JPH0621019B2 - Method for producing fine graphite powder dispersion slurry - Google Patents
Method for producing fine graphite powder dispersion slurryInfo
- Publication number
- JPH0621019B2 JPH0621019B2 JP61108695A JP10869586A JPH0621019B2 JP H0621019 B2 JPH0621019 B2 JP H0621019B2 JP 61108695 A JP61108695 A JP 61108695A JP 10869586 A JP10869586 A JP 10869586A JP H0621019 B2 JPH0621019 B2 JP H0621019B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- slurry
- graphite
- graphite powder
- pot
- 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
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法に関し、さら
に詳しくは特定のガス雰囲気下で粉砕した黒鉛微粉を含
酸素有機溶媒（分子式内に酸素原子を含む有機溶媒）に
分散して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。TECHNICAL FIELD The present invention relates to a method for producing a dispersion slurry of fine graphite powder used for a conductive coating agent, an industrial lubricant, an antistatic agent, and the like, and more specifically, a specific gas atmosphere. The present invention relates to a method for producing a graphite fine powder-dispersed slurry, which comprises dispersing graphite fine powder pulverized below into an oxygen-containing organic solvent (organic solvent containing oxygen atoms in the molecular formula) to form a slurry.
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、ポットミ
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
ミルあるいはポツ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500m2/gを超える
微粉が得られる。2. Description of the Related Art In order to make a dispersion slurry of fine graphite powder, it is first necessary to pulverize graphite. The crushing of graphite is performed by a vibration mill, a pot mill, etc., but it is known that crushing proceeds by changing the crushing atmosphere. That is, when the atmosphere in the vibrating ball mill or pot mill is crushed with helium gas, nitrogen gas, etc., finer powder is obtained than with crushing in air, and a fine powder having a specific surface area of more than 500 m 2 / g 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る場合、
前記のように不活性雰囲気下で粉砕し、その粉末を種々
の溶媒（分散媒）を用いてスラリーとする。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500m2/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 When particularly small fine powder is required in the graphite dispersion slurry,
As described above, the powder is ground under an inert atmosphere, and the powder is made into a slurry by using various solvents (dispersion media). The fine powder obtained by this pulverization has a large specific surface area measured by the BET method of 500 m 2 / g or more, and even when observed by a scanning electron microscope, the size of the primary particles is as small as 1 micron or less, but it is highly aggregated. There is.
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 a ketone or other organic dispersion medium, the particles are aggregated in the dispersion medium, and in order to evaluate the degree of dispersion, a laser diffraction type particle size distribution measuring device is used. Even when the particle size was measured by using, the specific surface area data and the measurement result corresponding to the observation result by the scanning electron microscope were not obtained.
本発明は粉砕した黒鉛（人造黒鉛又は天然黒鉛）の微粉
が分散媒の中でも凝集することなく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 crushed graphite (artificial graphite or natural graphite) is dispersed in a dispersion medium without agglomerating.
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 has been achieved as a result of various studies on a method for pulverizing graphite, a dispersion medium for making fine powder obtained thereby into a slurry, and their relations. It was found that a good slurry free from aggregation of fine powder can be obtained when and have a specific relationship.
即ち、本発明はO2ガスを実質的に含まず、ＣＯ２ガスま
たは不活性ガスを含むＣＯ２ガスの雰囲気下で粉砕を行
ない、得られた微粉を分子式内に酸素原子を含む有機溶
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 free of O 2 gas substantially, CO subjected to grinding in an atmosphere of CO 2 gas containing 2 gas or an inert gas, in an organic solvent containing the resulting oxygen atom fines in the molecular formula This is a method of dispersing it into 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動ボールミル、
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ガスまたは不活性ガスを含むＣＯ２ガスで置換
し、CO2ガス雰囲気とすることが必要である。雰囲気はC
O2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O2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CO2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。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 the crushing of graphite in the present invention, it is advisable to use a ball mill, a jet mill or the like in advance by a usual method to crush to about 10 microns. Next, this crushed product is rolled into a ball mill,
Grind with a vibrating ball mill. At that time through the ball mill was replaced with CO 2 gas including the CO 2 gas or an inert gas, it is necessary to CO 2 gas atmosphere. Atmosphere is C
100% O 2 gas is desirable, but contains substantially no O 2 gas,
That is, an inert gas such as N 2 or Ar may be contained as long as it does not contain O 2 other than those contained as impurities. However, the ambient gas is 30% to enhance the effect of CO 2 gas.
More than (volume) should be CO 2 gas. The crushing time varies depending on the type and capacity of the crusher, but in the above ball mill etc.
Grind for about 100 hours.
粉砕が終了したらその粉砕機内に分子式内に酸素原子を
含む有機溶媒を導入することが望ましい。粉砕した微粉
を空気中に瀑すと微粉の表面で空気中の酸素と反応し、
CO2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。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。After the pulverization is completed, it is desirable to introduce an organic solvent containing an oxygen atom in its molecular formula into the pulverizer. When crushed fine powder is dropped in the air, it reacts with oxygen in the air on the surface of the fine powder,
This is because the CO 2 crushing effect is diminished. The method of introducing the solvent into the crusher is to temporarily vacuum the inside of the crusher and then suck the solvent or press-fit. A slurry having good dispersibility can be obtained by further dispersing and mixing the mixture thus obtained using a ball mill or the like.
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 be varied over a wide range depending on the purpose of use, but most commonly, graphite fine powder having a concentration of 3 to 30% by weight is suitable for use.
分子式内に酸素原子を含む有機溶媒としてはメチルエチ
ルケトン（ＭＥＫ）、アセトン、メチルイソブチルケト
ン（ＭＩＢＫ）、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。Examples of the organic solvent containing an oxygen atom in its molecular formula include methyl ethyl ketone (MEK), acetone, methyl isobutyl ketone (MIBK), methyl-n-butyl ketone, methyl-
n-Propyl ketone, methanol, ethanol, butanol, acetic acid ester, acrylic acid and the like are suitable, and ketones are particularly preferable.
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。The slurry was diluted with the same dispersion medium to measure the particle size of the fine graphite powder of the slurry thus obtained. A laser diffraction type particle size distribution measuring device was used for measuring the particle size. As a result, it was found that the fine graphite powder had an average particle size of 1 micron or less and was hardly aggregated.
作 用 黒鉛をCO2系ガス雰囲気で粉砕し、それを分散媒として
分子式内に酸素原子を含む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分子式内に酸素原
子を含む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 agglomeration of fine graphite powder does not occur when crushing graphite in a CO 2 gas atmosphere and using an organic solvent containing oxygen atoms in the molecular formula as a dispersion medium is explained below. CO 2 gas acts on the surface of the graphite fine powder to generate a solvophilic functional group, and the existence of the surface prevents the aggregation of the fine powder in the organic solvent containing oxygen atoms in the molecular formula and promotes dispersion. It is thought that it depends.
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３のポットミルポットに
入れた。そこへ直径１０mmの鉄製ボールを１．２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 a raw material obtained by preliminarily crushing artificial graphite to an average particle size of 5.8 microns was weighed and put in a pot mill pot having an inner volume of 3. 1.2 iron balls having a diameter of 10 mm were put therein and used as a grinding medium. The pot was capped, the inside of the pot was once evacuated, and then Co 2 gas was sealed at 760 Torr, and the valve of the sealing line was closed to close the pot.
ポットをポットミル架台にのせ、回転数６０r.p.m.で６
５時間粉砕を行なった。Place the pot on the pot mill stand and rotate at 60 rpm for 6
Grinding was carried out for 5 hours.
粉砕が終了したポットを架台から取りはずし、ポット内
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６０r.p.m.で５０時間分散混合を行なった。混合
が終了してからポ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。The crushed pot was removed from the gantry, the gas in the pot was sucked up to a pressure of 50 Torr with a vacuum pump, and then 500 cc of methyl ethyl ketone was introduced into the pot. Then, put this pot on the pot mill stand again,
Dispersion and mixing were carried out at a rotation speed of 60 rpm for 50 hours. After the mixing was completed, the slurry in the pot was taken out and the particle size was measured using a laser diffraction type particle size distribution analyzer. As a result, the 50% cumulative average diameter was 0.37 micron.
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 to 3 and Comparative Examples 1 to 3 The same procedure as in Example 1 was performed, except that the atmosphere and the kind of the solvent in the pulverization were changed. Table 1 shows the conditions and results.
〔発明の効果〕 本発明によれば、雰囲気調整粉砕によって得られた黒鉛
の微粉を、産業上利用価値のの高い、分子式内に酸素原
子を含む有機溶媒へ良好に分散したスラリーとして得る
事が可能となり、黒鉛の利用上きわめて有用である。 [Effects of the Invention] According to the present invention, it is possible to obtain fine graphite powder obtained by atmosphere adjustment pulverization as a slurry having high industrial utility value and well dispersed in an organic solvent containing an oxygen atom in its molecular formula. It becomes possible and is extremely useful in using graphite.
Claims (1)
２ガスまたは不活性ガスを含むＣＯ２ガスの雰囲気下で
粉砕し、その黒鉛微粉に分子式内に酸素原子を含む有機
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。1. Graphite containing substantially no O 2 gas and CO
A method for producing a fine graphite powder-dispersed slurry, which comprises pulverizing in an atmosphere of 2 gas or CO 2 gas containing an inert gas and adding an organic solvent containing oxygen atoms in the molecular formula to the fine graphite 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 JPS62265110A (en) | 1987-11-18 |
| JPH0621019B2 true 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) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06102528B2 (en) * | 1988-09-13 | 1994-12-14 | 関西熱化学株式会社 | Purification method of quiche graphite |
| JPH06102529B2 (en) * | 1989-07-19 | 1994-12-14 | 関西熱化学株式会社 | Graphite purification method |
| KR101245815B1 (en) | 2011-07-14 | 2013-03-21 | 국립대학법인 울산과학기술대학교 산학협력단 | Edge-functionalized graphite via mechanic-chemical process and Manufacture of Its |
-
1986
- 1986-05-14 JP JP61108695A patent/JPH0621019B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62265110A (en) | 1987-11-18 |
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