TWI566819B - 自經塗佈之粒子製造碳物件 - Google Patents
自經塗佈之粒子製造碳物件 Download PDFInfo
- Publication number
- TWI566819B TWI566819B TW100141228A TW100141228A TWI566819B TW I566819 B TWI566819 B TW I566819B TW 100141228 A TW100141228 A TW 100141228A TW 100141228 A TW100141228 A TW 100141228A TW I566819 B TWI566819 B TW I566819B
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- particles
- article
- asphalt
- bitumen
- shape
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- 239000002245 particle Substances 0.000 title claims description 113
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 29
- 229910052799 carbon Inorganic materials 0.000 title claims description 21
- 239000010426 asphalt Substances 0.000 claims description 82
- 238000000576 coating method Methods 0.000 claims description 56
- 239000011248 coating agent Substances 0.000 claims description 49
- 239000007787 solid Substances 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 25
- 238000003763 carbonization Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000000571 coke Substances 0.000 claims description 6
- 239000011800 void material Substances 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
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- 239000000243 solution Substances 0.000 description 16
- 239000011295 pitch Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 229920000620 organic polymer Polymers 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 7
- 239000008096 xylene Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
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- 238000001125 extrusion Methods 0.000 description 3
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- 239000002243 precursor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000010420 art technique Methods 0.000 description 2
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- 238000009835 boiling Methods 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
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- 238000004626 scanning electron microscopy Methods 0.000 description 2
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
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- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004931 filters and membranes Substances 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 230000001172 regenerating effect Effects 0.000 description 1
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- 238000005245 sintering Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- C04B35/62802—Powder coating materials
- C04B35/62828—Non-oxide ceramics
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Description
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本發明之具體實例係關於碳質物件及製造該等碳質物件之方法。
碳質物件經常界定諸如機械部件、過濾基質、吸收材料或觸媒撐體之物體。碳質物件之性質包括適合於此類應用之孔隙率、重量、強度、溫度穩定性或惰性。舉例而言，固體碳或碳發泡體可形成碳質物件。
然而，用以製造具有所需性質之碳質物件的先前技術要求昂貴的專用前驅物及複雜的製程步驟。貫穿該等技術始終控制精確操作條件之困難限制了達成所需要的性質之能力。此外，用以產生碳發泡體之先前製程產出對於一些應用而言具有不足數量之不經濟的小批次。
用於製造該等物件之先前方法涉及到若干步驟，包括：a)任意混合黏結劑瀝青與碳粒子，b)形成該等物件之形狀，c)烘烤該等物件之所得預成形物，d)將不同的瀝青浸漬入該等預成形物中，及e)碳化該黏結劑及浸漬瀝青。由於在預成形物中的黏結劑瀝青需要浸漬以達成物件之所需密度，因此得到不足的碳。關於製程的不合需要之處在於，烘烤及浸漬步驟要求溫度的精確控制以避免瀝青流動及發泡。碳化亦導致重量損失及體積改變，從而導致在物件內產生裂縫、形狀發生變形及歸因於預成形物的組成中的黏結劑瀝青含量及不均一性而具有缺陷。
因此，存在對於碳質物件及製造碳質物件之方法的需要。
在一個具體實例中，一種製造物件之方法包括，藉由將瀝青塗層沈澱於在沈澱期間分散於懸浮液中之固體內核上來提供具有瀝青塗層之粒子，將粒子自懸浮液之液體分離，自粒子形成物件之形狀。將經形成為物件形狀之粒子加熱至高於400℃使得瀝青塗層碳化。粒子一旦在經形成為物件形狀之後即彼此互連且固定在一起，其中沿著該等粒子中之相毗連者的瀝青塗層彼此接觸且經碳化以產生物件。
根據一個具體實例，一種製造物件之方法包括，將由具有瀝青塗層的粒子形成之粉末衝壓成物件之形狀，其中該等粒子由於在壓力下彼此接觸而互連。將經衝壓成物件形狀之粉末加熱至高於400℃使得瀝青碳化。來自該等粒子中之相毗連者的瀝青因而碳化以提供具有經碳化材料之黏著網狀結構之物件。
對於一個具體實例，一種製造物件之方法包括，將溶解於溶劑中之瀝青溶液與固體顆粒物懸浮液混合，使得在所得混合物內相對於溶液內之瀝青之濃度降低可促進瀝青沈澱至固體顆粒物上。該方法另外包括將塗佈有瀝青的固體顆粒物之粒子自混合物之液體分離，及將自液體分離之粒子形成物件形狀，其中粒子藉由粒子之瀝青而彼此黏著。一旦將經形成為物件形狀的粒子加熱至高於400℃之後即將粒子之瀝青碳化，從而歸因於將粒子互連之瀝青之碳化來提供具有所需要的機械強度及組成之物件。
可藉由參考所提供之以下描述並結合隨附圖式來獲取本發明之更完整理解及其益處。
本發明之具體實例係關於自具有瀝青塗層的粒子製造碳質物件。加熱經形成為物件的形狀之粒子使得瀝青塗層碳化。粒子歸因於經形成為物件之形狀而彼此互連且固定在一起，其中沿著該等粒子中之相毗連者的瀝青塗層彼此接觸且經碳化以產生物件。
該等物件可包括開放的空隙空間且適合於眾多應用，諸如用於流體純化之過濾床、觸媒撐體、吸震器、吸附劑及輕質機械部件。因為碳在化學侵蝕性環境中(諸如在強鹼性及強酸性流體及氣體中)為惰性且在高溫下亦穩定，所以如本文中所描述而製造之物件包括具有均一孔分佈及所需要的孔大小之多孔碳物件，適用作在眾多工業應用中用於氣體及液體分離之過濾料及多孔膜。相比之下，諸如金屬及陶瓷膜之有機及無機過濾料及膜具有某些限制，包括有限的溫度範圍及溶液酸性且因為昂貴的前驅物及複雜的處理步驟及控制而不具有成本效率。與若未恰當地控制燒結溫度則熔化且變形之無機及金屬物件的製造不同，自粒子製得之物件在高於400℃下燒結時不會熔化或發生形狀變形，此係因為固體碳內核例如不在任何溫度下熔化，且在固體內核上之瀝青塗層最初將粒子固持在一起且自身在高於400℃下轉變為碳。
在一些具體實例中，粒子形成藉由將瀝青塗層塗覆於固體內核上而產生之粉末。固體內核為瀝青塗層提供支撐，同時在低於瀝青塗層軟化點之溫度下不發生分解或形狀變形。諸如研磨、粉碎或碾磨之方法可提供針對一些具體實例而調整尺寸之固體內核，以提供具有小於1毫米(mm)或小於0.5 mm之平均粒子大小的粒子。固體內核之組成取決於特定應用中指定之物件之所需最終組成及/或孔隙率。
固體內核之實例包括碳質材料，諸如焦炭、石墨或在經加熱至2200℃的石墨化溫度或以上之後即形成石墨之組成物。對於一些具體實例，不碳質之組成物可構成供瀝青塗層沈積之固體內核，且可存留於物件內或在製造物件期間移除以留下所得孔及經碳化之瀝青塗層。固體內核之此移除可包括固體內核之熱分解或化學溶解。
允許實現該移除之固體內核的適宜實例包括碳酸鋰、鋅、鋁及諸如聚乙烯之聚合物。在如本文中所描述將瀝青塗層碳化之後，鋅、碳酸鋰或鋁例如可藉由在酸性或鹼性溶液中處理而溶解。聚乙烯提供在瀝青塗層碳化期間且在高於瀝青塗層軟化點之溫度下分解之固體內核之實例。
在一些具體實例中，歸因於瀝青塗層之碳化及作為固體內核的碳質材料之使用或固體內核之移除，物件含有有限量之除碳以外的元素。如本文中所描述而製造之物件可因而在碳化之後含有以重量計至少95%的碳、以重量計至少98%的碳或以重量計至少99%的碳，且具有在約1%與約95%之間或小於約10%之孔隙率。在隨後加熱物件之後來自瀝青塗層之大於85%或大於90%的碳產率及瀝青塗層之均一性促進控制孔隙率且允許製造具有至少有限孔之物件(若想要的話)。
瀝青塗層覆蓋固體內核中之每一者的外表面之實質上所有部分或所有部分。安置於固體內核上之瀝青塗層的含量處於以重量計1%至80%或以重量計5%至50%的範圍中。在固體內核上之瀝青塗層的含量促進控制物件之孔隙率，此係因為瀝青塗層之含量可由塗佈條件調整且物件之孔隙率至少部分地基於本文教示中所給之瀝青塗層之含量。固體內核之粒子大小及分佈亦影響所製造之物件的孔隙率及孔大小。在沈積時且在加熱以使瀝青塗層碳化之前的瀝青塗層之碳含量超過50%、60%或70%。瀝青塗層之軟化點係指高於200℃或高於250℃之熔點。
在一些具體實例中，塗佈製程利用溶解於適宜溶劑中之瀝青(諸如石油瀝青或煤焦油瀝青)來形成塗層。用於溶解瀝青之適宜溶劑包括(例如且不加以限制)苯、甲苯、二甲苯、喹啉、四氫呋喃、萘、丙酮、環己烷、四氫萘、乙醚、水及甲基吡咯啶酮。在使用石油或煤焦油瀝青時，諸如甲苯、二甲苯、喹啉、四氫呋喃、四氫萘或萘之溶劑為適宜的。溶劑對瀝青之比率及所得瀝青溶液之溫度經控制以使得瀝青完全地或近乎完全地溶解於溶劑中。在一些具體實例中，在溶液中之溶劑對瀝青比率小於約4，小於約3，小於約2或小於約1。塗佈製程另外包括將固體內核混合於液體中且將所得懸浮液加熱至約20℃至約200℃之溫度。一旦接著將瀝青溶液引入於懸浮液中，則瀝青中之至少一部分沈澱至固體內核上以歸因於瀝青稀釋及/或溫度降低而形成瀝青塗層。固液分離回收待形成為物件之粒子。
一旦製備粒子，則產生物件之所需形狀及大小依賴於自粒子形成物件之物理屬性。形狀之此形成可在粒子之任何加熱之前發生，從而造成瀝青塗層之碳化。形成形狀之各種方法中之一者包括模製，諸如粒子之擠壓或鑄造。
對於一些具體實例，在模製期間粒子的壓縮可將粒子衝壓成界定物件之所需形狀，諸如板、桿或圓盤。模製可將每平方公分至少100公斤之壓力施加給粒子。在擠壓製程中，經由壓力差將粒子推動或抽吸通過具有對應橫截面之壓模以使具有所需要的物件形狀之粒子互連。在一些具體實例中，在高溫下(例如，高於瀝青塗層之軟化點)執行模製及/或在模製期間將添加劑(諸如針對瀝青塗層之溶劑)與粒子摻合會促進在一些具體實例中粒子形成為所需要的形狀。對於鑄造，粒子填充界定具有所需要的物件形狀之空穴的模具或壓模，且為了提供粒子之互連，粒子可經衝壓在一起及/或允許藉由在引入針對瀝青塗層的溶劑後的加熱或溶劑蒸發之後冷卻而固化。
在一些具體實例中，自粒子製造物件包括，將粒子與有機聚合物溶液混合以形成混合物，藉由擠壓、壓力模製(pressure molding)或頂注(tap casting)將混合物形成為物件之形狀，及將經形成為形狀之混合物加熱至高於50℃以蒸發有機聚合物溶液之溶劑，隨後在惰性氣體氛圍中加熱至高於400℃以分解有機聚合物溶液中之有機聚合物且使瀝青塗層碳化。有機聚合物溶液在物件製造期間促進粒子黏結在一起。適宜充當促進黏結劑之有機聚合物的實例包括聚乙烯醇、羧甲基纖維素、聚苯乙烯、聚乙酸乙烯酯、聚甲基丙烯酸甲酯、聚醯亞胺、含氟聚合物及聚丙烯腈。此等聚合化合物在高於400℃下分解且僅留下有限量之殘餘碳(例如以重量計小於物件的約5%或小於約10%)。溶劑溶解所選擇之有機聚合物且溶劑可選自水及其他有機溶劑。取決於有機聚合物溶液之黏度，有機聚合物之量處於以總固體重量計1%至10%的範圍中。
歸因於經形成為物件形狀，粒子彼此互連，其中沿著該等粒子中的相毗連者之瀝青塗層彼此接觸。在一些具體實例中，瀝青塗層提供粒子之全部黏著力，無需依賴於將黏結劑材料添加至粒子。物件可因此由經形成且碳化成物件之粒子組成或基本由經形成且碳化成物件之粒子組成。
在將粒子形成為所需要的形狀之後，於爐中在諸如氮氣之惰性氣體中加熱粒子來達成碳化。碳化係指主要行使增加粒子的碳/氫比率之功能的熱處理。在一些具體實例中，在惰性氛圍中且在至少400℃、約600℃至約1400℃、約700℃至約1300℃或約750℃至約1200℃之溫度下實行粒子之碳化達約0.1小時至約2小時。構成惰性氛圍之氣體的實例包括氮氣、氬氣、氦氣、二氧化碳、一氧化碳、氫氣或其組合。舉例而言，經形成為物件之形狀且接著在惰性氛圍中熱反應至至少650℃之粒子可產生物件。在一些具體實例中，碳化達到足夠之溫度(例如大於2000℃)以將粒子石墨化。
利用根據具有成本效率的前述技術製造之物件的應用自化學惰性、溫度穩定性及用以調整物件之可重現的特性(包括機械強度、孔隙率及孔大小)之能力獲益。一個實例利用自擠壓粒子而獲得之物件來作為沈積觸媒組成物之撐體。對於一個具體實例，使流體流以與形成過濾料和吸附劑中之一者的物件接觸之方式流過，從而自流體流移除污染物。使用該物件作為過濾膜允許顆粒物基於該物件的孔大小及孔隙率而根據大小選擇性地通過，諸如用作二氧化碳吸附劑材料之碳酸鈣。對於藉由加熱來再生吸附劑或觸媒組成物而言，使電流通過物件可提供接觸物件之任何介質的有效加熱，同時不會浪費能量來加熱具有流體(諸如蒸汽)的周邊區域。
圖1展示在將具有瀝青塗層100及固體內核102之粒子形成為一形狀以互連粒子之後且在碳化之前，在物件製造期間，穿過物件之部分的橫截面視圖。如所說明，在碳化之前藉由該形成而產生的在粒子之間的空隙空間促成物件之孔隙率。在將粒子形成為該形狀期間所施加之壓力量連同粒子之形狀及大小可影響物件密度及空隙空間之體積。
圖2說明穿過物件之碳質網狀結構200之部分的橫截面視圖，該碳質網狀結構200係如本文中所描述藉由自經塗佈的粒子移除內核而形成。在將粒子形成為一形狀以互連粒子之後，內核發生移除。僅來自粒子之塗層存留於物件內且經碳化以產生網狀結構200。
給出本發明之某些具體實例的以下實施例。藉由本發明之解釋來提供每一實施例，其為本發明的眾多具體實例中之一者，且不應將以下實施例解讀為限制或限定本發明之範疇。
實施例1：
在850℃下煅燒之具有8微米平均粒子大小之經煅燒的石油焦粉末如下塗佈有15%瀝青。藉由將34公克石油瀝青溶解於25公克二甲苯中來形成瀝青溶液。藉由將20公克焦炭粉末與130公克二甲苯混合來製備懸浮液。將瀝青溶液及懸浮液兩者加熱至沸點且接著混合在一起。將所得混合物在沸點下持續攪拌達五分鐘且隨後冷卻至周圍溫度(~23℃)。藉由過濾自混合物分離固體粒子，用二甲苯洗滌，且接著在真空下於100℃下乾燥達兩小時。經瀝青塗佈的焦炭粒子之所得乾燥固體粉末重達23.0公克，得到15%之瀝青塗層含量。
為形成形狀如圓盤之物件，將4公克經瀝青塗佈的焦炭粒子傾填至衝壓模(直徑1.25吋)中且在15噸之力下衝壓。接著將圓盤置於爐中且在氮氣氛圍中以1℃/分鐘之速率加熱至450℃且維持在此溫度下達4小時，且此後以5℃/分鐘之速率加熱至1000℃且保持在該溫度下達2小時。隨後，將爐冷卻至周圍溫度。在加熱之後圓盤重達3.82公克且具有保持為約1.25吋之直徑。在加熱之後圓盤之厚度經量測為4.2毫米(mm)。因而，將圓盤之密度計算為每立方公分1.15公克(g/cc)。因為焦炭粒子及經碳化的瀝青塗層具有接近2 g/cc之密度，所以圓盤之孔隙率為約43%。然而，圓盤具有高機械強度。如在圖1中所描繪，圓盤之掃描電子顯微鏡影像展示圓盤在互連粒子中間具有開放空隙空間且不論大小如何粒子均在邊緣處互連。
實施例2：
藉由將15公克碳酸鋰(Li2CO3)與25公克二甲苯球磨研磨達30分鐘來產生經研磨之碳酸鋰。接著藉由與在實施例1中將瀝青塗佈於焦炭粉末上的方式相同之方式來使經研磨的碳酸鋰塗佈有28%瀝青。另外，以與在實施例1中形成物件的方式相同之方式將4公克所得之經瀝青塗佈的碳酸鋰粉末衝壓成圓盤。
以與實施例1相似之方式加熱所得圓盤，但最終的碳化溫度為710℃而非1000℃。在碳化之後，將圓盤置於稀硝酸溶液中達三天以使得碳酸鋰溶解且濾去以留下形成圓盤之多孔碳網狀結構。在加熱及乾燥之後的圓盤重約0.85公克，得到約0.2 g/cc之密度及約90%之孔隙率。即使圓盤為多孔性的，圓盤仍具有機械強度。如以圖2來表示，圓盤之微結構的掃描電子顯微鏡影像展示與藉由複雜的製程及專用前驅物製造之一些碳發泡體相似之多孔性連續網狀結構。實施例1及實施例2表明使用經瀝青塗佈的粒子允許製造具有可控的孔隙率及孔大小之碳質物件。
實施例3：
為製備混合物，藉由將混合物球磨研磨達20分鐘來將10公克乙炔碳黑粉末(購自AlfaChemicals)均一地分散於250毫升二甲苯中。隨後，以與在實施例1中所描述的方式相同之方式來使碳黑粉末之顆粒物塗佈有24%瀝青。藉由以與在實施例1中所給出的方式相同之方式衝壓0.4公克此類經瀝青塗佈的碳黑粉末來製造圓盤。在710℃下將圓盤碳化。接著，圓盤之密度經量測為0.56 g/cc，孔隙率為68%。與在許多工業應用中適用作觸媒床及過濾料之基質類似，圓盤之橫截面微結構的掃描電子顯微鏡影像展示，所有奈米級碳粒子彼此互連以形成具有在10奈米與50奈米之間的均一奈米級孔之高度多孔性基質。
實施例4：
以與在實施例1中所描述的方式相同之方式，使20公克具有1微米平均粒子大小之經煅燒的焦炭粉末塗佈有15%的瀝青以提供經瀝青塗佈的焦炭粒子。藉由將10公克聚乙烯丁醛(Solutia公司之Butvar B-79)溶解於90公克50/50甲苯及甲醇混合物中來製得10%聚合物黏結劑溶液。藉由將5公克粒子與1公克聚合物黏結劑溶液混合來製備混合物。隨後，在直徑為1.25吋之壓模中以5噸之壓力衝壓1公克混合物。於70℃下在真空下乾燥所得圓盤達3小時且接著在爐中於氮氣下在850℃下加熱。圓盤此後具有1.1 g/cc之密度及40%之孔隙率。圓盤之橫截面微結構的掃描電子顯微鏡影像展示連續且均一之孔結構。在加熱期間聚乙烯丁醛分解，從而在圓盤中留下約3%之殘餘碳，或以圓盤之總重量計小於百萬分之600(ppm)的碳。
最後，應注意任何參考文獻之論述並不意謂承認其為本發明之先前技術，尤其對於公開日期可能在本申請案的優先權日期之後的任何參考文獻而言。同時，藉此將以下每一及每個申請專利範圍作為本發明之額外具體實例併入於此實施方式或說明書中。
儘管已詳細描述本文中所描述之系統及製程，但應理解可在不偏離如由以下申請專利範圍限定之本發明的精神及範疇之情況下做出各種改變、替換及變更。熟習此項技術者可能能夠研究較佳具體實例且識別出並未在本文中精確描述之用以實踐本發明之其他方式。發明人之意圖在於本發明之變體及等效物處於申請專利範圍之範疇內，同時說明書、摘要及圖式並非用以限制本發明之範疇。本發明特定地意欲如以下申請專利範圍及其等效物一樣廣泛。
100．．．瀝青塗層
102．．．固體內核
200．．．碳質網狀結構
圖1為根據本發明之一個具體實例，在製造用經塗佈的粒子形成之物件期間，物件之橫截面示意性表示。
圖2為根據本發明之一個具體實例，藉由自經塗佈的粒子移除內核而形成之碳質網狀結構的橫截面示意性描繪。
100．．．瀝青塗層
102．．．固體內核
Claims (18)
- 一種方法，其包含：藉由將瀝青塗層沈澱於在該沈澱期間分散於懸浮液中之固體內核上以提供粒子，將該等粒子自該懸浮液之液體分離，自該等粒子形成物件之形狀；及藉由將經形成為該形狀之該等粒子加熱至高於400℃來碳化該等瀝青塗層，使得因經形成為該形狀而彼此互連之該等粒子固定在一起，其中沿著該等粒子中之相毗連者的瀝青塗層彼此接觸且經碳化以產生該物件；其中在碳化期間且在高於該等瀝青塗層之軟化點之溫度下，該等固體內核分解。
- 如申請專利範圍第1項之方法，其進一步包含自該物件移除粒子中之固體內核以改變該物件之孔隙率。
- 如申請專利範圍第1項之方法，其中該物件之形成取決於該等瀝青塗層以達該等粒子之互連，而無需將黏結劑材料添加至該等粒子。
- 如申請專利範圍第1項之方法，其中該物件形狀之形成包括在模具中將該等粒子壓在一起。
- 如申請專利範圍第1項之方法，其中焦炭材料及碳酸鋰中之一者形成該等固體內核。
- 如申請專利範圍第1項之方法，其中在碳化之前該等瀝青塗層之碳含量為至少50%。
- 如申請專利範圍第1項之方法，其進一步包含一旦該等瀝青塗層碳化之後，即用溶劑自該物件溶解出該等粒子 的固體內核。
- 如申請專利範圍第1項之方法，其進一步包含至少部分地基於該等固體內核上之瀝青塗層的含量來控制該物件之孔隙率。
- 如申請專利範圍第1項之方法，其中以該等粒子之重量計，在該等固體內核上之瀝青塗層的含量為5%與50%之間。
- 如申請專利範圍第1項之方法，其中該等粒子之平均大小小於1毫米。
- 如申請專利範圍第1項之方法，其中在該等粒子間的空隙空間在碳化之前伴隨該形成產生，促成該物件之孔隙率。
- 一種方法，其包含：將由具有瀝青塗層的粒子形成之粉末壓成物件之形狀，其中該等粒子由於在壓力下彼此接觸而互連；及藉由將經壓成該物件之形狀的粉末加熱至高於400℃以使瀝青碳化，使得來自該等粒子中之相毗連者的瀝青經碳化以提供具有經碳化材料的黏著網狀結構之物件；其進一步包含移除該等粒子之內核，從而留下已經碳化之該瀝青。
- 如申請專利範圍第12項之方法，其中該壓在該等粒子間留下空隙空間，從而促成該物件之孔隙率。
- 如申請專利範圍第12項之方法，其中在高於該瀝青之軟化點之溫度下執行該壓，使得該瀝青填充在粒子中間 的空隙且該碳化將該瀝青轉化為碳，從而提供具有小於10%的孔隙率之該物件。
- 如申請專利範圍第12項之方法，其進一步包含將該粉末與聚合物溶液混合以形成混合物，接著在該壓期間，將該混合物以機械方式強壓成該形狀，其中藉由加熱至高於400℃之瀝青的碳化亦使該聚合物分解。
- 一種方法，其包含：將溶解於溶劑中之瀝青溶液與固體顆粒物懸浮液混合，以使得在所得混合物內相對於該溶液之瀝青濃度降低，促進該瀝青沈澱於該固體顆粒物上；將塗佈有該瀝青之固體顆粒物的粒子自該混合物之液體分離；將自該液體分離出之粒子形成為物件之形狀，其中該等粒子係藉由該等粒子之瀝青而彼此黏著；及藉由將經形成為該物件之形狀的粒子加熱至高於400℃來碳化該等粒子之瀝青，以提供具有所需要的機械強度及組成之物件，其係因使該等粒子互連的瀝青之碳化；其進一步包含移除該等粒子之內核，從而留下已經碳化之該瀝青。
- 如申請專利範圍第16項之方法，其進一步包含流經一流體，該流體係與形成過濾料和吸附劑中之一者的該物件接觸，以自該流體流移除污染物。
- 如申請專利範圍第16項之方法，其中該物件實質上係由經形成為該物件且經碳化之粒子組成。
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2011
- 2011-10-31 US US13/285,391 patent/US8703027B2/en active Active
- 2011-10-31 WO PCT/US2011/058562 patent/WO2012067800A1/en active Application Filing
- 2011-11-11 TW TW100141228A patent/TWI566819B/zh not_active IP Right Cessation
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| US4985184A (en) * | 1987-09-18 | 1991-01-15 | Mitsubishi Petrochemical Company Limited | Production of carbonaceous powders and their granulation |
Also Published As
| Publication number | Publication date |
|---|---|
| US8703027B2 (en) | 2014-04-22 |
| WO2012067800A1 (en) | 2012-05-24 |
| TW201231142A (en) | 2012-08-01 |
| US20120119398A1 (en) | 2012-05-17 |
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