CN108977096A - 一种耐水型聚氨酯胶膜的制备方法 - Google Patents
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Abstract
本发明公开了一种耐水型聚氨酯胶膜的制备方法,属于功能高分子材料技术领域。本发明将玻璃纤维与氢氟酸混合球磨,过滤,洗涤,得预处理玻璃纤维;将预处理玻璃纤维,有机酸,卡波姆,沼液,蔗糖,水混合发酵,过滤,洗涤,干燥,得改性玻璃纤维;将多元醇与三甲基己烷二异氰酸酯加热搅拌反应,随后加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液,碳化二亚胺和亚油酸,继续加热搅拌反应,出料,得水性聚氨酯乳化成膜液;将水性聚氨酯乳化成膜液涂覆在玻璃模具中,干燥,即得耐水型聚氨酯胶膜。本发明技术方案制备的耐水型聚氨酯胶膜具有优异的耐水性能和力学性能的特点。
Description
技术领域
本发明公开了一种耐水型聚氨酯胶膜的制备方法,属于功能高分子材料技术领域。
背景技术
聚氨酯,是聚氨基甲酸酯(Polyurethane,PU)的简称,是分子结构中的高分子链的主链上含有氨基甲酸酯-NHCOO-链接的高分子化合物,它是通过加聚而成的。聚氨酯自20世纪30年代在德国现世以来,因其具有良好的物理机械性能、优异的耐候性、耐疲劳性等特性,得到广泛而迅速的发展。聚氨酯作为纺织品整理剂开始在欧洲出现,通常为传统的溶剂型聚氨酯,与涂料、交联剂等复配,用于纺织品的涂层。但是有机溶剂在合成传统的溶剂型聚氨酯时,用量很大,这些有机溶剂包括苯、甲苯、氯苯、甲醇、丙酮、丁酮、二甲基甲酰胺等,有机溶剂的挥发会使传统的溶剂型聚氨酯产品中的挥发性有机化合物(VOC)含量高,不仅造成环境污染,而且也会对人体的健康产生危害,同时有机溶剂的大量使用也会不可避免的产生高额的生产成本。具有不燃、无毒、无污染等特点的水性聚氨酯(WPU)逐渐受到人们的青睐。
然而,由于亲水基团的引入导致水性聚氨酯胶膜的耐水性以及力学性能变差,从而限制了其应用。为了弥补水性聚氨酯的缺陷,提高其综合性能,扩大其应用范围,需要对其进行改性。
因此,如何改善传统聚氨酯胶膜耐水性能和力学性能无法进一步提升的缺点,以获取更高综合性能的聚氨酯胶膜,是其推广与应用于更广阔的领域,满足工业生产需求亟待解决的问题。
发明内容
本发明主要解决的技术问题是:针对传统的聚氨酯胶膜存在耐水性能和力学性能无法进一步提高的缺点,提供了一种耐水型聚氨酯胶膜的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种耐水型聚氨酯胶膜的制备方法,具体制备步骤如下:
(1)将玻璃纤维与氢氟酸按质量比1:10~1:20混合球磨,过滤,洗涤,得预处理玻璃纤维;
(2)按重量份数计,将20~30份预处理玻璃纤维,3~5份有机酸,3~5份卡波姆,3~5份沼液,0.3~0.5份蔗糖,40~60份水混合发酵,过滤,洗涤,干燥,得改性玻璃纤维;
(3)按重量份数计,依次取20~30份多元醇,40~50份三甲基己烷二异氰酸酯,2~3份扩链剂,2~3份增塑剂,2~3份催化剂,2~3份三氧化二锑,2~3份羟丙基纤维素钠,8~10份改性玻璃纤维,20~30份壳聚糖液,1~2份碳化二亚胺和3~5份亚油酸,将多元醇与三甲基己烷二异氰酸酯加热搅拌反应,随后加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液,碳化二亚胺和亚油酸,继续加热搅拌反应,出料,得水性聚氨酯乳化成膜液;
(4)将水性聚氨酯乳化成膜液涂覆在玻璃模具中,干燥,即得耐水型聚氨酯胶膜。
步骤(2)所述卡波姆为卡波姆934P,卡波姆974P或卡波姆971P中的任意一种。
步骤(2)所述有机酸为乙酸,腐植酸或富维酸中的任意一种。
步骤(3)所述多元醇为聚己二酸丁二醇酯二醇,聚碳酸酯二醇或聚己内酯二醇中的任意一种。
步骤(3)所述扩链剂为二羟甲基丁酸或二羟甲基丙酸中的任意一种。
步骤(3)所述增塑剂为邻苯二甲酸二正锌酯,邻苯二甲酸二丁酯或邻苯二甲酸二甲酯中的任意一种。
步骤(3)所述催化剂为为辛酸亚锡,异辛酸铅或二月桂酸二丁基锡中的任意一种。
本发明的有益效果是:
(1)本发明通过添加改性玻璃纤维,在制备过程中,玻璃纤维经过氢氟酸浸泡,使其表面出现大量的缺陷,接着将预处理玻璃纤维,有机酸,卡波姆,沼液,蔗糖,水混合发酵,体系中的噬酸微生物在玻璃纤维表面得以大量繁殖,使得卡波姆与微生物表面有机质形成氢键结合,产生较强的粘液凝胶网络结构,随后通过滴加氨水,使得卡波姆分子链上的羧基离子化,使得玻纤维表面带负电荷,由于同种电荷间相互排斥,使得玻璃纤维能够良好的分散在体系中,使得胶膜得致密度得到提升,从而使得胶膜的耐水性能和拉伸强度得到进一步的提升;
(2)本发明通过添加壳聚糖液和亚油酸,首先,由于壳聚糖大分子带有正电荷,能够吸引水性聚氨酯分子链的阴离子,避免水性聚氨酯分子链发生缠绕,使得形成的乳胶颗粒得以细化,提升了水性聚氨酯乳液的分散性,使得形成胶膜的致密度得到提升,从而进一步提升了胶膜的耐水性能和拉伸强度得到进一步的提升,其次,通过亚油酸改性,亚油酸的长链烷烃链可提供良好的柔韧性,从而使得体系的断裂伸长率得到进一步的提升。
具体实施方式
将壳聚糖与水按质量比1:50~1:100置于烧杯中,用玻璃棒搅拌10~20min,静置溶胀3~5h,将烧杯置于数显测速恒温磁力搅拌器中,于温度为80~85℃,转速为300~500r/min条件下,加热搅拌溶解40~60min后,得壳聚糖液;将玻璃纤维与质量分数为30~35%的氢氟酸按质量比1:10~1:20置于球磨机中,混合球磨40~60min,得混合球磨液,接着将混合球磨液过滤,得滤渣,接着将滤渣用质量分数为10~20%的氨水洗涤至洗涤液为中性,得预处理玻璃纤维;按重量份数计,将20~30份预处理玻璃纤维,3~5份有机酸,3~5份卡波姆,3~5份沼液,0.3~0.5份蔗糖,40~60份水置于发酵釜中,于温度为28~32℃,转速为200~300r/min条件下,混合发酵3~5天,得发酵混合液,再将发酵混合液过滤,得滤饼,接着用质量分数为20~30%得氨水将滤饼洗涤至洗涤液为中性,随后将洗涤后得滤饼置于烘箱中,于温度为105~110℃条件下,干燥至恒重,得改性玻璃纤维;按重量份数计,依次取20~30份多元醇,40~50份三甲基己烷二异氰酸酯,2~3份扩链剂,2~3份增塑剂,2~3份催化剂,2~3份三氧化二锑,2~3份羟丙基纤维素钠,8~10份改性玻璃纤维,20~30份壳聚糖液,1~2份碳化二亚胺和3~5份亚油酸,将多元醇与三甲基己烷二异氰酸酯置于三口烧瓶中,并将三口烧瓶置于数显测速恒温磁力搅拌器中,并以80~100mL/min速率向炉内通入氮气,于温度为70~80℃,转速为300~500r/min条件下,加热搅拌反应2~3h,随后向三口烧瓶中加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液,碳化二亚胺和亚油酸,于温度为75~85℃,转速为300~500r/min条件下,并以上述氮气保护下,加热搅拌反应1~2h后,出料,得水性聚氨酯乳化成膜液;将水性聚氨酯乳化成膜液涂覆在尺寸为120mm×120mm玻璃模具中,室温下放置,待膜表干后放入烘箱中,于温度为60~80℃条件下,干燥,即得耐水型聚氨酯胶膜。所述卡波姆为卡波姆934P,卡波姆974P或卡波姆971P中的任意一种。所述有机酸为乙酸,腐植酸或富维酸中的任意一种。所述多元醇为聚己二酸丁二醇酯二醇,聚碳酸酯二醇或聚己内酯二醇中的任意一种。所述扩链剂为二羟甲基丁酸或二羟甲基丙酸中的任意一种。所述增塑剂为邻苯二甲酸二正锌酯,邻苯二甲酸二丁酯或邻苯二甲酸二甲酯中的任意一种。所述催化剂为为辛酸亚锡,异辛酸铅或二月桂酸二丁基锡中的任意一种。
将壳聚糖与水按质量比1:100置于烧杯中,用玻璃棒搅拌20min,静置溶胀5h,将烧杯置于数显测速恒温磁力搅拌器中,于温度为85℃,转速为500r/min条件下,加热搅拌溶解60min后,得壳聚糖液;将玻璃纤维与质量分数为35%的氢氟酸按质量比1:20置于球磨机中,混合球磨60min,得混合球磨液,接着将混合球磨液过滤,得滤渣,接着将滤渣用质量分数为20%的氨水洗涤至洗涤液为中性,得预处理玻璃纤维;按重量份数计,将30份预处理玻璃纤维,5份有机酸,5份卡波姆,5份沼液,0.5份蔗糖,60份水置于发酵釜中,于温度为32℃,转速为300r/min条件下,混合发酵5天,得发酵混合液,再将发酵混合液过滤,得滤饼,接着用质量分数为30%得氨水将滤饼洗涤至洗涤液为中性,随后将洗涤后得滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,得改性玻璃纤维;按重量份数计,依次取30份多元醇,50份三甲基己烷二异氰酸酯,3份扩链剂,3份增塑剂,3份催化剂,3份三氧化二锑,3份羟丙基纤维素钠,10份改性玻璃纤维,30份壳聚糖液,2份碳化二亚胺和5份亚油酸,将多元醇与三甲基己烷二异氰酸酯置于三口烧瓶中,并将三口烧瓶置于数显测速恒温磁力搅拌器中,并以100mL/min速率向炉内通入氮气,于温度为80℃,转速为500r/min条件下,加热搅拌反应3h,随后向三口烧瓶中加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液,碳化二亚胺和亚油酸,于温度为85℃,转速为500r/min条件下,并以上述氮气保护下,加热搅拌反应2h后,出料,得水性聚氨酯乳化成膜液;将水性聚氨酯乳化成膜液涂覆在尺寸为120mm×120mm玻璃模具中,室温下放置,待膜表干后放入烘箱中,于温度为80℃条件下,干燥,即得耐水型聚氨酯胶膜。所述卡波姆为卡波姆934P。所述有机酸为乙酸。所述多元醇为聚己二酸丁二醇酯二醇。所述扩链剂为二羟甲基丁酸。所述增塑剂为邻苯二甲酸二正锌酯。所述催化剂为为辛酸亚锡。
将壳聚糖与水按质量比1:100置于烧杯中,用玻璃棒搅拌20min,静置溶胀5h,将烧杯置于数显测速恒温磁力搅拌器中,于温度为85℃,转速为500r/min条件下,加热搅拌溶解60min后,得壳聚糖液;按重量份数计,依次取30份多元醇,50份三甲基己烷二异氰酸酯,3份扩链剂,3份增塑剂,3份催化剂,3份三氧化二锑,3份羟丙基纤维素钠,10份玻璃纤维,30份壳聚糖液,2份碳化二亚胺和5份亚油酸,将多元醇与三甲基己烷二异氰酸酯置于三口烧瓶中,并将三口烧瓶置于数显测速恒温磁力搅拌器中,并以100mL/min速率向炉内通入氮气,于温度为80℃,转速为500r/min条件下,加热搅拌反应3h,随后向三口烧瓶中加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,玻璃纤维,壳聚糖液,碳化二亚胺和亚油酸,于温度为85℃,转速为500r/min条件下,并以上述氮气保护下,加热搅拌反应2h后,出料,得水性聚氨酯乳化成膜液;将水性聚氨酯乳化成膜液涂覆在尺寸为120mm×120mm玻璃模具中,室温下放置,待膜表干后放入烘箱中,于温度为80℃条件下,干燥,即得耐水型聚氨酯胶膜。所述有机酸为乙酸。所述多元醇为聚己二酸丁二醇酯二醇。所述扩链剂为二羟甲基丁酸。所述增塑剂为邻苯二甲酸二正锌酯。所述催化剂为为辛酸亚锡。
将壳聚糖与水按质量比1:100置于烧杯中,用玻璃棒搅拌20min,静置溶胀5h,将烧杯置于数显测速恒温磁力搅拌器中,于温度为85℃,转速为500r/min条件下,加热搅拌溶解60min后,得壳聚糖液;将玻璃纤维与质量分数为35%的氢氟酸按质量比1:20置于球磨机中,混合球磨60min,得混合球磨液,接着将混合球磨液过滤,得滤渣,接着将滤渣用质量分数为20%的氨水洗涤至洗涤液为中性,得预处理玻璃纤维;按重量份数计,将30份预处理玻璃纤维,5份有机酸,5份卡波姆,5份沼液,0.5份蔗糖,60份水置于发酵釜中,于温度为32℃,转速为300r/min条件下,混合发酵5天,得发酵混合液,再将发酵混合液过滤,得滤饼,接着用质量分数为30%得氨水将滤饼洗涤至洗涤液为中性,随后将洗涤后得滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,得改性玻璃纤维;按重量份数计,依次取30份多元醇,50份三甲基己烷二异氰酸酯,3份扩链剂,3份增塑剂,3份催化剂,3份三氧化二锑,3份羟丙基纤维素钠,10份改性玻璃纤维,30份壳聚糖液和5份亚油酸,将多元醇与三甲基己烷二异氰酸酯置于三口烧瓶中,并将三口烧瓶置于数显测速恒温磁力搅拌器中,并以100mL/min速率向炉内通入氮气,于温度为80℃,转速为500r/min条件下,加热搅拌反应3h,随后向三口烧瓶中加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液和亚油酸,于温度为85℃,转速为500r/min条件下,并以上述氮气保护下,加热搅拌反应2h后,出料,得水性聚氨酯乳化成膜液;将水性聚氨酯乳化成膜液涂覆在尺寸为120mm×120mm玻璃模具中,室温下放置,待膜表干后放入烘箱中,于温度为80℃条件下,干燥,即得耐水型聚氨酯胶膜。所述卡波姆为卡波姆934P。所述有机酸为乙酸。所述多元醇为聚己二酸丁二醇酯二醇。所述扩链剂为二羟甲基丁酸。所述增塑剂为邻苯二甲酸二正锌酯。所述催化剂为为辛酸亚锡。
将壳聚糖与水按质量比1:100置于烧杯中,用玻璃棒搅拌20min,静置溶胀5h,将烧杯置于数显测速恒温磁力搅拌器中,于温度为85℃,转速为500r/min条件下,加热搅拌溶解60min后,得壳聚糖液;将玻璃纤维与质量分数为35%的氢氟酸按质量比1:20置于球磨机中,混合球磨60min,得混合球磨液,接着将混合球磨液过滤,得滤渣,接着将滤渣用质量分数为20%的氨水洗涤至洗涤液为中性,得预处理玻璃纤维;按重量份数计,将30份预处理玻璃纤维,5份有机酸,5份卡波姆,5份沼液,0.5份蔗糖,60份水置于发酵釜中,于温度为32℃,转速为300r/min条件下,混合发酵5天,得发酵混合液,再将发酵混合液过滤,得滤饼,接着用质量分数为30%得氨水将滤饼洗涤至洗涤液为中性,随后将洗涤后得滤饼置于烘箱中,于温度为110℃条件下,干燥至恒重,得改性玻璃纤维;按重量份数计,依次取30份多元醇,50份三甲基己烷二异氰酸酯,3份扩链剂,3份增塑剂,3份催化剂,3份三氧化二锑,3份羟丙基纤维素钠,10份改性玻璃纤维,30份壳聚糖液,2份碳化二亚胺,将多元醇与三甲基己烷二异氰酸酯置于三口烧瓶中,并将三口烧瓶置于数显测速恒温磁力搅拌器中,并以100mL/min速率向炉内通入氮气,于温度为80℃,转速为500r/min条件下,加热搅拌反应3h,随后向三口烧瓶中加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液,碳化二亚胺,于温度为85℃,转速为500r/min条件下,并以上述氮气保护下,加热搅拌反应2h后,出料,得水性聚氨酯乳化成膜液;将水性聚氨酯乳化成膜液涂覆在尺寸为120mm×120mm玻璃模具中,室温下放置,待膜表干后放入烘箱中,于温度为80℃条件下,干燥,即得耐水型聚氨酯胶膜。所述卡波姆为卡波姆934P。所述有机酸为乙酸。所述多元醇为聚己二酸丁二醇酯二醇。所述扩链剂为二羟甲基丁酸。所述增塑剂为邻苯二甲酸二正锌酯。所述催化剂为为辛酸亚锡。
对比例:佛山某化工材料生产有限公司生产的聚氨酯胶膜。
将实例1至实例4所得的耐水型聚氨酯胶膜及对比例产品进行性能检测,具体检测方法如下:
1.将厚度为0.5mm的试件干燥至恒质量并剪裁成2cm×2cm,称质量记为m1,将其放入蒸馏水中常温浸泡24h后取出,并迅速用滤纸吸干试件表面的水分,立刻称质量记为m2。试件的吸水率按式(1)计算。
式(1):吸水率(%)=[(m2-m1)÷m1]×100%
2.根据GB/T040.3,将试件裁成哑铃型样条,采用Instron5567型万能材料试验机(美国Instron公司)测试其力学性能。拉伸速度100mm/min,夹具间距30mm,传感器灵敏度1kN。
具体检测结果如表1所示:
表1耐水型聚氨酯胶膜具体检测结果
检测项目 | 吸水率/% | 拉伸强度/MPa | 断裂伸长率/% |
实例1 | 6.04 | 18.63 | 612.31 |
实例2 | 8.51 | 16.47 | 561.48 |
实例3 | 24.18 | 13.71 | 516.34 |
实例4 | 45.86 | 11.24 | 264.18 |
对比例 | 86.12 | 98.7 | 187.61 |
由表1检测结果可知,本发明技术方案制备的耐水型聚氨酯胶膜具有优异的耐水性能和力学性能的特点,在功能高分子材料技术行业的发展中具有广阔的前景。
Claims (7)
1.一种耐水型聚氨酯胶膜的制备方法,其特征在于具体制备步骤如下:
(1)将玻璃纤维与氢氟酸按质量比1:10~1:20混合球磨,过滤,洗涤,得预处理玻璃纤维;
(2)按重量份数计,将20~30份预处理玻璃纤维,3~5份有机酸,3~5份卡波姆,3~5份沼液,0.3~0.5份蔗糖,40~60份水混合发酵,过滤,洗涤,干燥,得改性玻璃纤维;
(3)按重量份数计,依次取20~30份多元醇,40~50份三甲基己烷二异氰酸酯,2~3份扩链剂,2~3份增塑剂,2~3份催化剂,2~3份三氧化二锑,2~3份羟丙基纤维素钠,8~10份改性玻璃纤维,20~30份壳聚糖液,1~2份碳化二亚胺和3~5份亚油酸,将多元醇与三甲基己烷二异氰酸酯加热搅拌反应,随后加入扩链剂,增塑剂,催化剂,三氧化二锑,羟丙基纤维素钠,改性玻璃纤维,壳聚糖液,碳化二亚胺和亚油酸,继续加热搅拌反应,出料,得水性聚氨酯乳化成膜液;
(4)将水性聚氨酯乳化成膜液涂覆在玻璃模具中,干燥,即得耐水型聚氨酯胶膜。
2.根据权利要求1所述一种耐水型聚氨酯胶膜的制备方法,其特征在于:步骤(2)所述卡波姆为卡波姆934P,卡波姆974P或卡波姆971P中的任意一种。
3.根据权利要求1所述一种耐水型聚氨酯胶膜的制备方法,其特征在于:步骤(2)所述有机酸为乙酸,腐植酸或富维酸中的任意一种。
4.根据权利要求1所述一种耐水型聚氨酯胶膜的制备方法,其特征在于:步骤(3)所述多元醇为聚己二酸丁二醇酯二醇,聚碳酸酯二醇或聚己内酯二醇中的任意一种。
5.根据权利要求1所述一种耐水型聚氨酯胶膜的制备方法,其特征在于:步骤(3)所述扩链剂为二羟甲基丁酸或二羟甲基丙酸中的任意一种。
6.根据权利要求1所述一种耐水型聚氨酯胶膜的制备方法,其特征在于:步骤(3)所述增塑剂为邻苯二甲酸二正锌酯,邻苯二甲酸二丁酯或邻苯二甲酸二甲酯中的任意一种。
7.根据权利要求1所述一种耐水型聚氨酯胶膜的制备方法,其特征在于:步骤(3)所述催化剂为为辛酸亚锡,异辛酸铅或二月桂酸二丁基锡中的任意一种。
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