳液包括硫磺分散液乳化包覆处理的预聚物,所述预聚物由二异氰酸酯、蓖麻油、聚合物二元醇、扩链剂和中和剂反应得到;其中二异氰酸酯的异氰酸酯基:蓖麻油中羟基:聚合物二元醇中羟基:扩链剂中羟基:中和剂中胺基的摩尔比=(2.0~4.0):(1.0~1.5):(0.5~1.5):(0.5‑1.0):(0.45~1.2);所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.1%~1.5%。该水性聚氨酯乳液不仅可以有效防止水性聚氨酯乳液交联,提高胶乳利用率,延长存储时间,还可以显著改善采用水性聚氨酯乳液所制得可生物降解手套的降解性能、力学性能和漏水性能。
Description
技术领域
本发明涉及高分子化合物的组合物技术领域,更具体地,一种水性聚氨酯乳液、可生物降解手套及其制备方法和应用。
背景技术
水性聚氨酯是以水代替有机溶剂作为分散介质的新型聚氨酯体系,也称水分散聚氨酯、水系聚氨酯或水基聚氨酯。水性聚氨酯以水为溶剂,具有无污染、安全可靠、机械性能优良、相容性好、易于改性等优点,广泛应用于涂料、胶粘剂、织物涂层与整理剂、皮革涂饰剂、纸张表面处理剂和纤维表面处理剂。相比于丁腈手套,水性聚氨酯手套具备更好的柔软性、吸湿性和透气性,同时还兼顾耐腐蚀性、耐溶剂和生物相容性,是替代丁腈橡胶的理想材料。
而且,以丁腈橡胶为主的橡胶手套废品不能通过生物掩埋的方式进行降解,主要通过焚烧的方式进行处理,而焚烧一千克橡胶手套不仅需要0.65立方天然气,且燃烧过程还会产生0.98kg的二氧化碳气体。为解决丁腈橡胶的降解问题,现有技术中大多采用添加可降解助剂的方式来提高丁腈橡胶的降解性能。例如,现有技术中公开了一种可降解丁腈医用手套及其制备方法,通过在乳液配方中添加可生物降解且与丁腈胶乳相容性良好的丙烯腈接枝淀粉组分来提高丁腈医用手套的降解性能,但其降解率最高仅达到60%,断裂伸长率最高仅为521%,有待进一步提高。
发明内容
本发明的目的是克服现有丁腈手套可生物降解性能差,同时柔软性较差的缺陷和不足,提供一种水性聚氨酯乳液,该水性聚氨酯乳液以蓖麻油为多元醇,并与聚合物二元醇相配合,在二异氰酸酯、催化剂和扩链剂的作用下形成预聚物,并采用硫磺分散液对该预聚物进行乳化包覆处理。
本发明的另一目的是提供一种水性聚氨酯乳液的制备方法。
本发明的另一目的是提供一种聚氨酯手套材料。
本发明的又一目的是提供一种可生物降解手套。
本发明的又一目的是提供一种可生物降解手套的制备方法。
本发明上述目的通过以下技术方案实现:
一种水性聚氨酯乳液,包括硫磺分散液乳化包覆处理的预聚物,所述预聚物由二异氰酸酯、蓖麻油、聚合物二元醇、扩链剂和中和剂反应得到;
其中,所述二异氰酸酯的异氰酸酯基:蓖麻油中羟基:聚合物二元醇中羟基:扩链剂中羟基:中和剂中胺基的摩尔比=(2.0~4.0):(1.0~1.5):(0.5~1.5):(0.5-1.0):(0.45~1.2);所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.1%~1.5%。
本发明水性聚氨酯乳液以二异氰酸酯、蓖麻油和聚合物二元醇为聚合单体,在含有亲水基团(羟基)的扩链剂作用下扩链反应形成聚氨酯,中和成盐可进一步增强聚氨酯亲水基团的亲水性,有利于其在乳化过程中的亲疏水自组装,形成内核疏水、外壳亲水的聚氨酯微粒,疏水的硫磺颗粒被包载进聚氨酯微粒疏水内核中形成稳定的水性聚氨酯乳液。
优选地,所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.5%~1%;所述硫磺分散液中硫磺颗粒的D50为0.5~1.2μm;优选地,所述硫磺分散液中硫磺颗粒的D50为0.5~0.8μm。硫磺分散液中硫磺颗粒影响乳化的效果,硫磺颗粒的粒径越小,乳化效果越好,但基于加工工艺、成本等其他因素的考虑,当硫磺分散液中硫磺颗粒的D50为0.5~0.8μm时即可实现良好的乳化效果。
优选地,所述水性聚氨酯乳液的pH为8.5~9.5,在该pH范围内,可有效提高胶乳稳定性。
具体地,所述聚合物二元醇为聚酯二元醇、聚醚二元醇和聚碳酸酯二元醇中的一种或几种;
所述扩链剂为二羟甲基丙酸和/或二羟甲基丁酸;
所述中和剂为三乙胺、氢氧化钠、碳酸氢钠和氨水中的一种或几种;
所述二异氰酸酯为异氟尔酮二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯和L-赖氨酸二异氰酸酯中的一种或几种。
一种水性聚氨酯乳液的制备方法,包括以下步骤:
S1.将二异氰酸酯、蓖麻油、聚合物二元醇和催化剂混合均匀后在60~85℃条件下、惰性气氛中预聚反应45~150min,再加入扩链剂继续反应60~180min;然后加入稀释剂稀释,再将反应温度降至室温后加入中和剂反应形成预聚物;
S2.将硫磺分散液加入S1中的预聚物中进行乳化包覆处理,即可获得水性聚氨酯乳液;
其中,S2中所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.1%~1.5%,所述乳化包覆处理时间≥60min。
本发明水性聚氨酯乳液的制备方法,以蓖麻油为多元醇,与聚合物二元醇相配合,然后在二异氰酸酯、催化剂和扩链剂的作用下形成预聚物,同时采用硫磺分散液对上述预聚物进行乳化包覆处理形成水性聚氨酯乳液。其中,蓖麻油含有多羟基结构,相较于双羟基的聚合物二元醇可在一定程度提高水性聚氨酯的交联度;而且蓖麻油中含有双键结构,可在成膜过程中于加入交联剂共同作用促进水性聚氨酯进一步交联,进而提高水性聚氨酯的耐水性和力学性能。
聚合物分子量或者交联度不够,影响其力学性能和耐水性能。在乳化包覆处理过程中,硫磺添加量过多,不仅会使得预聚物包载不完全,而且会增大硫磺分布不均匀的概率,出现沉降现象;硫磺添加量过少,则会导致后续交联作用不明显。
具体地,上述稀释剂为丙酮和/或丁酮。
优选地,S2中所述乳化包覆处理的时间为80~120min。
本发明还保护一种聚氨酯手套材料,按重量份数计,包括以下组分,
水性聚氨酯乳液100份、氧化锌0.3~1.5份、二氧化钛0.4~2份、促进剂0.5~2份、防老化剂0.5~1份、分散剂0.02~0.1份、消泡剂0.02~0.1份和水5~100份;
所述水性聚氨酯乳液为上述水性聚氨酯乳液或者上述制备方法制备的水性聚氨酯乳液。
具体地,促进剂可以为二丁基二硫代氨基甲酸锌或二乙基二硫代氨基甲酸锌;防老化剂可以为N-(4-苯胺基苯基)马来酰亚胺;分散剂可以为高浓度分散剂NNO;消泡剂可以为聚醚改性乳液。
一种由上述聚氨酯手套材料制备得到可生物降解手套,也在本发明的保护范围之内。
本发明还保护一种可生物降解手套的制备方法,包括以下步骤:
S1.将手模加热后浸入到凝固液中,停留10~60s后取出烘干,烘干后迅速冷却浸渍到上述聚氨酯手套材料中,停留5~10s取出后烘干3~5min;然后再浸渍到质量百分数为0.05%~0.1%的聚丙烯酸溶液中,浸渍时间为2~10s,温度为30~50℃;
S2.将S1中浸渍后的手模进行硫化处理,硫化温度80~100℃,硫化时间20~30min,再将硫化后的产品清洗、烘干、脱模即得可生物降解手套。
其中,步骤S1中的凝固液为含有质量百分数为5%~15%的硝酸钙、质量百分数为0.1%~0.5%的润湿剂和质量百分数为3%~6%的脱模剂的水溶液。
与现有技术相比,本发明的有益效果是:
本发明以蓖麻油为多元醇并与聚合物二元醇相配合,然后在二异氰酸酯、催化剂和扩链剂的作用下形成预聚物,同时采用硫磺分散液对上述预聚物进行乳化包覆处理形成水性聚氨酯乳液,不仅可以有效防止水性聚氨酯乳液交联,提高胶乳利用率,延长存储时间,还可以显著改善采用水性聚氨酯乳液所制得可生物降解手套的降解性能、力学性能和漏水性能。
具体实施方式
下面结合具体实施方式对本发明作进一步的说明,但实施例并不对本发明做任何形式的限定。除非另有说明,本发明实施例采用的原料试剂为常规购买的原料试剂。
1、原料试剂
蓖麻油,市购可得,平行实验中均采用同种;
二异氰酸酯为异佛尔酮二异氰酸酯,市购可得,平行实验中均采用同种;
聚合物二元醇为聚己内酯二元醇,分子量为1000,牌号VOANOL 2110TB,厂家陶氏化学,平行实验中均采用同种;
催化剂为二月硅酸二丁基锡(DBTDL),市购可得,平行实验中均采用同种;
扩链剂为二羟甲基丁酸(DMBA),市购可得,平行实验中均采用同种;
硫磺、氧化锌和二氧化钛均市购可得,平行实验中均采用同种;
促进剂为二丁基二硫代氨基甲酸锌(ZDBC),市购可得,平行实验中均采用同种;
防老化剂为N-(4-苯胺基苯基)马来酰亚胺,市购可得,平行实验中均采用同种;
分散剂为分散剂NNO,市购可得,平行实验中均采用同种;
消泡剂为聚醚改性乳液,市购可得,平行实验中均采用同种。
2、性能测试
(1)拉伸强度和断裂伸长率:按照ASTM D412-2006a硫化橡胶和热塑性弹性体拉伸试验方法进行测试。
(2)漏水性能:按照EN455-1-2000进行漏水性能进行检测,测试数量100只。
(3)降解率:按照ASTM D5511-18进行测试。
水性聚氨酯乳液1
一种水性聚氨酯乳液,包括硫磺分散液乳化包覆处理的预聚物,所述预聚物由二异氰酸酯、蓖麻油、聚合物二元醇、扩链剂和中和剂反应得到;其中,所述二异氰酸酯的异氰酸酯基:蓖麻油中羟基:聚合物二元醇中羟基:扩链剂中羟基:中和剂中胺基的摩尔比=2.2:1.0:0.5:0.5:0.45。
上述水性聚氨酯乳液可以采用以下制备方法制得:
S1.先将蓖麻油在100℃条件下真空脱水120min,再将其与异佛尔酮二异氰酸酯、聚己内酯二元醇和催化剂混合均匀后在70℃条件下、惰性气氛中预聚反应50min,再加入扩链剂DMBA继续反应60min;然后加入10%的稀释剂丁酮稀释,再将反应温度降至室温后加入中和剂三乙胺进行中和反应,形成预聚物;
S2.将硫磺分散液加入S1中的预聚物中进行乳化包覆处理,即可获得水性聚氨酯乳液;
其中,S1中所述二异氰酸酯的异氰酸酯基:蓖麻油中羟基:聚合物二元醇中羟基:扩链剂中羟基:中和剂中胺基的摩尔比=2.2:1.0:0.5:0.5:0.45;
S2中所述硫磺分散液中硫磺颗粒的D50为0.6μm,S2中所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.5%,所述乳化包覆处理时间为120min。
水性聚氨酯乳液2~16
水性聚氨酯乳液2~16与水性聚氨酯乳液1基本相同,其主要区别如表1所示:
表1
实施例1~15
实施例1~15中聚氨酯手套材料的各组分的重量份数如表2所示。
表2实施例1~15中聚氨酯手套材料
上述聚氨酯手套材料可以采用以下制备方法得到:
将水性聚氨酯乳液、氯化锌、二氧化钛、促进剂、防老化剂、分散剂、消泡剂和水混合均匀,即可获得聚氨酯手套材料。
一种可生物降解胶手套由上述实施例1~15中聚氨酯手套材料按以下方法制备得到:
S1.将手模加热后浸入到凝固液中,停留10~60s后取出烘干,烘干后迅速冷却浸渍到实施例1~10聚氨酯手套材料中,停留5~10s取出后烘干3~5min;然后再浸渍到质量百分数为0.05%~0.1%的聚丙烯酸溶液中,浸渍时间为2~10s,温度为45℃;
S2.将S1中浸渍后的手模进行硫化处理,硫化温度80~100℃,硫化时间20~30min,再将硫化后的产品清洗、烘干、脱模即得可生物降解手套。
其中,步骤S1中的凝固液为含有质量百分数为5%~15%的硝酸钙、质量百分数为0.1%~0.5%的润湿剂和质量百分数为3%~6%的脱模剂的水溶液。
对比例1
一种聚氨酯手套材料,以重量份数计,包括与实施例1基本相同的组分及含量,其区别在于:水性聚氨酯乳液为水性聚氨酯乳液14。
对比例2
一种聚氨酯手套材料,以重量份数计,包括与实施例1基本相同的组分及含量,其区别在于:水性聚氨酯乳液为水性聚氨酯乳液15。
对比例3
一种聚氨酯手套材料,以重量份数计,包括与实施例1基本相同的组分及含量,其区别在于:水性聚氨酯乳液为水性聚氨酯乳液16。
对比例4
一种聚氨酯手套材料,以重量份数计,包括与实施例1基本相同的组分及含量,其区别在于:
采用水性聚氨酯乳液17,水性聚氨酯乳液17与水性聚氨酯乳液1的区别在于,制备方法中采用步骤S1形成预聚物后直接作为水性聚氨酯乳液17,未经过步骤S2的乳化包覆处理。
聚氨酯手套材料,以重量份数计,包括与实施例1基本相同的组分,其区别在于:采用水性聚氨酯乳液17替代水性聚氨酯乳液1,还包括相对于预聚物的质量百分数为0.5%的硫磺分散液,水性聚氨酯乳液17与硫磺分散液的总量为100份。
聚氨酯手套材料的制备方法为:将水性聚氨酯乳液17、相对于预聚物的质量百分数为0.5%的硫磺分散液、氧化锌、二氧化钛、促进剂、防老化剂、分散剂、消泡剂和水混合,得到聚氨酯手套材料。
一种可生物降解胶手套由上述对比例1~4中聚氨酯手套材料制得,其制备方法与实施例1相同。
按照上述提及的性能测试方法对各实施例和对比例中可生物降解手套的性能测试结果如表3所示。
表3各实施例和对比例的测试结果
由上表可以看出,本发明可生物降解胶手套的拉伸强度达到12~26MPa,断裂伸长率达到700%~890%,135天降解速率达到73%以上,且具备优异的耐水性能。
由实施例9和对比例1可知,乳化包覆处理时间过短,硫磺分散液的乳化效果较差,导致胶乳不会出现明显的预硫化从而可生物降解胶手套影响漏水性能;由对比例2和3可知,硫磺分散液中硫磺含量过少时,不仅使得可生物降解胶手套的拉伸强度下降,而且影响其漏水性能;硫磺分散液中硫磺含量过多时,则会明显降低可生物降解胶手套的断裂伸长率和降解率;由实施例1和对比例4可知,对硫磺进行乳化包覆处理后的胶乳长时间静置后手套的漏水性能明显更优,说明经过乳化包覆处理后的胶乳能够放置更长的时间,胶乳不会出现明显的预硫化从而影响漏水性能;同时发现乳化包覆处理后的胶乳具有更高的拉伸强度、断裂伸长率和135天降解速率。
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。
Claims (10)
1.一种水性聚氨酯乳液,其特征在于,包括硫磺分散液乳化包覆处理的预聚物,所述预聚物由二异氰酸酯、蓖麻油、聚合物二元醇、扩链剂和中和剂反应得到;
其中,所述二异氰酸酯的异氰酸酯基:蓖麻油中羟基:聚合物二元醇中羟基:扩链剂中羟基:中和剂中胺基的摩尔比=(2.0~4.0):(1.0~1.5):(0.5~1.5):(0.5-1.0):(0.45~1.2);
所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.1%~1.5%。
2.如权利要求1所述水性聚氨酯乳液,其特征在于,所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.5%~1%,或,所述硫磺分散液中硫磺颗粒的D50为0.5~1.2μm。
3.如权利要求2所述水性聚氨酯乳液,其特征在于,所述硫磺分散液中硫磺颗粒的D50为0.5~0.8μm。
4.如权利要求1所述水性聚氨酯乳液,其特征在于,所述水性聚氨酯乳液的pH为8.5~9.5,或,
所述聚合物二元醇为聚酯二元醇、聚醚二元醇和聚碳酸酯二元醇中的一种或几种;
所述扩链剂为二羟甲基丙酸和/或二羟甲基丁酸;
所述中和剂为三乙胺、氢氧化钠、碳酸氢钠和氨水中的一种或几种;
所述二异氰酸酯为异氟尔酮二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯和L-赖氨酸二异氰酸酯中的一种或几种。
5.权利要求1~4任一项所述水性聚氨酯乳液的制备方法,其特征在于,包括以下步骤:
S1.将二异氰酸酯、蓖麻油、聚合物二元醇和催化剂混合后在60~85℃条件下、惰性气氛中预聚反应45~150min,再加入扩链剂继续反应60~180min;然后加入稀释剂稀释,再将反应温度降至室温后加入中和剂反应形成预聚物;
S2.将硫磺分散液加入S1中的预聚物中进行乳化包覆处理,即可获得水性聚氨酯乳液;
其中,S2中所述硫磺分散液中硫磺相对于预聚物的质量百分数为0.1%~1.5%,所述乳化包覆处理时间≥60min。
6.如权利要求5所述制备方法,其特征在于,S2中所述乳化包覆处理的时间为80~120min。
7.一种聚氨酯手套材料,其特征在于,按重量份数计,包括以下组分,
水性聚氨酯乳液100份、氧化锌0.3~1.5份、二氧化钛0.4~2份、促进剂0.5~2份、防老化剂0.5~1份、分散剂0.02~0.1份、消泡剂0.02~0.1份和水5~100份;
所述水性聚氨酯乳液为权利要求1~4任一项所述的水性聚氨酯乳液或者权利要求5~6任一项所述制备方法制备的水性聚氨酯乳液。
8.如权利要求7所述聚氨酯手套材料,其特征在于,所述促进剂为二丁基二硫代氨基甲酸锌或二乙基二硫代氨基甲酸锌;
所述防老化剂为N-(4-苯胺基苯基)马来酰亚胺;
所述分散剂为高浓度分散剂NNO;所述消泡剂为聚醚改性乳液。
9.一种可生物降解手套,其特征在于,由权利要求7~8任一项所述聚氨酯手套材料制备得到。
10.一种可生物降解手套的制备方法,其特征在于,包括以下步骤:
S1.将手模加热后浸入到凝固液中,停留10~60s后取出烘干,烘干后迅速冷却浸渍到权利要求7~8任一项所述聚氨酯手套材料中,停留5~10s取出后烘干3~5min;然后再浸渍到质量百分数为0.05%~0.1%的聚丙烯酸溶液中,浸渍时间为2~10s,温度为30~50℃;
S2.将S1中浸渍后的手模进行硫化处理,硫化温度80~100℃,硫化时间20~30min,再将硫化后的产品清洗、烘干、脱模即得可生物降解手套。
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