CN110964167A - 一种聚酯型聚氨酯泡沫的制备方法 - Google Patents
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Abstract
本发明提供一种聚酯型聚氨酯泡沫的制备方法,制备的聚氨酯泡沫力学性能优异。所述制备方法为预聚体法,结合其中使用的催化剂组合,以及聚氨酯泡沫稳定剂,制备了聚氨酯泡沫。制备方法,A组份,聚氨酯预聚体:聚碳酸酯二元醇100份、异氰酸酯30‑50份、扩链剂2‑10份;B组份:催化剂0.2‑1.0份、发泡剂1‑5份、泡沫稳定剂1‑6份。
Description
技术领域
本发明涉及聚氨酯制品的制造领域,尤其涉及一种聚酯型聚氨酯泡沫的生产工艺。
背景技术
聚氨酯泡沫材料是聚氨酯材料中的一大类,按照所用原料不同分为聚醚型聚氨酯泡沫和聚酯型聚氨酯泡沫,作为泡沫清管器的主体材料,聚醚型聚氨酯泡沫材料的耐磨性和耐油性尚不能满足应用要求,聚氨酯型聚氨酯泡沫能够弥补此类性能不足。传统的聚氨酯泡沫大部分以聚醚型为主,涉及的聚酯型聚氨酯泡沫确实很少,并且大部分的传统聚氨酯泡以一步法制备,影响泡沫的不稳定性,容易造成泡沫的成型困难;大量采用物理发泡剂还会造成对环境的污染,也不利于形成密度较大的泡沫。作为清管器的主体材料,聚酯型聚氨酯泡沫是理想的首选材料。
发明内容
本发明的目的是提供一种聚酯型聚氨酯泡沫的制备方法。以此制备的聚酯型聚氨酯泡沫克服了一步法所造成的泡沫不稳定,成型困难的缺点和避免对环境造成污染,采用特殊的催化剂组合和自制的改性硅酮表面活性剂,制备的聚酯型聚氨酯泡沫具有优异的力学性能、耐磨性和耐油性,并具有较高密度。
本发明中一种聚酯型聚氨酯泡沫的制备方法,包括以下步骤:
1)A组份:聚氨酯预聚物的制备方法如下:以质量份计,聚碳酸酯二元醇100份、扩链剂2-10份、异氰酸酯30-50份,在60-75℃环境下反应1-3小时,得到聚氨酯预聚物;
2)B组份,制备方法如下:以质量份计,催化剂0.1-0.8份、发泡剂0.5-5份、泡沫稳定剂0.5-5份,按比例称量,均匀混合。
3)聚氨酯泡沫制备方法:将A组份和B组份在50-75℃下高速搅拌混合5-15s,立即浇注到温度为30-50℃的模具中,在30-50℃环境下熟化4-6小时,脱模后在室温下进一步熟化24-48h,得到聚氨酯泡沫。
其中,A组分中所述的聚碳酸酯二元醇数均分子量在1000-4000,为一种或几种不同数均分子量聚碳酸酯二元醇的混合物。
其中,A组分中所述的异氰酸酯为甲苯二异氰酸酯TDI-100、TDI-80中的一种或两种的混合物。
其中,A组份中所述的扩链剂为醇类扩链剂和胺类扩链剂,醇类扩链剂为1,4-丁二醇、一缩丙二醇、1,6-己二醇、新戊二醇、二缩三丙二醇、1,5-戊二醇,胺类扩链剂4,4′-二氨基-3,3′-二乙基-二苯基甲烷,3-氯-3’-乙基-4,4’-二氨基二苯甲烷,3,3’二氯-4,4’-二氨基二苯甲烷,二乙基甲苯二胺(DETDA),二甲硫基甲苯二胺DMTDA,A组份中所述的扩链剂为醇类扩链剂和胺类扩链剂中的一种或几种的混合物。
其中,A组份预聚体中异氰酸基团含量为4%-12%。
其中,B组份中所述的发泡剂为去离子水。
其中,B组份中所述的催化剂的组合为胺类催化剂和锡类催化剂的混合物,B组份中所述的胺类催化剂为乙二胺、三乙基胺、三甲基胺、N-甲基吗啉、N-乙基吗啉、N,N-二甲基苄胺,锡类催化剂为:辛酸亚锡、二月桂酸二丁基锡、二月桂酸二辛基锡、二油酸二丁基锡、醋酸锡、二醋酸二丁基锡、二醋酸二甲基锡、草酸亚锡。
其中,B组份中所述的泡沫稳定剂为有机硅酮表面活性剂,有机硅酮表面活性剂的摩尔质量2000g/mol,其中聚醚在硅酮表面活性剂中的含量为30%,聚醚中环氧乙烷/环氧丙烷比例为1/1,并且聚醚是丁基封端,封端率为95%。
其中,制备的聚酯型聚氨酯泡沫密度为70-320kg/m3.
本发明主要采用预聚体法,配合特殊的催化剂组合,并采用特殊结构的硅酮表面活性剂制备的聚酯型聚氨酯泡沫具有优异的力学性能、耐磨性和耐油性。
具体实施方式
下面结合实施实例对本发明做进一步的说明。
实施例按表1进行物料配比:
表1 实施例原料配比
实施例1:
A组份:聚氨酯预聚物的制备方法如下:以质量份计,按表1称量聚酯多元醇、扩链剂和异氰酸酯,在60℃环境下反应1小时,得到聚氨酯预聚物;
B组份,制备方法如下:
以质量份计,催化剂、发泡剂、泡沫稳定剂,按表1称量,均匀混合。
聚氨酯泡沫制备方法:
将A组份和B组份在50℃下高速搅拌混合5s,立即浇注到温度为30℃的模具中,在30℃环境下熟化4小时,脱模后在室温下进一步熟化24h,得到聚氨酯泡沫。
实施例2:
A组份:聚氨酯预聚物的制备方法如下:
以质量份计,按表1称量聚酯多元醇、扩链剂和异氰酸酯,在75℃环境下反应3小时,得到聚氨酯预聚物;
B组份,制备方法如下:
以质量份计,催化剂、发泡剂、泡沫稳定剂,按表1称量,均匀混合。
聚氨酯泡沫制备方法:
将A组份和B组份在75℃下高速搅拌混合15s,立即浇注到温度为50℃的模具中,在50℃环境下熟化6小时,脱模后在室温下进一步熟化48h,得到聚氨酯泡沫。
实施例3
A组份:聚氨酯预聚物的制备方法如下:
以质量份计,按表1称量聚酯多元醇、扩链剂、异氰酸酯,在70℃环境下反应2小时,得到聚氨酯预聚物;
B组份,制备方法如下:
以质量份计,催化剂、发泡剂、泡沫稳定剂,按表1称量,均匀混合。
聚氨酯泡沫制备方法:
将A组份和B组份在60℃下高速搅拌混合10s,立即浇注到温度为40℃的模具中,在40℃环境下熟化5小时,脱模后在室温下进一步熟化36h,得到聚氨酯泡沫。
实施例4
A组份:聚氨酯预聚物的制备方法如下:
以质量份计,按表1称量聚酯多元醇、扩链剂、异氰酸酯,在65℃环境下反应1.5小时,得到聚氨酯预聚物;
B组份,制备方法如下:
以质量份计,催化剂、发泡剂、泡沫稳定剂,按表1称量,均匀混合。
聚氨酯泡沫制备方法:
将A组份和B组份在65℃下高速搅拌混合12s,立即浇注到温度为45℃的模具中,在35℃环境下熟化5小时,脱模后在室温下进一步熟化30h,得到聚氨酯泡沫。
实施例5
A组份:聚氨酯预聚物的制备方法如下:
以质量份计,按表1称量聚酯多元醇、扩链剂、异氰酸酯,在70℃环境下反应2小时,得到聚氨酯预聚物;
B组份,制备方法如下:
以质量份计,催化剂、发泡剂、泡沫稳定剂,按表1称量,均匀混合。
聚氨酯泡沫制备方法:
将A组份和B组份在70℃下高速搅拌混合12s,立即浇注到温度为40℃的模具中,在45℃环境下熟化6小时,脱模后在室温下进一步熟化42h,得到聚氨酯泡沫。
实施例产品性能如表2:
表2 实施例产品性能
项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
密度(kg/m<sup>3</sup>) | 320 | 212 | 70 | 127 | 118 |
拉伸强度/MPa | 2.89 | 1.93 | 1.02 | 1.1 | 1.09 |
撕裂强度/kN·m<sup>-1</sup> | 8.95 | 7.5 | 3.02 | 5.3 | 4.6 |
回弹率/% | 33 | 32 | 30 | 31 | 31 |
拉断伸长率/% | 650 | 620 | 625 | 610 | 630 |
粘度过高和一步法的不稳定性的缺点,同时在半预聚体中使用胺类和醇类扩链剂的配合,制备的聚氨酯弹性体固化时间长,并且力学性能优越,耐磨性和耐油性优异。
具体实施方式
下面结合实施实例对本发明做进一步的说明。
实施例1
A组分:聚碳酸酯二醇PCL-1500(数均分子量1500)50份,聚二甲基甲基苯基硅氧烷碳二醇(数均分子量1000)2份,在120℃经氮气吹扫环境下除水2h,降至60℃时加入TDI-100 40份,反应1.5h,得到游离异氰酸根含量为4%的半预聚体。
B组份:聚碳酸酯二醇PCL-1500(数均分子量1500)50份、BDO 0.5份、催化剂辛酸亚锡0.01份;
弹性体:A组分与B组份以1∶1的比例混合,在60℃下搅拌30秒后,浇注到模具中,25度下固化4h,然后80℃下后硫化8h,得到聚氨酯弹性体。
实施例2
A组分:聚碳酸酯二醇PCL-4000(数均分子量4000)100份,聚二甲基甲基苯基硅氧烷碳二醇(数均分子量4000)4份,在120℃经氮气吹扫环境下除水2h,降至75℃时加入MDI-10070份,反应3h,得到游离异氰酸根含量为16%的半预聚体。
B组份:聚碳酸酯二醇PCL-1500(数均分子量1500)10份、二乙基甲苯二胺(DETDA)5份、催化剂N-乙基吗啉0.1份。
弹性体:A组分与B组份以1∶1的比例混合,在75℃下搅拌30秒后,浇注到模具中,30度下固化6h,然后80℃下后硫化8h,得到聚氨酯弹性体。
实施例3
A组分:聚碳酸酯二醇PCL-2000(数均分子量2000)75份,聚二甲基甲基苯基硅氧烷碳二醇(数均分子量3000)2份,在120℃经氮气吹扫环境下除水2h,降至70℃时加入MDI-50 60份,反应2h,得到游离异氰酸根含量为10%的半预聚体。
B组份:聚碳酸酯二醇PCL-3000(数均分子量3000)80份、二甲硫基甲苯二胺DMTDA 2份,1,6一己二醇2份、催化剂N,N,N′,N′-四甲基亚烷基二胺0.02份和二月桂酸二丁基锡0.01份。
弹性体:A组分与B组份以1∶1的比例混合,在75℃下搅拌30秒后,浇注到模具中,30度下固化5h,然后80℃下后硫化8h,得到聚氨酯弹性体。
实施例4
A组分:聚碳酸酯二醇PCL-3000(数均分子量2000)60份,聚二甲基甲基苯基硅氧烷碳二醇(数均分子量2000)3份,在120℃经氮气吹扫环境下除水2h,降至70℃时加入TDI-80 65份,反应2.5h,得到游离异氰酸根含量为12%的半预聚体。
B组份:聚碳酸酯二醇PCL-2000(数均分子量2000)75份、4,4′-二氨基-3,3′-二乙基-二苯基甲烷1份,三羟甲基丙烷0.5份、催化剂N,N’-二甲基吡啶0.01份和二油酸二辛基锡0.01份;
弹性体:A组分与B组份以1∶1的比例混合,在75℃下搅拌30秒后,浇注到模具中,25度下固化5h,然后80℃下后硫化8h,得到聚氨酯弹性体。
以上实施例1-4的测试性能实验结果如表1:
表1 实施例1-4的测试性能实验结果
项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
凝胶时间/min | 9 | 13 | 8 | 5 |
硬度/邵A | 72 | 40 | 61 | 85 |
拉伸强度/MPa | 38 | 30 | 34 | 42 |
撕裂强度/kN·m<sup>-1</sup> | 128 | 121 | 115 | 158 |
拉断伸长率/% | 510 | 640 | 550 | 420 |
DIN磨耗/mm<sup>3</sup> | 31 | 27 | 30 | 35 |
Claims (9)
1.一种聚酯型聚氨酯泡沫的制备方法,其特征在于,包括以下步骤:
1)A组份:聚氨酯预聚物的制备方法如下:以质量份计,聚碳酸酯二元醇100份、扩链剂2-10份、异氰酸酯30-50份,在60-75℃环境下反应1-3小时,得到聚氨酯预聚物;
2)B组份,制备方法如下:以质量份计,催化剂0.1-0.8份、发泡剂0.5-5份、泡沫稳定剂0.5-5份,按比例称量,均匀混合;
3)聚氨酯泡沫制备方法:将A组份和B组份在50-75℃下高速搅拌混合5-15s,立即浇注到温度为30-50℃的模具中,在30-50℃环境下熟化4-6小时,脱模后在室温下进一步熟化24-48h,得到聚氨酯泡沫。
2.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,A组分中所述的聚碳酸酯二元醇数均分子量在1000-4000,为一种或几种不同数均分子量聚碳酸酯二元醇的混合物。
3.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,A组分中所述的异氰酸酯为甲苯二异氰酸酯TDI-100、TDI-80中的一种或两种的混合物。
4.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,A组份中所述的扩链剂为醇类扩链剂和胺类扩链剂,醇类扩链剂为1,4-丁二醇、一缩丙二醇、1,6-己二醇、新戊二醇、二缩三丙二醇、1,5-戊二醇,胺类扩链剂4,4′-二氨基-3,3′-二乙基-二苯基甲烷,3-氯-3’-乙基-4,4’-二氨基二苯甲烷,3,3’二氯-4,4’-二氨基二苯甲烷,二乙基甲苯二胺(DETDA),二甲硫基甲苯二胺DMTDA,A组份中所述的扩链剂为醇类扩链剂和胺类扩链剂中的一种或几种的混合物。
5.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,A组份预聚体中异氰酸基团含量为4%-12%。
6.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,B组份中所述的发泡剂为去离子水。
7.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,B组份中所述的催化剂的组合为胺类催化剂和锡类催化剂的混合物,胺类催化剂为乙二胺、三乙基胺、三甲基胺、N-甲基吗啉、N-乙基吗啉、N,N-二甲基苄胺,锡类催化剂为:辛酸亚锡、二月桂酸二丁基锡、二月桂酸二辛基锡、二油酸二丁基锡、醋酸锡、二醋酸二丁基锡、二醋酸二甲基锡、草酸亚锡。
8.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,B组份中所述的泡沫稳定剂为有机硅酮表面活性剂,有机硅酮表面活性剂的摩尔质量2000g/mol,其中聚醚在硅酮表面活性剂中的含量为30%,聚醚中环氧乙烷/环氧丙烷比例为1/1,并且聚醚是丁基封端,封端率为95%。
9.根据权利要求1所述的聚酯型聚氨酯泡沫的制备方法,其特征在于,制备的聚酯型聚氨酯泡沫密度为70-320kg/m3。
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