CN109575866A - 一种湿固化聚氨酯热熔胶的制备方法 - Google Patents
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Abstract
本发明涉及本发明涉及一种湿固化聚氨酯热熔胶的制备方法,特别是一种适于家电领域粘接复合用的、具有流动性好且快速定位效果的单组份湿固化聚氨酯热熔胶的制备方法。步骤包括:(1)按预设比例,将聚醚多元醇、液态聚酯多元醇、固态聚酯多元醇,和抗氧剂加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;(2)降温至100℃,加入4,4’‑二苯基甲烷二异氰酸酯,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;(3)}加入硅烷偶联剂和催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;(4)氮气保护下快速出料,并封装于铝箔袋中即得。
Description
技术领域
本发明涉及一种湿固化聚氨酯热熔胶的制备方法,特别是一种适于家电领域粘接复合用的单组份湿固化聚氨酯热熔胶的制备方法。
背景技术
湿固化聚氨酯热熔胶是一类含有异氰酸酯端基的聚氨酯胶粘剂,应用时,先将其加热熔融后施胶,待胶层冷却物理固化后产生初步的粘接力,胶层中的端异氰酸酯基团再与空气中的湿气或被粘接基材表面的活泼氢物质发生化学反应,产生交联固化。所以,湿固化聚氨酯热熔胶不仅具有传统热塑性热熔胶的粘接性能,还能在交联固化后产生更高的内聚强度,具有优异的耐热性和耐候性。
其中,用于家电领域的湿固化聚氨酯热熔胶,一般是用来粘接ABS塑料和/或木材,这两类材料相对比较容易粘接,故其对胶粘剂粘接强度的要求不是特别高,一般该领域要求胶粘剂有较低的黏度,使其在施胶应用时具有较好的流动性,目前常规用于该领域的湿固化聚氨酯热熔胶在100℃的黏度在20000左右甚至更高;同时,该领域还要求胶粘剂有快速定位的特点,已达到高效生产的工艺需求,这就意味着胶粘剂的开放时间不能太长,目前常规用于该领域的湿固化聚氨酯热熔胶的开放时间普遍>45s。
而常规的配料体系中,产物的黏度越低,虽然流动性越好,但一般开放时间也越长,平衡难以保障。故,如何提供一种适于家电领域应用的,同时具备较低黏度和较短开放时间的湿固化聚氨酯热熔胶,成为待解决的问题。
发明内容
本发明的目的在于,解决上述技术问题,提供一种湿固化聚氨酯热熔胶的制备方法,使得通过本发明制备所得的湿固化聚氨酯热熔胶,同时具备较低黏度和较短开放时间的平衡特性,具有流动性好且快速定位的效果。
本发明所采用的技术方案为:一种湿固化聚氨酯热熔胶的制备方法,步骤如下:
(1)按预设比例,将聚醚多元醇、液态聚酯多元醇、固态聚酯多元醇,和抗氧剂加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;
(2)降温至100℃,加入4,4’-二苯基甲烷二异氰酸酯,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;
(3)加入硅烷偶联剂和催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;
(4)氮气保护下快速出料,并封装于铝箔袋中。
上述步骤(1)~(3)中,所有物料均以质量份数计,具体为:聚醚多元醇15~30份,液态聚酯多元醇18.5~25份,固态聚酯多元醇33~45份,抗氧剂0.2~0.5份,4,4’-二苯基甲烷二异氰酸酯15.2~17.75份,硅烷偶联剂0.5~1.5份,催化剂0.05~0.1份。
同时,聚醚多元醇具体为聚氧化丙烯二醇,其数均分子量为1000;
液态聚酯多元醇由聚己二酸新戊二醇酯二醇和己二酸/乙二醇/二甘醇共聚物混合而成,且聚己二酸新戊二醇酯二醇和己二酸/乙二醇/二甘醇共聚物的数均分子量均为2000;
固态聚酯多元醇由聚己二酸己二醇酯二醇和聚十二烷二酸己二醇酯二醇混合而成,且聚己二酸己二醇酯二醇的用量≥聚十二烷二酸己二醇酯二醇的用量;聚己二酸己二醇酯二醇的数均分子量为3000,聚十二烷二酸己二醇酯二醇的数均分子量为3500;
抗氧剂的牌号为1010;
硅烷偶联剂为γ-缩水甘油醚氧丙基三甲氧基硅烷;
催化剂为双吗啉基乙基醚,在本发明中,催化剂在反应即将结束时加入,其主要是催化产物于后期应用时与水汽的反应,增强交联,以达成较好的最终粘接效果。
本发明的创新之处及有益效果在于:设计了独特的原料配比及对应的制备步骤,特别是两种型态的聚酯多元醇的量选,以及催化剂的选定和加入时机,使得通过本发明制备所得的湿固化聚氨酯热熔胶,在100℃的黏度<11000,开放时间≤40s,具有较好的流动性和快速定位的效果,非常适于家电领域应用。
具体实施方式
下面通过实施例对本发明做进一步表述,但并不以此为限。
本发明中各实施例所涉及的原料信息如下:
聚醚多元醇:聚氧化丙烯二醇,数均分子量1000,简称LM1000;
液态聚酯多元醇:聚己二酸新戊二醇酯二醇,数均分子量2000,简称XCP-2000N;
液态聚酯多元醇你:己二酸/乙二醇/二甘醇共聚物,数均分子量2000,简称XCP-2016;
固态聚酯多元醇:聚己二酸己二醇酯二醇,数均分子量3000,简称XCP-3000H;
固态聚酯多元醇:聚十二烷二酸己二醇酯二醇,顺军分子量3500,简称C3002;
4,4’-二苯基甲烷二异氰酸酯:水白色固体,简称MDI。
实施例1:
一种湿固化聚氨酯热熔胶的制备方法,步骤如下:
(1)将30份LM1000、10份XCP-2000N、8.5份XCP-2016、25份XCP-3000H、8份C3002,和0.2份抗氧剂,加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;
(2)降温至100℃,加入17.75份MDI,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;
(3)加入0.5份硅烷偶联剂和0.05份催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;
(4)氮气保护下快速出料,并封装于铝箔袋中。
通过实施例1制备所得产物样品标记为A1。
实施例2:
(1)将15份LM1000、15份XCP-2000N、7.9份XCP-2016、30份XCP-3000H、15份C3002,和0.5份抗氧剂,加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;
(2)降温至100℃,加入16份MDI,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;
(3)加入1.5份硅烷偶联剂和0.1份催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;
(4)氮气保护下快速出料,并封装于铝箔袋中。
通过实施例2制备所得产物样品标记为A2。
实施例3:
(1)将18份LM1000、8份XCP-2000N、12份XCP-2016、35份XCP-3000H、10份C3002,和0.5份抗氧剂,加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;
(2)降温至100℃,加入15.2份MDI,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;
(3)加入1.5份硅烷偶联剂和0.1份催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;
(4)氮气保护下快速出料,并封装于铝箔袋中。
通过实施例3制备所得产物样品标记为A3。
实施例4:
(1)将16份LM1000、5份XCP-2000N、20份XCP-2016、20份XCP-3000H、20份C3002,和0.5份抗氧剂,加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;
(2)降温至100℃,加入17.2份MDI,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;
(3)加入1.2份硅烷偶联剂和0.1份催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;
(4)氮气保护下快速出料,并封装于铝箔袋中。
通过实施例4制备所得产物样品标记为A4。
性能测试:
将上述各实施例所得产物样品进行测试表征,其中,黏度测试参考GB/T 2749,开放时间测试参靠公司企业标准。
结果如下表1所示:
标记 | 黏度(mPa.s/100℃) | 开放时间(s) |
A1 | 8900 | 40 |
A2 | 10040 | 35 |
A3 | 9125 | 32 |
A4 | 9980 | 37 |
表1:测试结果。
Claims (6)
1.一种湿固化聚氨酯热熔胶的制备方法,其特征在于,包括如下步骤:
(1)按预设比例,将聚醚多元醇、液态聚酯多元醇、固态聚酯多元醇,和抗氧剂加入到反应釜中,搅拌均匀,加热升温至120℃~130℃,在真空度<100Pa条件下脱水2h;
(2)降温至100℃,加入4,4’-二苯基甲烷二异氰酸酯,搅拌,在真空度<100Pa、温度115℃~120℃条件下反应1h;
(3)加入硅烷偶联剂和催化剂,在真空度<100Pa、温度115℃~120℃条件下反应0.5h;
(4)氮气保护下快速出料,并封装于铝箔袋中即得;
所述步骤(1)~(3)中,所有物料均以质量份数计,具体为:
聚醚多元醇15~30份,液态聚酯多元醇18.5~25份,固态聚酯多元醇33~45份,抗氧剂0.2~0.5份,4,4’-二苯基甲烷二异氰酸酯15.2~17.75份,硅烷偶联剂0.5~1.5份,催化剂0.05~0.1份;且所述液态聚酯多元醇由聚己二酸新戊二醇酯二醇和己二酸/乙二醇/二甘醇共聚物混合而成;所述固态聚酯多元醇由聚己二酸己二醇酯二醇和聚十二烷二酸己二醇酯二醇混合而成。
2.如权利要求1所述的湿固化聚氨酯热熔胶的制备方法,其特征在于:所述聚己二酸新戊二醇酯二醇和所述己二酸/乙二醇/二甘醇共聚物的数均分子量均为2000。
3.如权利要求1所述的湿固化聚氨酯热熔胶的制备方法,其特征在于:所述聚己二酸己二醇酯二醇的用量≥所述聚十二烷二酸己二醇酯二醇的用量。
4.如权利要求3所述的湿固化聚氨酯热熔胶的制备方法,其特征在于:所述聚己二酸己二醇酯二醇的数均分子量为3000,聚十二烷二酸己二醇酯二醇的数均分子量为3500。
5.如权利要求1所述的湿固化聚氨酯热熔胶的制备方法,其特征在于:所述催化剂为双吗啉基乙基醚。
6.如权利要求3所述的湿固化聚氨酯热熔胶的制备方法,其特征在于:所述抗氧剂的牌号为1010;所述硅烷偶联剂为γ-缩水甘油醚氧丙基三甲氧基硅烷。
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