CN112831018B - 无溶剂合成革聚氨酯组合料及其制备方法 - Google Patents

无溶剂合成革聚氨酯组合料及其制备方法 Download PDF

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CN112831018B
CN112831018B CN202011633765.0A CN202011633765A CN112831018B CN 112831018 B CN112831018 B CN 112831018B CN 202011633765 A CN202011633765 A CN 202011633765A CN 112831018 B CN112831018 B CN 112831018B
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孙清峰
甘经虎
郭勇生
燕杰善
崔玉志
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Abstract

本发明涉及无溶剂合成革技术领域,具体涉及一种无溶剂聚氨酯合成革组合料及其制备方法。本发明所述的无溶剂合成革组合料,由A组分和B组分按100:40‑50的重量比混合组成;A组分为:聚酯多元醇、聚醚多元醇、聚酯醚、硬化剂、发泡剂、增稠剂、泡沫稳定剂、催化剂;B组分为聚酯改性MDI。本发明的无溶剂聚氨酯合成革组合料,生产和使用过程无溶剂,安全环保;同时制备的合成革涂层兼具聚酯和聚醚体系的优点,得到的制品不仅重量轻,而且力学性能优异、耐水解性能好。

Description

无溶剂合成革聚氨酯组合料及其制备方法
技术领域
本发明涉及聚氨酯合成革技术领域,具体涉及一种无溶剂合成革聚氨酯组合料及其制备方法。
背景技术
聚氨酯合成革属于聚氨酯微孔弹性体的一类,具有光泽柔和、自然,手感柔软,真皮感强的外观,具有与基材粘接性能优异、抗磨损、耐挠曲、抗老化等优异的机械性能,同时还具备耐寒性好、透气、可洗涤、加工方便、价格优廉等优点,是天然皮革的最为理想的替代品,广泛应用于服装、制鞋、箱包、家具等行业。
目前,聚氨酯合成革的生产还是采用溶剂型聚氨酯,在聚氨酯的生产和制造过程中都会用到大量的溶剂,如DMF、甲苯和丁酮等。不仅合成革生产过程中会造成溶剂污染,而且会引起产品的溶剂残留问题,从而限制产品进入高档市场领域。
为了解决聚氨酯合成革生产时的溶剂污染问题,目前主要采用水性聚氨酯或无溶剂聚氨酯替代溶剂型聚氨酯生产合成革。
专利CN201711500719.1中公开了一种无溶剂革用聚氨酯树脂及制备方法和应用,A组分含有重量百分比为30%~45%的聚醚酯多元醇-多异氰酸酯预聚体、重量百分比50%~65%的聚醚多元醇A和重量百分比0.3%~2.0%的水,B组分含有重量百分比为20%~60%的二异氰酸酯。该发明的无溶剂合成革的聚氨酯树脂在生产合成革时只需刮涂一刀无溶剂树脂,即可拥有面层、粘结层和发泡层结构,工艺过程简单,且物理机械性能优。但是其A组分和B组分只是简单的混合,使得无溶剂合成革的聚氨酯树脂的粘结力欠佳,进而造成聚氨酯树脂的剥离强度低。
专利CN201910676667.6中公开了一种无溶剂合成革用聚氨酯树脂及其制备方法,包含主剂A组分和固化剂B组分,主剂A组分由聚醚多元醇3000、聚醚多元醇2000、MDI-50、二甘醇组成;固化剂B组分由MDI-50、六亚甲基二异氰酸酯、二甘醇、有机催化剂组成;其提高了制备的无溶剂合成革用聚氨酯树脂的粘结力以及剥离强度。但是其耐水解性能不佳,且成膜时间较短,不利于操作。
发明内容
本发明的目的是提供一种无溶剂合成革聚氨酯组合料,生产和使用过程中均不使用无溶剂,同时由该组合料制备的无溶剂合成革兼具聚酯和聚醚体系的优点,得到的制品不仅重量轻(0.5-0.6g/cm3),而且力学性能优异、耐水解性能好,粘结性能好;本发明还提供其制备方法。
本发明所述的无溶剂合成革聚氨酯组合料,由A组分和B组分按100:40-50的重量比混合组成;
以质量百分数计,A组分为:
Figure BDA0002877706740000021
B组分为聚酯改性MDI,其NCO含量为8-12wt%。
聚酯多元醇的官能度为2,羟值为28-32mgKOH/g,数均分子量为4000;优选山东一诺威聚氨酯股份有限公司的PE2445。
聚醚多元醇为氧化乙烯封端的聚氧化丙烯三醇,官能度为4.5,数均分子量为8000-9000;优选蓝星东大的8005。
聚酯醚的官能度为2,羟值为80-100mgKOH/g,酸值≤0.05mgKOH/g;优选山东一诺威新材料有限公司的3500T。
硬化剂为官能度2,分子量400-600的小分子聚醚多元醇;优选蓝星东大的DL400。
增稠剂为气相白炭黑;优选赢创的疏水性R200。
发泡剂为水。
泡沫稳定剂为低雾化的聚硅氧烷-氧化烯烃嵌段共聚物,优选赢创的DC193。
催化剂为热敏性催化剂,优选赢创的SA-8。
聚酯改性MDI通过聚酯多元醇跟纯MDI、液化MDI在一定的温度下反应制得;优选山东一诺威聚氨酯股份有限公司的DXD-3310B。
本发明所述的无溶剂合成革聚氨酯组合料,步骤如下:
(1)A组分料:先将基于配方量的聚酯多元醇、聚醚多元醇、聚酯醚多元醇、硬化剂、增稠剂、发泡剂、泡沫稳定剂以及催化剂投入反应釜中搅拌,升温到50-60℃,在室温条件下,转速为40-50转/分钟,搅拌0.5-1.0小时,即得A组分;
(2)使用时,将A组分和B组分按质量比100:40-50混合均匀,然后滚涂到离型纸上,放入100-150℃烘箱中,待涂层开始乳白时,拿出烘箱覆盖无纺布,继续放入100-150℃烘箱熟化3-5min,即可得到无溶剂聚氨酯合成革。
与现有技术相比,本发明有以下有益效果:
(1)本发明在生产和使用过程中均无溶剂,安全环保;
(2)本发明采用聚醚多元醇和聚酯多元醇结合,聚醚多元醇、聚酯醚、聚酯多元醇相互协同作用,在降低制品重量的同时,保证了其依然具有较好的力学性能和耐水解性能;
(3)本发明采用气相白炭黑作为增稠剂,在不影响发泡的情况下,提高组合料的触变性,做涂层时流挂性好,不流淌;
(4)本发明采用热敏性催化剂延长了组合料的操作时间。
具体实施方式
以下结合实施例说明本发明,但不限定本发明。
实施例1
按以下原料配比和方法制备电池用发泡聚氨酯密封胶:
A组分为:
Figure BDA0002877706740000031
B组分为:
DXD-3310B 100kg。
称取60kg的PE2445,15kg的8005、15.5kg的3500T、5kg的DL400、3kg的R200、0.3kgH2O、1.0kgDC193以及0.5kg的SA-8投入反应釜中搅拌,升温到50℃,转速为40转/分钟,搅拌0.5小时,即得A组分;
将A组分和B组分(DXD-3310B)按质量比100:50混合均匀,然后滚涂到离型纸上,放入100-150℃烘箱中,待涂层开始乳白时,拿出烘箱覆盖无纺布,继续放入100-150℃烘箱熟化3-5min,即可得到无溶剂聚氨酯合成革。
实施例2
按以下原料配比和方法制备电池用发泡聚氨酯密封胶:
A组分为:
Figure BDA0002877706740000041
B组分为:
DXD-3310B 100kg。
称取54.8kg的PE2445,20kg的8005、20kg的3500T、3kg的DL400、1kg的R200、0.5kgH2O、0.5kgDC193以及0.2kg的SA-8投入反应釜中搅拌,升温到60℃,转速为50转/分钟,搅拌1小时,即得A组分;
将A组分和B组分(DXD-3310B)按质量比100:40混合均匀,然后滚涂到离型纸上,放入100-150℃烘箱中,待涂层开始乳白时,拿出烘箱覆盖无纺布,继续放入100-150℃烘箱熟化3-5min,即可得到无溶剂聚氨酯合成革。
实施例3
按以下原料配比和方法制备电池用发泡聚氨酯密封胶:
A组分为:
Figure BDA0002877706740000042
B组分为:
DXD-3310B 100kg。
称取50kg的PE2445,18kg的8005、18kg的3500T、10kg的DL400、2.4kg的R200、0.4kgH2O、0.8kgDC193以及0.4kg的SA-8投入反应釜中搅拌,升温到55℃,转速为55转/分钟,搅拌50min,即得A组分;
将A组分和B组分(DXD-3310B)按质量比100:50混合均匀,然后滚涂到离型纸上,放入100-150℃烘箱中,待涂层开始乳白时,拿出烘箱覆盖无纺布,继续放入100-150℃烘箱熟化3-5min,即可得到无溶剂聚氨酯合成革。
对比例1
本对比例与实施例3相比,不同点仅在于将A组分中聚醚多元醇8005、聚酯醚3500T全部替换为同等质量的聚酯多元醇PE2445。
对比例2
本对比例与实施例3相比,不同点仅在于将A组分中聚醚多元醇8005全部替换为同等质量的聚酯多元醇PE2445。
对比例3
本对比例与实施例3相比,不同点仅在于将A组分中聚醚多元醇8005替换为同等质量的聚醚多元醇330NG(分子量5000,官能度为3)。
对比例4
本对比例与实施例3相比,不同点仅在于将A组分中聚酯醚3500T替换为同等质量的聚醚多元醇330NG。
对比例5
本对比例与实施例3相比,不同点仅在于将A组分中硬化剂DL400替换为同等质量的乙二醇。
对比例6
本对比例与实施例3相比,不同点仅在于将A组分中气相白炭黑替换为同等质量亲水性SiO2
对比例7
本对比例与实施例3相比,不同点仅在于将A组分中热敏性催化剂SA-8替换为延迟性催化剂8154。
将实施例1-3和对比例1-7制得的无溶剂合成革进行性能测试,其中芯密度按照GB/T 6343-1995标准检测,断裂伸长率、拉伸强度按照GB/T6344-1996标准检测,撕裂强度按照GB/T 10808-2006标准检测,耐水解时间:在温度85℃,湿度85%条件下,力学性能保持在90%以上的时间。
测试结果如表1所示。
表1实施例1-3和对比例1-7制得的电池用发泡聚氨酯密封胶的性能测试结果
Figure BDA0002877706740000061
从表1可以看出,本发明的实施例1-3兼具了聚醚体系和聚酯体系的优点,在较低密度时,制品依然具有良好的力学性能和耐水解性能,对比例1-5对A组分中的聚醚多元醇、聚酯多元醇、聚酯醚、硬化剂进行了不同的替换,制备的产品在与实施例3密度基本一致的条件下,无法兼具良好的力学性能和耐水解性能;对比例6可以看出采用疏水性增稠剂以后,发泡正常,涂层不流淌;对比例7可以看出使用热敏性催化剂极大的延长了操作时间。

Claims (3)

1.一种无溶剂合成革聚氨酯组合料,其特征在于:由A组分和B组分按100:40-50的重量比混合组成;
以质量百分数计,A组分为:
Figure FDA0003526771250000011
B组分为聚酯改性MDI,其NCO含量为8-12wt%;
聚酯多元醇的官能度为2,羟值为28-32mgKOH/g,数均分子量为4000;
聚醚多元醇为氧化乙烯封端的聚氧化丙烯三醇,官能度为4.5,数均分子量为8000-9000;
聚酯醚的官能度为2,羟值为80-100mgKOH/g,酸值≤0.05mgKOH/g;
硬化剂为官能度2,分子量400-600的小分子聚醚多元醇;
增稠剂为气相白炭黑;
催化剂为热敏性催化剂。
2.根据权利要求1所述的无溶剂合成革聚氨酯组合料,其特征在于:发泡剂为水;泡沫稳定剂为聚硅氧烷-氧化烯烃嵌段共聚物。
3.一种权利要求1或2所述的无溶剂合成革聚氨酯组合料的制备方法,其特征在于:步骤如下:
(1)A组分料:先将基于配方量的聚酯多元醇、聚醚多元醇、聚酯醚、硬化剂、增稠剂、发泡剂、泡沫稳定剂以及催化剂投入应釜中搅拌,升温到50-60℃,在室温条件下,转速为40-50转/分钟,搅拌0.5-1.0小时,即得A组分;
(2)使用时,将A组分和B组分按质量比100:40-50混合均匀,然后滚涂到离型纸上,放入100-150℃烘箱中,待涂层开始乳白时,拿出烘箱覆盖无纺布,继续放入100-150℃烘箱熟化3-5min,即可得到无溶剂聚氨酯合成革。
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