TWI503273B - Porous carbon and a method for producing the same - Google Patents
Porous carbon and a method for producing the same Download PDFInfo
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- TWI503273B TWI503273B TW099119935A TW99119935A TWI503273B TW I503273 B TWI503273 B TW I503273B TW 099119935 A TW099119935 A TW 099119935A TW 99119935 A TW99119935 A TW 99119935A TW I503273 B TWI503273 B TW I503273B
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- particles
- carbon
- porous carbon
- metal
- metal particles
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 125
- 229910052799 carbon Inorganic materials 0.000 title claims description 122
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000002245 particle Substances 0.000 claims description 76
- 239000002923 metal particle Substances 0.000 claims description 63
- 239000011148 porous material Substances 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 30
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- 238000002296 dynamic light scattering Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 62
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 39
- 229910052697 platinum Inorganic materials 0.000 description 31
- 239000000395 magnesium oxide Substances 0.000 description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 22
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 17
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
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- 238000001179 sorption measurement Methods 0.000 description 3
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 2
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 2
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- RGISWSYUWAXSJH-UHFFFAOYSA-N 2-(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecoxy)-5-methylbenzene-1,4-diamine Chemical compound NC1=C(C=C(C(=C1)OC(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)N)C RGISWSYUWAXSJH-UHFFFAOYSA-N 0.000 description 1
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- YSZIUSQXDFVKDO-UHFFFAOYSA-N COC1=C(C=C(C=C1OC(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)N)N Chemical compound COC1=C(C=C(C=C1OC(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)N)N YSZIUSQXDFVKDO-UHFFFAOYSA-N 0.000 description 1
- LBDSWSAEQVNTIS-UHFFFAOYSA-N COC1=C(C=C(C=C1OC(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)N)N Chemical compound COC1=C(C=C(C=C1OC(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)N)N LBDSWSAEQVNTIS-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920000954 Polyglycolide Polymers 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- CQZITAWPXREEND-UHFFFAOYSA-N [C].Cl Chemical compound [C].Cl CQZITAWPXREEND-UHFFFAOYSA-N 0.000 description 1
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- VSRXQHXAPYXROS-UHFFFAOYSA-N azanide;cyclobutane-1,1-dicarboxylic acid;platinum(2+) Chemical compound [NH2-].[NH2-].[Pt+2].OC(=O)C1(C(O)=O)CCC1 VSRXQHXAPYXROS-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- GQHJPWVWMCOCEG-UHFFFAOYSA-N bis(4-amino-3-fluorophenyl)methanone Chemical compound C1=C(F)C(N)=CC=C1C(=O)C1=CC=C(N)C(F)=C1 GQHJPWVWMCOCEG-UHFFFAOYSA-N 0.000 description 1
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 description 1
- FNAQSUUGMSOBHW-UHFFFAOYSA-H calcium citrate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FNAQSUUGMSOBHW-UHFFFAOYSA-H 0.000 description 1
- 239000001354 calcium citrate Substances 0.000 description 1
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 229960004562 carboplatin Drugs 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229960005336 magnesium citrate Drugs 0.000 description 1
- 239000004337 magnesium citrate Substances 0.000 description 1
- 235000002538 magnesium citrate Nutrition 0.000 description 1
- 229940091250 magnesium supplement Drugs 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- AZQWKYJCGOJGHM-UHFFFAOYSA-N para-benzoquinone Natural products O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000004633 polyglycolic acid Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000004060 quinone imines Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 235000013337 tricalcium citrate Nutrition 0.000 description 1
- PLSARIKBYIPYPF-UHFFFAOYSA-H trimagnesium dicitrate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O PLSARIKBYIPYPF-UHFFFAOYSA-H 0.000 description 1
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Description
本發明係關於一種多孔質碳及製造方法,特別係關於一種於內部含有金屬粒子之多孔質碳及其製造方法。
含有金屬粒子之多孔質碳係工業價值高的觸媒,例如,利用活性碳高之吸附能而吸附反應物質,可以觸媒之金屬粒子反應。上述金屬粒子已知有鉑、銀、銅等,其用途有燃料電池用高活性電極、NOx、SOx分解過濾膜、鋰離子充電電池用電極材料等。
此處,上述含有金屬粒子之多孔質碳材料係已提出一種於碳擔體之表面、及細孔內部以金屬粒子為奈米程度微細地分散者,其製造方法係已提出一種使金屬粒子等、界面活性劑、熱硬化性樹脂等、與溶劑混合而加熱混合體以使之硬化後,再燒成而使之碳化的方法(參照下述專利文獻1)。
[專利文獻1]特開2005-314223號公報
但,在上述習知之方法中係於碳擔體之表面及細孔內部存在金屬粒子,故金屬粒子之表面呈露出狀態。因此,長期間使用時等有金屬粒子氧化,作為觸媒之功能降低等之課題。又,於以界面活性劑之靜電作用功能所產生的金屬粒子之分散中係亦有所謂產生無法使金屬粒子充分分散之課題。
因此本發明之目的在於提供一種可抑制金屬粒子氧化,同時並藉由使金屬粒子充分分散,可長期間維持金屬粒子之添加效果的多孔質碳及其製造方法。
本發明之多孔質碳,係構成間隙孔之外廓的碳質壁形成3次元網目構造,在臨近於上述碳質壁的上述間隙孔的位置形成微孔,其特徵在於:於上述碳質壁內分散金屬粒子,且上述金屬粒子之中至少一部分的金屬粒子係以粒子表面之一部分於上述微孔以露出狀態下配置。
如上述構成,若金屬粒子分散於碳質壁內,金屬粒子之表面的至少一部分受碳質被覆,故與露出狀態比較,可抑制金屬粒子氧化。因此,可長期間維持金屬粒子之添加效果。另一方面,金屬粒子之中至少一部分的金屬粒子係粒子表面的一部分於微孔以露出狀態下配置,故可充分發揮作為金屬粒子之觸媒等的功能。
又,若構成間隙孔之外廓的碳質壁形成3次元網目構造,且在臨近於碳質壁的間隙孔的位置形成微孔,可增大每單位量之吸附有效面積,或,增大在細孔之毛細管凝集量。尚且,若構成間隙孔之外廓的碳質壁形成3次元網目構造,亦可適應於其用途必須有彈力性之情形。
又,在本說明書中,細孔徑為2nm以下者稱為微孔,細孔徑為2~50nm者稱為間隙孔,細孔徑超過50nm者稱為巨孔,有時總稱此等之孔為細孔。
又,上述金屬粒子係可使用鉑、銀、銅、錫、鐵等,使用鉑時,可使用多孔質碳作為燃料電池用高活性電極或NOx、SOx分解過濾膜等,使用銀時,可使用多孔質碳作為汽車之排出氣體中的NOx、SOx等的吸附劑或氣體、液體中之殺菌過濾膜等,使用銅時,係可使用多孔質碳作為氨氣吸附分解觸媒、電刷材填充劑等,使用錫時係可使用多孔質碳作為低融點焊接粉末、鋰離子充電電池用電極材料等,使用鐵時係使用多孔質碳作為有機合成用觸媒、電刷材填充劑等。
宜以上述間隙孔之大小成為略相同的方式構成。
若以間隙孔之大小成為略相同的方式構成,使用精製或觸媒等為目的時,可充分達成其目的。
宜上述金屬粒子之平均粒徑為4~500nm。
金屬粒子之平均粒徑不足4nm時,金屬粒子易埋沒於碳質壁內之不佳情形,結晶構造無法維持而進行非晶化,故有時大小參差不齊、觸媒能力、作為金屬之特性無法發揮,另外,若金屬粒子之平均粒徑超過500nm,與碳質分離而析出,故成為無法進入碳壁之狀態,且金屬粒子之比表面積會降低,故有時觸媒能力降低。
又,上述金屬粒子之平均粒徑係藉動態光散射法測定時之值。
宜上述金屬粒子對構成上述碳質壁之碳與上述金屬粒子之總量的比率為0.5~90重量%。
金屬粒子之比率不足0.5質量%時係有時無法充分發揮金屬粒子之添加效果,另外,金屬粒子之比率超過90質量%之多孔質碳的製作很困難。
宜含有上述間隙孔及微孔之細孔中的孔徑為0.3~100nm。
細孔徑不足0.3nm者係很難製作,另外,若細孔徑超過100nm,每單位體積之碳質壁的量變少,恐無法保持3次元網目構造。
宜比表面積為100~1000m2
/g。
比表面積不足100m2
/g,氣孔之形成量不充分,有不形成三次元網目構造之問題,另外,若比表面積超過1000m2
/g,碳壁之形狀未能保持,有所謂粒子崩壞之問題。
宜上述間隙孔為開氣孔,成為氣孔部分連續之構成。
若為氣孔部分連續之構成,氣體之流動變順利,更易補充氣體。
本發明之多孔質碳的製造方法,其特徵在於具有如下步驟:使含有有機質樹脂之流動性材料、金屬粒子與鑄模粒子混合而製作混合物的步驟;使上述混合物於非氧化性環境加熱燒成而製作燒成物之步驟;除去上述燒成物中之上述鑄模粒子之步驟。
若為如此之方法,可製造上述之多孔質碳。此時,使混合物在非氧化性環境下加熱燒成而製作碳質壁時,其後,在成為間隙孔之部位存在鑄模粒子,故並非於該部位分散金屬粒子。又,即使使用融點低之金屬(融點低於加熱燒成時之溫度的金屬)作為金屬粒子,如上述般,若鑄模粒子存在,流動性材料以及金屬粒子鎖入於鑄模粒子間,故加熱燒成時即使金屬粒子溶解,可抑制金屬粒子從碳質壁溶出。進一步,若存在鑄模粒子,加熱燒成時碳質壁之厚度變小,故可抑制碳質壁內金屬粒子凝集,於碳質壁內可使金屬粒子奈米分散。
又,為順利地得到上述作用效果,鑄模粒子對流動性材料、金屬粒子、鑄模粒子之總量的比率,宜為30~80wt%。若鑄模粒子之比率太少,有時無法充分發揮鑄模粒子之添加效果,另外,若鑄模粒子之比率太多,產生碳質壁之厚度太小等之問題。
本發明之多孔質碳的製造方法,其特徵在於具有如下步驟:使含有有機質樹脂之流動性材料、在還原性環境下加熱燒成時含有金屬析出之金屬鹽的金屬成分、與鑄模粒子混合而製作混合物的步驟;使上述混合物於還原性環境下加熱燒成而製作燒成物之步驟;除去上述燒成物中之上述鑄模粒子之步驟。
若為如上述之方法,可製造上述之多孔質碳。此時,製作混合物之步驟時,只添加金屬粒子作為金屬成分時,在製作燒成物之步驟中只要在非氧化性環境下加熱燒即可,但添加含有金屬鹽作為金屬成分者時,在製作燒成物之步驟中必須在還原性環境下加熱燒成。又,於金屬成分係金屬鹽之外亦可含有金屬粒子。
又,在上述製造方法時,使用樹脂清漆作為流動性材料時,如示於圖11之概念圖,成為樹脂清漆與金屬鹽之錯合物。
本發明之多孔質碳的製造方法,其特徵在於具有如下步驟:含有具備於構造中含有金屬原子之有機質樹脂的流動性材料、與鑄模粒子混合而製作混合物的步驟;使上述混合物於非氧化性環境下加熱燒成而製作燒成物之步驟;除去上述燒成物中之上述鑄模粒子之步驟。
含有金屬作為微粒子之方法,上述之方法外,亦可使用於構造中含有金屬原子之高分子材料。例如,如卡鉑(Carboplatin)(參照圖10之概念圖)般,若使用於高分子材料之構造中含有鉑者,可得到上述之多孔質碳。
於上述鑄型粒子係宜為使用略同徑者。
若於鑄模粒子使用略同徑者,上述之間隙孔的大小成為略同等。
上述流動性材料宜為在200℃以下之溫度產生流動性之樹脂、或清漆狀之高分子樹脂。
就流動性材料而言,若使用在200℃以下之溫度產生流動性之樹脂、或清漆狀之高分子樹脂,可更順利地製作上述之多孔質碳。
但,流動性材料係不限於在200℃以下之溫度產生流動性之樹脂等,即使在200℃以下之溫度不產生流動性,只要為亦可溶於水或有機溶劑之高分子材料,可使用於本發明中。如此之材料可例示PVA(聚乙烯醇)、PET(聚對苯二甲酸乙二酯)樹脂、醯亞胺系樹脂、酚系樹脂等。
(1)流動性材料係宜為使用碳收率為40%以上85%以下者。若流動性材料之碳收率太小或太大(具體地,流動性材料之碳收率不足40%,或超過85%),有時成為未能保持三次元網目構造之碳粉末,但若使用碳收率為40%以上85%以下之流動性材料,除去鑄模粒子後,鑄模粒子存在之處可確實地得到具有成為連續孔之三次元網目構造的碳質壁。又,鑄模粒子若使用粒徑略同一者,可形成同一尺寸之連續孔,故可製作海綿狀且略籠狀之碳質壁。
又,流動性材料之碳收率若為上述範圍,微孔非常發達,故比表面積變大。但,流動性材料之碳收率即使為上述範圍,不使用鑄模粒子時係微孔不發達。
(2)藉由改變鑄模粒子之徑或有機質樹脂的種類,可調整細孔之徑、多孔質碳之細孔分布、及碳質壁的厚度。因此,藉由適當選擇鑄模粒子之徑與有機質樹脂之種類,俾具有更均一的細孔徑,亦可製作具有更大的細孔容量之多孔質碳。進一步,使用於碳源含有有機質樹脂之流動性材料,而且,不經過賦活處理步驟,可製作多孔質碳,故所得到之多孔質碳係成為非常高純度者。
(3)鑄模粒子宜為使用鹼土族金屬化合物。鹼土族金屬化合物可藉由弱酸或熱水除去(亦即,不使用強酸,可除去鑄模粒子),故在除去鑄模粒子之步驟中,可抑制多孔質碳本身的性狀變化者。又,使用弱酸時,有所謂除去速度變快之優點,另外,使用熱水時,有所謂可防止酸殘留而成為雜質之不佳情形的優點。又,在除去鑄模粒子之步驟中,已溶出之氧化物溶液可再使用來作為原料,可降低多孔質碳之製造成本。
(4)在除去鑄模粒子之步驟中係宜規制成除去後之鑄模粒子的殘留率為0.5%以下。若除去後之鑄模粒子的殘留率超過0.5%,殘留於間隙孔內之鑄模粒子變多,無法發揮作為細孔之角色的部位廣泛產生。又,亦恐很難適用於避免金屬雜質之用途。
若依本發明,可發揮如下之優異效果,即可抑制金屬粒子氧化,同時並藉由使金屬粒子充分分散,可長期間維持金屬粒子之添加效果。
以下,說明本發明之實施形態。
本發明之碳化物係使於單位構造中含有至少一個以上之氮或氟原子之聚醯亞胺或碳化收率超過40wt%之樹脂等(例如,酚樹脂或瀝清)、與金屬粒子等、氧化物粒子等、在溶液或粉末狀態中進行濕式或乾式混合,使混合物在非氧化性環境下、或減壓下[133Pa(1torr)以下]、或、在還原性環境下,以500℃以上之溫度進行碳化,洗淨處理所得到之碳與氧化物而得到,於其碳質壁內係分散金屬粒子之碳化物。
此處,於上述單位構造中含有至少一個以上之氮或氟原子之聚醯亞胺係可藉由酸成分與二胺成分之聚縮合而得到。但,此時,酸成分及二胺成分之任一者或兩者,必須含有一個以上之氮原子或氟原子。
具體上,藉由使聚醯亞胺之前驅體的聚醯胺酸成膜,加熱除去溶劑,俾得到聚醯胺酸膜。其次,藉由使所得到之聚醯胺酸膜以200℃以上進行熱醯亞胺化,俾製造聚醯亞胺。
前述二胺係可例示2,2-雙(4-胺基苯基)六氟丙烷[2,2-Bis(4-aminophenyl)hexafluoropropane]、2,2-雙(三氟甲基)-聯苯胺[2,2’-Bis(trifluoromethyl)-benzidine]、4,4’-二胺基八氟聯苯基、或3,3’-二氟-4,4’-二胺基二苯基甲烷、3,3’-二氟-4,4’-二胺基二苯基醚、3,3’-二(三氟甲基)-4,4’-二胺基二苯基醚、3,3’-二氟-4,4’-二胺基二苯基丙烷、3,3’-二氟-4,4’-二胺基二苯基六氟丙烷、3,3’-二氟-4,4’-二胺基二苯甲酮、3,3’,5,5’-四氟-4,4’-二胺基二苯基甲烷、3,3’,5,5’-四(三氟甲基)-4,4’-二胺基二苯基甲烷、3,3’,5,5’-四氟-4,4’-二胺基二苯基丙烷、3,3’,5,5’-四(三氟甲基)-4,4’-二胺基二苯基丙烷、3,3’,5,5’-四氟-4,4’-二胺基二苯基六氟丙烷、1,3-二胺基-5-(全氟壬基氧)苯、1,3-二胺基-4-甲基-5-(全氟壬基氧)苯、1,3-二胺基-4-甲氧基-5-(全氟壬基氧)苯、1,3-二胺基-2,4,6-三氟-5-(全氟壬基氧)苯、1,3-二胺基-4-氯-5-(全氟壬基氧)苯、1,3-二胺基-4-溴-5-(全氟壬基氧)苯、1,2-二胺基-4-(全氟壬基氧)苯、1,2-二胺基-4-甲基-5-(全氟壬基氧)苯、1,2-二胺基-4-甲氧基-5-(全氟壬基氧)苯、1,2-二胺基-3,4,6-三氟-5-(全氟壬基氧)苯、1,2-二胺基-4-氯-5-(全氟壬基氧)苯、1,2-二胺基-4-溴-5-(全氟壬基氧)苯、1,4-二胺基-3-(全氟壬基氧)苯、1,4-二胺基-2-甲基-5-(全氟壬基氧)苯、1,4-二胺基-2-甲氧基-5-(全氟壬基氧)苯、1,4-二胺基-2,3,6-三氟-5-(全氟壬基氧)苯、1,4-二胺基-2-氯-5-(全氟壬基氧)苯、1,4-二胺基-2-溴-5-(全氟壬基氧)苯、1,3-二胺基-5-(全氟己基氧)苯、1,3-二胺基-4-甲基-5-(全氟己基氧)苯、1,3-二胺基-4-甲氧基-5-(全氟己基氧)苯、1,3-二胺基-2,4,6-三氟-5-(全氟己基氧)苯、1,3-二胺基-4-氯-5-(全氟己基氧)苯、1,3-二胺基-4-溴-5-(全氟己基氧)苯、1,2-二胺基-4-(全氟己基氧)苯、1,2-二胺基-4-甲基-5-(全氟己基氧)苯、1,2-二胺基-4-甲氧基-5-(全氟己基氧)苯、1,2-二胺基-3,4,6-三氟-5-(全氟己基氧)苯、1,2-二胺基-4-氯-5-(全氟己基氧)苯、1,2-二胺基-4-溴-5-(全氟己基氧)苯、1,4-二胺基-3-(全氟己基氧)苯、1,4-二胺基-2-甲基-5-(全氟己基氧)苯、1,4-二胺基-2-甲氧基-5-(全氟己基氧)苯、1,4-二胺基-2,3,6-三氟-5-(全氟己基氧)苯、1,4-二胺基-2-氯-5-(全氟己基氧)苯、1,4-二胺基-2-溴-5-(全氟己基氧)苯、或不含有氟原子之對苯二胺(PPD)、二氧二苯胺等之芳香族二胺。又,上述二胺成分係可組合上述各芳香族二胺2種以上而使用。
另外,酸成分可舉例如含有氟原子之4,4-六氟異亞丙基二酞酸酐(6 FDA)、及不含有氟原子之3,4,3’,4’-聯苯基四羧酸二酐(BPDA)、均苯四甲酸二酐(PMDA)等。
又,使用來作為聚醯亞胺前驅體之溶劑的有機溶劑可舉例如N-甲基-2-吡咯烷酮、二甲基甲醯胺等。
醯亞胺化之方法係如示於公知之方法[例如,參照高分子學會編「新高分子實驗學」共立出版、1996年3月28日、第3卷高分子之合成、反應(2)158頁],亦可依加熱或化學醯亞胺化之任一方法,本發明係不受此醯亞胺化之方法影響。
進一步,聚醯亞胺以外之樹脂,可使用具有石油系煤焦瀝青、丙烯酸樹脂等具有40%以上之碳收率者。
另外,使用來作為上述氧化物之原料係鹼土族金屬氧化物(氧化鎂、氧化鈣等之外,亦可使用藉熱處理在熱分解過程狀態變化成氧化鎂、金屬有機酸(檸檬酸鎂、草酸鎂、檸檬酸鈣、草酸鈣等)、氯化物、硝酸鹽、硫酸鹽。
又,除去氧化物之洗淨液係宜可使用鹽酸、硫酸、硝酸、檸檬酸、醋酸、蟻酸等一般性無機酸,形成2mol/升以下之稀釋而使用。又,亦可使用80℃以上之熱水。
進一步,為得到本發明之多孔質碳係在非氧化環境下,宜為500℃以上、1500℃以下之溫度進行碳化。高碳收率之樹脂為高分子,故不足500℃時,有時碳化不充分,細孔之發達不充分,另外,1500℃以上係收縮率大,氧化物燒結,粗大化,故細孔尺寸變小而比表面積變小。
首先,如圖1(a)所示般,使作為碳前驅體之聚醯胺酸樹脂清漆(醯亞胺系樹脂)1、作為鑄模粒子之氧化鎂(MgO、平均結晶粒徑為100nm)2、作為金屬鹽之氯化鉑酸6以10:5:1之質量比混合。此時,聚醯胺酸樹脂清漆與氯化鉑酸6成為金屬錯合物。其次,如圖1(b)所示般使此混合物在氮環境中以1000℃熱處理1小時,而使氯化鉑酸6還原成鉑,且,使聚醯胺酸樹脂清漆1熱分解,俾製作含鉑粒子7之碳3。最後,如圖1(c)所示般,以1mol/升之比率添加所得到之碳3的硫酸溶液進行洗淨,使MgO完全溶出,俾得到具有多數孔4之多孔質碳5。又,在多孔質碳5中,上述鉑粒子7對構成碳質壁之碳與鉑粒子7之總量的比率為5質量%。
以下稱如此做法所製作之多孔質碳為本發明碳A1。
將本發明碳A1之STEM(掃描透過電子顯微鏡)照片表示於圖2中。從圖2明顯可知在多孔質碳內鉑粒子以奈米級分散。又,有關本發明碳A1,使除去氧化鎂前後之SEM(掃描電子顯微鏡)照片分別表示於圖3(a)[除去氧化鎂之前]及圖3(b)[除去氧化鎂之後]。從兩圖明顯可知,於除去氧化鎂之前係成為3次元網目構造,但除去氧化鎂之後係成為3次元網目構造(海綿狀之碳形狀)。更具體地,如圖4所示般,本發明碳A1的構造具有大小略同等之多數間隙孔10,於臨近碳質壁12的間隙孔10之位置形成微孔11,且於碳質壁12內存在鉑粒子7,此鉑粒子7之一部分成為露出於上述微孔11之構造。
又,在本發明碳A1中係碳部分之體積對碳壁全體的體積之比率為40%,微孔之孔徑為10nm,比表面積為700m2
/g。又,微孔之孔徑係使用HK法而計算,間隙孔之孔徑係使用BJH法而計算。
鉑粒子7對構成碳質壁12之碳與鉑粒子7之總量的比率分別為10質量%、15質量%、20質量%、30質量%、35質量%、45質量%、65質量%之外,其他係與上述實施例1同樣做法而製作多孔質碳。
使如此做法所製作之多孔質碳以下分別稱為本發明碳A2~A8。
除未添加作為鑄模粒子之氧化鎂外,其餘係與上述實施例1~實施例4同樣做法而製作多孔質碳。
使如此做法所製作之多孔質碳在以下分別稱為比較碳Z1~Z4。
硏究上述本發明碳A1~A8及比較碳Z1~Z4中之鉑的含量(鉑粒子7對構成碳質壁12之碳與鉑粒子7之總量的比例)與鉑之平均粒徑的關係,故其結果表示於圖5。
從圖5明顯可看出,在鉑含量為5質量%~35質量%之本發明碳A1~A6中鉑粒徑極小至約5nm,又,鉑含量各45質量%、65質量%之本發明碳A7、A8中,鉑粒徑小至約17nm以下。對此,比較碳Z1~Z4中係即使鉑含量為5質量%之比較碳Z1,鉑粒徑大至約18nm,在鉑含量為10質量%以上之比較碳Z2~Z4中鉑粒徑極大至約23nm以上。
此理由係完全未明確,但如本發明碳A1~A8,使用MgO填充劑時係在製造步驟之全體中藉MgO填充劑,微保持至碳壁之厚度不容許鉑粒子之凝集的程度,故推斷於多孔質碳之碳壁內可維持金屬粒子被奈米分散之狀態。然而,在比較碳Z1~Z4中係不使用MgO填充劑,故,推斷於熱處理時在聚醯胺酸樹脂清漆中引起鉑粒子之凝集,成為鉑之平均粒徑大者。
首先,使作為碳前驅體之聚乙烯醇、作為鑄模粒子之氧化鎂(MgO、平均粒徑為100nm)、作為金屬鹽之氧化錫以10:10:5之質量比混合。然後,使此混合物在氮環境中以1000℃進行熱處理1小時,而使氧化錫還原成錫,且,使聚乙烯醇熱分解,俾製作含錫之碳。最後,以1mol/升之比率添加所得到之碳的鹽酸溶液進行洗淨,使MgO完全溶出,俾得到具有多數孔之多孔質碳。又,在多孔質碳中,錫對構成碳質壁之碳與錫之總量的比率為55wt%。
以下稱如此做法所製作之多孔質碳為本發明碳B。
將本發明碳B之外觀照片表示於圖6。從圖6明顯可推測金屬之析出完全看不到,在多孔質碳內錫粒子被奈米級分散。
除未添加作為鑄模粒子之氧化鎂外,其餘係與上述實施例同樣做法而製作多孔質碳。
以下稱如此做法所製作之多孔質碳為比較碳Y。
將比較碳Y之外觀照片表示於圖7中。照片中之白粒子為所析出之金屬,從圖7明顯可知錫粒子凝集而析出於多孔質碳外。
成為上述外觀係如本發明碳B,使用MgO填充劑時係於多孔質碳之碳壁內包含金屬粒子之狀態即使在加熱燒成中亦可維持,故並非金屬析出於多孔質碳外。亦即,藉由存在MgO填充劑,可抑制於間隙孔溶出金屬。然而,可認為在比較碳Y中係不使用MgO填充劑,故較金屬粒子之融點還高溫之加熱燒成時,起因於被熔融之金屬溶出於間隙孔。
使與在上述實施例使用之混合物同一的混合物在氮環境中各以600℃、700℃、800℃、及900℃進行熱處理1小時後,以鹽酸溶液進行洗淨,使MgO完全溶出。繼而,進行以鹽酸溶液洗淨前後之碳的X線繞射,故其結果分別表示於圖8(以鹽酸溶液洗淨之前)及圖9(以鹽酸溶液洗淨之後)。
於圖8及圖9可明顯看出,在700℃以下進行熱處理時,無論以鹽酸溶液洗淨之前後而存在SnO2
,可看出以800℃進行熱處理時,以鹽酸溶液洗淨之前係不存在SnO2
,但以鹽酸溶液洗淨之後而存在SnO2
。然而,可看出在900℃以下進行熱處理時,無論以鹽酸溶液洗淨之前後而未存在SnO2
。因此,使用氧化錫作為金屬鹽時,確實地進行氧化錫之還原處理,係可知熱處理溫度宜為900℃以上。
本發明係可使用來作為氣體吸附、分解材料、燃料電池用高活性電極、氣體、液體中之殺菌過濾膜、電刷材填充劑、低融點焊接粉末、鋰離子充電電池用電極材等。
1...聚醯胺酸樹脂清漆(醯亞胺系樹脂)
2...氧化鎂
3...碳
4...孔
5...多孔質碳
6...氯化鉑酸
7...鉑粒子
[圖1]係表示本發明碳之製造步驟的圖,圖1(a)係表示混合有聚醯胺酸樹脂清漆與氧化鎂、氯化鉑酸之狀態的說明圖,圖1(b)係表示熱處理混合物之狀態的說明圖,圖1(c)係表示多孔質碳之說明圖。
[圖2]係本發明碳A1之STEM(掃描透過電子顯微鏡)照片。
[圖3]係除去本發明碳A1中之氧化鎂的前後之SEM(掃描透過電子顯微鏡)照片,圖3(a)係除去氧化鎂之前的照片、圖3(b)係除去氧化鎂之後的照片。
[圖4]係表示本發明碳的狀態之說明圖。
[圖5]係表示本發明碳A1~A8及比較碳Z1~Z4中之鉑的含量與鉑之平均粒徑的關係之圖表。
[圖6]係本發明碳B之外觀照片。
[圖7]係比較碳Y之外觀照片。
[圖8]係以鹽酸溶液洗淨前之碳的X線繞射圖。
[圖9]係以鹽酸溶液洗淨後之碳的X線繞射圖。
[圖10]係表示於構造中含有金屬原子之高分子材料的狀態之概念圖。
[圖11]係表示樹脂清漆與金屬鹽之錯合物的狀態之概念圖。
1...聚醯胺酸樹脂清漆(醯亞胺系樹脂)
2...氧化鎂
3...碳
4...孔
5...多孔質碳
6...氯化鉑酸
7...鉑粒子
Claims (8)
- 一種多孔質碳,係構成間隙孔之外廓的碳質壁形成3次元網目構造,在臨近於上述碳質壁的上述間隙孔的位置形成微孔,其特徵在於:於上述碳質壁內分散金屬粒子,且上述金屬粒子之中至少一部分的金屬粒子係以粒子表面之一部分於上述微孔以露出狀態下配置,上述金屬粒子之平均粒徑(動態光散射法)為4~500nm,上述金屬粒子對構成上述碳質壁之碳與上述金屬粒子之總量的比率為0.5~90wt%,上述間隙孔為開氣孔,成為氣孔部分連續之構成,上述碳質壁係由碳收率為40~85%之流動性材料所形成者。
- 如申請專利範圍第1項之多孔質碳,其中含有上述間隙孔及微孔之細孔中的孔徑為0.3~100nm。
- 如申請專利範圍第1或2項中任一項之多孔質碳,其中比表面積為100~1000m2 /g。
- 一種多孔質碳的製造方法,其特徵在於具有如下步驟:使含有有機質樹脂之流動性材料、金屬粒子與鑄模粒子混合而製作混合物的步驟;使上述混合物於非氧化性環境加熱燒成而製作燒成物之步驟; 除去上述燒成物中之上述鑄模粒子之步驟,前述流動材料的碳收率為40~85%。
- 一種多孔質碳的製造方法,其特徵在於具有如下步驟:使含有有機質樹脂之流動性材料、在還原性環境加熱燒成時含有金屬析出之金屬鹽的金屬成分、與鑄模粒子混合而製作混合物的步驟;使上述混合物於還原性環境加熱燒成而製作燒成物之步驟;除去上述燒成物中之上述鑄模粒子之步驟,前述流動材料的碳收率為40~85%。
- 一種多孔質碳的製造方法,其特徵在於具有如下步驟:含有具備於構造中含有金屬原子之有機質樹脂的流動性材料、與鑄模粒子混合而製作混合物的步驟;使上述混合物於非氧化性環境加熱燒成而製作燒成物之步驟;除去上述燒成物中之上述鑄模粒子之步驟,前述流動材料的碳收率為40~85%。
- 如申請專利範圍第4~6項中任一項之多孔質碳的製造方法,其中於上述鑄模粒子中係使用略同徑者。
- 如申請專利範圍第4~6項中任一項之多孔質碳的製造方法,其中就上述流動性材料而言,使用在200℃以下之溫度產生流動性的樹脂、或清漆狀之高分子樹脂。
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2009
- 2009-06-19 JP JP2009145953A patent/JP5636171B2/ja active Active
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2010
- 2010-06-14 KR KR1020117026652A patent/KR101714096B1/ko active IP Right Grant
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- 2010-06-14 WO PCT/JP2010/060046 patent/WO2010147087A1/ja active Application Filing
- 2010-06-14 EP EP10789462.8A patent/EP2444369A4/en not_active Withdrawn
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JP2006062954A (ja) * | 2004-07-30 | 2006-03-09 | Nard Inst Ltd | 活性炭の製法 |
JP2008207072A (ja) * | 2007-02-23 | 2008-09-11 | Osaka Industrial Promotion Organization | 多孔性炭素支持体に埋設させたナノ粒子系触媒及びその作製方法 |
Also Published As
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EP2444369A1 (en) | 2012-04-25 |
US9248442B2 (en) | 2016-02-02 |
JP5636171B2 (ja) | 2014-12-03 |
WO2010147087A1 (ja) | 2010-12-23 |
KR20120039517A (ko) | 2012-04-25 |
JP2011001224A (ja) | 2011-01-06 |
KR101714096B1 (ko) | 2017-03-08 |
TW201119939A (en) | 2011-06-16 |
EP2444369A4 (en) | 2016-07-13 |
US20120077670A1 (en) | 2012-03-29 |
CN102414122B (zh) | 2014-05-14 |
CN102414122A (zh) | 2012-04-11 |
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