JPS6227474A - Production of electrically conductive coating fluid - Google Patents

Production of electrically conductive coating fluid

Info

Publication number
JPS6227474A
JPS6227474A JP60168407A JP16840785A JPS6227474A JP S6227474 A JPS6227474 A JP S6227474A JP 60168407 A JP60168407 A JP 60168407A JP 16840785 A JP16840785 A JP 16840785A JP S6227474 A JPS6227474 A JP S6227474A
Authority
JP
Japan
Prior art keywords
tin oxide
binder resin
dispersant
conductive coating
solvent
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
Application number
JP60168407A
Other languages
Japanese (ja)
Other versions
JPH06898B2 (en
Inventor
Kaoru Yamamoto
薫 山本
Makoto Nakahira
中平 誠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Takiron Co Ltd
Original Assignee
Takiron Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Takiron Co Ltd filed Critical Takiron Co Ltd
Priority to JP60168407A priority Critical patent/JPH06898B2/en
Publication of JPS6227474A publication Critical patent/JPS6227474A/en
Publication of JPH06898B2 publication Critical patent/JPH06898B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE:To produce the title coating soln. which causes neither agglomeration nor precipitation of an ultrafine powder of tin oxide and which can maintain a uniform composition over a long period of time, by mixing a predried ultrafine powder of tin oxide and a binder resin with a dehydrated solvent. CONSTITUTION:A tin oxide dispersion obtd. by dispersing an ultrafine particle of tin oxide immediately after predrying in a dispersant soln. immediately after dehydration is mixed with a binder resin soln. obtd. by dissolving a binder resin immediately after predrying in a solvent immediately after dehydration.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、バインダー樹脂を含む溶剤中に酸化錫超微粒
子を分散させてなる導電性塗布液の製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing an electrically conductive coating liquid by dispersing ultrafine tin oxide particles in a solvent containing a binder resin.

〔従来の技術〕[Conventional technology]

上記種類の導電性塗布液は、プラスチック材の表面電気
抵抗値を小さくして塵埃の吸着を防止するためのコーテ
ィング剤としての用途に適する。
The above-mentioned type of conductive coating liquid is suitable for use as a coating agent for reducing the surface electrical resistance of plastic materials and preventing dust adsorption.

このような導電性塗布液は、従来、三酸化アンチモンで
ドーピングした酸化錫の超微粒子を、酸化錫に対して0
.5〜5tmt%の分散剤を溶解した溶液中に混入する
ことによって酸化錫分散液を作成し、この酸化錫分散液
をバインダー樹脂溶液と混合することによって製造して
いた。
Conventionally, such conductive coating liquids are made by using ultrafine particles of tin oxide doped with antimony trioxide, which have a zero resistance to tin oxide.
.. A tin oxide dispersion was prepared by mixing 5 to 5 tmt% of a dispersant into a solution, and the tin oxide dispersion was mixed with a binder resin solution.

このような従来方法において、分散剤の溶剤にはキシレ
ン、トルエン等の芳香族系溶剤又はメチルイソブチルケ
トン、メチルエチルケトン等のケトン類に属する溶剤が
用いられ、分散剤には界面活性剤(例えば、第−工業製
薬部製の商品名5AS−13,味の素■製の商品名93
等)が用いられ、酸化錫超微粒子には例えば三菱金属製
の商品名T−l等が用いられる。一方、バインダー樹脂
には例えば塩化ビニル樹脂、アクリル系樹脂、ポリエス
テル系樹脂等が用いられ、バインダー樹脂の溶剤にはシ
クロヘキサノン、メチルイソブチルケトン。
In such conventional methods, aromatic solvents such as xylene and toluene, or solvents belonging to ketones such as methyl isobutyl ketone and methyl ethyl ketone are used as the solvent for the dispersant, and a surfactant (for example, -Product name 5AS-13 manufactured by Industrial Pharmaceutical Department, Product name 93 manufactured by Ajinomoto ■
etc.) are used, and as the tin oxide ultrafine particles, for example, Mitsubishi Metals' product name T-1 or the like is used. On the other hand, the binder resin used is, for example, vinyl chloride resin, acrylic resin, polyester resin, etc., and the binder resin solvent is cyclohexanone or methyl isobutyl ketone.

七ロ、ソルブ、芳香族系溶剤等が用いられる。また、酸
化錫超微粒子と分散剤溶液との混合、酸化錫分散液とバ
インダー樹脂溶液との混合にはホモジナイザー、ボール
ミル、サンドミル等の攪拌装置が使用される。
Solvents, solvents, aromatic solvents, etc. are used. Further, a stirring device such as a homogenizer, a ball mill, or a sand mill is used to mix the ultrafine tin oxide particles and the dispersant solution, and to mix the tin oxide dispersion and the binder resin solution.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

しかし、上記した従来方法によって製造した導電性塗布
液を製造後放置すると数日間で酸化錫超微粒子が他の成
分から分離して凝集したり沈澱したりすることが多々あ
った。
However, if a conductive coating solution produced by the above conventional method is left to stand after production, the ultrafine tin oxide particles often separate from other components and aggregate or precipitate within several days.

本願発明者はこの点について調査を重ねた結果、酸化錫
超微粒子の凝集や沈澱が、分散剤溶液に混入する前の酸
化錫超微粒子の表面に若干の水分が吸着担持されている
こと2分散剤の溶剤やバインダー樹脂の溶剤に水分が含
まれていること9等に基づいていることを突き止め、さ
らに酸化錫超微粒子に水分が吸着担持されたり溶剤に水
分が含まれるのはそれらを使用する前の保存中であるこ
とを突き止めた。
As a result of repeated investigations on this point, the inventor of the present application has found that the agglomeration and precipitation of ultrafine tin oxide particles is due to a small amount of water being adsorbed and supported on the surface of ultrafine tin oxide particles before being mixed into the dispersant solution.2. We found out that water is contained in the solvent of the binder resin and the solvent of the binder resin, and furthermore, we found that water is adsorbed and supported on ultrafine tin oxide particles and that water is contained in the solvent. I found out that the previous one was being saved.

本発明はこのような調査の結果なされたもので、製造後
に長期間放置しておいても当該導電性塗布液中に分散さ
れている酸化錫超微粒子がa集や沈澱を起こさず、長期
に亘って均一組成が維持される導電性塗布液の製造方法
を提案することを目的とする。
The present invention was made as a result of such research, and the tin oxide ultrafine particles dispersed in the conductive coating solution do not aggregate or precipitate even if left for a long period of time after manufacture, and can be maintained for a long period of time. The purpose of the present invention is to propose a method for producing a conductive coating liquid that maintains a uniform composition throughout.

〔問題点を解決するための手段〕[Means for solving problems]

上記問題点を解決するため、本発明は、分散剤溶液中に
酸化錫超微粒子を混入することにより作成した酸化錫分
散液をバインダー樹脂溶液と混合する導電性塗布液の製
造方法において、酸化錫超微粒子を分散剤溶液中に混入
する直前に予備乾燥すると共に、分散剤の溶剤及びバイ
ンダー樹脂の溶剤を、分散剤及びバインダー樹脂を溶解
させる直前に脱水し、さらにバインダー樹脂を溶剤に溶
解させる直前に予備乾燥する点に要旨を有する。
In order to solve the above problems, the present invention provides a method for producing a conductive coating liquid in which a tin oxide dispersion prepared by mixing ultrafine tin oxide particles into a dispersant solution is mixed with a binder resin solution. Pre-drying the ultrafine particles immediately before mixing them into the dispersant solution, dehydrating the dispersant solvent and binder resin solvent immediately before dissolving the dispersant and binder resin, and further dissolving the binder resin in the solvent. The main point is to pre-dry it.

〔作 用〕[For production]

上記手段によると、分散剤溶液に混入する酸化錫超微粒
子の表面に吸着担持されていた水分が該溶液への混入に
先立って取り除かれる。また、分散剤の溶剤やバインダ
ー樹脂の溶剤に含まれていた水分が、これらの溶剤への
分散剤の溶解やバインダー樹脂の溶解に先立って取り除
かれる。さらにバインダー樹脂が溶剤に溶解される直前
に予備乾燥される。
According to the above means, water adsorbed and carried on the surface of ultrafine tin oxide particles mixed into the dispersant solution is removed prior to mixing into the solution. In addition, water contained in the solvent of the dispersant and the solvent of the binder resin is removed prior to dissolving the dispersant and the binder resin in these solvents. Furthermore, the binder resin is pre-dried immediately before being dissolved in the solvent.

以下、実験例を示して本発明方法を説明する。The method of the present invention will be explained below with reference to experimental examples.

〔実験例〕[Experiment example]

酸化錫分散液及びバインダー樹脂溶液を次に述べる方法
によって別個に作成した。
A tin oxide dispersion and a binder resin solution were prepared separately by the method described below.

(al酸化錫分散液の作成 シリカゲル適量を投入して脱水した直後のキシレン41
2 、5 ccに味の素側製の商品名9sを分散剤とし
て2.06g溶解させ、この分散剤溶液に、乾燥器内に
105.5℃、3時間放置して予備乾燥した酸化錫超微
粒子(三菱金属■製の商品名T−1) 206゜4gを
混入し、直径15CI11のボールミル中で約2日間分
散処理した。
(Preparation of al tin oxide dispersion) Xylene 41 immediately after adding an appropriate amount of silica gel and dehydrating
2.06g of Ajinomoto brand 9s as a dispersant was dissolved in 2.5 cc, and tin oxide ultrafine particles (pre-dried by standing in a dryer at 105.5°C for 3 hours) were added to this dispersant solution. 206° (4 g) of T-1 (trade name, manufactured by Mitsubishi Metals Ltd.) was mixed in and dispersed in a ball mill with a diameter of 15 CI11 for about 2 days.

(b)バインダー樹脂溶液の作成 シリカゲル適量を投入して脱水した直後のシクロへキサ
ノン412.5ccに50〜60°Cで乾燥したポリ塩
化ビニル樹脂(商品名リューロン800BL) 41.
3gを溶解させ、これに安定剤として日東化成■製の商
品名112000E 1.24gを混入した。
(b) Preparation of binder resin solution Add a suitable amount of silica gel to 412.5 cc of cyclohexanone immediately after dehydration, and dry at 50 to 60°C. Polyvinyl chloride resin (trade name: Lyuron 800BL) 41.
3 g was dissolved, and 1.24 g of Nitto Kasei ■ trade name 112000E was mixed therein as a stabilizer.

次に、上記方法で作成した酸化錫分散液にバインダー樹
脂溶液を混入し、上記のボールミルを使用して3日間分
散処理することによって導電性塗布液を調製した。
Next, a binder resin solution was mixed into the tin oxide dispersion prepared by the above method, and a conductive coating liquid was prepared by performing a dispersion treatment for 3 days using the above ball mill.

他方、比較例として、上記した酸化錫超微粒子の予備乾
燥並びにキシレン、シクロヘキサノン。
On the other hand, as a comparative example, the above-described pre-drying of ultrafine tin oxide particles, xylene, and cyclohexanone were used.

ポリ塩化ビニル樹脂の脱水を行うことな(、それ以外は
上記と同一条件で導電性塗布液を調製した。
A conductive coating liquid was prepared under the same conditions as above except that the polyvinyl chloride resin was not dehydrated.

〔実験結果の考察〕[Consideration of experimental results]

上記の実験例において調製した本発明方法による導電性
塗布液は約3箇月間の長期保存によっても酸化錫超微粒
子の凝集や沈澱がほとんど起こらなかった。また、上記
期間保存後の導電性塗布液をプラスチック板に塗布した
後のプラスチック板の表面状況は良好であった。
The conductive coating liquid according to the method of the present invention prepared in the above experimental example showed almost no aggregation or precipitation of ultrafine tin oxide particles even after long-term storage for about 3 months. Furthermore, the surface condition of the plastic plate after the conductive coating liquid was applied to the plastic plate after storage for the above-mentioned period was good.

これに対し、比較例による導電性塗布液は、調製後の数
日間の保存中に酸化錫超微粒子の沈澱が起こり始めた。
On the other hand, in the conductive coating liquid according to the comparative example, ultrafine tin oxide particles began to precipitate during storage for several days after preparation.

本発明方法において、分散剤の溶剤としては上記したキ
シレンのほかにトルエン等の芳香族系溶剤やメチルイソ
ブチルケトン、メチルエチルケトン等のケトン類の属す
る溶剤を使用でき、バインダー樹脂としては上記したポ
リ塩化ビニル樹脂のほかにアクリル系樹脂やポリエステ
ル系樹脂等を使用でき、バインダー樹脂の溶剤としては
上記したシクロヘキサノンのほかにメチルイソブチルケ
トン、セロソルブ、芳香族系溶剤等を使用でき、さらに
脱水剤としては上記したシリカゲルのほかにゼオライト
等も使用できる。
In the method of the present invention, as the solvent for the dispersant, in addition to the above-mentioned xylene, aromatic solvents such as toluene and solvents belonging to ketones such as methyl isobutyl ketone and methyl ethyl ketone can be used, and as the binder resin, the above-mentioned polyvinyl chloride can be used. In addition to resins, acrylic resins and polyester resins can be used, and as solvents for the binder resin, in addition to the above-mentioned cyclohexanone, methyl isobutyl ketone, cellosolve, aromatic solvents, etc. can be used, and as dehydrating agents, the above-mentioned solvents can be used. In addition to silica gel, zeolite etc. can also be used.

〔発明の効果〕〔Effect of the invention〕

本発明によると、長期間放置しても酸化錫超微粒子の凝
集や沈澱が起こりに<<、品質の安定した導電性塗布液
を製造できる。
According to the present invention, it is possible to produce a conductive coating liquid with stable quality, which does not cause agglomeration or precipitation of ultrafine tin oxide particles even if left for a long period of time.

ところで、本発明方法は、酸化錫微粒子を分散剤溶液に
混入する直前に予備乾燥することによってその表面に吸
着担持されていた水分の分散剤溶液中への混入を防止す
ると共に、分散剤及びバインダー樹脂の各溶剤に分散剤
やバインダー樹脂を溶解させる直前にそれらの溶剤を脱
水し、さらにバインダー樹脂を溶剤への溶解前に予備乾
燥することによって、分散剤溶液やバインダー樹脂溶液
への水分の混入を防止するものである。
By the way, in the method of the present invention, by pre-drying the tin oxide fine particles immediately before mixing them into the dispersant solution, it is possible to prevent the water adsorbed and supported on the surface of the particles from being mixed into the dispersant solution, and also to prevent the water adsorbed on the surface of the tin oxide particles from being mixed into the dispersant solution. By dehydrating the dispersant and binder resin immediately before dissolving them in each solvent of the resin, and pre-drying the binder resin before dissolving it in the solvent, it is possible to prevent water from entering the dispersant solution or binder resin solution. This is to prevent

このような本発明方法に対して、導電性塗布液を製造後
にその中へシリカゲルやゼオライト等の脱水剤を投入し
て該塗布液中の水分を取り除くことも考えられる。しか
し、この方法では、分散剤溶液に混入する前の酸化錫超
微粒子に吸着担持されていた水分を十分に取り除くこと
は難しく、本発明方法のように予備乾燥によってその水
分を取り除く場合に比べるとその効果に格段の差異があ
る。また、導電性塗布液に脱水剤を投入すると、該塗布
液中に溶解しているバインダー樹脂が脱水剤に付着して
該脱水剤の分離に困難をきたすほか、分離できたとして
も脱水剤の表面がバインダー樹脂による樹脂膜で覆われ
ているためにその再生が困難である。バインダー樹脂溶
液に脱水剤を投入することによって水分を取り除く場合
についても同様のことがいえる。従って、このような不
都合を生じることのない本発明方法は脱水剤の再生再使
用を可能にし、経済性に富む方法であるといえる。
Regarding such a method of the present invention, it is also conceivable to remove moisture from the conductive coating liquid by adding a dehydrating agent such as silica gel or zeolite into the conductive coating liquid after manufacturing the conductive coating liquid. However, with this method, it is difficult to sufficiently remove the moisture adsorbed and supported on the ultrafine tin oxide particles before they are mixed into the dispersant solution, and compared to the method of the present invention in which the moisture is removed by pre-drying. There is a marked difference in the effects. Furthermore, when a dehydrating agent is added to a conductive coating liquid, the binder resin dissolved in the coating liquid adheres to the dehydrating agent, making it difficult to separate the dehydrating agent, and even if it is separated, the dehydrating agent is Since the surface is covered with a resin film made of binder resin, it is difficult to regenerate it. The same can be said of the case where water is removed by adding a dehydrating agent to the binder resin solution. Therefore, the method of the present invention, which does not cause such inconvenience, enables the dehydrating agent to be recycled and reused, and can be said to be a highly economical method.

なお、本発明方法では、酸化錫超微粒子を予備乾燥する
こと、分散剤及びバインダー樹脂の各溶剤を使用前に脱
水すること及びバインダー樹脂を予備乾燥することにつ
いて触れているに過ぎないが、このことは分散剤を使用
前に脱水することを除外する趣旨ではない。即ち、分散
剤溶液はシリカゲル等の脱水剤を投入することによって
容易に脱水でき、脱水剤の再生再使用も容易であるが、
分散剤を使用前に脱水しておいてもよく、むしろこの操
作を行うことが導電性塗布液の酸化錫超微粒子の凝集や
沈澱を抑制する上で好ましい。
Note that the method of the present invention only mentions pre-drying the ultrafine tin oxide particles, dehydrating the dispersant and binder resin solvents before use, and pre-drying the binder resin. This is not to exclude dehydration of the dispersant before use. That is, the dispersant solution can be easily dehydrated by adding a dehydrating agent such as silica gel, and the dehydrating agent can be easily recycled and reused.
The dispersant may be dehydrated before use, and it is preferable to perform this operation in order to suppress agglomeration and precipitation of ultrafine tin oxide particles in the conductive coating liquid.

Claims (1)

【特許請求の範囲】[Claims] (1)分散剤溶液中に酸化錫超微粒子を混入することに
より作成した酸化錫分散液をバインダー樹脂溶液と混合
する導電性塗布液の製造方法において、酸化錫超微粒子
を分散剤溶液中に混入する直前に予備乾燥すると共に、
分散剤の溶剤及びバインダー樹脂の溶剤を、分散剤及び
バインダー樹脂を溶解させる直前に脱水し、さらにバイ
ンダー樹脂を溶剤に溶解させる直前に予備乾燥すること
を特徴とする導電性塗布液の製造方法。
(1) In a method for producing a conductive coating liquid in which a tin oxide dispersion prepared by mixing ultrafine tin oxide particles into a dispersant solution is mixed with a binder resin solution, ultrafine tin oxide particles are mixed into the dispersant solution. In addition to pre-drying immediately before
A method for producing a conductive coating liquid, which comprises dehydrating a dispersant solvent and a binder resin solvent immediately before dissolving the dispersant and binder resin, and pre-drying the binder resin immediately before dissolving the binder resin in the solvent.
JP60168407A 1985-07-29 1985-07-29 Method for producing conductive coating liquid Expired - Fee Related JPH06898B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60168407A JPH06898B2 (en) 1985-07-29 1985-07-29 Method for producing conductive coating liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60168407A JPH06898B2 (en) 1985-07-29 1985-07-29 Method for producing conductive coating liquid

Publications (2)

Publication Number Publication Date
JPS6227474A true JPS6227474A (en) 1987-02-05
JPH06898B2 JPH06898B2 (en) 1994-01-05

Family

ID=15867547

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60168407A Expired - Fee Related JPH06898B2 (en) 1985-07-29 1985-07-29 Method for producing conductive coating liquid

Country Status (1)

Country Link
JP (1) JPH06898B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62252481A (en) * 1986-04-24 1987-11-04 Catalysts & Chem Ind Co Ltd Electrically conductive paint
CN100389157C (en) * 2005-08-16 2008-05-21 上海天鑫环境科技有限公司 Novel electrically-conducting paint preparation method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59102932A (en) * 1982-12-02 1984-06-14 Mitsubishi Plastics Ind Ltd Coating of electrically-conductive transparent paint

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59102932A (en) * 1982-12-02 1984-06-14 Mitsubishi Plastics Ind Ltd Coating of electrically-conductive transparent paint

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62252481A (en) * 1986-04-24 1987-11-04 Catalysts & Chem Ind Co Ltd Electrically conductive paint
JPH0219150B2 (en) * 1986-04-24 1990-04-27 Catalysts & Chem Ind Co
CN100389157C (en) * 2005-08-16 2008-05-21 上海天鑫环境科技有限公司 Novel electrically-conducting paint preparation method

Also Published As

Publication number Publication date
JPH06898B2 (en) 1994-01-05

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