CN112703394A - 气体检测器 - Google Patents

气体检测器 Download PDF

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Publication number
CN112703394A
CN112703394A CN201980053883.3A CN201980053883A CN112703394A CN 112703394 A CN112703394 A CN 112703394A CN 201980053883 A CN201980053883 A CN 201980053883A CN 112703394 A CN112703394 A CN 112703394A
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CN
China
Prior art keywords
gas
filter
organic polymer
membrane
siloxane
Prior art date
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Pending
Application number
CN201980053883.3A
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English (en)
Inventor
竹内雅人
古野纯平
福井健太
井泽邦之
佐井正和
三桥弘和
谷口卓史
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Public University Legal Person Osaka
Figaro Engineering Inc
New Cosmos Electric Co Ltd
University Public Corporation Osaka
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Public University Legal Person Osaka
Figaro Engineering Inc
New Cosmos Electric Co Ltd
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Publication date
Application filed by Public University Legal Person Osaka, Figaro Engineering Inc, New Cosmos Electric Co Ltd filed Critical Public University Legal Person Osaka
Publication of CN112703394A publication Critical patent/CN112703394A/zh
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Abstract

本申请在气体传感器的壳体内收纳有气体检测部，经由安装于壳体的过滤器将壳体外的气氛气导入气体检测部。过滤器具有为透气性且用于除去硅氧烷的有机高分子过滤器以及用于除去醇且使检测对象气体透过的无机过滤器。

Description

气体检测器
技术领域
本发明涉及气体传感器等的气体检测器，特别涉及其过滤器。
背景技术
已知将PTFE(聚四氟乙烯)等有机高分子透气性膜作为气体传感器的过滤器(专利文献1)。还开发了具有高的气体透过性和高的气体选择性的气体选择性透过膜(非专利文献1)。不论是PTFE膜的情况还是气体选择性透过膜的情况下，都是分子量小的氢、甲烷等气体快速透过膜，分子量大的甲苯等气体仅能缓慢透过膜。
气体传感器存在容易因硅氧烷而中毒的问题。由于硅氧烷的分子量大，所以有机高分子透气性膜有希望作为硅氧烷的过滤器。然而，由于有机高分子透气性膜根据分子量来筛选气体，所以在检测甲烷、LPG、CO等检测对象气体时，并不适合除去乙醇。此外，乙醇是日常产生的杂质气体的代表，会妨碍检测对象气体的检测。作为杂质气体，在乙醇以外还有丙酮、异丙醇、甲醇等。
现有技术文献
专利文献
专利文献1：日本特开2008-128687A
专利文献2：WO2017-138190A
非专利文献
非专利文献1：Energy-efficient polymeric gas separation membranes for asustainable future:A review；Davide F.Sanders,et al.Polymer 54(2013)4719-4761
发明内容
发明所要解决的问题
本发明的课题在于提供除去硅氧烷和乙醇等杂质气体的气体检测器用的过滤器。
用于解决问题的手段
本发明的特征在于：在经由过滤器将气氛气导入气体检测部的气体检测器中，过滤器具有：透气性且用于除去硅氧烷、使检测对象气体透过的包含有机高分子膜的有机高分子过滤器；以及用于除去醇且使检测对象气体透过的无机过滤器。优选气体检测器为气体传感器，除了具有气体检测部和过滤器以外，还具有收纳气体检测部且安装有过滤器的壳体。另外过滤器也可以设置在气体传感器的壳体的外部。例如，可以将没有过滤器的气体传感器收纳在抽吸管的基端等，在管的前端等去往气体传感器的气体流路的上游侧设置本发明的过滤器。这样设置，过滤器的作用也相同。
在本发明中，在过滤器设置透气性且用于除去硅氧烷的有机高分子过滤器、和用于除去醇且使检测对象气体透过的无机过滤器。有机高分子过滤器根据分子量等来筛选气体，阻止硅氧烷的透过。有机高分子过滤器的材料中有PTFE膜等的氟树脂膜、作为气体选择性透过膜已知的高透气性的有机高分子的合成树脂膜等。氟树脂膜中，有像PTFE这样的透气性比较低的膜，以及像Teflon AF(Teflon是E.I.Dupont的注册商标)、Hyflon AD(Hyflon是Solvay的注册商标)、Cytop(Cytop是旭玻璃的商标)等这样高透气性的气体选择性透过膜等。另外，有机高分子膜可以是纤维素膜、岩藻依聚糖膜、壳聚糖膜等的多糖类的膜。有机高分子膜有透气性，根据分子量或者除了分子量以外还利用膜与分子的相互作用来筛选气体。而且有机高分子膜的种类是任意的。这些膜从外部气体中将分子量大的硅氧烷除去，使甲烷、LPG、CO等的检测对象气体、以及乙醇等的醇透过。此外，LPG比甲烷难以通过有机高分子过滤器，但由于只要检测出高浓度的LPG即可，所以有机高分子过滤器不妨碍LPG的检测。
无机过滤器包含活性炭、硅胶、沸石、中孔二氧化硅、硅酸铝等的无机吸附剂、或贵金属、金属氧化物等的氧化催化剂等。上述的氧化催化剂优选为在由上述的无机吸附剂形成的载体担载贵金属催化剂、金属氧化物催化剂等的氧化催化剂而成的催化剂、或在不为吸附剂的高分子的纤维(例如PTFE纤维)固定贵金属催化剂或金属氧化物催化剂等的氧化催化剂而成的催化剂，特别优选为在上述的无机吸附剂或高分子的纤维担载贵金属催化剂而成的催化剂。无机吸附剂吸附乙醇、甲醇、异丙醇等醇，此外也吸附丙酮等。氧化催化剂将这些杂质气体氧化而将其除去，如果在无机吸附剂担载氧化催化剂，则会产生杂质气体的吸附和氧化的2个过程。无机过滤器的形态为任意，例如活性炭的情况下，可以为粒状，也可以为由纤维状活性炭形成的片状。这些无机吸附剂的大部分，除了MS5A(分子筛5A)等的细孔径小的吸附剂以外，也吸附硅氧烷。
有机高分子过滤器和无机过滤器哪一个配置在外气侧都没有关系，但优选由无机过滤器处理透过有机高分子过滤器的气氛气。特别是优选用包含氧化催化剂的无机过滤器处理透过有机高分子过滤器的气氛气。如果在比氧化催化剂靠上游侧将硅氧烷除去，则除了能够防止气体检测部的中毒以外，还可以防止氧化催化剂的中毒。最优选在无机过滤器的外侧(外气侧)和内侧(气体检测部侧)的双方都设置有机高分子过滤器。这样设置，能够充分保护气体检测部不中毒。
在使有机高分子过滤器和无机过滤器为一体的情况下，可以在片状的无机过滤器层叠有机高分子过滤器，也可以进而将片状的无机过滤器作为支撑层形成有机高分子膜。后者的情况下，无机过滤器的纤维或颗粒与有机高分子膜一体化。
在本发明中，利用有机高分子膜将硅氧烷从外气除去，利用无机过滤器将醇除去。因此，气体检测器或气体传感器能够没有硅氧烷导致的中毒且没有因醇引起的误报地检测甲烷、LPG、CO等检测对象气体。
优选有机高分子膜含有酸性基团或碱性基团。特别优选有机高分子膜为具有羧基的羧甲基纤维素的膜、硫酸化纤维素的膜、岩藻依聚糖的膜、其他酸性多糖类的膜或具有氨基的壳聚糖的膜。
有机高分子膜由于硅氧烷的透过慢，而且硅氧烷对膜的溶解热或吸附热大，所以被认为在膜内长时间存在。然而，可以认为如果硅氧烷在膜内积累，则硅氧烷会透过膜，而使气体检测部中毒。
发明人们确认了如果在中孔二氧化硅中导入磺基，则硅氧烷会发生聚合(专利文献2)。聚合机理被认为是通过磺基的硅氧烷的水解。吸附在中孔二氧化硅的细孔内的硅氧烷分子通过吸附脱附平衡而能够脱离到气相中，但在有机高分子膜中扩散的硅氧烷分子应当移动较为受限制。因此，比磺基的酸性弱的羧基、磷酸基等也应该能够固定硅氧烷使其聚合。另外由于硅氧烷的聚合被认为是水解，因此氨基、碱性羟基等的碱性基团也应该能够使硅氧烷聚合。
Nafion(Nafion是E.I.Dupont的注册商标)具有氟树脂的骨架和磺基，能够以溶液的形态获得。因此，容易在气体选择性透过膜中掺混Nafion，例如在气体选择性透过膜材料的溶液混合Nafion溶液进行成膜即可。另外也可以将具有碱性羟基的有机高分子阴离子离子导电体掺混到气体选择性透过膜材料中。
多糖类中有羧甲基纤维素这样的具有羧基的多糖、岩藻依聚糖、硫酸化纤维素这样的具有磺基的多糖、壳聚糖这样的具有氨基的多糖。另外，多糖类通常容易成膜，且多糖类的膜具有透气性。因此如果使用这些膜，能够将硅氧烷利用聚合等在膜内化学固定。
附图说明
图1是表示实施例的气体传感器的截面图。
图2是实施例中的层叠膜的截面图。
图3是实施例中的芯片的俯视图。
图4是表示实施例中的气体传感器的驱动模式的图。
图5是表示实施例和比较例对硅氧烷(D5×20ppm)的耐久性的图。
图6是将实施例和比较例的对乙醇200ppm的灵敏度换算为甲烷表示的图。
具体实施方式
以下表示用于实施本发明的最优实施例。
实施例
图1～图4表示实施例的气体传感器2，图5、图6表示试验结果。气体传感器2例如具有Si芯片4，Si芯片4为气体检测部的例子。Si芯片4被收纳于陶瓷等的壳体5，由芯片粘接等固定于壳体5内。陶瓷的盖6覆盖壳体5的开口部，从多个开口7将壳体外的气氛气向过滤器8供给。在盖6的内表面(Si芯片4侧的面)安装有膜状的过滤器8。过滤器8由有机高分子过滤器10和活性炭过滤器14的二层构成，有机高分子过滤器10被配置在壳体5的外气侧，活性炭过滤器14被配置在Si芯片4侧。活性炭过滤器14为无机过滤器的例子，可以为氧化催化剂过滤器等，优选在无机过滤器的两侧配置有机高分子过滤器10。另外，无机过滤器也可以叠层不同种类的过滤器来使用。此外，气体检测部的种类和壳体的结构是任意的。另外，Si芯片4的焊盘经由引线16，与设置于壳体5的端子17连接。
图2表示过滤器8的结构。有机高分子过滤器10是在多孔质的支撑膜11上层叠有透气性有机高分子膜12而成的，但也可以没有支撑膜11。支撑膜11为具有连续气孔的合成树脂或多糖类的膜，膜厚例如为1μm～100μm左右。透气性有机高分子膜12例如膜厚为0.1μm～5μm左右。活性炭过滤器14在实施例中由厚度1mm左右的纤维状活性炭的片形成，但也可以为粒状活性炭，还可以为硅胶、中孔二氧化硅、沸石、硅酸铝等，材质和形状是任意的。另外，也可以代替活性炭过滤器14，使用在这些吸附剂上担载贵金属等的氧化催化剂而成的过滤器或在高分子的纤维中固定有贵金属等的氧化催化剂而成的过滤器。
透气性有机高分子膜12为由多糖类的膜或合成高分子形成的气体选择性透过膜。在多糖类的膜中，由于长链状的分子容易规则地排列，所以容易产生连续的微孔。而且该微孔会成为气体的扩散路径，微孔的大小确定能够透过的分子的大小，不使分子大小大的硅氧烷透过，而使氢、甲烷、LPG、CO、乙醇等透过。合成高分子的气体选择性透过膜通常为高透气性的，气体的透过性依赖于分子大小，虽然使氢、甲烷、CO、LPG、乙醇等透过，但不透过硅氧烷。另外，高分子膜12能够通过浇铸、旋涂、喷涂、辊涂等来成膜。
如果在透气性有机高分子膜12(以下简称为高分子膜12)中导入羧基、磺基、磷酸基等的酸性基团、或氨基、碱性羟基等的碱性基团，这些基团会与硅氧烷分子的-(O-Si-O)-的部分结合。如果膜中的硅氧烷浓度增加，则硅氧烷分子的-(O-Si-O)-的部分被水解而聚合，在膜中被完全固定。因此，即使长时间暴露于高浓度的硅氧烷，硅氧烷也不会透过有机高分子过滤器10。
优选的高分子膜12为羧甲基纤维素、硫酸化纤维素、岩藻依聚糖、壳聚糖等的多糖类膜，具有羧基(羧甲基纤维素)、磺基(硫酸化纤维素和岩藻依聚糖)、氨基(壳聚糖)等的酸性基团或碱性基团。在多糖类的膜以外，也可以在合成树脂的气体选择性透过膜中导入酸性基团或碱性基团。例如在氟树脂系的气体选择性透过膜中掺混Nafion等的质子导电性高分子，或掺混氢氧根离子导电性高分子。
图3表示Si芯片4，Si芯片4在腔室26上具有包括电极和加热器的微热板20。加热板20被横梁24支撑，在加热板20上设置有膜状的金属氧化物半导体22。28为焊盘。
气体检测部不限于Si芯片4，气体的检测材料不限于金属氧化物半导体。例如可以将接触燃烧催化剂作为气体检测材料，在该情况下，将膜状的接触燃烧催化剂设置在加热板20上，或者在未图示的加热器线圈支撑接接触燃烧催化剂，均为任意。另外，在金属氧化物半导体22的情况下，也可以被加热板20以外的部件支撑。此外，作为气体检测部，也可以使用电化学气体传感器，该电化学气体传感器在液体或固体的电解质中连接有检测电极和对电极、或者除此之外还连接有参照电极。
图4表示气体传感器2的工作模式。气体传感器2以周期P工作，每1周期在时间T1期间被加热到250℃～450℃左右(实施例中为400℃)的工作温度，由加热时的金属氧化物半导体的电阻值，检测气体。
图5表示对硅氧烷的耐久试验(20ppm的D5中暴露10天)的结果。使用的气体传感器为图1～图3的气体传感器，实线的实施例中同时使用高分子膜(羧甲基纤维素)和片状活性炭，比较例中仅使用片状活性炭。测定氢100ppm中的输出，使用对氢浓度的输出的依赖性的初始值，换算成氢浓度。从100ppm的位移表示气体传感器的中毒的程度，在因硅氧烷导致的中毒中，通常浓度换算的输出增加。同样测定甲烷1000ppm中的输出，评价对硅氧烷的耐久性。通过设置有机高分子过滤器10，能够减小硅氧烷的影响。此外，由此可知，在代替活性炭过滤器14使用氧化催化剂过滤器的情况下，也能够通过有机高分子过滤器10防止氧化催化剂过滤器的中毒。
图6表示与乙醇200ppm的输出相等的甲烷浓度，A为无过滤器的比较例，B为仅高分子膜(羧甲基纤维素)的比较例，C为高分子膜(羧甲基纤维素)+片状活性炭的实施例。仅高分子膜时不能除去乙醇，但通过活性炭就除去了乙醇。
符号说明
2 气体传感器
4 Si芯片(气体检测部)
5 壳体
6 盖
7 开口
8 过滤器
10 有机高分子过滤器
11 支撑膜
12 透气性有机高分子膜
14 活性炭过滤器(无机过滤器)
16 引线
17 端子
20 微热板
22 金属氧化物半导体
24 横梁
26 腔室
28 焊盘

Claims (6)

1.一种气体检测器，其特征在于，在经由过滤器将气氛气导入气体检测部的气体检测器中，所述过滤器具有：
透气性且用于除去硅氧烷、使检测对象气体透过的包含有机高分子膜的有机高分子过滤器；以及
用于除去醇且使检测对象气体透过的无机过滤器。
2.根据权利要求1所述的气体检测器，其特征在于，所述气体检测器为气体传感器，其除了具有所述气体检测部和所述过滤器以外还具有收纳所述气体检测部且安装有所述过滤器的壳体。
3.根据权利要求2所述的气体检测器，其特征在于，在所述壳体内的位置关系上，所述有机高分子过滤器被配置在外气侧，所述无机过滤器被配置在气体检测部侧。
4.根据权利要求1～3中任一项所述的气体检测器，其特征在于，所述无机过滤器含有氧化催化剂。
5.根据权利要求1～4中任一项所述的气体检测器，其特征在于，所述有机高分子膜含有酸性基团或碱性基团。
6.根据权利要求5所述的气体检测器，其特征在于，所述有机高分子膜为具有羧基的羧甲基纤维素的膜、硫酸化纤维素的膜、岩藻依聚糖的膜或具有氨基的壳聚糖的膜。
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