CN114231019B - 一种高耐磨抗腐蚀洗地机聚氨酯轮胎 - Google Patents

一种高耐磨抗腐蚀洗地机聚氨酯轮胎 Download PDF

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CN114231019B
CN114231019B CN202111522920.6A CN202111522920A CN114231019B CN 114231019 B CN114231019 B CN 114231019B CN 202111522920 A CN202111522920 A CN 202111522920A CN 114231019 B CN114231019 B CN 114231019B
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史春晓
史玉林
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Anhui Yulin New Material Technology Co ltd
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Abstract

本发明涉及一种高耐磨抗腐蚀洗地机聚氨酯轮胎，属于聚氨酯技术领域，该聚氨酯轮胎通过如下步骤制备：第一步、将聚酯多元醇、扩链剂和异氰酸酯混合，搅拌反应，然后加入端羟基液体橡胶、催化剂，搅拌得到A组分；第二步、将聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯混合，加热反应，得到低聚物，然后依次加入异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂、抗水解剂，搅拌得到B组分；第三步、将A组分和B组分混合，灌注于轮胎模具中固化后得到一种高耐磨抗腐蚀洗地机聚氨酯轮胎。加入的扩链剂和抗水解剂，提高材料的强度、抗水解，对提高该高耐磨抗腐蚀洗地机聚氨酯轮胎的寿命具有良好的促进作用。

Description

一种高耐磨抗腐蚀洗地机聚氨酯轮胎
技术领域
本发明属于聚氨酯技术领域，具体地，涉及一种高耐磨抗腐蚀洗地机聚氨酯轮胎。
背景技术
聚氨酯是一种性能介于橡胶与塑料之间的高分子合成材料，其特点是硬度调整范围宽，既有橡胶的弹性又有塑料的硬度，聚氨酯弹性体具有很好的机械性能，耐磨性能和回弹性能。但是聚氨酯除了要具有耐磨、回弹效果好外，还需要产品具有极佳的耐低温效果以及超强的耐水解性能。
常规的聚氨酯材料，绝大多数都是由聚酯合成的，这样的产品虽然有较好的强度，回弹性，但由于产品中含有酯键，使用过程中会由于湿气的进入而发生水解，影响产品的寿命。
发明内容
为了解决背景技术中提到的技术问题，本发明提供一种高耐磨抗腐蚀洗地机聚氨酯轮胎。
本发明的目的可以通过以下技术方案实现：
一种高耐磨抗腐蚀洗地机聚氨酯轮胎，包括如下重量份原料：A组分100份、B组分90-110份；
A组分包括聚酯多元醇、扩链剂、异氰酸酯、端羟基液体橡胶、催化剂；B组分包括聚碳酸酯二醇、聚四氢呋喃二醇、对苯二异氰酸酯、异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂、抗水解剂；
所述扩链剂通过如下步骤制备：
步骤S11、在温度为0℃条件下，将对硝基苯酚、四氢呋喃和三乙胺混合，然后加入甲基丙烯酰氯，加完后保持温度不变，继续搅拌反应10h，反应结束后，将得到的反应液减压浓缩除去溶剂，然后用氯仿溶解，然后依次用1％的盐酸溶液、3％的氢氧化钠溶液洗涤，洗涤结束后除去溶剂，得到助剂；
步骤S12、在氮气保护条件下，将助剂和对苯二酚混合，加入氯铂酸，然后缓慢滴加1,3,5,7-四甲基环四硅氧烷，升温至65℃，加完后保持温度不变，搅拌12h，然后升温至75℃，搅拌20h，结束后进行减压蒸馏得到环状基体；
Figure BDA0003408438970000021
步骤S13、将环状基体加入反应釜中，然后加入催化剂悬浮液，在温度为50℃，常压、氢气条件下搅拌反应10h，反应结束后，减压抽滤，将得到的滤液转移至旋转蒸发仪中，在温度为45℃条件下，减压浓缩至滤液体积不变，得到扩链剂。
本发明制得的扩链剂属于胺类的扩链剂，通过对环状基体结构中的硝基进行还原，制得含有端氨基的扩链剂，胺类的扩链剂与异氰酸酯基团生成脲结构。从分子结构上看，脲键的引入有利于提高体系中的氢键密度和有序度，即形成氢键交联点，对于提高材料的强度具有良好的促进作用；此外，该扩链剂中含有Si-O-Si链，交织成网状结构，具有很强的无机材料的特征，同时不易水解，耐高温性能也得到提升。
进一步地，步骤S11中对硝基苯酚、甲基丙烯酰氯、四氢呋喃和三乙胺的用量比为0.015mol：0.015mol：40mL：2mL；
进一步地，步骤S12中助剂、1,3,5,7-四甲基环四硅氧烷、氯铂酸和对苯二酚的用量比为7g：4g：20μL：0.1g；步骤S13中催化剂悬浮液为钯/炭催化剂和乙酸乙酯按照用量比1g：100mL混合而成，环状基体、催化剂悬浮液的用量比为1g：10mL。
抗水解剂通过如下步骤制备：
在温度为180℃、氮气保护条件下，将异氰酸丙基三乙氧基硅烷加入3-甲基-1-苯基-2-环丁磷烯-1-氧化物，搅拌反应4h，得到抗水解剂。其中3-甲基-1-苯基-2-环丁磷烯-1-氧化物的添加量为异氰酸丙基三乙氧基硅烷质量的0.75％。异氰酸丙基三乙氧基硅烷中的异氰酸酯基在3-甲基-1-苯基-2-环丁磷烯-1-氧化物的催化作用下发生缩合生成含有N＝C＝N官能团的抗水解剂。对于酯类的抗水解性能具有促进作用，同时，硅氧烷结构在温和条件下发生缩合，形成交联结构，防止低分子量的抗水解剂迁移，影响稳定性，本发明中的抗水解剂对于提高该高耐磨抗腐蚀洗地机聚氨酯轮胎的寿命，具有良好的促进作用。
所述聚氨酯轮胎包括如下步骤制备：
第一步、在温度为95℃条件下，将聚酯多元醇、扩链剂和异氰酸酯混合10min，然后降温至70℃，搅拌反应60min，然后加入端羟基液体橡胶、催化剂，搅拌至NCO含量为3-6％，得到A组分；
第二步、将聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯混合，加热至95℃，混合均匀，然后降温至70℃，搅拌反应60min，得到低聚物，然后依次加入异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂、抗水解剂，搅拌至NCO含量为7-10％，得到B组分；
第三步、将A组分和B组分混合，灌注于轮胎模具中固化后得到一种高耐磨抗腐蚀洗地机聚氨酯轮胎。
进一步地，第一步中端羟基液体橡胶为端羟基聚丁二烯丙烯腈，催化剂为三乙烯二胺、四甲基二亚乙基三胺中的一种。
进一步地，第一步中聚酯多元醇、扩链剂和异氰酸酯的用量质量比为10：1.2-2：1-1.2，聚酯多元醇、端羟基液体橡胶、催化剂的用量质量比为10：2-5：2-3。
进一步地，第二步中聚碳酸酯二醇的分子量约为1000、聚四氢呋喃二醇的分子量约为2000；聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯的质量比为10：1-13：1.2-2，低聚物、异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂和抗水解剂的质量比为10：16-18：0.01-0.05：0.1-0.5：0.5。抗氧化剂为抗氧剂168，紫外线吸收剂为UV328。
进一步地，异氰酸酯为二苯基甲烷二异氰酸酯、甲苯-2,4-二异氰酸酯、异佛尔酮二异氰酸酯中的一种或多种按照任意比例混合。
进一步地，聚酯多元醇通过如下步骤制备：
将二元酸和多元醇以质量比为10：7的比例混合，加入钛酸四异丙酯，在氮气保护条件下加热至233℃，制得聚酯多元醇，其中，二元酸为癸二酸，多元醇为新成二醇和三羟甲基丙烷以质量比10-50：0.5的混合物。
本发明的有益效果：
本发明在制备一种高耐磨抗腐蚀洗地机聚氨酯轮胎的过程中加入了扩链剂，制得的扩链剂属于胺类的扩链剂，通过对环状基体结构中的硝基进行还原，制得含有端氨基的扩链剂，胺类的扩链剂与异氰酸酯基团生成脲结构。从分子结构上看，脲键的引入有利于提高体系中的氢键密度和有序度，即形成氢键交联点，对于提高材料的强度具有良好的促进作用；此外，该扩链剂中含有Si-O-Si链，交织成网状结构，具有很强的无机材料的特征，同时不易水解，耐高温性能也得到提升。
另外还制备了抗水解剂，该抗水解剂中的硅氧烷结构在温和条件下发生缩合，形成交联结构，防止低分子量的抗水解剂迁移，影响稳定性，本发明中的抗水解剂，对于提高该高耐磨抗腐蚀洗地机聚氨酯轮胎的寿命具有良好的促进作用。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
制备扩链剂：
步骤S11、在温度为0℃条件下，将对硝基苯酚、四氢呋喃和三乙胺混合，然后加入甲基丙烯酰氯，加完后保持温度不变，继续搅拌反应10h，反应结束后，将得到的反应液减压浓缩除去溶剂，然后用氯仿溶解，然后依次用1％的盐酸溶液、3％的氢氧化钠溶液洗涤，洗涤结束后除去溶剂，得到助剂；控制对硝基苯酚、甲基丙烯酰氯、四氢呋喃和三乙胺的用量比为0.015mol：0.015mol：40mL：2mL；
步骤S12、在氮气保护条件下，将助剂和对苯二酚混合，加入氯铂酸，然后缓慢滴加1,3,5,7-四甲基环四硅氧烷，升温至65℃，加完后保持温度不变，搅拌12h，然后升温至75℃，搅拌20h，结束后进行减压蒸馏得到环状基体；控制助剂、1,3,5,7-四甲基环四硅氧烷、氯铂酸和对苯二酚的用量比为7g：4g：20μL：0.1g；
步骤S13、将环状基体加入反应釜中，然后加入催化剂悬浮液，在温度为50℃，常压、氢气条件下搅拌反应10h，反应结束后，减压抽滤，将得到的滤液转移至旋转蒸发仪中，在温度为45℃条件下，减压浓缩至滤液体积不变，得到扩链剂。控制催化剂悬浮液为钯/炭催化剂和乙酸乙酯按照用量比1g：100mL混合而成，环状基体、催化剂悬浮液的用量比为1g：10mL。
实施例2
制备抗水解剂：
在温度为180℃、氮气保护条件下，将异氰酸丙基三乙氧基硅烷加入3-甲基-1-苯基-2-环丁磷烯-1-氧化物，搅拌反应4h，得到抗水解剂。其中3-甲基-1-苯基-2-环丁磷烯-1-氧化物的添加量为异氰酸丙基三乙氧基硅烷质量的0.75％。
实施例3
制备聚酯多元醇：
将二元酸和多元醇以质量比为10：7的比例混合，加入钛酸四异丙酯，在氮气保护条件下加热至233℃，反应至酸值降为1mgKOH/g以下，羟值为114mgKOH/g以下停止反应，制得聚酯多元醇，其中，二元酸为癸二酸，多元醇为新成二醇和三羟甲基丙烷以质量比10-50：0.5的混合物。
实施例4
制备聚氨酯轮胎：
第一步、在温度为95℃条件下，将实施例3制得的聚酯多元醇、实施例1制得的扩链剂和二苯基甲烷二异氰酸酯混合10min，然后降温至70℃，搅拌反应60min，然后加入端羟基聚丁二烯丙烯腈、三乙烯二胺，搅拌至NCO含量为3-6％，得到A组分；控制聚酯多元醇、扩链剂和二苯基甲烷二异氰酸酯的用量质量比为10：1.2-2：1-1.2，聚酯多元醇、端羟基聚丁二烯丙烯腈、三乙烯二胺的用量质量比为10：2-5：2-3。
第二步、将聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯混合，加热至95℃，混合均匀，然后降温至70℃，搅拌反应60min，得到低聚物，然后依次加入异佛尔酮二异氰酸酯、抗氧剂168、紫外线吸收剂UV328、抗水解剂，搅拌至NCO含量为7-10％，得到B组分；聚碳酸酯二醇的分子量约为1000、聚四氢呋喃二醇的分子量约为2000；聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯的质量比为10：1-13：1.2-2，低聚物、异佛尔酮二异氰酸酯、抗氧剂168、紫外线吸收剂UV328和实施例2制得的抗水解剂的质量比为10：16-18：0.01-0.05：0.1-0.5：0.5。
第三步、将A组分和B组分混合，灌注于轮胎模具中固化后得到一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其中，按重量份计A组分100份、B组分90-110份。
实施例5
制备聚氨酯轮胎：
第一步、在温度为95℃条件下，将实施例3制得的聚酯多元醇、实施例1制得的扩链剂和二苯基甲烷二异氰酸酯混合10min，然后降温至70℃，搅拌反应60min，然后加入端羟基聚丁二烯丙烯腈、三乙烯二胺，搅拌至NCO含量为3-6％，得到A组分；控制聚酯多元醇、扩链剂和二苯基甲烷二异氰酸酯的用量质量比为10：1.2-2：1-1.2，聚酯多元醇、端羟基聚丁二烯丙烯腈、三乙烯二胺的用量质量比为10：2-5：2-3。
第二步、将聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯混合，加热至95℃，混合均匀，然后降温至70℃，搅拌反应60min，得到低聚物，然后依次加入异佛尔酮二异氰酸酯、抗氧剂168、紫外线吸收剂UV328、抗水解剂，搅拌至NCO含量为7-10％，得到B组分；聚碳酸酯二醇的分子量约为1000、聚四氢呋喃二醇的分子量约为2000；聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯的质量比为10：1-13：1.2-2，低聚物、异佛尔酮二异氰酸酯、抗氧剂168、紫外线吸收剂UV328和实施例2制得的抗水解剂的质量比为10：16-18：0.01-0.05：0.1-0.5：0.5。
第三步、将A组分和B组分混合，灌注于轮胎模具中固化后得到一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其中，按重量份计A组分100份、B组分90-110份。
实施例6
制备聚氨酯轮胎：
第一步、在温度为95℃条件下，将实施例3制得的聚酯多元醇、实施例1制得的扩链剂和二苯基甲烷二异氰酸酯混合10min，然后降温至70℃，搅拌反应60min，然后加入端羟基聚丁二烯丙烯腈、三乙烯二胺，搅拌至NCO含量为3-6％，得到A组分；控制聚酯多元醇、扩链剂和二苯基甲烷二异氰酸酯的用量质量比为10：1.2-2：1-1.2，聚酯多元醇、端羟基聚丁二烯丙烯腈、三乙烯二胺的用量质量比为10：2-5：2-3。
第二步、将聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯混合，加热至95℃，混合均匀，然后降温至70℃，搅拌反应60min，得到低聚物，然后依次加入异佛尔酮二异氰酸酯、抗氧剂168、紫外线吸收剂UV328、抗水解剂，搅拌至NCO含量为7-10％，得到B组分；聚碳酸酯二醇的分子量约为1000、聚四氢呋喃二醇的分子量约为2000；聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯的质量比为10：1-13：1.2-2，低聚物、异佛尔酮二异氰酸酯、抗氧剂168、紫外线吸收剂UV328和实施例2制得的抗水解剂的质量比为10：16-18：0.01-0.05：0.1-0.5：0.5。
第三步、将A组分和B组分混合，灌注于轮胎模具中固化后得到一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其中，按重量份计A组分100份、B组分90-110份。
对比例1
将实施例5中的扩链剂换成3,3'-二氯4,4'-二氨基二苯基甲烷，其余原料及制备过程保持不变。
对比例2
与实施例5相比，不添加抗水解剂，其余原料及制备过程保持不变。
对实施例4-6和对比例1-2制得的材料进行测试；耐水解性测试：测试样片规格200mm*200mm*10mm；根据ASTMD412标准测试拉伸强度，然后将测试样片被放置在70℃，95％相对湿度条件下进行水解，在设定水解时间后取出样片，置于23℃，50％相对湿度条件下调节24h。调节完成以后，样片被切成哑铃状测试样条，根据ASTMD412标准测试拉伸强度保持率(％)，测试结果如下表1所示：
表1
实施例4 实施例5 实施例6 对比例1 对比例2
水解7d 115 115 115 105 99
水解14d 109 109 109 92 73
水解21d 104 104 104 80 55
从上表1可知，本发明制得的材料具有良好的耐水解性，提高产品的使用寿命。
在说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (7)

1.一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，包括如下重量份原料：A组分100份、B组分90-110份；所述A组分包括聚酯多元醇、扩链剂、异氰酸酯、端羟基液体橡胶、催化剂；所述B组分包括聚碳酸酯二醇、聚四氢呋喃二醇、对苯二异氰酸酯、异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂、抗水解剂；
所述扩链剂通过如下步骤制备：
在氮气保护条件下，将助剂和对苯二酚混合，加入氯铂酸，然后滴加1,3,5,7-四甲基环四硅氧烷，升温至65℃，加完后保持温度不变，搅拌12h，然后升温至70-80℃，搅拌20h，得到环状基体；控制助剂、1,3,5,7-四甲基环四硅氧烷、氯铂酸和对苯二酚的用量比为7g：4g：20μL：0.1g；
将环状基体加入反应釜中，然后加入催化剂悬浮液，在温度为50℃，常压、氢气条件下搅拌反应10h，得到扩链剂；控制环状基体、催化剂悬浮液的用量比为1g：10mL；
所述助剂通过如下步骤制备：
在温度为0℃条件下，将对硝基苯酚、四氢呋喃和三乙胺混合，然后加入甲基丙烯酰氯，加完后保持温度不变，继续搅拌反应10h，得到助剂；控制对硝基苯酚、甲基丙烯酰氯、四氢呋喃和三乙胺的用量比为0.015mol：0.015mol：40mL：2mL。
2.根据权利要求1所述的一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，抗水解剂通过如下步骤制备：
在温度为180℃、氮气保护条件下，将异氰酸丙基三乙氧基硅烷加入3-甲基-1-苯基-2-环丁磷烯-1-氧化物，搅拌反应4h，得到抗水解剂。
3.根据权利要求2所述的一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，3-甲基-1-苯基-2-环丁磷烯-1-氧化物的添加量为异氰酸丙基三乙氧基硅烷质量的0.75％。
4.根据权利要求1所述的一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，包括如下步骤制备：
第一步、在温度为95℃条件下，将聚酯多元醇、扩链剂和异氰酸酯混合10min，然后降温至70℃，搅拌反应60min，然后加入端羟基液体橡胶、催化剂，搅拌得到A组分；
第二步、将聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯混合，加热至95℃，混合均匀，然后降温至70℃，搅拌反应60min，得到低聚物，然后依次加入异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂、抗水解剂，搅拌得到B组分；
第三步、将A组分和B组分混合，灌注于轮胎模具中固化后得到一种高耐磨抗腐蚀洗地机聚氨酯轮胎。
5.根据权利要求4所述的一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，第一步中聚酯多元醇、扩链剂和异氰酸酯的用量质量比为10：1.2-2：1-1.2，聚酯多元醇、端羟基液体橡胶、催化剂的用量质量比为10：2-5：2-3。
6.根据权利要求4所述的一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，第二步中聚碳酸酯二醇、聚四氢呋喃二醇和对苯二异氰酸酯的质量比为10：1-13：1.2-2，低聚物、异佛尔酮二异氰酸酯、抗氧化剂、紫外线吸收剂和抗水解剂的质量比为10：16-18：0.01-0.05：0.1-0.5：0.5。
7.根据权利要求1所述的一种高耐磨抗腐蚀洗地机聚氨酯轮胎，其特征在于，异氰酸酯为二苯基甲烷二异氰酸酯、甲苯-2,4-二异氰酸酯、异佛尔酮二异氰酸酯中的一种或多种按照任意比例混合。
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