CN107075257B - 增粘剂及其连续过程 - Google Patents
增粘剂及其连续过程 Download PDFInfo
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- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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Abstract
一种松香分散体是以该松香分散体的总干重计80％至98％干重的松香树脂和2％至20％干重的分散剂的反应产物。该松香树脂通过以下方法中的至少一种方法进行处理：由原材料松香进行a)改性、b)氢化或歧化、以及c)聚合或酯化。该分散剂选自C18‑C32脂肪族羧酸、烯烃(甲基)丙烯酸共聚物、以及其它酸/酸酐改性聚合物。还包括一种用于制备该松香分散体的连续过程和一种包含该松香分散体的粘合剂配方。
Description
技术领域
本发明涉及一种增粘剂，具体地说，涉及一种松香分散体，以及一种用于制备松香分散体的连续过程。
背景技术
增粘剂是用于配制粘合剂以增加粘性(即粘合剂的粘着性)的化学化合物。松香或松香树脂是压敏粘合剂中广泛使用的增粘剂之一，并且压敏粘合剂通常由丙烯酸类聚合物乳液制成。在应用之前，利用专门选择的分散剂通过分批方法将松香制成松香分散体。
在粘合剂领域中希望提供一种具有改进的环粘性和抗剪切性性能的松香分散体。还希望提供一种用于制备松香分散体的连续过程。
发明内容
本发明提供一种松香分散体，其是以所述松香分散体的总干重计80％至98％干重的松香树脂和2％至20％干重的分散剂的反应产物。所述松香树脂通过以下方法中的至少一种方法进行处理：由原材料松香进行a)改性、b)氢化或歧化、以及c)聚合或酯化。所述分散剂选自C18-C32脂肪族羧酸、烯烃(甲基)丙烯酸共聚物、以及其它酸/酸酐改性聚合物。
本发明进一步提供一种用于制备松香分散体的连续过程，所述连续过程包含以下步骤：将熔融分散相料流与熔融连续相料流合并到机械分散器中。所述熔融分散相包含所述松香树脂，并且所述熔融连续相包含水。将所述分散剂加入到所述分散相、所述连续相、或者这两者中。
本发明进一步提供一种粘合剂配方，其包含丙烯酸类聚合物乳液和以所述丙烯酸类聚合物乳液的总干重计1％至50％干重的松香分散体。
具体实施方式
本发明的松香分散体是以所述松香分散体的总干重计a)80％至98％、优选地85％至95％、并且更优选地88％至93％干重的松香树脂和b)2％至20％、优选地5％至15％、并且更优选地7％至12％干重的分散剂的反应产物。
松香树脂
本发明中使用的松香树脂通过以下方法中的至少一种方法进行处理：由原材料松香(诸如脂松香、妥尔油松香和木松香)进行a)改性、b)氢化或歧化、以及c)聚合或酯化。在松香树脂通过上述方法中的至少两种方法进行处理的情况下，方法b)和c)的处理顺序没有具体地限制，只是如果既使用改性方法又使用聚合方法，那么改性方法之后必须，但不一定直接跟随聚合方法。松香树脂的合适实例包括分别通过改性、氢化、歧化和聚合原材料松香获得的改性松香、氢化松香、歧化松香和聚合松香，以及另外通过用醇或环氧化合物酯化原材料松香获得的松香酯。改性松香的合适实例包括通过用不饱和酸改性原材料松香获得的不饱和改性松香和通过用酚改性原材料松香获得的酚改性松香。不饱和酸的合适实例包括丙烯酸、甲基丙烯酸、富马酸和马来酸。酚的合适实例包括苯酚和烷基酚。改性方法没有具体地限制，并且通常采用将原材料松香与酚或不饱和酸混合并且将其加热的方法。
用于由原材料松香和醇制备松香酯的醇的合适实例包括：一价醇，诸如甲醇、乙醇和丙醇；二价醇，诸如乙二醇、二甘醇、丙二醇和新戊二醇；三价醇，诸如甘油、三羟甲基乙烷和三羟甲基丙烷；四价醇，诸如季戊四醇和二甘油；以及六价醇，诸如二季戊四醇。优选地，醇为甘油，并且更优选地，醇为季戊四醇。松香酯的酯化方法没有具体地限制，并且采用将原材料松香与醇混合并且在任选的酯化催化剂的存在下加热所述混合物的方法。由歧化松香制备的松香酯(即歧化松香酯)是优选的。
松香树脂的酸值和软化点根据其种类而变化。酸值通常为1至50KOH mg/g，优选地为1至15KOH mg/g，并且软化点为25℃至150℃，优选地为60℃至120℃。
可以使用其它增粘剂树脂代替本发明的松香树脂，并且达到类似的性能。其它增粘剂树脂的合适实例包括：萜烯和改性萜烯；脂肪族、脂环族和芳香族树脂，诸如C5脂肪族树脂、C9芳香族树脂、以及C5/C9脂肪族/芳香族树脂；氢化烃类树脂；萜烯-酚树脂；以及其任何组合。
分散剂
本发明的分散剂选自：C18-C32脂肪族羧酸，优选地C18-C28脂肪族羧酸，并且更优选地C20-C26脂肪族羧酸；烯烃(甲基)丙烯酸共聚物，优选地具有10wt％至30wt％(甲基)丙烯酸的那些，并且更优选地具有15wt％至25wt％(甲基)丙烯酸的那些；以及其它酸/酸酐改性(共)聚合物，诸如部分水解的聚乙烯醇、苯乙烯马来酸酐共聚物、马来酸酐改性的聚乙烯、聚丙烯或聚烯烃共聚物、马来酸酐改性的苯乙烯-二烯嵌段共聚物，以及其任何组合。优选地，分散剂选自烯烃(甲基)丙烯酸共聚物，并且烯烃(甲基)丙烯酸共聚物的合适实例包括乙烯甲基丙烯酸共聚物、乙烯丙烯酸共聚物、丙烯甲基丙烯酸共聚物、丙烯丙烯酸共聚物。优选地，烯烃(甲基)丙烯酸共聚物是乙烯(甲基)丙烯酸共聚物，并且更优选地，是乙烯丙烯酸共聚物。
任选地，常规的离子或非离子表面活性剂可以与以上分散剂组合使用。优选地，表面活性剂是阴离子表面活性剂，并且阴离子表面活性剂的合适实例选自磺酸酯、磷酸酯、羧酸酯、以及其任何组合。优选地，阴离子表面活性剂是磺酸酯(诸如烷基单酯磺基琥珀酸酯)和磷酸酯(诸如聚氧乙烯壬基苯基醚支链磷酸酯)。
连续过程
本发明的松香分散体通过将熔融分散相料流与熔融连续相料流合并到机械分散器中来制备。熔融分散相料流含有松香树脂，所述松香树脂在室温下优选地为固体，但在较高温度下熔融。熔融连续相料流含有水。所述连续过程是挤出(或熔融捏合)工艺，其包括熔融挤出和复合挤出。
在熔融挤出中，将通常为薄片或颗粒形式的松香树脂输送到挤出机中以熔融。通过加热的导管将熔融松香树脂送入，成为熔融松香树脂料流。将该料流与连续相料流连接并且最终合并到机械分散器中。如果需要将中和剂、填料、稳定剂、颜料或其它非反应性化合物引入到分散相料流中，则在挤出之前有利地进行此类添加，并且通过化合物挤出将各成分共混。
可以将分散剂加入到a)分散相、b)连续相、或者c)这两者中。优选将分散剂优选地通过挤出机的入口加入到分散器上游的分散相中。
优选地，松香分散体基本上不含有机溶剂，即其含有以分散体的总重量计小于3％、优选地小于2％、更优选地小于1％、更优选地小于0.5％、更优选地小于0.2％、并且最优选地小于0.1％重量的有机溶剂。在松香分散体中可以存在的在所述界限内的溶剂是烃基溶剂，优选地是芳香族溶剂、并且更优选地是甲苯。
应用
通过本发明的方法获得的松香分散体被用作粘合剂配方(诸如丙烯酸压敏粘合剂)中的增粘剂分散体。丙烯酸压敏粘合剂通过将松香分散体复配在丙烯酸类聚合物乳液中而获得。
丙烯酸类聚合物没有具体地限制，并且在制备丙烯酸压敏粘合剂时可以使用各种已知的均聚物或共聚物。丙烯酸类聚合物的合适实例包括(甲基)丙烯酸酯(诸如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯和(甲基)丙烯酸-2-乙基己酯)的单体和官能单体(诸如(甲基)丙烯酸、(甲基)丙烯酸缩水甘油酯、(甲基)丙烯酸2-羟基乙酯和(甲基)丙烯酰胺)的聚合产物。其它可共聚的单体(诸如乙酸乙烯酯和苯乙烯)也可用于所述聚合。
(甲基)丙烯酸酯为主要成分的丙烯酸类聚合物的玻璃化转变温度没有具体地限制，但是通常为-90至0℃，并且优选地为-80至-10℃。如果玻璃化转变温度高于0℃，则粘性降低，而且如果其低于-90℃，则粘合性趋于降低。进一步地，丙烯酸类聚合物的分子量没有具体地限制，但是为了更好的粘合，其重均分子量优选地为100,000至1,000,000、并且更优选地为150,000至500,000。
在粘合剂配方中，松香分散体以丙烯酸类聚合物的总干重计优选地为1％至50％干重、更优选地为10％至40％干重。
实例
I.原材料
*S-202松香树脂的酸值为小于15KOH mg/g，以及软化点为90℃。
II.测试方法
使粘合剂层压体在测试实验室中在受控环境(22-24℃，45-55％相对湿度)下调节至少过夜之后，在所述粘合剂层压体上进行性能测试，至少过夜。
1.环粘性测试
根据FINAT(Féderation Internationale des fabricants et transformateursd'Adhésifs et Thermocollants)测试方法No.9，在不锈钢(SS)和高密度聚乙烯(HDPE)测试板上测试所制备的粘合剂层压体，其中破坏模式为粘合破坏，除非另外指定。与其中破坏模式为粘合破坏的实例相比，其中破坏模式为纸张撕裂的粘合剂层压体实例(如下所述)具有更好的环粘性性能。环粘性测试也在老化之后进行(老化-环粘性)。将制备的粘合剂层压体放入65℃温度和80％湿度的烘箱中4天。然后将层压体放置在受控环境(22-24℃，50-60％相对湿度)中至少过夜，之后进行测试。
2.抗剪切性测试
FINAT测试方法No.8被称为抗剪切性测试，其中破坏模式为内聚破坏。
III.实例
1.本发明的松香分散体1和2的制备
按照以下方法制备松香分散体1：
设置双螺杆挤出机，其中电动机速度为250rpm，排出压力为2.0巴，排出温度为86℃，以及乳化区温度为100℃。选择S-202松香和PRIMACOR EAA 5980i分散剂，并且将其进料速率分别设置为3.27kg/h和0.36kg/h。S-202松香与PRIMACOR EAA 5980i分散剂的干重比为9比1。所选择的S-202松香、PRIMACOR EAA 5980i分散剂、初始水(90℃，13.9ml/min)和氢氧化钾溶液(90℃，在水中为50％，0.48ml/min)通过在双螺杆挤出机中复合挤出熔融共混。然后在双螺杆挤出机中用水(90℃，46.56ml/min)稀释熔融共混的材料以形成松香分散体。所得到的松香分散体的体积平均粒径为752nm(Malvern Zetasizer Nano ZS，下文相同)，固体含量为50.24％，粘度为246cps(Brookfield RVDV数字粘度计，63#心轴，30rpm，下文相同)，以及pH为7.8(Mettler Toledo SevenEasyTM pH计，下文相同)。
松香分散体2根据松香分散体1的制备而制备，但是使用二甲基乙醇胺(DMEA)(90℃，在水中为50％，2ml/min)代替氢氧化钾溶液，并且S-202松香与PRIMACOR EAA5980i分散剂的干重比为85比15。所得到的松香分散体的体积平均粒径为620nm，固体含量为50.79％，粘度为650cps，以及pH为7.3。
2.对比松香分散体1的制备
使用传统的低分子量分散剂、RHODAFAC RE-610表面活性剂制备对比松香分散体1。将50g的S-202松香、5g的乙酸丁酯和5g的RHODAFAC RE-610表面活性剂加入到烧瓶中并且加热至95℃。熔融后，向烧瓶中加入50g沸水，搅拌10分钟，从而制备成对比松香分散体1。将所述分散体冷却至室温，并且用氨中和至pH 6.5～7.5。所得到的松香分散体的体积平均粒径为500nm，固体含量为52.31％，粘度为90cps，以及pH为7.2。
3.压敏粘合剂(PSA)的制备
松香分散体1和2以及对比松香分散体1分别用于制备压敏粘合剂1与2以及对比压敏粘合剂1。SNOWTACK SE780G松香分散体是劳特化工有限公司的市售松香分散体，并且用于制备对比压敏粘合剂2。
将ROBOND PS-7851丙烯酸类聚合物、以上松香分散体中的任一种、以ROBOND PS-7851丙烯酸类聚合物和松香分散体的总湿重计0.3％湿重的AEROSOL GPG润湿剂和0.4％湿重的SURFYNOL 440润湿剂在搅拌下加入到烧瓶中用以制备压敏粘合剂。松香分散体与ROBOND PS-7851丙烯酸类聚合物的干重比为0.325。将ACRYSOL RM-8W增稠剂和氨加入到烧瓶中，以将压敏粘合剂的粘度调节至400cps至800cps，以及将最终pH调节至7至8。对于PSA1、PSA 2、对比PSA 1和对比PSA 2，压敏粘合剂的实际粘度分别为500cps、650cps、630cps和550cps(Brookfield，LVDV，63#，30rpm)以及最终pH分别为7.8、7.5、7.2和7.9。
4.粘合剂层压体的制备
将压敏粘合剂以干重计22g/m2的量涂布到纸张剥离衬垫上，并且进行干燥以制备粘合剂层压体。将粘合剂层与纸张的粗糙非光泽的一面接触，得到粘合剂片。
IV.结果
表1
*破坏模式为纸张撕裂。
对于所有以上性能测试，即包括基于不锈钢(SS)和高密度聚乙烯(HDPE)的那些的抗剪切性测试和环粘性测试(以及老化-环粘性测试)，所得到的值越高，性能越好。对于其中破坏模式为纸张撕裂的PSA实例(PSA 1和2)，与其中破坏模式为粘合破坏的PSA实例(对比PSA 1和2)相比，它们具有更好的环粘性性能。保留值是老化测试与非老化测试的比率，表明老化后PSA实例的保留性能。
从上表1可以清楚看出，与使用普通分散剂的对比PSA 1和对比PSA 2相比，使用乙烯丙烯酸共聚物分散剂，即PRIMACOR EAA 5980i分散剂的PSA 1和2显示出显著改进的(更高值)抗剪切性和SS环粘性(基于老化和没有老化的不锈钢)性能，以及可接受的HDPE环粘性(基于高密度聚乙烯)性能。
Claims (9)
1.一种松香分散体，其是以所述松香分散体的总干重计80％至98％干重的松香树脂和2％至20％干重的分散剂的反应产物，其中，所述松香树脂通过以下方法中的至少一种方法进行处理：由原材料松香进行a)改性、b)氢化或歧化，以及c)聚合或酯化，所述分散剂是烯烃(甲基)丙烯酸共聚物，并且所述松香树脂的酸值为1至50KOH mg/g，以及软化点为25至150℃。
2.根据权利要求1所述的松香分散体，其中，以所述松香分散体的总干重计，所述松香树脂为85％至95％干重以及所述分散剂为5％至15％干重。
3.根据权利要求1所述的松香分散体，其中，以所述松香分散体的总干重计，所述松香树脂为88％至93％干重以及所述分散剂为7％至12％干重。
4.根据权利要求1所述的松香分散体，其中，所述松香树脂是歧化松香酯。
5.根据权利要求1所述的松香分散体，其中，所述分散剂是乙烯-丙烯酸共聚物。
6.一种用于制备根据权利要求1所述的松香分散体的连续过程，其包含以下步骤：将熔融分散相料流与熔融连续相料流合并到机械分散器中；其中，所述熔融分散相包含所述松香树脂，并且所述熔融连续相包含水；以及将所述分散剂加入到所述分散相、所述连续相、或者这两者中。
7.根据权利要求6所述的连续过程，其中，所述连续过程是挤出过程。
8.一种粘合剂配方，其包含丙烯酸类聚合物乳液和以所述丙烯酸类聚合物乳液的总干重计1％至50％干重的根据权利要求1所述的松香分散体。
9.根据权利要求8所述的粘合剂配方，其中，所述丙烯酸类聚合物乳液的玻璃化转变温度为-90至0℃，以及重均分子量为100,000至1,000,000。
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- 2014-10-31 BR BR112017008433-3A patent/BR112017008433B1/pt active IP Right Grant
- 2014-10-31 WO PCT/CN2014/090001 patent/WO2016065604A1/en active Application Filing
- 2014-10-31 CN CN201480082958.8A patent/CN107075257B/zh active Active
- 2014-10-31 JP JP2017522920A patent/JP6681889B2/ja active Active
- 2014-10-31 RU RU2017117181A patent/RU2678276C2/ru active
- 2014-10-31 EP EP14904886.0A patent/EP3212716A4/en active Pending
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Also Published As
| Publication number | Publication date |
|---|---|
| RU2678276C2 (ru) | 2019-01-24 |
| WO2016065604A1 (en) | 2016-05-06 |
| RU2017117181A (ru) | 2018-11-21 |
| JP2018503700A (ja) | 2018-02-08 |
| BR112017008433A2 (pt) | 2018-01-23 |
| EP3212716A1 (en) | 2017-09-06 |
| MX2017005266A (es) | 2017-08-18 |
| EP3212716A4 (en) | 2018-08-01 |
| BR112017008433B1 (pt) | 2021-11-03 |
| CN107075257A (zh) | 2017-08-18 |
| RU2017117181A3 (zh) | 2018-11-21 |
| US10544335B2 (en) | 2020-01-28 |
| JP6681889B2 (ja) | 2020-04-15 |
| US20170313913A1 (en) | 2017-11-02 |
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