CN101384666A - 用于由软木颗粒制备成型体的方法 - Google Patents
用于由软木颗粒制备成型体的方法 Download PDFInfo
- Publication number
- CN101384666A CN101384666A CNA2007800053702A CN200780005370A CN101384666A CN 101384666 A CN101384666 A CN 101384666A CN A2007800053702 A CNA2007800053702 A CN A2007800053702A CN 200780005370 A CN200780005370 A CN 200780005370A CN 101384666 A CN101384666 A CN 101384666A
- Authority
- CN
- China
- Prior art keywords
- cork
- polymer
- formed body
- vinyl
- acrylate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Abstract
本发明涉及用于由软木颗粒制备成型体的方法，其中用热塑性聚合物粘结软木颗粒，其特征在于，该热塑性聚合物以其水中可再分散的聚合物粉末的形式加以使用，其包含一种或更多种基础聚合物、一种或更多种保护胶体以及任选的抗结块剂。
Description
技术领域
本发明涉及用于由软木颗粒制备成型体的方法，其中用热塑性聚合物粘结软木颗粒。
背景技术
在制备用于制备瓶塞软木的软木塞中，每年产生相当大量的废软木。将它们研磨成软木颗粒(软木粉)(传输软木)，并用作由软木颗粒制备成型体的基本原料。为此将软木颗粒与合成聚合物混合，随后压制成为成型体。
DE 1 620 777 A公开了由软木颗粒和聚氨酯制备的软木成型体。在使用聚氨酯作为粒状软木的粘结剂时的缺点是，由此获得的成型体无法进行热塑性再加工。
DE 196 29 017同样涉及软木颗粒与聚氨酯的粘结，但其中还描述了使用热塑性聚合物作为粘结剂。在软木加工中，乙烯-乙酸乙烯酯共聚物、聚氯乙烯和热塑性弹性体(TPE)是常用的热塑性粘结剂。利用热塑性聚合物能够通过挤出或压延而热塑性加工软木颗粒。但缺点是，基于成型体的总重量，必须使用的热塑性塑料的高含量通常为50至70重量％，从而获得所需的机械强度。另一个缺点在于，由于聚合物含量高，导致成型体不再具有天然软木的外观。
因此，本发明的目的在于开发能够由软木颗粒和热塑性聚合物制备成型体的方法，其能够更少量使用热塑性塑料，虽然确保成型体的机械强度高，其仍然能够进行热塑性再加工，并且能够获得具有天然软木外观的成型体。
发明内容
本发明涉及用于由软木颗粒制备成型体的方法，其中用热塑性聚合物粘结软木颗粒，其特征在于，该热塑性聚合物以其水中可再分散的聚合物粉末的形式加以使用，其包含一种或更多种聚合物、一种或更多种保护胶体以及任选存在的抗结块剂。
能够在存在保护胶体的情况下通过干燥聚合物的对应的含水分散体而获得的粉末组合物称作水中可再分散的聚合物粉末。借助于该制备过程，分散体的细碎的树脂由足够量的水溶性保护胶体包覆。在干燥时，保护胶体发挥阻止颗粒结块的外套的作用。于水中再次分散时，保护胶体再次溶于水中，并获得原始聚合物颗粒的含水分散体(Schulze J.in TIZ，No.9，1985)。
合适的聚合物是基于一种或更多种选自以下组中的单体：乙烯基酯、(甲基)丙烯酸酯、乙烯基芳烃、烯烃、1，3-二烯烃及卤乙烯以及任选存在的可与其共聚合的其他单体。
合适的乙烯基酯是具有1至12个碳原子的羧酸的乙烯基酯。优选为乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、2-乙基己酸乙烯酯、月桂酸乙烯酯、乙酸1-甲基乙烯酯、新戊酸乙烯酯以及具有9至11个碳原子的α-分支单羧酸的乙烯基酯，如VeoVa9R或VeoVa10R(Resolution公司的商品名)。特别优选为乙酸乙烯酯。
合适的选自丙烯酸酯或甲基丙烯酸酯的单体是具有1至15个碳原子的非分支或分支型醇的酯。优选的甲基丙烯酸酯或丙烯酸酯是丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸叔丁酯、甲基丙烯酸叔丁酯、丙烯酸2-乙基己酯。特别优选为丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸正丁酯、丙烯酸叔丁酯及丙烯酸2-乙基己酯。
乙烯基芳烃优选为苯乙烯、甲基苯乙烯和乙烯基甲苯。优选的卤乙烯是氯乙烯。优选的烯烃是乙烯和丙烯，而优选的二烯烃是1，3-丁二烯和异戊二烯。
基于单体混合物的总重量，任选还可共聚合0.1至5重量％的辅助单体。优选使用0.5至2.5重量％的辅助单体。辅助单体的实例是：烯键式不饱和的单羧酸及二羧酸，优选为丙烯酸、甲基丙烯酸、富马酸及马来酸；烯键式不饱和的羧酰胺及腈，优选为丙烯酰胺及丙烯腈；富马酸及马来酸的单酯及二酯，如二乙酯及二异丙酯；马来酸酐；烯键式不饱和的磺酸及其盐，优选为乙烯基磺酸或2-丙烯酰胺基-2-甲基丙磺酸。其他的实例是预交联共聚单体，如多重烯键式不饱和的共聚单体，如邻苯二甲酸二烯丙酯、己二酸二乙烯酯、马来酸二烯丙酯、甲基丙烯酸烯丙酯或氰脲酸三烯丙酯；或后交联共聚单体，如丙烯酰胺基羟基乙酸(AGA)、甲基丙烯酰胺基羟基乙酸甲酯(MAGME)、N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺、N-羟甲基氨基甲酸烯丙酯；N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺及N-羟甲基氨基甲酸烯丙酯的烷基醚，如异丁氧基醚或酯。环氧基官能的共聚单体也是合适的，如甲基丙烯酸缩水甘油酯及丙烯酸缩水甘油酯。其他的实例是硅官能的共聚单体，如丙烯酰氧基丙基三(烷氧基)硅烷及甲基丙烯酰氧基丙基三(烷氧基)硅烷、乙烯基三烷氧基硅烷及乙烯基甲基二烷氧基硅烷，其中例如可含有乙氧基及乙氧基丙二醇醚基作为所述烷氧基。还述及具有羟基或CO基的单体，如甲基丙烯酸羟烷基酯及丙烯酸羟烷基酯，如丙烯酸羟乙基酯、丙烯酸羟丙基酯、丙烯酸羟丁基酯、甲基丙烯酸羟乙基酯、甲基丙烯酸羟丙基酯或甲基丙烯酸羟丁基酯，以及诸如双丙酮丙烯酰胺及丙烯酸乙酰基乙酰氧基乙酯或甲基丙烯酸乙酰基乙酰氧基乙酯的化合物。
单体的选择和/或共聚单体的重量份的选择，通常使得玻璃化转变温度Tg≤120℃，优选为-40℃至+120℃，更优选为-20℃至+80℃。该聚合物的玻璃化转变温度Tg可利用差示扫描量热法(DSC)由已知的方式测得。Tg也可利用Fox方程预先进行近似计算。依照Fox T.G.，Bull.Am.Physics Soc.1，3，page 123(1956)：
1/Tg＝x1/Tg1+x2/Tg2+…+xn/Tgn
其中xn代表单体n的以重量％/100计的质量分数，而Tgn代表单体n的均聚物以开尔文计的玻璃化转变温度。均聚物的Tg值记载于“聚合物手册(Polymer Handbook)”，第二版，J.Wiley & Sons，New York(1975)。
优选为包含一种或更多种选自以下组中的单体的均聚物或共聚物：乙酸乙烯酯、具有9至11个碳原子的α-分支单羧酸的乙烯基酯、氯乙烯、乙烯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸2-乙基己酯和苯乙烯。特别优选为乙酸乙烯酯和乙烯的共聚物；乙酸乙烯酯、乙烯和具有9至11个碳原子的α-分支单羧酸的乙烯基酯的共聚物；丙烯酸正丁酯和丙烯酸2-乙基己酯和/或甲基丙烯酸甲酯的共聚物；苯乙烯和一种或更多种选自以下组中的单体的共聚物：丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸正丁酯和丙烯酸2-乙基己酯；乙酸乙烯酯和一种或更多种选自以下组中的单体的共聚物：丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸正丁酯、丙烯酸2-乙基己酯和任选的乙烯；1，3-丁二烯和苯乙烯和/或甲基丙烯酸甲酯以及任选的其他丙烯酸酯的共聚物；其中所述混合物任选还可含有一种或更多种上述的辅助单体。
以已知的方式在存在保护胶体的情况下，根据乳液聚合法或者根据悬浮聚合法，优选根据乳液聚合法，制备聚合物，其中聚合作用的温度通常为20℃至100℃，优选为60℃至90℃，在气态共聚单体如乙烯共聚合期间，通常也可在5巴至100巴之间的压力下进行。使用对于乳液聚合或悬浮聚合常用的水溶性或单体可溶性引发剂或氧化还原引发剂组合引发聚合反应。在聚合反应期间可以使用调节物质以控制分子量。可以在任选与乳化剂相结合的情况下使用保护胶体以进行稳定化。
为了稳定化聚合批次常用的保护胶体例如是部分水解或完全水解的聚乙烯醇；聚乙烯吡咯烷酮；聚乙烯醇缩醛；水溶性形式的多糖，如淀粉(直链淀粉及支链淀粉)，纤维素及其羧甲基衍生物、甲基衍生物、羟乙基衍生物及羟丙基衍生物；蛋白质，如酪蛋白或酪蛋白酸盐、大豆蛋白、明胶；木质素磺酸盐；合成聚合物，如聚(甲基)丙烯酸、(甲基)丙烯酸酯与羧基官能的共聚单体单元的共聚物、聚(甲基)丙烯酰胺、聚乙烯基磺酸及其水溶性共聚物；三聚氰胺甲醛磺酸盐、萘甲醛磺酸盐、苯乙烯马来酸共聚物及乙烯基醚马来酸共聚物。优选为部分水解或完全水解的聚乙烯醇。特别优选为水解度为80至95摩尔％且在浓度为4％的水溶液中的
粘度为1至30毫帕斯卡·秒(
法，在20℃下，DIN 53015)的部分水解的聚乙烯醇。
由此获得的含水分散体的固体含量为30至75重量％，优选为50至60重量％。
任选在添加其他保护胶体作为干燥助剂之后对该分散体实施干燥，例如利用流化床干燥、冻干或喷干，以制备水中可再分散的聚合物粉末组合物。优选对分散体实施喷干。在此，于常规的喷干装置内实施喷干，其中可利用单料喷嘴、双料喷嘴或多料喷嘴或者利用转盘实施雾化。取决于装置、树脂的Tg及预期的干燥度，通常选定出口温度为45℃至120℃，优选为60℃至90℃。由固体含量调节待雾化物料的粘度，从而获得小于500毫帕斯卡·秒(20转及23℃下的Brookfield粘度)，优选小于250毫帕斯卡·秒的数值。该待雾化的分散体的固体含量大于35％，优选大于40％。
以该分散体的聚合物成分为基准，干燥助剂的总使用量通常为0.5至30重量％。换而言之，以聚合物部分为基准，该干燥过程之前保护胶体的总使用量应为至少1至30重量％；以形成薄膜的聚合物部分为基准，优选使用总计5至20重量％的保护胶体。
合适的干燥助剂例如是上述的保护胶体。
已反复证实，基于基础聚合物，含量最高为1.5重量％的抑泡剂在雾化期间是有利的。通过提高抗结块性以提高存储稳定性，特别是在具有低玻璃态转化温度的粉末的情况下，以聚合物成分的总重量为基准，所得粉末可含有优选为1至30重量％的抗结块剂。抗结块剂的实例是：碳酸钙、碳酸镁、滑石、石膏、二氧化硅、高岭土如偏高岭土、硅酸盐，其粒径优选为10纳米至10微米。
更优选的再分散粉末组合物含有乙酸乙烯酯和乙烯的共聚物或者乙酸乙烯酯、乙烯和具有9至11个碳原子的α-分支单羧酸的乙烯基酯的共聚物，作为基础聚合物，以及部分水解的聚乙烯醇作为保护胶体。
软木颗粒以平均粒径为0.05至500mm的颗粒或软木粉的形式存在。特别合适的还有软木颗粒，其是在制造其他软木物品如瓶塞软木时作为废物产生的(传输软木)，并且例如通过研磨而达到所期望的粒径。
例如在热混合器内将水中可再分散的聚合物粉末与软木颗粒混合以制备成型体。在此，均基于软木和聚合物的总重量，聚合物粉末的添加比例为4至70重量％，优选为10至60重量％，更优选为10至40重量％，并通过传统的热塑性成型技术如挤出、注射、压制、造粒和压延而加工成为成型体。加工温度通常为60℃至200℃，优选为90℃至150℃。优选在提高的压力下进行操作。
该混合物任选还包含其他添加剂，例如润滑剂，如硬脂酸钙、增塑剂、抗氧剂、UV稳定剂、染料、颜料、填料、加工助剂，或用于后交联的过氧化物，如过氧二碳酸盐。在水中可再分散的聚合物粉末还可加入包含传统热塑性塑料、弹性体和热固性塑料的混合物中。
该方法适合于制备基于软木的各种不同的成型体。其实例是瓶塞软木、板状的绝热材料及隔音材料、密封垫、防震材料、墙涂层、地板涂层及办公用品。其他实例是用于制鞋业、服装业、家具业、运动器材业、娱乐业和建筑业中的材料。
该方法的特征在于，以相对较少量的可再分散的聚合物粉末获得具有高机械强度的成型体。因为聚合物粘结剂的含量少，所以保留了软木的天然外观。尤其是优选的由聚乙烯醇稳定化的可再分散的聚合物粉末中聚乙烯醇含量带来高的机械强度。在使用基础聚合物的Tg为-40℃至+60℃的聚合物粉末时，所得成型体的特征在于，机械强度高且弹性高。
具体实施方式
以下实施例用于进一步阐述本发明：
以下材料用于测试：
来自Wacker化学股份公司的可再分散的聚合物粉末Vinnex LL2504：
基于Tg为-7℃的乙酸乙烯酯-乙烯共聚物的由聚乙烯醇稳定化的聚合物粉末。
来自Amorin的软木BD 0.5/1：
粒径为0.5至1mm的软木颗粒。
K值为70且肖氏A硬度为70的热稳定化的增塑剂S-PVC。
将所述材料以表中所列的用量比例加以混合，并加工成为成型体。
将该混合物在Collin双辊轧机上于150℃至170℃的温度下轧制成厚度为1mm的轧片。
使用Collin标准压机将该混合物在150℃至170℃的温度下压制成厚度为4mm的压片。
根据ISO 1183测定轧片的密度，并根据ISO 1184测定压片的密度。
利用根据ISO 8307的方法测定压片的回弹性，并利用根据ISO 868的方法测定压片的肖氏A硬度。
在拉伸实验中测定轧片的机械强度，根据ISO 527-1/2测定伸长率，并根据ISO 527-1/3测定断裂强度。
结果汇总于表中。
表：
| 配制品 | 实施例1 | 实施例2 | 实施例3 | 比较例4 |
| RD粉末[重量份] | 20 | 30 | 40 | |
| 软木颗粒[重量份] | 80 | 70 | 60 | 60 |
| S-PVC[重量份] | 40 | |||
| 轧片密度[kg/m3] | 0.4060 | 0.6373 | 0.6028 | 0.6376 |
| 压片密度[kg/m3] | 0.6469 | 0.6644 | 0.7093 | 0.7044 |
| 回弹性[％] | 28 | 24 | 20 | 23 |
| 肖氏A硬度 | 80.5 | 80.5 | 79.8 | 79.6 |
| 伸长率[％] | 15.75 | 48.77 | 53.52 | 12.08 |
| 断裂强度[mpa] | 3.21 | 4.51 | 5.82 | 2.51 |
拉伸实验的结果表明，与以传统方式用PVC粘结的软木成型体(比较例4)相比，根据本发明所制的成型体的伸长率明显更高且断裂强度更高(实施例3)。
Claims (10)
1、用于由软木颗粒制备成型体的方法，其中用热塑性聚合物粘结所述软木颗粒，其特征在于，该热塑性聚合物以其水中可再分散的聚合物粉末的形式加以使用，该水中可再分散的聚合物粉末包含一种或更多种聚合物、一种或更多种保护胶体以及任选存在的抗结块剂。
2、根据权利要求1的方法，其特征在于，所述水中可再分散的聚合物粉末包含基于一种或更多种选自以下组中的单体的聚合物：乙烯基酯、(甲基)丙烯酸酯、乙烯基芳烃、烯烃、1，3-二烯烃及卤乙烯以及任选存在的可与上述单体共聚合的其他单体。
3、根据权利要求1或2的方法，其特征在于，所述水中可再分散的聚合物粉末包含玻璃化转变温度Tg为-20℃至+80℃的聚合物。
4、根据权利要求1至3之一的方法，其特征在于，所述水中可再分散的聚合物粉末含有包含一种或更多种选自以下组中的单体的均聚物或共聚物：乙酸乙烯酯、具有9至11个碳原子的α-分支单羧酸的乙烯基酯、氯乙烯、乙烯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸2-乙基己酯和苯乙烯，以及部分水解的聚乙烯醇作为保护胶体。
5、根据权利要求1至4之一的方法，其特征在于，所述软木颗粒以粒径为0.05至5mm的颗粒或软木粉的形式存在。
6、根据权利要求1至5之一的方法，其特征在于，基于软木和聚合物的总重量，所述水中可再分散的聚合物粉末的添加比例为4至70重量％。
7、根据权利要求1至6之一的方法，其特征在于，通过传统的热塑性成型技术，如挤出、注塑、压制、造粒和压延，而加工成为成型体。
8、利用权利要求1至7之一的方法由软木颗粒制得的成型体。
9、根据权利要求8的成型体用于瓶塞软木、板状的绝热材料及隔音材料、密封垫、防震材料、墙涂层、地板涂层及办公用品的用途。
10、根据权利要求8的成型体用于制鞋业、服装业、家具业、运动器材业、娱乐业和建筑业中的材料的用途。
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| PCT/EP2007/051102 WO2007093521A1 (de) | 2006-02-13 | 2007-02-06 | Verfahren zur herstellung von formteilen aus korkpartikeln |
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| CN (1) | CN101384666B (zh) |
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| CN102494135A (zh) * | 2011-12-15 | 2012-06-13 | 上海市电力公司 | 一种油浸式电力变压器用软木橡胶混合密封圈 |
| CN103849155A (zh) * | 2012-12-07 | 2014-06-11 | 成都俊马密封制品有限公司 | 纤维软木橡胶密封材料及其制备方法 |
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| US9688040B2 (en) | 2012-06-08 | 2017-06-27 | Nomacorc Llc | Method of preparing a closure for a product-retaining container |
| CN106957521A (zh) * | 2017-02-27 | 2017-07-18 | 佛山市因诺维生物科技有限公司 | 一种用于建筑领域的新型吸音材料及其制备方法 |
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- 2006-02-13 DE DE102006006579A patent/DE102006006579A1/de not_active Withdrawn
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- 2007-02-06 CN CN2007800053702A patent/CN101384666B/zh not_active Expired - Fee Related
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| CN110983912A (zh) * | 2019-12-25 | 2020-04-10 | 山东森盟工艺制品有限公司 | 软木预聚体的制备方法及其应用和软木地面的施工方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| DE502007001036D1 (de) | 2009-08-20 |
| EP1984452B1 (de) | 2009-07-08 |
| EP1984452A1 (de) | 2008-10-29 |
| KR20080089475A (ko) | 2008-10-06 |
| CN101384666B (zh) | 2012-11-21 |
| US20080300345A1 (en) | 2008-12-04 |
| WO2007093521A1 (de) | 2007-08-23 |
| ATE435889T1 (de) | 2009-07-15 |
| JP2009526884A (ja) | 2009-07-23 |
| KR100967575B1 (ko) | 2010-07-05 |
| US8283394B2 (en) | 2012-10-09 |
| DE102006006579A1 (de) | 2007-08-23 |
| JP4960975B2 (ja) | 2012-06-27 |
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