JP4046785B2 - Non-conductive carbonaceous powder and method for producing the same - Google Patents
Non-conductive carbonaceous powder and method for producing the same Download PDFInfo
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- JP4046785B2 JP4046785B2 JP15048396A JP15048396A JP4046785B2 JP 4046785 B2 JP4046785 B2 JP 4046785B2 JP 15048396 A JP15048396 A JP 15048396A JP 15048396 A JP15048396 A JP 15048396A JP 4046785 B2 JP4046785 B2 JP 4046785B2
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
Description
【０００１】
【発明の属する技術分野】
本発明は非導電性炭素質粉体に関し、更に詳しくは高い遮光性、黒色度及び非導電性が要求される用途において使用される非導電性炭素質粉体であって、プリント基板の着色、ブラウン管のシャドウマスク、液晶表示装置用カラーフィルターのブラックマトリックス等に非導電性黒色層を与えることができる非導電性炭素質粉体に関する。
【０００２】
【従来の技術】
従来、ブラウン管のシャドウマスク、液晶表示装置用カラーフィルターのブラックマトリックス等の製造に際しては、非導電性黒色塗膜を与える塗料が求められてきた。従来、これらの塗料に使用される黒色顔料としては、酸化鉄系黒色顔料或いは黄色、赤色及び青色等の有機顔料を配合してなる黒色顔料が使用されてきた。
【０００３】
【発明が解決しようとする課題】
しかしながら、これらの顔料を用いて形成される塗膜では黒色隠蔽度が不十分であることや、材料自体が高価であるという欠点を有している。
カーボンブラック等の炭素質粉体は黒色度が優れ、安価であることから上記の如き用途の塗料の顔料として広く使用されてきたが、炭素質粉体には本来導電性があり、非導電性が要求される場合には適しておらず、非導電性が要求される用途に使用する場合には、塗料中の炭素質粉体の含量を極端に低くしなければならないという問題を有していた。
【０００４】
これらの問題に対し、本発明者らは、既にに炭素質粉体に静電的吸引力により絶縁化物を直接吸着させる、或いは結合剤を用いて炭素質粉体の表面の一部に絶縁化物を固定する方法を提案しているが、直接静電的吸引力で絶縁化物を付着させる場合は、絶縁化物が炭素質粉体から剥がれやすく、塗料中に炭素質粉体に付着していない絶縁化物が多く存在し、これらの付着していない絶縁化物が、塗膜にした場合に膜の均一性や遮光性を低下させる原因となる。又、結合剤を用いた場合、炭素質粉体に付着していない絶縁化物の量を抑えることができるが、炭素質粉体、或いは絶縁化物に結合剤を導入する操作は、一般に複雑で、充分な絶縁化効果を持つ結合剤の結合活性は高く、空気中の水分で結合活性が失活するため、品質の安定した非導電性炭素質粉体を大量に作製する際には問題がある。
【０００５】
更に、絶縁化物として使用される微粒子の粒子径は、炭素質粉体の遮光性を損なわないためには充分に小さくする必要があるが、微粒子の粒子径を小さくすると、その凝集力が強くなり、凝集構造を破壊することが困難となるため、絶縁化物は微粒子の集合体として炭素質粉体に吸着し、結果としてその遮光性を低下させることとなる。
【０００６】
従って本発明の目的は、炭素質粉体表面と絶縁化物の両者に対し、強い親和性を有する有機高分子化合物を用いることで、炭素質粉体の少なくとも一部に絶縁化物を選択的に吸着及び被覆する操作を簡便に行うことができ、且つ絶縁化物の剥離や凝集も起こりにくくすることで、炭素質材料の導電性を排除し、塗膜に絶縁性を付与することが可能な黒色塗料に用いることができる非導電性炭素質粉体を提供することである。
【０００７】
【課題を解決するための手段】
上記目的は以下の本発明によって達成される。即ち、本発明は、炭素質粉体の表面の少なくとも一部が、炭素質粉体に対し親和性を有する有機高分子化合物、及び該有機高分子化合物に対して親和性を有する絶縁化物の少なくとも１種で被覆され、前記有機高分子化合物が、イミニウムイオン生成基を有することを特徴とする非導電性炭素質粉体、及びその製造方法である。
【０００８】
炭素質粉体の表面の少なくとも一部を、前記の如き炭素質粉体に対し親和性を有する有機高分子化合物、及び該有機高分子化合物に対し親和性を有する絶縁化物で被覆することによって、炭素質粉体の導電性を排除し、塗膜に絶縁性を付与することが可能な黒色塗料に用いることができる非導電性炭素質粉体を提供することができる。
【０００９】
本発明では、炭素質粉体の有する固有の導電性及び塗膜中の炭素質粉体の連鎖による塗膜の導電性を、炭素質粉体の少なくとも表面の一部を絶縁化物で被覆することによって、炭素質粉体相互の連鎖を遮断して導電性を無くし、これらの非導電性炭素質粉体を塗料に使用することによって、形成される塗膜の絶縁化を図ることができる。
又、この時、炭素質粉体表面の少なくとも一部を、炭素質粉体に対し親和性を有する有機高分子化合物で覆い、更に該有機高分子化合物に対し親和性を有する絶縁化物で覆うことで、膜の均一性や遮光性を損なわず、塗膜を得る操作も簡便に行うことができる。
【００１０】
【発明の実施の形態】
次に好ましい実施の形態を挙げて本発明を更に詳しく説明する。
本発明でいう非導電性炭素質粉体とは、炭素質粉体の表面の少なくとも一部が、炭素質粉体に対して親和性を有する有機高分子化合物、及び該有機高分子化合物に対して親和性を有する絶縁化物によって被覆された炭素質粉体である。
【００１１】
本発明で使用する炭素質粉体としては、例えば、ケッチェンブラック、アセチレンブラック、ファーネスブラック等のカーボンブラックや、天然又は人造の黒鉛等があり、その他のカーボンホイスカー、カーボンファイバーやグラファイトファイバー、カーボンナノチューブ等の短繊維等を挙げることができ、これらの炭素質粉体は単独で使用することができる他、２種以上を組み合わせて使用することもできる。
【００１５】
上記炭素質粉体の表面を被覆する炭素質粉体に対し親和性を有する有機高分子化合物が、Ｎ−アルキルアミノベンゾフェノン等のアミノベンゾフェノン類やＮ−アルキルカプロラクタム等のラクタム類からの、いわゆるイミニウムイオンを生成する官能基を有する場合には、炭素質粉体の種類や極性基の有無を問わず、その表面に対し著しい親和性を有するため、極性基の少ない炭素質粉体を用いる場合や、より選択的な有機高分子化合物の吸着が必要な場合は特に好ましく用いられる。
【００１７】
更に、炭素質粉体に対して、種類の有無を問わず、その表面に対し著しい親和性を有するアミノベンゾフェノン類やラクタム類等のイミニウムイオン生成基を有する有機高分子化合物は、本発明で使用される絶縁化物に対しても良好な親和性を有するため、表面の酸化物層が少ない絶縁化物を用いる場合等は特に好ましく使用される。
【００１８】
上記炭素質粉体を被覆する絶縁化物としては、金属化合物の加水分解物、部分加水分解物、無機化合物粒子、及びそれらの混合物から選択された少なくとも１種の無機粒子である。これらの無機粒子のうちで、加水分解物又は部分加水分解物としては、無機金属塩、有機酸塩、有機金属化合物、有機金属錯体、及びそれらの誘導体の１種又は２種以上を組み合わせて加水分解又は部分加水分解した無機粒子を使用することができる。
これらの無機粒子は、炭素質粉体表面に有機高分子化合物を介して吸着し、その場で殆ど凝集することなく絶縁化物として析出するため、炭素質粉体の少なくとも一部を絶縁化物で被覆することができる。
【００１９】
これらの加水分解物又は部分加水分解物から得られる絶縁化物は、その大きさが数μｍ以下のいわゆる超微粒子である場合が殆どであって、炭素質粉体の表面に析出した場合も、その遮光性を全く損なわずに絶縁性のみを炭素質粉体に付与することが可能となる。
上記炭素質粉体の表面を被覆する絶縁化物のうち、無機化合物粒子としては、酸化アルミニウム、酸化チタン、酸化鉄及び二酸化ケイ素等の金属酸化物、及び窒化ケイ素、窒化アルミニウム等の金属窒化物、及びフッ化マグネシウム等の金属フッ化物、及び炭化アルミニウム等の金属炭化物等の非導電性の微粒子の１種又は２種以上を組み合わせて使用することができる。
【００２０】
又、黒色塗膜を形成する塗料組成物に合せて、これらの無機化合物粒子の表面を改質し、その表面に親水性又は新油性を持たせることもできる。これらの無機化合物粒子は、非導電性であれば特に限定されないが、安価で取扱が容易であり、又、有機高分子化合物との親和性に優れ、且つ人体に対しても無害な二酸化ケイ素微粒子が好ましい。
これらの無機化合物粒子はその大きさを任意に選択することが可能なので、炭素質粉体が複雑な形状を持ち、その一部を加水分解物、及び部分加水分解物からの絶縁化物で被覆しただけでは、炭素質粉体同士の連鎖を防げない場合には特に好ましく用いることができる。
【００２１】
本発明においては、上記絶縁化物として前記加水分解物又は部分加水分解物と無機化合物微粒子とを組み合わせて用いることも可能である。この組合せを用いて本発明の非導電性炭素質粉体を製造した場合、絶縁化物のうちの加水分解物又は部分加水分解物は、それ自身が炭素質粉体表面に有機高分子化合物を介して析出すると同時に、炭素質粉体表面に吸着した無機化合物粒子と無機物膜を形成して炭素質粉体表面を被覆することも可能となる。
又、本発明で使用する絶縁化物は、炭素質粉体を含む塗料中における炭素質粉体の微小化及び粒子径の均一安定化等の分散安定化剤としての効果も有する。
【００２２】
本発明の非導電性炭素質粉体の実現のためには、予め炭素質粉体に対して親和性を有する上記有機高分子化合物を炭素質粉体の少なくとも一部に吸着させた後、絶縁化物を添加及び吸着させて非導電性炭素質粉体とする場合と、炭素質粉体を分散させた溶剤中で炭素質粉体に対して親和性を有する有機高分子化合物を合成し、その表面の少なくとも一部に吸着させた後、絶縁化物を添加及び吸着させて非導電性炭素質粉体とする場合が挙げられ、必要に応じて両者を選択することができる。
【００２３】
本発明の非導電性炭素質粉体の製造は、炭素質粉体の表面に対して親和性を有する有機高分子化合物を使用することで、結合剤の結合活性を保持するために大気中の水分との接触を極力避ける等の複雑な操作を要した従来法に比べ、同等の特性を容易に実現することが可能となる。
【００２４】
以上の本発明において炭素質粉体の表面を被覆するために使用する有機高分子化合物、及び該有機高分子化合物に対して親和性を有する絶縁化物の使用量は、被覆されるべき炭素質粉体の表面積にもよるが、一般的には炭素質粉体１００重量部当たり有機高分子化合物が約０．１〜２００重量部、好ましくは約１０〜１００重量部であり、絶縁化物が約０．１〜３００重量部、好ましくは約１０〜２００重量部である。有機高分子化合物及び絶縁化物の使用量が多すぎると、炭素質粉体の優れた遮光性が損われ、一方、使用量が少なすぎると炭素質粉体の絶縁性が低下する。
【００２５】
【実施例】
次に実施例及び比較例を挙げて本発明を更に具体的に説明する。尚、例中、「部」は重量部を意味する。体積抵抗値は、炭素質粉体をエポキシ樹脂に対して５０重量％分散させ、この分散ペーストをＩＴＯ成膜済みガラス基板板上に塗布し、１５０℃で９０分間乾燥後、厚さ方向の抵抗値を測定して求めた。
実施例１
（１）炭素質粉体分散液
ＭＣＦ＃９７０（三菱化学（株）製、カーボンブラック顔料） ５部
エタノール ９５部
からなる混合物を撹拌混合し、炭素質粉体分散液を得た。
【００２６】
（２）有機高分子化合物による被覆
上記（１）の炭素質粉体分散液 ９６部
両末端をε−カプロラクトンで封止したポリアクリル酸 ４部
（分子量１万）
からなる混合物を２５℃で３時間撹拌し、カーボンブラック表面への有機高分子化合物の吸着処理を行った。
（３）絶縁化物による被覆
上記（２）の炭素質粉体分散液 ８７部
テトラエトキシシラン １０部
０．００１Ｎ塩酸水溶液 ３部
からなる混合物を２５℃で１０時間撹拌し、炭素質粉体表面へ有機高分子化合物を介してテトラエトキシシランの加水分解物による被覆処理を行った。
以上得られた加水分解物被覆炭素質粉体を濾過及び洗浄して未反応物を除去した後、充分乾燥し、粉砕して本発明の非導電性炭素質粉体を得た。
【００２７】
実施例２
（１）炭素質粉体分散液
ＭＣＦ＃９７０（三菱化学（株）製、カーボンブラック顔料） ５部
エタノール ９５部
からなる混合物を撹拌混合し、炭素質粉体分散液を得た。
（２）有機高分子化合物による被覆
上記（１）の炭素質粉体分散液 ９５部
２−メチル２−オキサゾリン ３部
アクリル酸 ２部
からなる混合物を２５℃で８時間撹拌し、カーボンブラック表面への有機高分子化合物の吸着処理を行った。
【００２８】
（３）絶縁化物による被覆
上記（２）の炭素質粉体分散液 ８７部
テトラエトキシシラン １０部
０．００１Ｎ塩酸水溶液 ３部
からなる混合物を２５℃で１０時間撹拌し、炭素質粉体表面へ有機高分子化合物を介してテトラエトキシシランの加水分解物による被覆処理を行った。
以上得られた加水分解物被覆炭素質粉体を濾過及び洗浄して未反応物を除去した後、充分乾燥し、粉砕して本発明の非導電性炭素質粉体を得た。
【００２９】
比較例１
実施例１で有機高分子化合物による被覆処理を行わず、炭素質粉体分散液８７重量部にテトラエトキシシラン１０重量部と０．００１Ｎ塩酸水溶液３重量部を加え、２５℃で１０時間撹拌した後、実施例１と同様の操作で炭素質粉体を取出した。
（体積抵抗値の測定例）
ＭＣＦ＃９７０単独、各実施例及び比較例における炭素質粉体の体積抵抗値を表１に示す。
【００３０】
【表１】
【００３１】
【発明の効果】
以上の如き本発明によれば、炭素質粉体の表面の少なくとも一部を前記の如き炭素質粉体に対し親和性を有するイミニウムイオン生成基を有する有機高分子化合物、及び該有機高分子化合物に対し親和性を有する絶縁化物で被覆することによって、炭素質粉体の導電性を排除し、塗膜に絶縁性を付与することが可能な黒色塗料に用いることができる非導電性炭素質粉体を提供することができる。
【００３２】
本発明では、炭素質粉体の有する固有の導電性及び塗膜中の炭素質粉体の連鎖による塗膜の導電性を、炭素質粉体の少なくとも表面の一部を絶縁化物で被覆することによって、炭素質粉体相互の連鎖を遮断して導電性を無くし、これらの非導電性炭素質粉体を塗料に使用することによって、形成される塗膜の絶縁化を図ることができる。
又、この時、炭素質粉体表面の少なくとも一部を炭素質粉体に対し親和性を有するイミニウムイオン生成基を有する有機高分子化合物で覆い、更に該有機高分子化合物に対し親和性を有する絶縁化物で覆うことで、膜の均一性や遮光性を損なわず、塗膜を得る操作も簡便に行うことができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a non-conductive carbonaceous powder, and more specifically, a non-conductive carbonaceous powder used in applications requiring high light-shielding property, blackness and non-conductivity, The present invention relates to a nonconductive carbonaceous powder capable of providing a nonconductive black layer on a shadow mask of a cathode ray tube, a black matrix of a color filter for a liquid crystal display device, or the like.
[0002]
[Prior art]
Conventionally, in the production of a shadow mask for a cathode ray tube, a black matrix for a color filter for a liquid crystal display device, and the like, a paint that gives a non-conductive black coating film has been demanded. Conventionally, as black pigments used in these paints, iron oxide black pigments or black pigments formed by blending organic pigments such as yellow, red and blue have been used.
[0003]
[Problems to be solved by the invention]
However, a coating film formed using these pigments has a drawback that the black concealment degree is insufficient and the material itself is expensive.
Carbon black and other carbonaceous powders have been widely used as paint pigments for the above-mentioned applications because of their excellent blackness and low cost. However, carbonaceous powders are inherently conductive and non-conductive. However, when used in applications where non-conductivity is required, the content of carbonaceous powder in the paint must be extremely low. It was.
[0004]
In response to these problems, the present inventors have already adsorbed the insulating material directly to the carbonaceous powder by electrostatic attraction, or the insulating material is partly attached to the surface of the carbonaceous powder using a binder. However, if the insulator is attached directly by electrostatic attraction, the insulator is easily peeled off from the carbonaceous powder, and the insulation that does not adhere to the carbonaceous powder in the paint is used. There are a lot of chemicals, and these non-adhered insulating materials cause a reduction in film uniformity and light-shielding properties when formed into a coating film. In addition, when a binder is used, the amount of insulating material not attached to the carbonaceous powder can be suppressed, but the operation of introducing the binder into the carbonaceous powder or insulating material is generally complicated. The binding activity of a binder with sufficient insulation effect is high, and the binding activity is deactivated by moisture in the air, so there is a problem when producing a large quantity of non-conductive carbonaceous powder with stable quality .
[0005]
Furthermore, the particle size of the fine particles used as the insulating material needs to be sufficiently small so as not to impair the light-shielding property of the carbonaceous powder. However, if the particle size of the fine particles is small, the cohesive force becomes strong. Since it becomes difficult to destroy the aggregate structure, the insulating material is adsorbed on the carbonaceous powder as an aggregate of fine particles, and as a result, the light shielding property is lowered.
[0006]
Accordingly, an object of the present invention is to selectively adsorb the insulator on at least a part of the carbonaceous powder by using an organic polymer compound having a strong affinity for both the carbonaceous powder surface and the insulator. In addition, a black paint that can easily perform the covering operation, and also prevents the insulation from being peeled off or aggregated, thereby eliminating the conductivity of the carbonaceous material and imparting insulation to the coating film. It is providing the nonelectroconductive carbonaceous powder which can be used for.
[0007]
[Means for Solving the Problems]
The above object is achieved by the present invention described below. That is, the present invention provides an organic polymer compound in which at least a part of the surface of the carbonaceous powder has an affinity for the carbonaceous powder, and at least an insulating material having an affinity for the organic polymer compound. coated with one, it said organic polymer compound is a non-conductive carbonaceous particles, and a manufacturing method thereof, wherein Rukoto which have a iminium ion forming group.
[0008]
By covering at least a part of the surface of the carbonaceous powder with an organic polymer compound having affinity for the carbonaceous powder as described above, and an insulating material having affinity for the organic polymer compound, It is possible to provide a non-conductive carbonaceous powder that can be used in a black paint capable of eliminating the conductivity of the carbonaceous powder and imparting insulating properties to the coating film.
[0009]
In the present invention, the intrinsic conductivity of the carbonaceous powder and the conductivity of the coating film due to the chain of the carbonaceous powder in the coating film are coated with an insulator on at least a part of the surface of the carbonaceous powder. Thus, the chain between the carbonaceous powders is interrupted to eliminate the conductivity, and by using these non-conductive carbonaceous powders in the paint, the formed coating film can be insulated.
At this time, at least a part of the surface of the carbonaceous powder is covered with an organic polymer compound having an affinity for the carbonaceous powder, and further covered with an insulating material having an affinity for the organic polymer compound. Thus, the operation of obtaining the coating film can be easily performed without impairing the uniformity and light shielding property of the film.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
Next, the present invention will be described in more detail with reference to preferred embodiments.
The non-conductive carbonaceous powder referred to in the present invention is an organic polymer compound in which at least a part of the surface of the carbonaceous powder has affinity for the carbonaceous powder, and the organic polymer compound. It is a carbonaceous powder coated with an insulating material having affinity.
[0011]
Examples of the carbonaceous powder used in the present invention include carbon black such as ketjen black, acetylene black, and furnace black, natural or artificial graphite, and other carbon whiskers, carbon fibers, graphite fibers, and carbon. Short fibers such as nanotubes can be mentioned, and these carbonaceous powders can be used alone or in combination of two or more.
[0015]
Organic polymer compounds having an affinity for the carbonaceous powder covering the surface of the carbonaceous powder are so-called “I” from aminobenzophenones such as N-alkylaminobenzophenone and lactams such as N-alkylcaprolactam. When having functional groups that generate minium ions, regardless of the type of carbonaceous powder and the presence or absence of polar groups, it has significant affinity for the surface, so when using carbonaceous powders with few polar groups It is particularly preferably used when more selective adsorption of an organic polymer compound is required.
[0017]
Furthermore, an organic polymer compound having an iminium ion-generating group such as aminobenzophenones and lactams having a remarkable affinity for the surface of carbonaceous powders, regardless of the type, is used in the present invention. Since it has a good affinity for the insulator used, it is particularly preferably used when an insulator having a small oxide layer on the surface is used.
[0018]
The insulating material covering the carbonaceous powder is at least one kind of inorganic particles selected from hydrolysates of metal compounds, partial hydrolysates, inorganic compound particles, and mixtures thereof. Among these inorganic particles, the hydrolyzate or partial hydrolyzate may be an inorganic metal salt, an organic acid salt, an organometallic compound, an organometallic complex, or a combination of one or more of these derivatives. Decomposed or partially hydrolyzed inorganic particles can be used.
These inorganic particles are adsorbed on the surface of the carbonaceous powder through the organic polymer compound, and are deposited as an insulating material with almost no agglomeration in situ, so at least a part of the carbonaceous powder is coated with the insulating material. can do.
[0019]
Insulations obtained from these hydrolysates or partial hydrolysates are mostly so-called ultrafine particles having a size of several μm or less, and even when precipitated on the surface of carbonaceous powder, Only the insulating property can be imparted to the carbonaceous powder without impairing the light shielding property.
Among the insulators covering the surface of the carbonaceous powder, as inorganic compound particles, metal oxides such as aluminum oxide, titanium oxide, iron oxide and silicon dioxide, and metal nitrides such as silicon nitride and aluminum nitride, One kind or two or more kinds of non-conductive fine particles such as metal fluoride such as magnesium fluoride and metal carbide such as aluminum carbide can be used in combination.
[0020]
Moreover, according to the coating composition which forms a black coating film, the surface of these inorganic compound particle | grains can be modify | reformed, and the hydrophilicity or new oil property can be given to the surface. These inorganic compound particles are not particularly limited as long as they are non-conductive, but are inexpensive, easy to handle, excellent in affinity with organic polymer compounds, and harmless to the human body. Is preferred.
Since these inorganic compound particles can be arbitrarily selected in size, the carbonaceous powder has a complicated shape, and a part thereof is coated with a hydrolyzate and an insulator from the partial hydrolyzate. If it is not possible to prevent chaining of carbonaceous powders, it can be particularly preferably used.
[0021]
In the present invention, the hydrolyzate or partial hydrolyzate and inorganic compound fine particles can be used in combination as the insulating material. When the non-conductive carbonaceous powder of the present invention is produced using this combination, the hydrolyzate or partial hydrolyzate of the insulating material itself has an organic polymer compound interposed on the surface of the carbonaceous powder. At the same time, the inorganic compound particles adsorbed on the surface of the carbonaceous powder and an inorganic film can be formed to coat the surface of the carbonaceous powder.
The insulating material used in the present invention also has an effect as a dispersion stabilizer such as miniaturization of the carbonaceous powder and uniform stabilization of the particle diameter in the coating material containing the carbonaceous powder.
[0022]
In order to realize the non-conductive carbonaceous powder of the present invention, the organic polymer compound having an affinity for the carbonaceous powder is adsorbed on at least a part of the carbonaceous powder and then insulated. When a non-conductive carbonaceous powder is added and adsorbed to form a non-conductive carbonaceous powder, an organic polymer compound having an affinity for the carbonaceous powder is synthesized in a solvent in which the carbonaceous powder is dispersed. In some cases, after adsorbing on at least a part of the surface, an insulator is added and adsorbed to form a non-conductive carbonaceous powder, and both can be selected as necessary.
[0023]
In the production of the non-conductive carbonaceous powder of the present invention, an organic polymer compound having affinity for the surface of the carbonaceous powder is used to maintain the binding activity of the binder in the atmosphere. Compared to conventional methods that require complicated operations such as avoiding contact with moisture as much as possible, it is possible to easily realize equivalent characteristics.
[0024]
The amount of the organic polymer compound used for coating the surface of the carbonaceous powder in the present invention and the insulating material having an affinity for the organic polymer compound is the carbonaceous powder to be coated. Although it depends on the surface area of the body, generally, the organic polymer compound is about 0.1 to 200 parts by weight, preferably about 10 to 100 parts by weight, and the insulator is about 0 per 100 parts by weight of the carbonaceous powder. 0.1 to 300 parts by weight, preferably about 10 to 200 parts by weight. If the amount of the organic polymer compound and the insulating material used is too large, the excellent light-shielding property of the carbonaceous powder is impaired. On the other hand, if the amount used is too small, the insulating property of the carbonaceous powder decreases.
[0025]
【Example】
Next, the present invention will be described more specifically with reference to examples and comparative examples. In the examples, “parts” means parts by weight. The volume resistance is 50% by weight of carbon powder dispersed in an epoxy resin. This dispersion paste is applied onto a glass substrate plate with ITO film formed, dried at 150 ° C. for 90 minutes, and then resistance in the thickness direction. The value was determined by measurement.
Example 1
(1) Carbonaceous powder dispersion MCF # 970 (manufactured by Mitsubishi Chemical Corporation, carbon black pigment) A mixture of 95 parts of ethanol and 95 parts of ethanol was stirred and mixed to obtain a carbonaceous powder dispersion.
[0026]
(2) Coating with organic polymer compound 96 parts of carbonaceous powder dispersion of (1) above 4 parts of polyacrylic acid with both ends sealed with ε-caprolactone (molecular weight 10,000)
The mixture consisting of was stirred at 25 ° C. for 3 hours, and an organic polymer compound was adsorbed onto the carbon black surface.
(3) Coating with insulating material Carbonaceous powder dispersion of (2) above 87 parts tetraethoxysilane 10 parts 0.001 N aqueous hydrochloric acid solution 3 parts is stirred at 25 ° C. for 10 hours to the surface of carbonaceous powder The coating process with the hydrolyzate of tetraethoxysilane was performed through the organic polymer compound.
The hydrolyzate-coated carbonaceous powder obtained above was filtered and washed to remove unreacted materials, and then sufficiently dried and pulverized to obtain the nonconductive carbonaceous powder of the present invention.
[0027]
Example 2
(1) Carbonaceous powder dispersion MCF # 970 (manufactured by Mitsubishi Chemical Corporation, carbon black pigment) A mixture of 95 parts of ethanol and 95 parts of ethanol was stirred and mixed to obtain a carbonaceous powder dispersion.
(2) Coating with organic polymer compound Carbonaceous powder dispersion liquid of above (1) 95 parts 2-methyl 2-oxazoline 3 parts A mixture of 2 parts acrylic acid is stirred at 25 ° C. for 8 hours to the surface of carbon black The organic polymer compound was adsorbed.
[0028]
(3) Coating with insulating material Carbonaceous powder dispersion of (2) above 87 parts tetraethoxysilane 10 parts 0.001 N aqueous hydrochloric acid solution 3 parts is stirred at 25 ° C. for 10 hours to the surface of carbonaceous powder The coating process with the hydrolyzate of tetraethoxysilane was performed through the organic polymer compound.
The hydrolyzate-coated carbonaceous powder obtained above was filtered and washed to remove unreacted materials, and then sufficiently dried and pulverized to obtain the nonconductive carbonaceous powder of the present invention.
[0029]
Comparative Example 1
In Example 1, the coating treatment with the organic polymer compound was not performed, and 10 parts by weight of tetraethoxysilane and 3 parts by weight of 0.001N hydrochloric acid aqueous solution were added to 87 parts by weight of the carbonaceous powder dispersion, followed by stirring at 25 ° C. for 10 hours. Thereafter, the carbonaceous powder was taken out by the same operation as in Example 1.
(Measurement example of volume resistivity)
Table 1 shows the volume resistance values of the carbonaceous powder in MCF # 970 alone, each of Examples and Comparative Examples.
[0030]
[Table 1]
[0031]
【The invention's effect】
According to the present invention as described above, at least a part of the surface of the carbonaceous powder has an iminium ion-forming group having affinity for the carbonaceous powder as described above, and the organic polymer. Non-conductive carbonaceous material that can be used in black paints that can provide conductivity to the coating film by eliminating the electrical conductivity of the carbonaceous powder by coating with an insulator having an affinity for the compound. Powders can be provided.
[0032]
In the present invention, the intrinsic conductivity of the carbonaceous powder and the conductivity of the coating film due to the chain of the carbonaceous powder in the coating film are coated with an insulator on at least a part of the surface of the carbonaceous powder. Thus, the chain between the carbonaceous powders is interrupted to eliminate the conductivity, and by using these non-conductive carbonaceous powders in the paint, the formed coating film can be insulated.
At this time, at least a part of the surface of the carbonaceous powder is covered with an organic polymer compound having an iminium ion-forming group having an affinity for the carbonaceous powder, and the affinity for the organic polymer compound is further increased. By covering with the insulating material which has, the operation which obtains a coating film can also be performed simply, without impairing the uniformity and light-shielding property of a film | membrane.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP15048396A JP4046785B2 (en) | 1996-05-23 | 1996-05-23 | Non-conductive carbonaceous powder and method for producing the same |
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| JP15048396A JP4046785B2 (en) | 1996-05-23 | 1996-05-23 | Non-conductive carbonaceous powder and method for producing the same |
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| Publication Number | Publication Date |
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| JP4046785B2 true JP4046785B2 (en) | 2008-02-13 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH11181324A (en) * | 1997-12-24 | 1999-07-06 | Mitsubishi Chemical Corp | Carbon black |
| JP3632558B2 (en) * | 1999-09-17 | 2005-03-23 | 日立化成工業株式会社 | Epoxy resin composition for sealing and electronic component device |
| JP4872154B2 (en) * | 2000-12-28 | 2012-02-08 | 株式会社島津製作所 | Method for producing fine hollow carbon |
| US6834439B2 (en) | 2002-05-21 | 2004-12-28 | Mitutoyo Corporation | Measuring tool, encoder and producing method of encoder |
| JP4543695B2 (en) * | 2004-02-18 | 2010-09-15 | 住友ベークライト株式会社 | Coated carbon material powder and method for producing the same |
| JP6294951B2 (en) * | 2016-01-26 | 2018-03-14 | デクセリアルズ株式会社 | HEAT CONDUCTIVE SHEET, HEAT CONDUCTIVE SHEET MANUFACTURING METHOD, HEAT DISSIBLING MEMBER AND SEMICONDUCTOR DEVICE |
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| JPS6060974A (en) * | 1983-09-14 | 1985-04-08 | ダイセル化学工業株式会社 | Manufacture of ceramic sintered formed body |
| JPH0730269B2 (en) * | 1986-09-04 | 1995-04-05 | 大日精化工業株式会社 | Surface treatment method for carbon black for powder coating |
| JPH0742473B2 (en) * | 1988-08-29 | 1995-05-10 | 株式会社ブリヂストン | Electrorheological liquid |
| JPH0316910A (en) * | 1989-06-14 | 1991-01-24 | Mitsubishi Kasei Corp | Fluid having electroviscous effect |
| JPH05213611A (en) * | 1991-08-09 | 1993-08-24 | Asahi Glass Co Ltd | Treatment of graphitic powder and graphite powder for making them hydrophilic |
| JPH05192146A (en) * | 1991-11-11 | 1993-08-03 | Osaka Gas Co Ltd | Active carbon and its production |
| DE4309700C2 (en) * | 1993-03-25 | 1995-02-23 | Sigri Great Lakes Carbon Gmbh | Process for the production of a laminate from metal and graphite |
| US5807494A (en) * | 1994-12-15 | 1998-09-15 | Boes; Ralph Ulrich | Gel compositions comprising silica and functionalized carbon products |
| JPH08245210A (en) * | 1995-03-09 | 1996-09-24 | New Oji Paper Co Ltd | Production of metal oxide carrying activated carbon |
| JP3577129B2 (en) * | 1995-03-22 | 2004-10-13 | 大日本印刷株式会社 | Non-conductive carbonaceous powder and method for producing the same |
| JPH08291295A (en) * | 1995-04-21 | 1996-11-05 | Tokai Carbon Co Ltd | Carbon fine powder for electroviscous fluid and its production |
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