JP4741196B2 - フラーレン類の残留溶媒の除去方法 - Google Patents
フラーレン類の残留溶媒の除去方法 Download PDFInfo
- Publication number
- JP4741196B2 JP4741196B2 JP2004123370A JP2004123370A JP4741196B2 JP 4741196 B2 JP4741196 B2 JP 4741196B2 JP 2004123370 A JP2004123370 A JP 2004123370A JP 2004123370 A JP2004123370 A JP 2004123370A JP 4741196 B2 JP4741196 B2 JP 4741196B2
- Authority
- JP
- Japan
- Prior art keywords
- fullerenes
- toluene
- residual
- solvent
- ppm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims description 35
- 229910003472 fullerene Inorganic materials 0.000 title claims description 34
- 239000013557 residual solvent Substances 0.000 title claims description 12
- 238000000034 method Methods 0.000 title claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 84
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- 206010042674 Swelling Diseases 0.000 claims description 4
- 230000008961 swelling Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 description 5
- 230000001766 physiological effect Effects 0.000 description 5
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229940117389 dichlorobenzene Drugs 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/44—Elemental carbon, e.g. charcoal, carbon black
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/152—Fullerenes
- C01B32/156—After-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Medicinal Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Carbon And Carbon Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Description
〔1〕溶媒トルエンが残留するフラーレン類を、10Torr以下の減圧度において300℃以上600℃以下の温度で加熱処理してトルエン残留量を890ppm以下にまで低減することを特徴とするフラーレン類の残留溶媒の除去方法。
〔2〕20時間以上加熱することを特徴とする上記〔1〕の残留溶媒の除去方法。
〔3〕加熱処理前に、トルエンを添加して膨潤処理することを特徴とする上記〔1〕または〔2〕のフラーレン類の残留溶媒の除去方法。
<実施例1>
上記MF試料5gを粉砕(メノウ乳鉢)し、ガラス容器に入れて、減圧加熱装置内で加熱処理した。
残留トルエン量が17200ppmのMF試料において,10Torrの減圧0℃で24時間の加熱処理の前に、前処理として、MF試料と同重量以上のトルエンを加えて1時間放置し、MF試料を膨潤させた。この場合の残留トルエン量を示した。残留トルエン量は、この前処理を行わない場合の約1/10にまで減少することがわかる。
Claims (3)
- 溶媒トルエンが残留するフラーレン類を、10Torr以下の減圧度において300℃以上600℃以下の温度で加熱処理してトルエン残留量を890ppm以下にまで低減することを特徴とするフラーレン類の残留溶媒の除去方法。
- 20時間以上加熱することを特徴とする請求項1に記載の残留溶媒の除去方法。
- 加熱処理前に、トルエンを添加して膨潤処理することを特徴とする請求項1または2に記載のフラーレン類の残留溶媒の除去方法。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004123370A JP4741196B2 (ja) | 2004-04-19 | 2004-04-19 | フラーレン類の残留溶媒の除去方法 |
PCT/JP2005/007742 WO2005102925A1 (ja) | 2004-04-19 | 2005-04-18 | フラーレン類の残留溶媒の除去方法 |
CNA2005800117989A CN1942397A (zh) | 2004-04-19 | 2005-04-18 | 富勒烯类的残留溶剂的去除方法 |
US11/579,000 US20070172411A1 (en) | 2004-04-19 | 2005-04-18 | Method of removing residual solvent from fullerene |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004123370A JP4741196B2 (ja) | 2004-04-19 | 2004-04-19 | フラーレン類の残留溶媒の除去方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2005306636A JP2005306636A (ja) | 2005-11-04 |
JP4741196B2 true JP4741196B2 (ja) | 2011-08-03 |
Family
ID=35196881
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2004123370A Expired - Lifetime JP4741196B2 (ja) | 2004-04-19 | 2004-04-19 | フラーレン類の残留溶媒の除去方法 |
Country Status (4)
Country | Link |
---|---|
US (1) | US20070172411A1 (ja) |
JP (1) | JP4741196B2 (ja) |
CN (1) | CN1942397A (ja) |
WO (1) | WO2005102925A1 (ja) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5576720B2 (ja) * | 2010-06-11 | 2014-08-20 | ビタミンC60バイオリサーチ株式会社 | フラーレンの高濃度飽和炭化水素溶液の製造方法 |
CN111156790B (zh) * | 2018-12-21 | 2020-12-29 | 中国科学院化学研究所 | 一种去除富勒烯固体中残留溶剂的方法 |
CN111547706B (zh) * | 2020-05-11 | 2022-12-06 | 赤峰福纳康生物技术有限公司 | 一种脱除富勒烯溶剂残留的方法 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0558611A (ja) * | 1991-09-02 | 1993-03-09 | Idemitsu Kosan Co Ltd | フラーレン類の精製方法 |
US5364993A (en) * | 1993-01-21 | 1994-11-15 | Inrad, Inc. | Selective functionalization of fullerenes |
US5354926A (en) * | 1993-02-23 | 1994-10-11 | E. I. Du Pont De Nemours And Company | Fluoroalkylated fullerene compounds |
JP2003089510A (ja) * | 2001-09-11 | 2003-03-28 | Denso Corp | カーボンナノチューブの精製方法 |
-
2004
- 2004-04-19 JP JP2004123370A patent/JP4741196B2/ja not_active Expired - Lifetime
-
2005
- 2005-04-18 CN CNA2005800117989A patent/CN1942397A/zh active Pending
- 2005-04-18 WO PCT/JP2005/007742 patent/WO2005102925A1/ja active Application Filing
- 2005-04-18 US US11/579,000 patent/US20070172411A1/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
CN1942397A (zh) | 2007-04-04 |
WO2005102925A1 (ja) | 2005-11-03 |
US20070172411A1 (en) | 2007-07-26 |
JP2005306636A (ja) | 2005-11-04 |
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