JPS62265110A - Production of slurry containing dispersed fine graphite powder - Google Patents
Production of slurry containing dispersed fine graphite powderInfo
- Publication number
- JPS62265110A JPS62265110A JP61108695A JP10869586A JPS62265110A JP S62265110 A JPS62265110 A JP S62265110A JP 61108695 A JP61108695 A JP 61108695A JP 10869586 A JP10869586 A JP 10869586A JP S62265110 A JPS62265110 A JP S62265110A
- Authority
- JP
- Japan
- Prior art keywords
- graphite
- slurry
- fine powder
- oxygen
- dispersed
- 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.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000002002 slurry Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000000843 powder Substances 0.000 claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 17
- 239000010439 graphite Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 18
- 238000010298 pulverizing process Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002612 dispersion medium Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 4
- 229910021383 artificial graphite Inorganic materials 0.000 abstract description 3
- 239000002216 antistatic agent Substances 0.000 abstract description 2
- 239000000314 lubricant Substances 0.000 abstract description 2
- 229910021382 natural graphite Inorganic materials 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000012799 electrically-conductive coating Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 238000000227 grinding Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- -1 Acetate ester Chemical class 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は導電性塗剤、工業用潤滑剤、帯電防止剤等に利
用される黒鉛微粉の分散スラリーの製造スラリーとする
ことからなる黒鉛微粉分散スラリーの製造法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to the production of a graphite fine powder dispersion slurry that is used in conductive coatings, industrial lubricants, antistatic agents, etc. Concerning the manufacturing method.
従来の技術
黒鉛微粉の分散スラリーをつくるには先ず黒鉛を粉砕す
ることが必要である。黒鉛の粉砕は振動ミル、ボットミ
ル等によって行われるが、粉砕の雰囲気を変えることで
粉砕が進むことが知られている。すなわち、振動ボール
ミルあるいはボットミル内の雰囲気をヘリウムガス、窒
素ガス等にして粉砕を行なうと空気中で粉砕するよりも
、微細な粉末が得られ、比表面積が５０Ｏｎ？／ｇを超
える微粉が得られる。BACKGROUND OF THE INVENTION In order to create a dispersed slurry of fine graphite powder, it is first necessary to crush the graphite. Grinding of graphite is carried out using a vibrating mill, a bot mill, etc., and it is known that the grinding progresses by changing the grinding atmosphere. In other words, if the atmosphere inside the vibrating ball mill or bot mill is helium gas, nitrogen gas, etc., a finer powder can be obtained than by grinding in air, and the specific surface area will be 50 On? /g of fine powder is obtained.
発明が解決しようとする問題点
黒鉛分散スラリーで特に小さい微粉を必要とすこの粉砕
によって得られた微粉はＢＥＴ法による比表面積の測定
値が５００ ｒｄ／ｇ以上と大きく、走査型電子顕微、
鏡による観察でも、１次粒子の大きさが１ミクロン以下
と小さいが大きく凝集している。Problems to be Solved by the Invention Particularly small fine powder is required for graphite dispersion slurry.The fine powder obtained by this pulverization has a large specific surface area measured by the BET method of 500 rd/g or more, and is suitable for scanning electron microscopy,
Even when observed using a mirror, the primary particles are small, less than 1 micron in size, but are largely aggregated.
しかし、この方法によって得られた微粉をケトン、その
他の有機質分散媒に分散させた場合、分散媒中で粒子同
志が凝集してしまい、分散の程度を評価する為、レーザ
ー回折式粒度分布測定機を用いて粒度測定を行なっても
、上記比表面積データ及び走査型電子顕微鏡による観察
結果と対応した測定結果が得られなかった。However, when the fine powder obtained by this method is dispersed in ketone or other organic dispersion medium, the particles tend to aggregate together in the dispersion medium. Even when the particle size was measured using a method, measurement results corresponding to the specific surface area data and the observation results using a scanning electron microscope could not be obtained.
本発明は粉砕した黒鉛（人造黒鉛又は天然黒鉛）の微粉
が分散−の中でも凝集することな（分散したスラリーを
提供することを目的とする。An object of the present invention is to provide a slurry in which fine powder of pulverized graphite (artificial graphite or natural graphite) is dispersed without agglomerating during dispersion.
問題点を解決するための手段
本発明は黒鉛の粉砕方法、それによって得られた微粉を
スラリーにするための分散媒及びこれらの関連について
種々研究した結果到達したもので、粉砕の雰囲気と分散
媒とが特定の関係にある場合に微粉の凝集のない良好な
スラリーが得られることが判明したものである。Means for Solving the Problems The present invention was arrived at as a result of various studies on a graphite pulverization method, a dispersion medium for turning the resulting fine powder into a slurry, and the relationship between these. It has been found that a good slurry without agglomeration of fine powder can be obtained when there is a specific relationship between the two.
即ち、本発明は０２ガスを実質的に含まず、ＣＯ□を主
体とするガスの雰囲気下で粉砕を行ない、得られた微粉
を含酸素有機溶媒に分散させてスラリーとする方法であ
る。That is, the present invention is a method in which pulverization is carried out in an atmosphere of gas that does not substantially contain 02 gas and is mainly composed of CO□, and the resulting fine powder is dispersed in an oxygen-containing organic solvent to form a slurry.
本発明における黒鉛の粉砕において予め通常の方法でボ
ールミル、ジェットミル等を用い、１０ミクロン程度に
粉砕しておくとよい。次にこの粉砕物を転勤ボールミル
、振動ボールミル等で粉砕する。その際ボールミル等の
中をＣＯ２系ガスで置換し、ＣＯ□ガス雰囲気とするこ
とが必要である。雰囲気はＣＯ２ガス１００％が望まし
いが、実質的にＯ２ガスを含まず、即ち不純物程度とし
て含まれるもの以外の０．を含まなければ、Ｎ２やＡｒ
等の不活性ガスは含まれていてもよい。ただしＣＯ□ガ
スによる効果を高めるには雰囲気ガスは３０％（容積）
以上をＣＯ２ガスとすべきである。本明細書においては
このようなガスをＣＯ□系ガスと称する。粉砕時間は粉
砕機の種類、容量等によって変わるが、前記のボールミ
ル等では１次粒子として１ミクロン程度にするには１〜
１００時間位粉砕する。In pulverizing graphite in the present invention, it is preferable to previously pulverize the graphite to about 10 microns using a ball mill, jet mill, etc. in a conventional manner. Next, this pulverized material is pulverized using a transfer ball mill, a vibrating ball mill, or the like. At that time, it is necessary to replace the inside of a ball mill or the like with CO2-based gas to create a CO□ gas atmosphere. It is desirable that the atmosphere be 100% CO2 gas, but it does not substantially contain O2 gas, that is, it contains 0.0% CO2 gas other than that contained as impurities. If it does not contain N2 or Ar
Inert gases such as may also be included. However, to increase the effect of CO□ gas, the atmospheric gas should be 30% (volume).
The above should be CO2 gas. In this specification, such a gas is referred to as a CO□-based gas. The grinding time varies depending on the type of grinder, capacity, etc., but with the ball mills mentioned above, it takes about 1 to 1 micron to make the primary particles about 1 micron.
Pulverize for about 100 hours.
粉砕が終了したらその粉砕機内に面接合酸素有機溶媒を
導入することが望ましい。粉砕した微粉を空気中に渇す
と微粉の表面で空気中の酸素と反応し、ＣＯｚ粉砕効果
が減殺されるからである。粉砕機内に導入する方法は粉
砕機内を一旦真空にした上で溶媒を吸引するかあるいは
圧入等による。After the pulverization is completed, it is desirable to introduce the surface-binding oxygen organic solvent into the pulverizer. This is because when the pulverized fine powder is exposed to air, the surface of the fine powder reacts with oxygen in the air, reducing the COz pulverization effect. The method for introducing the solvent into the pulverizer is to first create a vacuum inside the pulverizer and then suck the solvent, or to press it into the pulverizer.
こうして得られた混合物をボールミル等を用いてさらに
分散混合する事で分散性のよいスラリーを得ることがで
きる。By further dispersing and mixing the mixture thus obtained using a ball mill or the like, a slurry with good dispersibility can be obtained.
スラリーの濃度は用途目的に応じ広範囲に変えることが
できるが、最も一般的には黒鉛微粉３〜３０重量％のも
の・が使用に適する。The concentration of the slurry can vary widely depending on the intended use, but 3 to 30% by weight of fine graphite powder is most commonly suitable for use.
含酸素有機溶媒としてはメチルエチルケトン（ＭＦ、Ｋ
） 、アセトン、メチルイソブチルケトン（Ｍ Ｉ Ｂ
Ｋ） 、メチル−ｎ−ブチルケトン、メチル−ｎ−プ
ロピルケトン、メタノール、エタノール、ブタノール、
酢酸エステル、アクリル酸などが適し、特にケトン類が
好ましい。Methyl ethyl ketone (MF, K
), acetone, methyl isobutyl ketone (M I B
K), methyl-n-butyl ketone, methyl-n-propyl ketone, methanol, ethanol, butanol,
Acetate ester, acrylic acid, etc. are suitable, and ketones are particularly preferred.
このようにして得られたスラリーの黒鉛微粉の粒度を測
定するためスラリーをその同一分散媒で希釈した。粒度
の測定はレーザー回折式粒度分布測定゛器を用いた。そ
の結果黒鉛微粉は平均粒径が１ミクロン以下であり、殆
んど凝集していないことがわかった。To measure the particle size of graphite fines in the slurry thus obtained, the slurry was diluted with the same dispersion medium. The particle size was measured using a laser diffraction particle size distribution analyzer. As a result, it was found that the graphite fine powder had an average particle size of 1 micron or less and was hardly agglomerated.
作用
黒鉛をＣ（ｈ系ガス雰囲気で粉砕し、それを分散媒とし
て含酸素有機溶媒を用いた場合に黒鉛微粉の凝集がなぜ
起らないかについては、黒鉛の粉砕中にＣＯ２ガスが黒
鉛微粉表面に作用して、親溶媒性の官能基を生成し、そ
の表面の存在によって含酸素有機溶媒中で微粉の凝集が
さまたげられ、分散が促進される事によると考えられる
。The reason why graphite fine powder does not agglomerate when graphite is crushed in a C (h) gas atmosphere and an oxygen-containing organic solvent is used as a dispersion medium is as follows. This is thought to be due to the fact that it acts on the surface to generate solvent-philic functional groups, and its presence on the surface prevents aggregation of the fine powder in the oxygen-containing organic solvent and promotes dispersion.
実施例１
人造黒鉛を、平均粒度５．８ミクロンに予備粉砕した原
料を２０ｇ′秤量して、内容量３１のポットミルポット
に入れた。そこへ直径１０鶴の鉄製ボールを１．２１入
れ、粉砕媒体とした。ポットにふたをして、ポット内を
一旦真空にした上で、Ｃｏ２ガスを７６０Ｔｏｒｒ封入
し、封入ラインの弁を締めてポットを密閉状態とした。Example 1 20 g' of raw material prepared by pre-pulverizing artificial graphite to an average particle size of 5.8 microns was weighed and placed in a pot mill pot with an internal capacity of 31 μm. 1.21 iron balls each having a diameter of 10 mm were placed therein to serve as a grinding medium. The pot was covered with a lid, the inside of the pot was once evacuated, and then Co2 gas was sealed at 760 Torr, and the valve of the filling line was closed to seal the pot.
ポットをポットミル架台にのせ、回転数６゜ｒ、ｐ、ｍ
、で６５時間粉砕を行なった。Place the pot on the pot mill stand and rotate at 6゜r, p, m.
, for 65 hours.
粉砕が終了したポットを架台から取りはずし、ポー／
ト内のガスを真空ポンプで圧力５０Ｔｏｒｒ迄吸引した
後、今度は５００ｃｃのメチルエチルケトンをポット内
に導入した。次いで、このポットを再びポットミル架台
にのせ、回転数６ Ｏｒ、ｐ、ｍ、で５０時間分散混合
を行なった。混合が終了してからボット内のスラリーを
取り出し、レーザー回折式粒度分布測定器を用いて粒度
測定を行なった所、５０％累積平均径が０．３７ミクロ
ンとなった。Once the pot has been crushed, remove it from the stand and place it in the pot.
After the gas in the pot was sucked up to a pressure of 50 Torr using a vacuum pump, 500 cc of methyl ethyl ketone was introduced into the pot. Next, this pot was placed on the pot mill stand again, and dispersion mixing was performed for 50 hours at a rotation speed of 6 Or, p, m. After the mixing was completed, the slurry in the bot was taken out and the particle size was measured using a laser diffraction particle size distribution analyzer, and the 50% cumulative average diameter was found to be 0.37 microns.
実施例２〜３．比較例１〜３
実施例１と同様にし、但し、粉砕における雰囲気及び溶
媒の種類を変えて実施した。第１表にその条件及び結果
を示す。Examples 2-3. Comparative Examples 1 to 3 Comparative Examples 1 to 3 were carried out in the same manner as in Example 1, except that the atmosphere and type of solvent used during pulverization were changed. Table 1 shows the conditions and results.
Claims (1)
の雰囲気下で粉砕し、その微粉に含酸素有機溶媒を加え
てスラリーとすることを特徴とする黒鉛微粉分散スラリ
ーの製造法。A method for producing a fine graphite powder dispersion slurry, which comprises pulverizing graphite in an atmosphere of CO_2-based gas that does not substantially contain O_2 gas, and adding an oxygen-containing organic solvent to the fine powder to form a slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61108695A JPH0621019B2 (en) | 1986-05-14 | 1986-05-14 | Method for producing fine graphite powder dispersion slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61108695A JPH0621019B2 (en) | 1986-05-14 | 1986-05-14 | Method for producing fine graphite powder dispersion slurry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62265110A true JPS62265110A (en) | 1987-11-18 |
| JPH0621019B2 JPH0621019B2 (en) | 1994-03-23 |
Family
ID=14491296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61108695A Expired - Lifetime JPH0621019B2 (en) | 1986-05-14 | 1986-05-14 | Method for producing fine graphite powder dispersion slurry |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0621019B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02167808A (en) * | 1988-09-13 | 1990-06-28 | Kansai Coke & Chem Co Ltd | Purification of kish graphite |
| JPH0350110A (en) * | 1989-07-19 | 1991-03-04 | Kansai Coke & Chem Co Ltd | Method for highly purifying graphite |
| JP2014520751A (en) * | 2011-07-14 | 2014-08-25 | ユニスト・アカデミー―インダストリー・リサーチ・コーポレーション | Graphite with edge functionalized by mechanochemical method and method for producing the same |
-
1986
- 1986-05-14 JP JP61108695A patent/JPH0621019B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02167808A (en) * | 1988-09-13 | 1990-06-28 | Kansai Coke & Chem Co Ltd | Purification of kish graphite |
| JPH0350110A (en) * | 1989-07-19 | 1991-03-04 | Kansai Coke & Chem Co Ltd | Method for highly purifying graphite |
| JP2014520751A (en) * | 2011-07-14 | 2014-08-25 | ユニスト・アカデミー―インダストリー・リサーチ・コーポレーション | Graphite with edge functionalized by mechanochemical method and method for producing the same |
| JP2016029014A (en) * | 2011-07-14 | 2016-03-03 | ユニスト・アカデミー—インダストリー・リサーチ・コーポレーションＵｎｉｓｔ Ａｃａｄｅｍｙ−Ｉｎｄｕｓｔｒｙ Ｒｅｓｅａｒｃｈ Ｃｏｒｐｏｒａｔｉｏｎ | Method of producing graphite with edges functionalized by mechanochemical method |
| US9656871B2 (en) | 2011-07-14 | 2017-05-23 | Unist (Ulsan National Institute Of Science And Technology) | Edge-functionalized graphitic material through mechanochemical process and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0621019B2 (en) | 1994-03-23 |
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