CN109098006B - 一种夹布橡胶材料及其制备方法 - Google Patents

一种夹布橡胶材料及其制备方法 Download PDF

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CN109098006B
CN109098006B CN201810554027.3A CN201810554027A CN109098006B CN 109098006 B CN109098006 B CN 109098006B CN 201810554027 A CN201810554027 A CN 201810554027A CN 109098006 B CN109098006 B CN 109098006B
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肖风亮
吴斌
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Guangzhou Mechanical Engineering Research Institute Co Ltd
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Abstract

本发明公开了一种夹布橡胶材料，使用涤棉织物作为骨架材料，使用聚氨酯弹性体溶液作为底涂胶，使用丁腈橡胶混炼胶作为面涂胶。本发明所述夹布橡胶材料中，涤棉织物不需要进行特殊RFL等预处理措施，而是使用所述聚氨酯弹性体溶液处理，即可获得优良的粘结能力；本发明通过特定的骨架材料、底涂胶、面涂胶的选择，使得所述夹布橡胶材料具有吸水率低、粘合强度保持能力强、硫化后产品尺寸稳定性好特点，特别适用于海上风机主轴密封的骨架材料。同时，本发明还公开一种所述夹布橡胶材料的制备方法。

Description

一种夹布橡胶材料及其制备方法
技术领域
本发明涉及一种橡胶材料及其制备方法，尤其是一种夹布橡胶材料及其制备方法。
背景技术
风机轴承密封用夹布油封通常使用夹布橡胶与唇口橡胶复合而成，其中夹布橡胶作为骨架材料使用，主要利用其可剖分的特点，适用于在线安装，确保在风机20年寿命历程中能够在线更换密封件。CN201310349219.8涉及到了一种风机旋转轴密封用胶料，是风机密封唇口胶部分，没有涉及到作为骨架材料使用的夹布橡胶制造。CN 201310143915.3涉及到了一种夹布油封制备方法，但该夹布油封中的夹布橡胶材料是丁腈橡胶和棉织物制造，不能适应耐海水要求，只能在润滑油中使用，涉及到海水盐雾时候不具备尺寸稳定性。CN201010195243.7涉及到了一种丁腈夹布橡胶制造方法，该专利适用于制造尺寸精度高的V型密封圈，不能作为耐海水的骨架材料使用。由于一般的丁腈棉织物组合的夹布橡胶具有吸潮率高、不利于它在雨雪天气以及高湿度、高盐雾的海上风机上使用。
发明内容
基于此，本发明的目的在于克服上述现有技术的不足之处而提供一种黏合强度高、耐海水老化后粘合强度保持率高、尺寸稳定性好的夹布橡胶材料。该夹布橡胶适用于制造超大规格海上风机主轴的夹布油封。
为实现上述目的，本发明所采取的技术方案为：一种夹布橡胶材料，使用涤棉织物作为骨架材料，使用聚氨酯弹性体溶液作为底涂胶，使用丁腈橡胶混炼胶作为面涂胶。
优选地，所述聚氨酯弹性体溶液包含以下重量份的成分：聚合物二元醇100份、二异氰酸酯28.8～34.2份、扩链剂8.7～12.8份、溶剂100～200份、催化剂0.01～0.03份；其中，所述聚合物二元醇为以新戊二醇为起始剂合成的聚碳酸酯二醇，所述聚合物二元醇的分子量为1000～3000；所述二异氰酸酯为碳化二亚胺改性MDI。
由于聚碳酸酯二醇在相同条件普遍具有远高于其他二醇的粘度，粘度高，对反应的控制难度就高。MPD型聚碳酸酯二元醇是指以MPD(新戊二醇)为起始剂合成的聚碳酸酯二元醇，具有比以1,4-BDO、1,6-HDO或者环己烷二甲醇等更低的粘度、更好的反应操控性和更优异的低温性能。
MPD型聚碳酸酯二元醇既保留了聚碳酸酯二元醇软段赋予MPU的高耐水解性、耐热性和耐化学性能，又规避了EG、BDO或HDO等二元醇起始剂合成的聚碳酸酯二元醇粘度高、活性高和反应操作难度高的问题；其次，分子量选择1000～3000，这是合成弹性体类TPU较常使用的分子量区间，既可以保证合成的弹性体具有足够的强度和综合性能，又不至于因为原料分子量影响过程反应合成控制，分子量高反应慢、粘度高、强度低，分子量低反应快、在溶剂中分散好、反应不易控制、合成的弹性体刚性强、弹性差。选择碳化二亚胺改性的MDI是因为纯MDI自聚很严重，并且不易储存，对二元醇、扩链剂、空气和溶剂中的水分敏感，细微的原料品质波动都可能对合成的产品性能造成严重的影响。碳化二亚胺改性MDI本身含有MDI的二聚体和三聚体，自聚合程度远远低于纯MDI，并且储存不需要冷库保持，常温为液态。碳化二亚胺通常用作聚氨酯的耐水解添加剂，碳化二亚胺改性MDI一般官能度2.1～2.2，可以形成微交联结构，同时，合成的弹性体还具有较好的耐水解性能。
本发明合成的该聚氨酯弹性体在溶剂中具有线性结构，当涂布后，高温硫化时，具有进一步反应交联的特性，不需要再添加硫化剂，也不需要进行混炼。这种交联反应可以大幅度改善涤棉帆布的粘合性能，赋予涤棉帆布良好的粘结能力，为下一步与丁腈橡胶粘合以及在海水中老化后粘合力持久保持打下基础。
优选地，所述聚合物二元醇的分子量为2000；所述二异氰酸酯的官能度为2.1。基于粘度、反应速率、和物理机械性能考虑，2000分子量的最适宜。碳化二亚胺改性MDI二异氰酸酯官能度2.1是最为常见和最易获得的原料之一。
更优选地，所述催化剂为2,3-二氯苯甲酰氯、间对苯二甲酰氯中的至少一种；所述扩链剂为二甘醇胺；所述溶剂为甲乙酮、甲基异丁酮、乙酸乙酯中的至少一种。
优选地，所述涤棉织物中，涤含量为60-70％，棉含量为40-30％，单位面积的质量为230～260g/m2。值得注意的是，此处的含量均指质量百分含量。
单纯使用棉帆布，由于棉帆布吸水返潮率非常高，吸水后体积膨胀就使得密封制品的尺寸发生变化，进而影响到唇口橡胶尺寸，使得产品过盈量变化，从而导致油脂泄露或者早期密封失效或者产品寿命急剧缩短。涤纶吸湿性极低，可以有效的保持产品在潮湿环境下几何尺寸，并用一部分棉，可以有效的改善夹布的柔软度、粘合力、提高半成品成型能力。
优选地，所述丁腈橡胶混炼胶采用无锌的硫化体系，配方中不含有金属氧化物。
金属氧化物会显著提高海水的渗透和吸附性能，显著降低黏合强度以及增大产品的体积膨胀。使用低吸潮的炭黑和填料，优选半补强炭黑、热裂法炭黑，以及硫酸钡等。
优选地，所述丁腈橡胶混炼胶包含以下重量份的成分：丁腈橡胶100份、防老剂RD1.5份、防老剂ZMBI 1.5份、C9石油树脂3份、N774炭黑50份、过氧化二异丙苯2份、三丙烯基异氰脲酸酯1.0份。
优选地，所述丁腈橡胶为JSR N220s丁腈橡胶。NBR生胶优选丙烯腈质量百分比含量40％的牌号，随着丙烯腈含量提高，有利于降低橡胶吸水速率，同时提高过氧化物对丁腈橡胶交联键稳定性。
优选地，所述聚氨酯弹性体溶液的制备方法为：将二异氰酸酯、催化剂、脱水后的聚合物二元醇投料于40～50℃的溶剂中，在温度为40～50℃、100～300转/分钟的搅拌速率下反应2～2.5小时，得到预聚体；将扩链剂投入预聚体中，在温度为40～50℃、200～400转/分钟的搅拌速率下反应0.5～2.5小时，得到聚氨酯弹性体溶液。
同时，本发明还公开一种所述的夹布橡胶材料的制备方法，包括如下步骤：
(1)在聚氨酯弹性体溶液中加入有机溶剂，得到稀溶液，然后采用刮刀浸浆方式将稀溶液涂在涤棉织物上，干燥后得到聚氨酯弹性体涂层处理的涤棉织物；
(2)将丁腈橡胶混炼胶溶解在有机溶剂中，得到丁腈橡胶胶浆；
(3)将步骤(1)得到的聚氨酯弹性体涂层处理的涤棉织物，采用刮刀涂布的方式，面涂步骤(2)得到的丁腈橡胶胶浆，干燥后得到夹布橡胶材料。
优选地，所述步骤(1)中，稀溶液中的固体质量百分含量为18～22％；所述步骤(2)中，丁腈橡胶胶浆中的固体质量百分含量为45～55％。
稀溶液18～22％固含量可以有效保证溶液的粘度，将其中聚氨酯弹性体不仅仅是分布在涤棉布的纱线的缝隙之间，而是进一步润湿并扩散到纱线内部，这种充分的混合有利于黏合强度提高和保持。丁腈橡胶胶浆45～55％固含量作为覆盖胶使用，较高固含量可以节省溶剂、提高涂覆效率。
优选地，所述步骤(1)中，所述聚氨酯弹性体涂层处理的涤棉织物中，所述聚氨酯弹性体的挂胶量为30～35g/m2；所述步骤(3)中，所述夹布橡胶材料中，所述丁腈橡胶的挂胶量为160～190g/m2。
挂胶量大小与使用涤棉布单位面积质量正相关，以此来保证单位质量的涤棉布上含有的聚氨酯弹性体质量(约13％质量比)和丁腈橡胶质量(约70％质量比)恒定。这两个质量恒定是为了实现最终产品黏合强度稳定和硬度稳定。
优选地，所述步骤(1)和所述步骤(2)中的有机溶剂为甲苯、乙酸乙酯、乙酸丁酯中的至少一种。
相对于现有技术，本发明的有益效果为：
本发明所述夹布橡胶材料中，涤棉织物不需要进行特殊RFL等预处理措施，而是使用所述聚氨酯弹性体溶液处理，即可获得优良的粘结能力；本发明通过特定的骨架材料、底涂胶、面涂胶的选择，使得所述夹布橡胶材料具有吸水率低、粘合强度保持能力强、硫化后产品尺寸稳定性好特点，特别适用于海上风机主轴密封的骨架材料。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。本发明实施例中，只是列举了具体的例子对本申请进行了具体说明，但是实施例中的例子并不代表本申请全部的保护范围，只要在本申请全部保护范围中的技术方案均能达到本申请的效果，在此并不一一进行敖述。
实施例1
本发明所述夹布橡胶材料的一种实施例，本实施例所述夹布橡胶材料通过以下方法制备所得：
(1)底涂胶聚氨酯弹性体溶液制备
①将MPD型聚碳酸酯二醇在100℃真空脱水2小时，降至室温，N2保护；
②取甲乙酮150g，加热至40℃，加入100g脱水MPD型聚碳酸酯二元醇(分子量为1000～3000)和0.02g 2,3-二氯苯甲酰氯、30g碳化二亚胺改性MDI，控制温度40℃，在200转/分钟的搅拌速率下反应2.5小时，反应完成得到预聚体；
③加入9.2g二甘醇胺扩链剂于预聚体中，维持温度40℃，在300转/分钟的搅拌速率下反应0.5小时，然后降温至室温，N2保护，得到聚氨酯弹性体溶液。
(2)浸涂涤棉布制备
将底涂胶用甲苯稀释到20％固含量，使用TC110-1型(70％涤/30％棉)涤棉帆布，单位面积质量为230g/m2，采用浸涂方法通过底涂胶溶液，干燥后获得单位面积质量为260g/m2，即上胶量为30g/m2的聚氨酯溶液涂层处理的涤棉布。
(3)面涂胶丁腈橡胶胶浆制备
按JSR N220s丁腈橡胶100份、防老剂RD(2,2,4-三甲基-1,2-二氢化喹啉聚合体)1.5份、防老剂ZMBI(2-硫醇基苯骈咪唑锌盐)1.5份、C9树脂3份、N774炭黑50份、DCP(过氧化二异丙苯)2份、TAIC(三丙烯基异氰脲酸酯)1.0份的配合比例制备丁腈橡胶混炼胶，将丁腈橡胶混炼胶溶解在甲苯中，制备出成固含量50％的丁腈橡胶胶浆。
(4)涤棉夹布橡胶材料制备
将聚氨酯弹性体涂层处理的涤棉帆布，采用刮刀涂布的方式通过丁腈橡胶胶浆，干燥后获得单位面积质量为420g/m2，即上胶量160g/m2的涤棉布夹布橡胶材料。
实施例2
本发明所述夹布橡胶材料的一种实施例，本实施例所述夹布橡胶材料通过以下方法制备所得：
将实施例1中涤棉布使用TC110-6C1型涤棉布(60％涤/40％棉)代替，其单位面积质量为260g/m2，相应的聚氨酯弹性体上胶量提高到35g/m2，丁腈橡胶上胶量提高到190g/m2，其它保持不变。
对比例1
实施例1中丁腈橡胶采用有氧化锌的硫黄硫化系统代替，其他不变，具体配方如下：
JSR N220s丁腈橡胶100份、氧化锌5.0份、硬脂酸1份、防老剂RD 1.5份、防老剂ZMBI 1.5份、C9树脂3份、N774炭黑50份、硫黄0.3份、TMTD2.0份、DM 1.5份。
对比例2
实施例2中使用全棉帆布代替涤棉帆布，其他不变。
对比例3
实施例1中取消聚氨酯溶液涂层的步骤，同时将丁腈橡胶挂胶量从160g/m2提高到190g/m2，弥补减少的30g/m2的聚氨酯弹性体，保持总挂胶量不变。
表1给出了实施例1～2和对比例1～3的性能数据比较分析。其中丁腈橡胶硫化胶、涤棉夹布橡胶两种试样均是170℃×10分钟模压硫化获得；夹布橡胶剥离强度试样硫化条件是170℃×15分钟。
表1实施例与对比例夹布橡胶材料性能数据
Figure BDA0001680862960000071
从表1中可以看出：
(1)实施例1～2与对比例1相比，含有金属氧化物硫黄硫化丁腈橡胶其吸水能力迅速增大，对夹布粘合强度保持能力同时显著下降；
(2)实施例1～2与对比例2相比，更换成全棉帆布后，相对涤棉帆布，其夹布橡胶吸水能力大大增加，耐海水后力学性能下降显著，粘合强度保持率降低到47.5％。
(3)实施例1～2与对比例3相比，当取消聚氨酯涂层之后，夹布橡胶初始粘合强度很低，体现出了聚氨酯涂层在硫化过程中对涤纶纤维的表面活化和改性作用。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (5)

1.一种夹布橡胶材料，其特征在于，使用涤棉织物作为骨架材料，使用聚氨酯弹性体溶液作为底涂胶，使用丁腈橡胶混炼胶作为面涂胶；
所述聚氨酯弹性体溶液包含以下重量份的成分：聚合物二元醇100份、二异氰酸酯28.8~34.2份、扩链剂8.7~12.8份、溶剂100~200份、催化剂 0.01~0.03份；其中，所述聚合物二元醇为以新戊二醇为起始剂合成的聚碳酸酯二醇，所述聚合物二元醇的分子量为1000~3000；所述二异氰酸酯为碳化二亚胺改性MDI；
所述聚氨酯弹性体溶液的制备方法为：将二异氰酸酯、催化剂、脱水后的聚合物二元醇投料于40~50℃的溶剂中，在温度为40~50℃、100~300转/分钟的搅拌速率下反应2~2.5小时，得到预聚体；将扩链剂投入预聚体中，在温度为40~50℃、200~400转/分钟的搅拌速率下反应0.5~2.5小时，得到聚氨酯弹性体溶液；
所述涤棉织物中，涤含量为60-70%wt，棉含量为40-30% wt，单位面积的质量为230~260g/m2；
所述丁腈橡胶混炼胶采用无锌的硫化体系，配方中不含有金属氧化物；所述丁腈橡胶混炼胶包含以下重量份的成分：丁腈橡胶 100份、防老剂RD 1.5份、防老剂ZMBI 1.5份、C9石油树脂3份、N774炭黑 50份、过氧化二异丙苯2份、三丙烯基异氰脲酸酯1.0份。
2.如权利要求1所述的夹布橡胶材料，其特征在于，所述催化剂为2,3-二氯苯甲酰氯、间对苯二甲酰氯中的至少一种；所述扩链剂为二甘醇胺；所述溶剂为甲乙酮、甲基异丁酮、乙酸乙酯中的至少一种。
3.一种如权利要求1或2所述的夹布橡胶材料的制备方法，其特征在于，包括如下步骤：
（1）在聚氨酯弹性体溶液中加入有机溶剂，得到稀溶液，然后采用刮刀浸浆方式将稀溶液涂在涤棉织物上，干燥后得到聚氨酯弹性体涂层处理的涤棉织物；
（2）将丁腈橡胶混炼胶溶解在有机溶剂中，得到丁腈橡胶胶浆；
（3）将步骤（1）得到的聚氨酯弹性体涂层处理的涤棉织物，采用刮刀涂布的方式，面涂步骤（2）得到的丁腈橡胶胶浆，干燥后得到夹布橡胶材料。
4.如权利要求3所述的夹布橡胶材料的制备方法，其特征在于，所述步骤（1）中，稀溶液中的固体质量百分含量为18~22%；所述步骤（2）中，丁腈橡胶胶浆中的固体质量百分含量为45~55%。
5.如权利要求3所述的夹布橡胶材料的制备方法，其特征在于，所述步骤（1）中，所述聚氨酯弹性体涂层处理的涤棉织物中，所述聚氨酯弹性体的挂胶量为30~35g/m2；所述步骤（3）中，所述夹布橡胶材料中，所述丁腈橡胶的挂胶量为160~190g/m2。
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