CN114957598B - 一种低熔点高硬度tpu及其制备方法 - Google Patents
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Abstract
本发明属于聚氨酯弹性体领域,涉及一种低熔点高硬度TPU及其制备方法。通过在扩链剂组分引入双酚芴类衍生物,并在特定组成(双酚芴衍生物与仲胺的质量比为1~9:1)协同作用下,采用双螺杆挤出机一步法反应制得。所述TPU熔点在60‑100℃,硬度高达55‑80D,同时兼具优异的溶解性和耐磨性,特别适用于油墨、磨粉、底漆领域。
Description
技术领域
本发明为聚氨酯领域,涉及一种低熔点高硬度热塑性聚氨酯(TPU)的制备及应用。
背景技术
热塑性聚氨酯(TPU)由于其线性结构,可通过热熔或溶解进行加工,性能介于橡胶与塑料之间,硬度范围在55A-80D。
通常高硬度与低熔点是相矛盾的性能。专利CN 108976380公布了一种低熔点快成型热塑性聚氨酯,通过软段结晶可得到低熔点的TPU,但其硬度通常在58D以下,且Tg低于-30℃。专利CN 110922557公布了一种高硬度热塑性聚氨酯,其通过引入一元醇组分,在特定组成下得到超硬的TPU,但其熔点远高于140℃。
油墨、磨粉、底漆等特定领域通常希望TPU加工方便,如低熔点、易溶解、高Tg。因此,上述问题的存在限制了TPU在油墨、磨粉、底漆等特定领域的使用。
发明内容
本发明的目的是提供一种低熔点高硬度的TPU,解决传统TPU高硬度与低熔点难以兼得的问题。
为达到上述目的,本发明提供一种低熔点高硬度TPU,其包含下述重量份的组分组成:
a)多元醇50~80份
b)二异氰酸酯15~40份
c)扩链剂5~10份;
所述扩链剂为双酚芴衍生物与仲胺的混合物。
其中,双酚芴衍生物具有如下结构式:
R1、R2为相互独立的羟基(-OH)、线性或支化烷羟基醚(-O-CnH2n-OH,n=1~4)。
进一步的,所述多元醇组分的数均分子量优选为500-3000g/mol,可以是聚酯多元醇、聚醚多元醇、聚己内酯多元醇或其组合物。
所述聚酯多元醇是由己二酸与二元醇通过行业公知的聚酯多元醇合成工艺制得,或者是聚碳酸酯多元醇;
其中所述二元醇选自乙二醇、二乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、一缩二乙二醇、一缩二丙二醇、新戊二醇、3-甲基-1,5-戊二醇、甲基丙二醇中的任意一种或至少两种的组合,优选为聚己二酸乙二醇(PEBA)酯、聚己二酸乙二醇酯(PEA)、聚己二酸新戊二醇酯(PNA)中的任意一种或至少两种的组合。
所述聚醚多元醇是以含活泼氢化合物作为起始剂与环氧化合物开环聚合制得;
其中所述含活泼氢化合物选自乙二醇、一缩二乙二醇、1,2-丙二醇中的任意一种或至少两种的组合,优选1,2-丙二醇;
所述环氧化合物选自环氧丙烷、四氢呋喃、环氧乙烷中的任意一种或至少两种的组合,优选四氢呋喃。
所述聚己内酯多元醇是以小分子醇作为起始剂与ε-己内酯开环聚合制得;
所述小分子醇起始剂选自乙二醇、1,4-丁二醇、新戊二醇中任意一种或至少两种的组合,优选新戊二醇。
进一步的,所述二异氰酸酯组分可以是芳香族二异氰酸酯、脂肪族二异氰酸酯或其组合物;
所述芳香族二异氰酸酯包括二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、对苯二异氰酸酯中一种或多种,优选二苯基甲烷二异氰酸酯(MDI);
所述脂肪族二异氰酸酯包括六亚甲基二异氰酸酯、4,4-二环己基甲烷二异氰酸酯、异氟尔酮二异氰酸酯、环己烷二亚甲基二异氰酸酯中一种或多种,优选异氟尔酮二异氰酸酯(IPDI)。
进一步的,所述扩链剂组分中双酚芴衍生物与仲胺的质量比为(1~9):1,优选(3~6):1;
所述仲胺包括4,4-双仲丁氨基二苯基甲烷、1,4-双仲丁氨基苯、聚天门冬胺中一种或多种。
进一步的,本发明还提供所述低熔点高硬度TPU的制备方法,可采用一步法,将多元醇、二异氰酸酯、扩链剂按配方比例混合均匀,再经双螺杆反应挤出、造粒、干燥制得。挤出温度100-200℃,优选140-180℃。造粒水温5-30℃,优选10-20℃。干燥温度30-50℃。
本发明的低熔点高硬度TPU熔点在60-100℃,硬度高达55-80D,可以应用在油墨、磨粉、底漆等领域。
本发明的特点和有益效果在于:扩链剂组分为双酚芴类衍生物与仲胺协同组合,在特定组合配比下得到兼具低熔点、高硬度的TPU树脂,同时兼具优异的溶解性和耐磨性,特别适用于油墨、磨粉、底漆领域。
具体实施方式
下面通过具体的实施例对本发明的技术方案作进一步的说明。
原料来源:
双酚芴衍生物(R1,R2为-OH):美国Sigma-Aldrich公司。
双酚芴衍生物(R1,R2为-OCH2CH2OH):上海麦克林生化科技有限公司。
仲胺(4,4-双仲丁氨基二苯基甲烷):万华化学集团股份有限公司。
仲胺(1,4-双仲丁氨基苯):美国Hanson公司。
仲胺(聚天门冬胺):Desmophen NH1220、Desmophen NH1420、Desmophen NH1520,德国科思创公司。
六亚甲基二异氰酸酯(HDI)、二苯基甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(T-80)、4,4-二环己基甲烷二异氰酸酯(HMDI)、异氟尔酮二异氰酸酯(IPDI),万华化学集团股份有限公司;
聚己二酸乙二醇丁二醇酯(PEBA):数均分子量2000g/mol,万华化学集团股份有限公司;
聚己二酸新戊二醇酯(PNA):数均分子量1000g/mol,万华化学集团股份有限公司;
聚己二酸乙二醇酯(PEA):数均分子量2500g/mol,万华化学集团股份有限公司;
聚己内酯(NPG-PCL):数均分子量2000g/mol,日本大赛璐有机合成公司;
聚四氢呋喃醚二醇:数据分子量2000g/mol,德国BASF公司。
实施例1
一种低熔点高硬度TPU,其原料组成及重量比如下:
A)多元醇65份:聚己二酸乙二醇丁二醇酯(PEBA),数均分子量2000g/mol。
B)二异氰酸酯27份:六亚甲基二异氰酸酯(HDI)。
C)扩链剂8份:双酚芴衍生物(R1,R2为-OH)、仲胺(4,4-双仲丁氨基二苯基甲烷),两者重量比5:1。
采用一步法将上述组成混合均匀,再经双螺杆反应挤出制得TPU,挤出温度140℃,造粒温度10℃,干燥温度30℃。
实施例2
一种低熔点高硬度TPU,其原料组成及重量比如下:
A)多元醇50份:聚己二酸乙二醇酯(PEA),数均分子量2500g/mol。
B)二异氰酸酯40份:甲苯二异氰酸酯(T-80)。
C)扩链剂10份:双酚芴衍生物(R1,R2为-OH)、仲胺(1,4-双仲丁氨基苯),两者重量比3:1。
采用一步法将上述组成混合均匀,再经双螺杆反应挤出制得TPU,挤出温度160℃,造粒温度15℃,干燥温度35℃。
实施例3
一种低熔点高硬度TPU,其原料组成及重量比如下:
A)多元醇80份:聚己二酸新戊二醇酯(PNA),数均分子量1000g/mol。
B)二异氰酸酯15份:二苯基甲烷二异氰酸酯(MDI)。
C)扩链剂5份:双酚芴衍生物(R1,R2为-OH)、仲胺(聚天门冬胺,DesmophenNH1220),两者重量比6:1。
采用一步法将上述组成混合均匀,再经双螺杆反应挤出制得TPU,挤出温度180℃,造粒温度20℃,干燥温度40℃。
实施例4
一种低熔点高硬度TPU,其原料组成及重量比如下:
A)多元醇75份:聚己内酯多元醇(NPG-PCL),数均分子量2000g/mol。
B)二异氰酸酯17份:4,4-二环己基甲烷二异氰酸酯(HMDI)。
C)扩链剂8份:双酚芴衍生物(R1,R2为-OCH2CH2OH)、仲胺(聚天门冬胺,DesmophenNH1420),两者重量比4:1。
采用一步法将上述组成混合均匀,再经双螺杆反应挤出制得TPU,挤出温度175℃,造粒温度15℃,干燥温度35℃。
实施例5
一种低熔点高硬度TPU,其原料组成及重量比如下:
A)多元醇57份:聚四氢呋喃醚二元醇(PTMG),数均分子量2000g/mol。
B)二异氰酸酯35份:异氟尔酮二异氰酸酯(IPDI)。
C)扩链剂8份:双酚芴衍生物(R1,R2为-OCH2CH2OH)、仲胺(聚天门冬胺,DesmophenNH1520),两者重量比4:1。
采用一步法将上述组成混合均匀,再经双螺杆反应挤出制得TPU,挤出温度200℃,造粒温度20℃,干燥温度50℃。
对比例1
参照实施例1方法制备TPU,不同之处仅在于扩链剂组分替换为等重量单独的双酚芴衍生物(R1,R2为-OH),其他原料及用量不变,制得TPU。
对比例2
参照实施例1方法制备TPU,不同之处仅在于扩链剂组分替换为等重量单独的仲胺(4,4-双仲丁氨基二苯基甲烷),其他原料及用量不变,制得TPU。
对比例3
参照实施例1方法制备TPU,不同之处仅在于扩链剂组分中双酚芴衍生物(R1,R2为-OH)与仲胺(4,4-双仲丁氨基二苯基甲烷)重量比为20:1,其他原料及用量不变,制得TPU。
分别对上述TPU样品进行硬度、熔点、溶解性、磨耗进行测试。
测试项目 | 硬度/shore D | 熔点/℃ | 15wt%乙酸乙酯溶解性 | 磨耗/mm3 |
测试方法 | ASTM D2240 | 毛细管流变仪 | 静置24h观察 | ISO 4649 |
实施例1 | 76 | 75 | 可溶 | 15 |
实施例2 | 80 | 85 | 可溶 | 10 |
实施例3 | 75 | 70 | 可溶 | 20 |
实施例4 | 77 | 80 | 可溶 | 25 |
实施例5 | 78 | 82 | 可溶 | 20 |
对比例1 | 70 | 185 | 不溶 | 30 |
对比例2 | 35 | 120 | 不溶 | 65 |
对比例3 | 60 | 160 | 不溶 | 50 |
根据本发明制备的TPU具有低熔点、高硬度的特征,同时具备优异的溶解性和耐磨性。
Claims (12)
2.根据权利要求1所述的低熔点高硬度TPU,其中,多元醇是聚酯多元醇、聚醚多元醇中的至少一种。
3.根据权利要求2所述的低熔点高硬度TPU,其中,所述多元醇的数均分子量为500-3000g/mol。
4.根据权利要求2所述的低熔点高硬度TPU,其中,所述聚酯多元醇是聚碳酸酯多元醇,或聚己内酯多元醇,或由己二酸与二元醇制得,其中所述二元醇选自乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、一缩二乙二醇、一缩二丙二醇、新戊二醇、3-甲基-1,5-戊二醇、甲基丙二醇中的至少一种。
5.根据权利要求2所述的低熔点高硬度TPU,其中,所述聚醚多元醇是以含活泼氢化合物作为起始剂与环氧化合物开环聚合制得;
其中所述含活泼氢化合物选自乙二醇、一缩二乙二醇、1,2-丙二醇中的至少一种;所述环氧化合物选自环氧丙烷、四氢呋喃、环氧乙烷中的至少一种。
6.根据权利要求4所述的低熔点高硬度TPU,其中,所述聚己内酯多元醇是以小分子醇作为起始剂与ε-己内酯开环聚合制得;
所述小分子醇选自乙二醇、1,4-丁二醇、新戊二醇中的至少一种。
7.根据权利要求1所述的低熔点高硬度TPU,其中,二异氰酸酯组分是芳香族二异氰酸酯、脂肪族二异氰酸酯中的至少一种。
8.根据权利要求7所述的低熔点高硬度TPU,其中,所述芳香族二异氰酸酯包括二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、对苯二异氰酸酯中的至少一种;
所述脂肪族二异氰酸酯包括六亚甲基二异氰酸酯、4,4-二环己基甲烷二异氰酸酯、异氟尔酮二异氰酸酯、环己烷二亚甲基二异氰酸酯中的至少一种。
9.根据权利要求1所述的低熔点高硬度TPU,其中扩链剂组分双酚芴衍生物与仲胺的质量比为3~6:1。
10.根据权利要求1-9任一项所述的低熔点高硬度TPU的制备方法,采用一步法,将多元醇、二异氰酸酯、扩链剂混合均匀,再经双螺杆挤出、造粒、干燥制得TPU树脂颗粒。
11.根据权利要求10所述的制备方法,其中,挤出温度100-200℃,造粒水温5-30℃,干燥温度30-50℃。
12.根据权利要求1-9任一项所述的低熔点高硬度TPU在油墨、磨粉、底漆领域的应用。
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