CN102307655A - 吸附介质 - Google Patents
吸附介质 Download PDFInfo
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- CN102307655A CN102307655A CN2009801563434A CN200980156343A CN102307655A CN 102307655 A CN102307655 A CN 102307655A CN 2009801563434 A CN2009801563434 A CN 2009801563434A CN 200980156343 A CN200980156343 A CN 200980156343A CN 102307655 A CN102307655 A CN 102307655A
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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Abstract
公开了一种用于吸附系统的吸附介质和其制备方法。该介质包含较薄载体层如纸张，吸附剂如沸石和未活化沥青基碳纤维。较薄层、多孔介质提供了较快质量流的优点。因为该沥青基碳纤维未活化，所以它们保持其高热导率，因此，提供通过该介质的快速和高效的热扩散。
Description
发明背景
该公开内容涉及吸附系统。尤其是用于该系统的吸附介质。
技术领域
吸附系统如HVAC系统、液体和气体提纯、溶剂和汽油蒸气回收和除臭、吸着冷却工艺、某些大宗气体分离等有时使用吸附介质以除去气体混合物中的气相杂质或较强吸附的主要组分。吸附工艺和吸着冷却工艺通常采用一些设置在金属容器中的吸附介质，其可自支撑或含在金属筛网或表面上。将该吸附剂与含有吸附性组分的流体或气体料流在吸附所需条件范围内接触。
一些常规吸附介质由薄片或层如纸张、金属箔、聚合物膜等以及吸附剂材料如硅胶、活性氧化铝、活性碳和分子筛如沸石等组成。这些吸附剂片或层与常规珠粒、挤出物或颗粒相比更薄。因为更薄的介质提供从气相或液相进料到吸附部位的较短路径长度，所以通过这些吸附剂的传质比珠粒或颗粒更快。此外，大孔尺寸分布，特别是在含吸附剂的湿直纹纸张中的数量级一般来说可比通常吸附剂珠粒的数量级大。该较大的大孔尺寸还相对于珠粒或颗粒提高了介质的传质。
由于快速传质，在某些应用中可能变得难以消散吸附热。在吸附剂由薄膜或薄层介质组成时尤其如此，该介质通常具有低热导率。例如，纸张的热导率仅为0.05W/mK。就此为了显示其确实如此，Styrofoam，一种已知绝热体的热导率为0.033W/mK。该较低热导率引起整个物质热消散较慢。因此，实际上在吸附循环过程中加热吸附剂纸张或某些其他薄层吸附剂可减慢达到平衡，由此降低较薄吸附介质的吸附速度或传质益处。相似地，在脱附中，由于脱附除去热量，吸附剂的温度可以显著降低，这可减缓介质的脱附速度。
需要一种吸附介质，其提供了薄层(例如片、膜、箔、盘、纸张等)介质的传质优点，同时避免了与薄层介质中的吸附热消散有关的问题。
发明概述
本公开内容提供了一种吸附介质，该介质包含至少一种载体材料，吸附剂和5-30重量％未活化沥青基碳纤维。
本公开内容还提供了一种吸附介质，该介质包含至少一种选自纸张、金属箔和聚合物膜的载体材料，吸附剂和5-30重量％未活化沥青基碳纤维，其中该介质包含多孔薄层。
本公开内容还提供了一种制备吸附介质的方法，该方法包括提供包含水、原纤化聚合物纤维和沸石粉末的纸浆，并将沥青基碳纤维配制到纸浆中。
附图简述
图1显示了不含沥青基碳纤维的吸附介质在第一加载循环后的热流和表面温度对时间的图。
图2A显示了含沥青基碳纤维的图1中所示的介质在第一加载循环后的热流和表面温度对时间的图。
图2B显示了含沥青基碳纤维的图1中所示的介质在第二加载循环后的热流和表面温度对时间的图。
图2C显示了含沥青基碳纤维的图1中所示的介质在第三加载循环后的热流和表面温度对时间的图。
图2D显示了含沥青基碳纤维的图1中所示的介质在第四加载循环后的热流和表面温度对时间的图。
发明详述
本公开内容涉及吸附介质。该介质可用于非工业工艺和工业工艺如HVAC系统、液体和气体提纯、溶剂和汽油蒸气回收、大宗分离和除臭。具体而言，例如，该介质可用于吸附转轮如UOP LLC描述于US 7,166,149的那些，变压和变温吸附工艺如UOP LLC描述于US 6,293,998的那些或吸着激冷器如UOP LLC描述于US 6,102,107的那些。US 6,102,107公开一种吸附介质如层压到热交换器的板翅或管的第一和第二侧的纸层。使该吸附剂与含有吸附性组分的流体或气体料流在吸附和脱附所需条件范围内接触。该介质的一种形式尤其可以以涂层施用于热交换器表面上。
本公开内容的介质优选为由载体材料组成的介质的薄层，其可为纸张，例如由纤维材料组成。该介质还包含粘合剂、干燥剂或吸附材料和沥青基碳纤维。在一些情况下，该介质可为自支撑的。该介质可为纸张、金属箔、聚合物膜等。纸张类型的吸附剂的实例由UOP LLC公开于US5,650,221中并将其引入本文作为参考。该吸附剂纸层由载体材料组成，该载体材料可为纤维材料。它还包含吸附剂和粘合剂。该纤维材料包括纤维素纤维、合成纤维和其混合物。优选原纤化纤维，即在其端部分裂并形成原纤维，即比纤维轴细得多的细纤维或丝。可用于介质的吸附纸张的原纤化合成有机纤维的实例为原纤化芳族聚酰胺和丙烯酸类纤维。
该芳族聚酰胺可为人造纤维，其中形成纤维的物质为长链合成聚酰胺，其中至少85％酰胺(--CO--NH--)连接基团直接连接在两个芳族环上。优选芳族聚酰胺的实例为Twaron或KEVLAR。Twaron，可来自TeijinAramid，为耐热和强对芳族聚酰胺纤维，且可以以各种长度和原纤化程度得到。可用于该介质的Twaron的实例为Twaron 1094和1099。KEVLAR也是一种对芳族聚酰胺。它可来自E.I.du Pont de Nemours & Company且可以市购作为精制浆用于形成纸张，如KEVLAR 303浆。在精制过程中，通过施加高剪切将芳族聚酰胺纤维轴在端部分裂为原纤维，由此形成树状结构。在纸板的制造中，已发现原纤维互锁以提高该纸板的强度。芳族聚酰胺可在至多450℃的氧化氛围中稳定。其他耐高温芳族聚酰胺如可来自DuPont的NOMEX也适用于介质中纸张的形成。
该吸附材料可为能吸附吸附性组分如水、二氧化碳、烃类、氮气等的任何材料。这类材料可为无定形固体或结晶化合物。实例包括硅胶、活性氧化铝、活性碳、分子筛和其混合物。可用作吸附剂的其他材料例如包括卤化化合物如卤素盐，包括氯化物、溴化物和氟化物。
分子筛包括沸石分子筛。沸石为结晶硅铝酸盐组合物，其具有微孔且具有由顶点共享的AlO2和SiO2四面体形成的三维氧化物骨架。在介质中均可使用天然存在沸石和合成沸石。沸石的非限制性实例为结构类型为八面沸石、A、β等的沸石种类。八面沸石类型的沸石包括DDZ-70、Y-54、Y-74、Y-84、Y-85、蒸汽锻烧的稀土交换的Y-54、低铈稀土交换的Y-84、低铈稀土交换的沸石LZ-210以及其他八面沸石类型的沸石如沸石X和其混合物。DDZ-70为稀土交换的钠Y沸石如Y-54，其按照描述于均给予UOP LLC的US 5,512,083和US 5,667,560的方法蒸汽锻烧，将它们的整个内容引入本文作为参考。八面沸石类型的沸石为具有三维大孔结构的沸石，该结构由次级结构单元4元环、6元环和双6元环构成。八面沸石类型的沸石孔的直径为
在这些沸石中包括合成原态的沸石和与其他阳离子，例如Ca+交换的那些。非沸石分子筛为不含作为基本骨架组分的AlO2和SiO2四面体的那些，但是其显示出沸石的离子交换和/或吸附特性。也可用于该介质中的非沸石分子筛吸附剂的非限制性实例包括磷酸铝盐(aluminophosphate)或AlPO分子筛，磷酸硅铝(silicoaluminophosphate)，或SAPO分子筛，硅质岩(silicalite)I和硅质岩II或其他纯二氧化硅分子筛，和钛硅酸盐(titanosilicate)分子筛。
沸石分子筛的孔尺寸可通过采用不同金属阳离子而改变。例如钠沸石A具有
的明显孔尺寸，而钙沸石A具有的明显孔尺寸。本文所用短语“明显孔尺寸”可定义为所述分子筛在通常条件下的最大关键尺寸。明显孔尺寸比有效孔直径大，后者可定义为沸石结构中适当硅酸盐环的自由直径(free diameter)。呈锻烧形式的沸石分子筛可由以下通式表示：
Me2/nO:Al2O3:xSiO2:yH2O，
其中Me为阳离子，x具有2到无穷大的值，n为阳离子价态且y具有2-10的值。商业上已知为类型13X的分子筛组成的通式为1.0±0.2Na2O:1.00Al2O3:2.5±0.5SiO2加结合水。类型13X的立方晶体结构的特征在于具有可通过容许关键尺寸至多为
的分子的孔开口得到的相互连接的晶体内空隙的三维网络。该空隙体积为沸石的51体积％且大多数吸附在晶体空隙中进行。
该吸附剂可通过常规涂覆方法如滑流涂覆、浸渍、喷涂、幕涂、电泳涂覆和其组合涂覆在纸张、箔、膜、片或筛网上。或者，可将该吸附剂在纸张的生产过程中掺入纸片或也可使用在纸张的生产过程中掺入吸附剂和此后用吸附剂涂覆的组合。
如上所述，优选该介质由多孔薄层组成。尤其优选该层为大孔薄层。优选该介质具有基本均匀的厚度且为0.10-1.00mm(0.004-0.04英寸)厚。因此，该介质为吸附珠粒或颗粒厚度的1/2至1/20。因此，该介质提供较短的扩散程，这允许出入介质的较快传质速度。
该介质包含至少30重量％(30％)吸附剂。然而，吸附剂的重量百分数可对介质的厚度具有一定依赖性。例如如果最终厚度或厚度(caliper)为至少0.375mm(0.015英寸)厚，则它可更易于制备75-80重量％沸石纸张。优选该介质不大于1.00mm(0.040英寸)厚且含有大于60重量％吸附剂。在该介质中优选的吸附剂含量范围为60-85重量％。此外，该吸附剂可包含均匀的密度，其可通过调节配料(纸浆)组成、湿成层条件和压延处理而调节为0.5-1.1g/cm3。
该介质还包含沥青基碳纤维。优选该沥青基碳纤维未活化，然而，可使用未活化和活化沥青基碳的共混物，只要该介质如下所述包含5-30重量％未活化沥青基碳。在活性碳中，在碳化之后或碳化期间将碳加热，吹蒸汽或氧化以形成微孔性，这提供了吸附容量。因此，活性碳纤维有时用于补充或代替吸附剂如沸石。
通常将碳在反应性气体如二氧化碳存在下加热到至少800℃的温度以活化。这些氧化条件降低了沥青基碳纤维的热导率。根据US 6,800,364，在空气中在25℃下各向同性的沥青基纤维的热导率为10Watt/m-K。活化后，各向同性的沥青基纤维的热导率为0.25Watt/m-K(Vittorio等，TheTransport Properties of Activated Carbon Fibers，J.Mater.Res.，第6卷，第4期，1991年4月，第782页)。因此，未活化各向同性沥青基碳纤维的热导率比活化的各向同性沥青基碳纤维大40倍。中间相沥青基碳纤维将显示出在活化和未活化沥青基碳纤维之间相同或较大不同的热导率。可能活化的中间相沥青基碳纤维将产生热导率甚至更大的降低，因为中间相沥青基碳纤维通常具有比各向同性的沥青基碳纤维更高的热导率。因此，在活化时，更可能显著降低。
优选，该介质包含5-30重量％未活化沥青基碳纤维。更优选，该介质包含10-20重量％未活化沥青基碳纤维。这些量的沥青基碳纤维用于提供所需热导率。该介质如芳族聚酰胺-沸石-碳纤维复合材料的热导率预期与碳纤维的体积分数呈比例，无需为线性比例，且还与碳纤维纵横比有关，其在介质中优选为5∶1-20∶1。因此，例如仅1-2重量％碳纤维(这将就给定组分密度的体积百分数而言为0.5-1)的少量的材料不足以引起该介质传热能力的有效增加。此外，如果沥青基碳纤维以30重量％以上的水平使用，则吸附剂粉末的水平肯定会降低太多而不能另外将足够的芳族聚酰胺纤维掺入该片中以得到适当强度并且所得吸附纸张的容量将会太低而不能用于吸附工艺应用中。
所用沥青基碳纤维为含碳材料，其源于由石油或煤形成的中间相沥青。事实上该沥青基碳纤维可为任何市售沥青基碳纤维。优选，该沥青基碳纤维与纸张相比具有较高的热导率。该较高的热导率为20-1000W/mK。该沥青基碳纤维也可具有1.00-3.00g/cc的密度和5.00微米(0.0002英寸)至15微米(0.0006英寸)的直径。该类沥青基碳纤维包括可得自CytecIndustries of New Jersey和Toray Carbon Fibers America，Inc.ofAlabama的那些。
为了制备包含纸张层的介质层，例如将沥青基碳纤维配制到纸张配料中(淤浆)中，其如上所述还含有水、原纤化聚合物纤维如TWARON或KEVLAR浆、沸石粉末和絮凝添加剂。该纸张配料还可包含有机胶乳和/或无机氧化物粘合剂。这些片通过使配料在造纸机中湿成层而制备。所得纸张可配置有至多85重量％沸石粉末且可用于快速循环吸附工艺如变压吸附、变温吸附、变真空吸附和其组合以及吸附加热和冷却工艺。如上所述，优选该碳纤维没有活化，或者如果活化了，则仍含5-30重量％未活化沥青基碳纤维。只要至少5-30重量％未活化沥青基碳纤维使该介质可保持其热导率。
在较薄层介质中，传质比可使用珠粒或颗粒的吸附剂明显更高和更快。这是因为较薄介质提供了从气相或液相进料至平均吸附部位的显著较短的路径长度。此外，吸附介质的大孔尺寸分布的数量级一般来说比通常吸附珠粒的数量级大。该较大大孔尺寸还相对于颗粒珠粒提高了该介质的传质。
然而，在常规介质中，更快的传质可能变得难以消散吸附热。事实上，由于吸附具有高吸附热的分子，加热吸附剂可实际减慢达到平衡，因此降低较薄吸附介质的吸附速度和传质益处。相似地，在脱附下，由于脱附的热量去除而降低吸附剂温度，这降低了该介质的脱附性能。
如图1和2A-2B所示和下文所述，介质中的沥青基碳纤维极大地改善了该介质的热导率，因此利于吸附热的扩散。因此，该介质提供了由该介质的厚度导致的增加的质量流并提供了从沥青基碳纤维的必要热消散。
图1显示了吸附介质在下文说明的第一加载循环之后的热流和表面温度，该吸附介质为芳族聚酰胺/沸石纸张，不含沥青基碳纤维。图2A-2D显示了含20重量％THORNEL商标的沥青基碳纤维的吸附介质在四个加载循环之后的热流和表面温度。在图1和2A-2D中所示实例中，所用沸石为Y-54沸石。
为测量图1和2A-2D中所示的热流和表面温度，将热流转换器和热电偶与该介质连接。该介质的位置与热流转换器(BF-02，来自VatellElectronics)接触，其夹在介质样品和恒温为30.0℃的高热导率受热器之间。所用受热器为在恒温浴相反侧具有快速流体循环的薄不锈钢工作台。与吸附相关的样品中产生或除去的热量因此通过热流转换器通入和通出该受热器，只要样品温度与该受热器的温度不同，由此在热流转换器中产生与热流的大小成比例的电压信号。具有数毫秒响应时间的精细量规热电偶的位置与介质样品的另一侧接触。
排出样品池和连接的真空系统。然后进行第一加载或计量进料循环。具体而言，在30.0℃的温度下将10托水蒸气计量加入计量加料容器中，其然后向样品池打开，开始将水蒸气吸附到片状样品中。随着水吸附进行且吸附热引起片状样品的温度变化而测量表面温度和热流。使该介质冷却至30.0℃的环境温度。然后进行第二加载循环。相似地，如上所述将另外10托水蒸气计量加料加入该系统。测量表面温度和热流。该水蒸气加载或计量加料程序对不含沥青基碳纤维的介质总共进行4次，且对含沥青基碳纤维的介质总共进行4次。在该工艺中可利用的水吸附容量基本饱和。
随着用水将该介质变得越加饱和，在各水蒸气计量加料后，测量较小的表面温度增加和降低的热流电压。这与现有技术已知的一致；吸附热取决于对沸石的加载百分数。例如，在图2A中所示的沥青基碳纤维介质的第一加载循环中，表面温度达到62℃。然而，在图2B所示的第二加载中，表面温度仅达到35℃。此外，如图2A-2D所示和下文所述，通过热流测量的介质达到环境温度的时间随着各循环缩短。
在不含沥青基碳纤维的介质的第一加载循环中，表面温度达到43℃。热流达到0.34Watt/cm2。热流在450秒后回到0Watt/cm2且表面温度在450秒后冷却至环境温度(30.0℃)。这些结果显示在图1中。在第二加载循环中(未显示)，表面温度达到37℃。热流达到0.23Watt/cm2。热流在250秒后回到0Watt/cm2且表面温度在250秒后冷却至环境温度。在第三加载循环中(未显示)，表面温度开始为37℃。热流达到0.5Watt/cm2。在150秒后，热流回到0Watt/cm2且表面温度冷却至环境温度。在第四加载循环中(未显示)，表面温度为31℃。热流达到0.1Watt/cm2。在120秒后，热流回到0Watt/cm2且表面温度冷却至环境温度。
如图2A所示，在含沥青基碳纤维的介质的第一加载循环中，表面温度达到62℃。热流达到0.59Watt/cm2。热流在200秒后回到0Watt/cm2且表面温度在200秒后冷却至环境温度(30.0℃)。在图2B中所示的第二加载中，表面温度达到35℃。热流达到0.13Watt/cm2。热流在130秒后回到0Watt/cm2且在表面温度在180秒后冷却至环境温度。在图2C中所示的第三加载中，表面温度开始为30.5℃。热流达到0.09Watt/cm2。热流在90秒后回到0Watt/cm2且表面温度在160秒(在该数据中有干些扰且冷却时间中有不确定度)后似乎冷却至环境温度。在图2D中所示的第四加载中，表面温度为30℃。热流达到0.3Watt/cm2。在50秒后，热流回到0Watt/cm2且表面温度冷却至环境温度。
图1和2A-2D基本显示了相对于时间而言的热消散量。如上所述，在含沥青基碳纤维的介质中的吸附过程中产生的热量的消散比在不含沥青基碳纤维的介质中的吸附过程中产生的热量快得多。例如，在使用沥青基碳纤维介质的第一运转中热流回到0Watt/cm2耗时仅200秒，而在使用不含沥青基碳纤维的碳纤维介质的第一运转中热流回到0Watt/cm2耗时450秒。同样，由含沥青基碳纤维的介质的吸附热产生的表面温度的增加冷却至环境温度比不含沥青基碳纤维的介质的表面温度的增加冷却至环境温度快得多。相对于时间的热流和表面温度的这些测量值是沥青基碳纤维介质提供的热消散的改善的真正度量。
在另外的形式中，将介质适当涂覆在例如热交换器的表面上。在该形式中，介质可由有机淤浆中的有机硅氧烷树脂与沸石吸附剂组成或可由含水淤浆中的无机粘合剂与沸石吸附剂组成。该介质还可由沥青基碳纤维组成。这些沥青基碳纤维优选未活化，然而，它们可包含活化和未活化沥青基碳纤维的混合物。该介质和提供的涂覆方法使介质可涂覆在比常规介质相对较大且更复杂或盘旋状表面积(例如波浪形表面)。设计将粘合剂固化为硬质吸附剂涂层的热处理方法以避免降低沥青基碳纤维的热导率性能。例如涂料淤浆的挥发性组分通过在惰性或还原氛围中或在真空下加热至450-600℃而除去。
尽管就示例性实施方案而言已描述了该介质，但它并不限于此。而是所附权利要求书应宽范围解释以包括其他变体和实施方案，其可由本领域熟练技术人员在不背离等同物的目标和范围下做出。本公开内容用于包括本文所述任意修改或变化。因此要求保护参考前述说明和附图的如上所述的设备。
Claims (10)
1.一种吸附介质，其包含
至少一种载体材料；
吸附剂；和
5-30重量％未活化沥青基碳纤维。
2.权利要求1的介质，其中所述载体材料选自纸张、金属箔和聚合物膜。
3.权利要求1的介质，其中所述吸附剂由沸石组成。
4.权利要求1的介质，其包含至少60重量％吸附剂。
5.权利要求1的介质，其具有0.10-1.00mm的基本均匀的厚度。
6.权利要求1的介质，其包含20重量％所述沥青基碳纤维。
7.权利要求1的介质，其中由吸附热产生的所述介质的表面温度的增加比不含沥青基碳纤维的类似介质的表面温度的增加更快回到环境温度。
8.权利要求1的介质，其中所述介质包含多孔薄层。
9.权利要求2的介质，其中所述载体材料为对芳族聚酰胺。
10.权利要求3的介质，其中所述沸石为八面沸石类型的沸石。
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| Application Number | Priority Date | Filing Date | Title |
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| US12146508P | 2008-12-10 | 2008-12-10 | |
| US61/121,465 | 2008-12-10 | ||
| PCT/US2009/058675 WO2010068326A1 (en) | 2008-12-10 | 2009-09-29 | Adsorbent media |
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| US (1) | US20110281721A1 (zh) |
| JP (1) | JP2012511425A (zh) |
| CN (1) | CN102307655A (zh) |
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| US9428639B2 (en) * | 2009-10-22 | 2016-08-30 | Profile Products Llc | Flocculant composition for dewatering solids laden slurries |
| US8323747B2 (en) * | 2010-06-25 | 2012-12-04 | Uop Llc | Zeolite containing wash coats for adsorber heat exchangers and temperature controlled adsorbers |
| US8506782B2 (en) * | 2010-08-13 | 2013-08-13 | Southwest Research Institute | Electrophoretic deposition of adsorbent media |
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| US4134743A (en) * | 1970-03-31 | 1979-01-16 | Gas Developments Corporation | Desiccant apparatus and method |
| EP0162645A1 (en) * | 1984-05-11 | 1985-11-27 | Masami Harada | Carbon-fiber-covered material |
| DE4200995C2 (de) * | 1991-01-21 | 2002-02-14 | Seibu Giken Fukuoka Kk | Verfahren zur Herstellung eines wabenförmigen Gasadsorptionselements oder eines wabenförmigen Katalysatorträgers |
| EP0517189A1 (en) * | 1991-06-03 | 1992-12-09 | Kuraray Co., Ltd. | Sheet containing activated carbon fiber, process for producing the same and use of the same |
| JPH0617321A (ja) * | 1992-06-25 | 1994-01-25 | Morinobu Endo | ピッチ系活性炭素繊維 |
| FR2698098B1 (fr) * | 1992-11-13 | 1994-12-16 | Ceca Sa | Blocs adsorbants pour pompes à chaleur chimiques et leur procédé d'obtention. |
| US6045700A (en) * | 1996-07-29 | 2000-04-04 | Solutia Inc. | Retrievable organic carbon scavengers for cleaning of contaminated surface water sediments |
| EP1143658A1 (en) * | 2000-04-03 | 2001-10-10 | Canal+ Technologies Société Anonyme | Authentication of data transmitted in a digital transmission system |
| US20040231828A1 (en) * | 2003-05-22 | 2004-11-25 | Dunne Stephen R. | Adsorber generator for use in sorption heat pump processes |
| US7166149B2 (en) * | 2004-01-12 | 2007-01-23 | Uop Llc | Adsorption process for continuous purification of high value gas feeds |
| JP2007245025A (ja) * | 2006-03-16 | 2007-09-27 | Mitsubishi Chemicals Corp | 吸着シート、吸着素子およびその製造方法ならびにこれらの用途 |
| JP4891011B2 (ja) * | 2006-09-13 | 2012-03-07 | 帝人株式会社 | 補強材・放熱材に適する炭素繊維集合体 |
| JP2008266586A (ja) * | 2007-03-27 | 2008-11-06 | Toyoda Gosei Co Ltd | 低電気伝導性高放熱性高分子材料及び成形体 |
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2009
- 2009-09-29 US US13/133,251 patent/US20110281721A1/en not_active Abandoned
- 2009-09-29 CA CA2746345A patent/CA2746345A1/en not_active Abandoned
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| CA2746345A1 (en) | 2010-06-17 |
| JP2012511425A (ja) | 2012-05-24 |
| US20110281721A1 (en) | 2011-11-17 |
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