CN1198109A - 经真空闪蒸蒸发的聚合物复合材料 - Google Patents
经真空闪蒸蒸发的聚合物复合材料 Download PDFInfo
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Abstract
公开了一种在真空下制备聚合物复合层的方法。具体地说,公开的方法包括把盐类溶于一种单体溶液中,溶液真空闪蒸蒸发,闪蒸蒸发后的溶液冷凝成液膜并将冷凝的液膜在底材上形成聚合物复合层。
Description
发明领域
本发明一般涉及一种在真空下制备聚合物复合层的方法。
具体地说,本发明涉及将盐类溶于一种单体溶液中、将该溶液闪蒸蒸发,并将蒸发后的溶液在基材上形成聚合物复合层。
发明背景
具有至少一个聚合物层的层压结构已被证实可用于多种用途,包括但不限于电子器件诸如电路元件和电致变色器件、包装材料以及太阳能反射器。也含离子或盐的聚合物层显示出在单个聚合物层中不存在的特性,因而,含有离子或盐类的聚合物或复合聚合物层,可能显示出各种特性,诸如较高的离子导电率,这些特性可使这些聚合物优于不含离子或盐类的聚合物,更适用于一些特殊用途。
本领域的技术人员已知有若干种在真空条件下大批生产聚合物和聚合物复合层的技术。例如使用包括但不限于挤压和单体涂布设备,诸如辊涂机、凹槽辊涂机、线绕刮涂杆(wound rod)刮板和槽孔口模等方法把液态单体或含有离子或盐类的液态单体溶液涂布在底材上并使之固化。
单体流体的真空闪蒸蒸发也已被证实是在层压结构内产生聚合物薄层的一种有用的工艺。但是,本技术领域的技术人员一直避免采用真空闪蒸蒸发法来形成聚合物复合层。盐类蒸发所需的温度一般太高,以致不允许按照闪蒸蒸发法把盐类包含在单体蒸发中。例如,本文参考文献中美国专利4,954,371“单体流体的闪蒸蒸发”公开了一种在低于该材料分解温度和聚合温度的温度下连续供应一种可聚合和/或可交联材料的方法。该物质被雾化成粒径从1到50微米的液滴。然后,上述液滴与加热到该物质的沸点以上的加热面接触但低于裂解温度,在真空下汽化。该方法指出,通过把上述蒸气在底材上冷凝成液体后,就可以将该物质进行聚合或交联,在层压结构中生成非常薄的聚合物层。
采用真空闪蒸蒸发法所提供的聚合物层,比其它方法生成的聚合物层具有一些优点,包括但不限于,生成更加均匀和更薄聚合物层的能力,残留在聚合物层下面的气体量较少,聚合物层内密度较大,聚合物层表面更光滑。
因此,本领域的技术人员会很有兴趣拥有一种能生成含有离子或盐类的聚合物复合层并拥有真空闪蒸蒸发法优点的方法。
发明概述
本发明依赖于下述意外发现,即:溶于单体溶液的盐类在完全溶剂化的情况下,按照真空闪蒸蒸发法,可与单体一起蒸发,并从而可用于在真空下生成复合聚合物层。具体地说,按照本发明,一种盐首先在一种单体溶液中实行完全溶剂化。然后,这一混合物可按照真空闪蒸蒸发法用来生成聚合物复合层。同时,在闪蒸蒸发之前,还可以把溶剂、光固化剂、增粘剂或滑爽剂混合加到上述单体/盐混合物中。优选实施方案的描述
在本发明的优选实施方案中,把一种盐溶于或溶剂化于一种可聚合和/或可交联的物质中,典型地是含有至少一种液态单体的单体溶液中,以生成一种可聚合的复合材料。这种盐可以是能在溶液中发生离解生成离子的任何离子型化合物,包括但不限于二元盐和配盐。凡本文中使用的配盐术语,均指具有两种以上元素的任何盐。在需要时,可加入其它组分,例如可以加入一种溶剂,以帮助该盐在该单体溶液实现溶剂化;也可加入一种增粘剂以帮助在基材上生成复合聚合物;或者加入一种光引发剂以帮助复合聚合物的聚合。一旦该盐溶解或溶剂化,则应将可聚合的复合材料按照真空闪蒸蒸发工艺进行加工;在加工过程中,可聚合的复合材料可以在真空下以基本均一的气相形式被连续地供应。这样,这种方法可让可聚合复合材料沉积在基材上,并在真空下生成复合聚合物层。
该可聚合复合材料在低于该材料分解温度和聚合温度的温度下被连接供应。该材料被雾化成粒径从约1到约50微米或更小的液滴。典型使用超声发生器进行雾化。也可以静电雾化。在约1千伏到约20千伏的高压下进行静电雾化,可以生成更加均匀的液滴,还可以改进蒸发过程。此外,还可使液滴带有电荷,使液滴被吸往带有相反电荷的加热面,从而增加液滴的通过量。然后,液滴因与被加热到该物质的沸点以上、但低于可能引起裂解的温度的加热面接触而蒸发。然后,蒸气与基材接触,该材料在基材上冷凝成液膜,然后发生聚合或交联,在真空下生成一层复合聚合物层。
优选是在进行闪蒸蒸发之前让该盐在单体溶液尽可能最大限度地充分溶剂化。溶剂化程度愈完全,则与单体溶液一起蒸发并进入聚合物复合层的盐量或离子量愈多。而且,盐与单体的浓度比,可以通过改变单体溶液中的盐量来加以调节。从单体中不加盐开始,可以加盐达到任何所需要的浓度,直至单体溶液达到饱和为止。
实例
按下列条件进行试验,将150毫升聚乙二醇二丙烯酸酯、150毫升聚乙二醇甲醚、15毫升丙烯酸增粘剂、30毫升从纽约HawthornCiba/Geigy公司买来的Darocure 4265光引发剂与20克LiCF3SO3混合,直至LiCF3SO3在混合物中完全溶剂化为止。然后,按照本发明的真空闪蒸蒸发法将该混合物纳入多层的层状复合材料中。该层状复合材料由放在交指型电容器结构内、位于两层铝之间的一层复合聚合物材料组成,其中每个层都是真空沉积的。然后,用标准电压计对多层层状复合材料进行测试,其电导与电解质材料相一致,说明LiCF3SO3盐的离子已经夹杂在聚合物中。
虽然上面对本发明的优选实施方案作了说明,但很明显,本领域的技术人员在更广泛的方面不背离本发明的情况下可以作出许多更改和改动。因此,所附的权利要求将覆盖落入本发明精神和范围的所有此类改动和更改。
Claims (6)
1.一种在真空下供应可聚合复合材料均匀蒸气的方法,所述方法包括:
a)将一种盐溶于一种单体中以生成所述复合材料,
b)在低于复合材料分解温度和聚合温度的温度下将所述复合材料的液流输送到真空环境中,
c)将此液流雾化成液滴流;和
d)让所述液滴与加热面接触而发生汽化,加热面的温度应保持在或高于所述复合材料的沸点,但低于所述液滴在汽化前发生裂解的温度。
2.权利要求1所述的方法,该方法用于在真空环境中将一层可聚合复合材料沉积在基材上,该方法进而包括下列步骤:
e)至少把所述基材的一部分保持在低于所述复合材料的沸点以下,并且在压力低于所述汽化的复合材料的区域内,使汽化后的复合材料正向流向所述基材;和
f)把汽化的复合材料流导向所述基材上。
3.权利要求2所述的方法,其中,所述的材料在其沸点或低于其沸点的温度下是化学不稳定的。
4.权利要求1所述的方法,其中雾化包括:
超声振动一个设备和分散以液滴形式送入该设备的复合材料。
5.权利要求4所述的方法,其中分散包括:
用所述复合材料涂布设备尖端处的一个端面;
超声振动所述端面,从而把所述液滴从端面的四周分散。
6.权利要求1所述的方法,其中雾化包括:
静电喷雾所述复合材料。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/508,278 US5681615A (en) | 1995-07-27 | 1995-07-27 | Vacuum flash evaporated polymer composites |
US08/508,278 | 1995-07-27 |
Publications (2)
Publication Number | Publication Date |
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CN1198109A true CN1198109A (zh) | 1998-11-04 |
CN1083301C CN1083301C (zh) | 2002-04-24 |
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Application Number | Title | Priority Date | Filing Date |
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CN96197266A Expired - Lifetime CN1083301C (zh) | 1995-07-27 | 1996-07-25 | 经真空闪蒸蒸发的聚合物复合材料 |
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Country | Link |
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US (1) | US5681615A (zh) |
EP (1) | EP0843599B1 (zh) |
JP (1) | JP3197563B2 (zh) |
KR (1) | KR100275191B1 (zh) |
CN (1) | CN1083301C (zh) |
AT (1) | ATE207390T1 (zh) |
CA (1) | CA2226496C (zh) |
DE (1) | DE69616344T2 (zh) |
ES (1) | ES2163647T3 (zh) |
MX (1) | MX9800732A (zh) |
WO (1) | WO1997004885A1 (zh) |
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US5032461A (en) * | 1983-12-19 | 1991-07-16 | Spectrum Control, Inc. | Method of making a multi-layered article |
US4842893A (en) * | 1983-12-19 | 1989-06-27 | Spectrum Control, Inc. | High speed process for coating substrates |
EP0242460A1 (en) * | 1985-01-18 | 1987-10-28 | SPECTRUM CONTROL, INC. (a Pennsylvania corporation) | Monomer atomizer for vaporization |
US4954371A (en) * | 1986-06-23 | 1990-09-04 | Spectrum Control, Inc. | Flash evaporation of monomer fluids |
DE3786063T2 (de) * | 1986-06-23 | 1993-09-09 | Spectrum Control Inc | Bedampfen von fluessigen monomeren. |
US5260095A (en) * | 1992-08-21 | 1993-11-09 | Battelle Memorial Institute | Vacuum deposition and curing of liquid monomers |
-
1995
- 1995-07-27 US US08/508,278 patent/US5681615A/en not_active Expired - Lifetime
-
1996
- 1996-07-25 CA CA002226496A patent/CA2226496C/en not_active Expired - Lifetime
- 1996-07-25 ES ES96927258T patent/ES2163647T3/es not_active Expired - Lifetime
- 1996-07-25 AT AT96927258T patent/ATE207390T1/de active
- 1996-07-25 KR KR1019980700495A patent/KR100275191B1/ko not_active IP Right Cessation
- 1996-07-25 WO PCT/US1996/012288 patent/WO1997004885A1/en active IP Right Grant
- 1996-07-25 DE DE69616344T patent/DE69616344T2/de not_active Expired - Lifetime
- 1996-07-25 EP EP96927258A patent/EP0843599B1/en not_active Expired - Lifetime
- 1996-07-25 CN CN96197266A patent/CN1083301C/zh not_active Expired - Lifetime
- 1996-07-25 JP JP50776497A patent/JP3197563B2/ja not_active Expired - Lifetime
-
1998
- 1998-01-26 MX MX9800732A patent/MX9800732A/es unknown
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1097472C (zh) * | 1998-08-07 | 2003-01-01 | 拜尔公司 | 蒸发热塑性聚合物的聚合物溶液的方法 |
CN101801545A (zh) * | 2007-02-06 | 2010-08-11 | 赛昂能源有限公司 | 可聚合单体与不可聚合载体溶剂/盐混合物/溶液的共闪蒸 |
CN101801545B (zh) * | 2007-02-06 | 2013-06-26 | 赛昂能源有限公司 | 可聚合单体与不可聚合载体溶剂/盐混合物/溶液的共闪蒸 |
Also Published As
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JPH11506045A (ja) | 1999-06-02 |
CA2226496C (en) | 2002-04-30 |
KR100275191B1 (ko) | 2001-02-01 |
EP0843599A1 (en) | 1998-05-27 |
JP3197563B2 (ja) | 2001-08-13 |
US5681615A (en) | 1997-10-28 |
DE69616344D1 (de) | 2001-11-29 |
CN1083301C (zh) | 2002-04-24 |
WO1997004885A1 (en) | 1997-02-13 |
CA2226496A1 (en) | 1997-02-13 |
DE69616344T2 (de) | 2002-07-11 |
MX9800732A (es) | 1998-11-29 |
ES2163647T3 (es) | 2002-02-01 |
ATE207390T1 (de) | 2001-11-15 |
KR19990035835A (ko) | 1999-05-25 |
EP0843599B1 (en) | 2001-10-24 |
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