CN111548722B - 一种生活饮用水接触级聚氨酯防水涂料及其制备方法 - Google Patents
一种生活饮用水接触级聚氨酯防水涂料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种生活饮用水接触级聚氨酯防水涂料,由以下组分按照以下重量份组成:异氰酸酯6.2~10.7、聚醚多元醇35.0~55.0、对苯二甲酸二辛酯8.0~12.0、钛白粉2.0~5.0、滑石粉15.0‑29.0、重钙3.0~29.0、煅烧高岭土2.0~7.0、催化剂0.05~0.3、潜固化剂0.5~1.3、稳定剂0.05~0.13。该产品可溶性重金属均未检出,特此制备样品送至国家建筑工程质量监督检验中心,经检测该产品完全符合GB/T17219‑1998《生活饮用水输配水设备及防护材料安全性评价规定》和GB/T5750.4‑2006《生活饮用水卫生标准检验方法感官性状和物理指标》技术标准要求。
Description
技术领域
本发明涉及一种生活饮用水接触级聚氨酯防水涂料及其制备方法。
背景技术
聚氨酯防水涂料多为含有多种溶剂和增塑剂的油性防水涂料,很难满足卫生部下发的《生活饮用水输配水设备及防护材料安全性评价规定》、《饮用水化学处理剂卫生安全评价规定》、《饮水处理器卫生安全与功能评价规定》、《反渗透饮水处理装置卫生安全与功能评价规定》、《生活饮用水卫生标准检验方法》等标准要求,适用于饮用水以及饮用水处理剂直接接触的物质和产品指用于供水系统的输配水管、设备、机械部件(如阀门、加氯设备、水处理剂加入器等)以及防护材料(如涂料、内衬等)。这些产品不得污染水质,浸泡水必须通过毒理学实验,基因突变试验和哺乳动物细胞染色体畸变试验必须为阴性,产品所用的原材料必须使用食品级等技术要求。因此提高聚氨酯防水涂料的环保性能,满足生活饮用水相关技术标准要求显得尤为重要。
发明内容
本发明提供了生活饮用水接触级聚氨酯防水涂料及其制备方法,本发明方法通过聚合恒温制备成生活饮用水接触级聚氨酯防水涂料,它能满足《生活饮用水输配水设备及防护材料安全性评价规定》和《生活饮用水卫生标准检验方法》中重金属含量、VOC含量等技术要求。
一种生活饮用水接触级聚氨酯防水涂料,由以下组分按照以下重量份组成:
进一步地,所述的异氰酸酯由TDI、MDI或者PAPI按照任意比例混合而成。所述的TDI为甲苯二异氰酸酯(toluene diisocyanate);所述的MDI为二苯基甲烷二异氰酸酯(4,4`~diphenylmethane diisocyanate);所述的PAPI为多亚甲基多苯基异氰酸酯(polymethylene polyphenlene isocyanate)。
进一步地,所述的聚醚多元醇由聚氧化丙烯二醇、甘油氧化丙烯聚醚三醇、甘油氧化丙烯聚醚三醇、聚四氢呋喃醚二醇按照任意比例混合而成。
聚氧化丙烯二醇(polyoxypropylene glycol 1000),分子量1000;聚氧化丙烯二醇(polyoxypropylene glycol 2000),分子量2000;甘油氧化丙烯聚醚三醇(Glycerolpropylene oxide polyether triol 330N)聚四氢呋喃醚二醇(Polytetrahydrofuranether glycol)
进一步地,所述的滑石粉采用可溶性重金属未检出级别的滑石粉的滑石粉。
进一步地,所述的煅烧高岭土采用可溶性重金属未检出级别的煅烧高岭土。
进一步地,所述的钛白粉采用可溶性重金属未检出级别的钛白粉。
进一步地,所述的重钙采用可溶性重金属未检出级别的重钙。
进一步地,催化剂:主要为二月桂酸二丁基锡或者异辛酸铋。
进一步地,潜固化剂:酮亚胺、醛亚胺或者氨酯二噁唑烷。
进一步地,稳定剂:有机弱酸类:水杨酸、草酸或者苯甲酸。
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为200-600转/min,对反应釜进行加热,当反应釜温度升至70~80℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至115~125℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.095~-0.1Mpa之间持续抽真空2~5小时,之后关闭真空泵;
接着使反应釜温度冷却至45~55℃后,加入异氰酸酯,之后恒温1~2小时;
接着使反应釜升温至55~65℃后恒温1~2小时;
接着使反应釜升温至65~75℃后恒温1~2小时;
接着使反应釜升温至75~85℃后恒温1~2小时;
之后再在75~85℃加入催化剂后恒温1~2小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,恒温50~100分钟并在恒温过程中检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,打开与反应釜连接的真空泵并在真空度为--0.095~-0.1MPa下持续抽真空20~40分钟,之后逐步降低搅拌速度至停止,最后静置5~10min即得。
清理基面,保证无尖锐物或凸起。
清扫表面的尘土和杂质,基层要干燥,坚实,干净,无尘无油污。
对细部节点部位进行节点加强,采用一布两涂对阴阳角、管道管根处进行细部节点加强。
大面积涂刷第一遍,待表面干燥后进行刮涂第二遍,两遍总干膜涂刷厚度不低于1.5mm。
干燥后养护1周,进行闭水实验,验收合格后即可进行保护层或隔离层下道工序施工。
教之前的现有技术,本发明的有益之处在于:本发明通过对异氰酸酯的不同选择,采用不同的合成工艺制备出的聚氨酯防水涂料,根据GB/T19250-2013《聚氨酯防水涂料》标准测试结果可以看出,具有有害物质限量含量低,很多项均未检出,物理性能指标在完全满足I型的技术指标前提下,比传统市售产品具有良好的环保性,且该产品可溶性重金属均未检出,特此制备样品送至国家建筑工程质量监督检验中心,经检测该产品完全符合GB/T17219-1998《生活饮用水输配水设备及防护材料安全性评价规定》和GB/T5750.4-2006《生活饮用水卫生标准检验方法感官性状和物理指标》技术标准要求。
具体实施方式
下面结合具体实施例对本发明进行进一步阐述。
实施例1
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为200转/min,对反应釜进行加热,当反应釜温度升至70℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至度115℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.095Mpa之间持续抽真空2小时,之后关闭真空泵;
脱水完成之后关闭真空阀然后50℃后加入TDI和MDI-50恒温2小时;
然后升温至65℃恒温2小时;
升温至75℃恒温2小时;
之后再在75℃加入催化剂并恒温2小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,恒温50~100分钟并在恒温过程中检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,打开与反应釜连接的真空泵并在真空度为--0.095MPa下持续抽真空20分钟,之后逐步降低搅拌速度至停止,最后静置5min即得。
实施例2
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为400转/min,对反应釜进行加热,当反应釜温度升至75℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至度115℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.098Mpa之间持续抽真空5小时,之后关闭真空泵;
脱水完成之后关闭真空阀和并设定温度为50℃,待温度冷却至50℃后加入TDI和MDI-50恒温2小时;
然后升温至65℃恒温2小时;
升温至75℃恒温2小时;
之后再在75℃加入催化剂并恒温2小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,恒温50~100分钟并在恒温过程中检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,打开与反应釜连接的真空泵并在真空度为--0.098MPa下持续抽真空30分钟,之后逐步降低搅拌速度至停止,最后静置7min即得。
实施例3
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为300转/min,对反应釜进行加热,当反应釜温度升至75℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至度120℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.1Mpa之间持续抽真空2小时,之后关闭真空泵;
脱水完成之后关闭真空阀和并设定温度为60℃,待温度冷却至60℃后加入异氰酸酯恒温1小时;
然后升温至75℃恒温1小时;
升温至85℃恒温1小时;
之后再在85℃加入催化剂并恒温1小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,恒温50分钟后,打开与反应釜连接的真空泵并在真空度为--0.095MPa下持续抽真空40分钟,之后逐步降低搅拌速度至停止,最后静置10min即得。
实施例4
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为500转/min,对反应釜进行加热,当反应釜温度升至75℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至度120℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.097Mpa之间持续抽真空5小时,之后关闭真空泵;
脱水完成之后关闭真空阀和并设定温度为60℃,待温度冷却至60℃后加入异氰酸酯恒温1小时;
然后升温至75℃恒温1小时;
升温至85℃恒温1小时;
之后再在85℃加入催化剂并恒温1小时;
之后在85℃下依次加入潜固化剂和稳定剂,恒温60分钟后,打开与反应釜连接的真空泵并在真空度为-0.1MPa下持续抽真空40分钟,之后逐步降低搅拌速度至停止,最后静置10min即得。
实施例5
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为500转/min,对反应釜进行加热,当反应釜温度升至70℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至度115℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.095Mpa之间持续抽真空3小时,之后关闭真空泵;
脱水完成之后关闭真空阀和并设定温度为60℃,待温度冷却至60℃后加入异氰酸酯恒温1小时;
然后升温至75℃恒温1小时;
升温至85℃恒温1小时;
之后再在85℃加入催化剂并恒温1小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,恒温50~100分钟并在恒温过程中检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,打开与反应釜连接的真空泵并在真空度为--0.095~-0.1MPa下持续抽真空20~40分钟,之后逐步降低搅拌速度至停止,最后静置5~10min即得。
实施例6
一种生活饮用水接触级聚氨酯防水涂料的制备方法,包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为-600转/min,对反应釜进行加热,当反应釜温度升至80℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至度125℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.097Mpa之间持续抽真空3小时,之后关闭真空泵;
脱水完成之后关闭真空阀和并设定温度为60℃,待温度冷却至60℃后加入异氰酸酯恒温1小时;
然后升温至75℃恒温1小时;
升温至85℃恒温1小时;
之后再在85℃加入催化剂并恒温1小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,恒温50~100分钟并在恒温过程中检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,打开与反应釜连接的真空泵并在真空度为--0.095~-0.1MPa下持续抽真空20~40分钟,之后逐步降低搅拌速度至停止,最后静置5min即得。
施工流程:
施工准备→基层处理→细部附加防水层施工→大面积刮涂施工→养护→闭水试验→保护、隔离层施工。
将上述实施例1-6所得的产品按照GB/T19250-2013标准技术指标A类、B/T17219-1998《生活饮用水输配水设备及防护材料安全性评价规定》、和GB/T5750.4-2006《生活饮用水卫生标准检验方法感官性状和物理指标》进行检测得结果如表1和表2所示。
从有害物质限量技术数据可以看出,实验1-6均满足GB/T19250-2013技术标准要求,VOC含量方面均小于10g/L,其他有害物质均未检出,环保性能方面均优于国家标准,经国家建筑工程质量监督检验中心测试,技术指标均满足GB/T17219-1998《生活饮用水输配水设备及防护材料安全性评价规定》和GB/T5750.4-2006《生活饮用水卫生标准检验方法感官性状和物理指标》的技术标准要求。符合国家饮用水接触级技术要求。
中试产品送国家建筑工程质量监督检验中心检测,该产品通过了GB/T 17219-1998《生活饮用水输配水设备及防护材料的安全性评价标准》,GB/T 5750.4-2006《生活饮用水标准检验方法感官性状和物理指标》等检测标准,有16种以上的有害物质检测数据均低于国家生活饮用水的技术指标。
从以上检验报告数据可以看出,无论从气味还是金属限量,还是其他表征数据,经检验均超越国家技术指标的要求。
有害物质限量中可挥发性有机化合物(VOC)的数据一直在7~10g/L的范围内徘徊,有以下原因造成:
测试方法测试方法未考虑到聚氨酯预留的端-NCO基团与H20的恒温。
单组分聚氨酯产品预留的端-NCO与空气中的水恒温,一个H2O释放出CO2,质量差为26,也就是说参与恒温的1molH2O,释放出1molCO2,质量损耗差值为26g。根据配方的设计,恰巧测试出的VOC值恰是释放出的质量差损耗。如聚氨酯固化原理恒温方程式所示:
物质限量超出。
本发明所用化学原料缩写、商品名与中英文名称对照如下:
TDI甲苯二异氰酸酯(toluene diisocyanate);
MDI二苯基甲烷二异氰酸酯(4,4`-diphenylmethane diisocyanate);
PAPI多亚甲基多苯基异氰酸酯(polymethylene polyphenlene isocyanate);
N210聚氧化丙烯二醇(polyoxypropylene glycol 1000),分子量1000;
N220聚氧化丙烯二醇(polyoxypropylene glycol 2000),分子量2000;
330N甘油氧化丙烯聚醚三醇(Glycerol propylene oxide polyether triol330N)
PTMG聚四氢呋喃醚二醇(Polytetrahydrofuran ether glycol)
DINP邻苯二甲酸二异壬酯(diisononyl phthalate);
DOTP对苯二甲酸二辛酯(dioctyl terephthalate);
DIDP邻苯二甲酸二异癸酯(diisodecyl phthalate);
DINCH环己烷1,2-二甲酸二异壬基酯(Diisononyl cyclohexane 1,2-diformate)。
滑石粉(talcumpowder)800目-2000目
煅烧高岭土(calcined kaolin)1000-2000目
钛白粉(Titanium dioxide)金红石型钛白粉
碳酸钙(Calcium carbonate)800-2000目
硅藻土(Diatomite)SiO2≥80%以上
以上所述实施例仅仅是本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案作出的各种变形和改进,均应落入本发明的权利要求书确定的保护范围内。
Claims (8)
1.一种生活饮用水接触级聚氨酯防水涂料,其特征在于:由以下组分按照以下重量份组成:
异氰酸酯 6.2~10.7
聚醚多元醇 35.0~55.0
对苯二甲酸二辛酯 8.0~12.0
钛白粉 2.0~5.0
滑石粉 15.0-29.0
重钙 3.0~29.0
煅烧高岭土 2.0~7.0
催化剂 0.05~0.3
潜固化剂 0.5~1.3
稳定剂 0.05~0.13,
所述的异氰酸酯为TDI;
所述的生活饮用水接触级聚氨酯防水涂料由以下方法制备而成:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为200-600转/min,对反应釜进行加热,当反应釜温度升至70~80℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至115~125℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.095~-0.1Mpa之间持续抽真空2~5小时,之后关闭真空泵;
接着使反应釜温度冷却至45~55℃后,加入异氰酸酯,之后恒温1~2小时;
接着使反应釜升温至55~65℃后恒温1~2小时;
接着使反应釜升温至65~75℃后恒温1~2小时;
接着使反应釜升温至75~85℃后恒温1~2小时;
之后再在75~85℃加入催化剂后恒温1~2小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,之后恒温50~100分钟,之后打开与反应釜连接的真空泵对反应釜抽真空,并在真空度-0.095~-0.1MPa下持续抽真空20~40分钟,之后逐步降低搅拌速度至静止,最后静置5~10min即得;
所述的异氰酸酯由TDI组成;在加入潜固化剂和稳定剂之后的恒温50~100分钟过程中,检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,即打开与反应釜连接的真空泵对反应釜抽真空。
2.根据权利要求1所述的一种生活饮用水接触级聚氨酯防水涂料,其特征在于:所述的聚醚多元醇由聚氧化丙烯二醇、甘油氧化丙烯聚醚三醇、甘油氧化丙烯聚醚三醇、聚四氢呋喃醚二醇中的一种组成或其中两种以上按照任意比例混合而成。
3.根据权利要求1所述的一种生活饮用水接触级聚氨酯防水涂料,其特征在于:所述的滑石粉采用可溶性重金属未检出级别的滑石粉。
4.根据权利要求1所述的一种生活饮用水接触级聚氨酯防水涂料,其特征在于:所述的煅烧高岭土采用可溶性重金属未检出级别的煅烧高岭土。
5.根据权利要求1所述的一种生活饮用水接触级聚氨酯防水涂料,其特征在于:所述的钛白粉采用可溶性重金属未检出级别的钛白粉。
6.根据权利要求1所述的一种生活饮用水接触级聚氨酯防水涂料,其特征在于:所述的重钙采用可溶性重金属未检出级别的重钙;所述的催化剂为二月桂酸二丁基锡或者异辛酸铋。
7.根据权利要求1所述的一种生活饮用水接触级聚氨酯防水涂料,其特征在于:所述的潜固化剂为酮亚胺、醛亚胺或者氨酯二噁唑烷;所述的稳定剂为水杨酸、草酸或者苯甲酸。
8.根据权利要求1-7中任一项所述的一种生活饮用水接触级聚氨酯防水涂料的制备方法,其特征在于:包括如下步骤:
将聚醚多元醇、对苯二甲酸二辛酯加入反应釜中,开启并设定搅拌速度为200-600转/min,对反应釜进行加热,当反应釜温度升至70~80℃后,依次加入钛白粉、滑石粉、重钙、煅烧高岭土,当反应釜温度升温至115~125℃之间时,打开与反应釜连接的真空泵对反应釜抽真空,并使反应釜在真空度为-0.095~-0.1Mpa之间持续抽真空2~5小时,之后关闭真空泵;
接着使反应釜温度冷却至45~55℃后,加入异氰酸酯,之后恒温1~2小时;
接着使反应釜升温至55~65℃后恒温1~2小时;
接着使反应釜升温至65~75℃后恒温1~2小时;
接着使反应釜升温至75~85℃后恒温1~2小时;
之后再在75~85℃加入催化剂后恒温1~2小时;
之后在75~85℃下依次加入潜固化剂和稳定剂,之后恒温50~100分钟,之后打开与反应釜连接的真空泵对反应釜抽真空,并在真空度-0.095~-0.1MPa下持续抽真空20~40分钟,之后逐步降低搅拌速度至静止,最后静置5~10min即得;
所述的异氰酸酯由TDI组成;在加入潜固化剂和稳定剂之后的恒温50~100分钟过程中,检测游离TDI的百分含量是否低于0.3%,当检测的游离TDI的百分含量低于0.3%后,即打开与反应釜连接的真空泵对反应釜抽真空。
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