JPS6139685B2 - - Google Patents
Info
- Publication number
- JPS6139685B2 JPS6139685B2 JP1621680A JP1621680A JPS6139685B2 JP S6139685 B2 JPS6139685 B2 JP S6139685B2 JP 1621680 A JP1621680 A JP 1621680A JP 1621680 A JP1621680 A JP 1621680A JP S6139685 B2 JPS6139685 B2 JP S6139685B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- tio
- content
- coating layer
- ethanol
- 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
Links
- 239000000843 powder Substances 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000011247 coating layer Substances 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 4
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 18
- 229910006404 SnO 2 Inorganic materials 0.000 description 11
- 239000010410 layer Substances 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 2
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Conductive Materials (AREA)
- Photoreceptors In Electrophotography (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【発明の詳細な説明】
この発明は、良好な導電性を有し、特に通電感
熱紙や静電記録紙などの複写用紙の導電層形成に
使用される白色複合粉末の製造法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a white composite powder that has good electrical conductivity and is particularly used for forming a conductive layer on copy paper such as electrically conductive thermal paper and electrostatic recording paper. .
一般に、通電感熱紙や静電記録紙などの複写用
紙における導電層の形成には、白色の色調を有
し、かつ導電性の良好な粉末が必要とされてい
る。しかしながら、現在通電感熱紙の導電層に使
用されているヨウ化銅（Cul）粉末は、良好な導
電性をもつものの完全な白色を呈するものではな
く、その上に製造が不安定であるため均一なもの
を安定的に製造することが難しく、さらにヨウ素
のもつ毒性の点でも問題があるものである。一方
静電記録紙の場合には、通電感熱紙に比して、そ
の導電層は導電性が低くてもよい、すなわち高抵
抗をもつものでよいことから、例えば硫酸アンモ
ンや塩化アンモンなどの無機電解質、あるいは有
機電解質が使用されているが、これら白色の電解
質には、大気中および紙中の水分が吸着する性質
があるため、この吸着水分によつて導電層の抵抗
が変化してしまい、安定的導電性を確保すること
が困難であるという問題点があるものであつた。 Generally, to form a conductive layer on copy paper such as electrically conductive thermal paper or electrostatic recording paper, a powder having a white tone and good conductivity is required. However, although the copper iodide (Cul) powder currently used in the conductive layer of current-carrying thermal paper has good conductivity, it does not exhibit a perfect white color, and is unstable in production, so it cannot be uniformly produced. It is difficult to stably produce iodine, and there is also a problem in terms of the toxicity of iodine. On the other hand, in the case of electrostatic recording paper, compared to current-carrying thermal paper, its conductive layer may have low conductivity, that is, it may have high resistance. Electrolytes or organic electrolytes are used, but these white electrolytes have the property of adsorbing moisture in the air and paper, so this adsorbed moisture changes the resistance of the conductive layer. The problem was that it was difficult to ensure stable conductivity.
本発明者等は、上述のような観点から、白色を
呈し、かつ良好な導電性を安定的に有する、特に
通電感熱紙や静電記録紙などの複写用紙の導電層
形成に使用するのに適した粉末を、品質および毒
性上の問題なく、低コストで製造すべく研究を行
なつた結果、酸化チタン（以下TiO2で示す）粉
末を加熱水に分散させたものからなる加熱懸濁液
に、エタノールに塩化錫（以下SnCl4で示す）と
塩化アンチモン（以下SbCl3で示す）を溶解した
ものからなる溶液を加えると、エタノールノは加
熱水と接触することで瞬時に蒸発すると同時に加
水分解が起つて、アンチモン（Sb）が均一に固
溶した酸化錫（以下SnO2で示す）が前記TiO2粉
末の表面に析出し、しかも前記加水分解による
Sb含有SnO2のTiO2粉末表面への析出は前記TiO2
のもつ活性によつて著しく促進されるものである
ため、前記Sb含有SnO2は均一な層厚に析出する
ものであり、さらにこの結果得られた複合粉末
は、白色を呈すると共に、良好な導電性を有し、
しかも吸湿性がなく、品質的に安定したたもので
あるという知見を得たのである。 From the above-mentioned viewpoints, the present inventors have developed a paper that exhibits white color and stably has good conductivity, and that is particularly suitable for use in forming a conductive layer on copying paper such as current-carrying thermal paper and electrostatic recording paper. As a result of our research to produce a suitable powder at low cost without quality or toxicity problems, we have developed a heated suspension consisting of titanium oxide (hereinafter referred to as TiO 2 ) powder dispersed in heated water. When a solution consisting of tin chloride (hereinafter referred to as SnCl 4 ) and antimony chloride (hereinafter referred to as SbCl 3 ) dissolved in ethanol is added to ethanol, the ethanol instantly evaporates upon contact with heated water and simultaneously adds water. As decomposition occurs, tin oxide (hereinafter referred to as SnO 2 ) in which antimony (Sb) is uniformly dissolved is precipitated on the surface of the TiO 2 powder, and furthermore, due to the hydrolysis
The precipitation of Sb-containing SnO 2 on the TiO 2 powder surface is caused by the precipitation of Sb-containing SnO 2 on the TiO 2 powder surface.
The Sb-containing SnO 2 precipitates in a uniform layer thickness, and the resulting composite powder exhibits a white color and good conductivity. have sex,
Moreover, they found that it is not hygroscopic and has stable quality.
この発明は、上記知見にもとづいてなされたも
のであつて、１〜10m2／ｇの比表面積を有する
TiO2粉末を加熱水中に分散させたものからなる
加熱懸濁液に、エタノールに78〜783ｇ／の
SnCl4と0.085〜8.59ｇ／のSbCl3を溶解したも
のからなる溶液を加えることによつて、前記
TiO2粉末の表面を、Sb：0.1〜１重量％未満を含
有し、残りが実質的にSnO2からなる全体割合で
５〜67重量％の被覆層で被覆してなる白色導電性
複合粉末を製造することに特徴を有するものであ
る。 This invention was made based on the above findings, and has a specific surface area of 1 to 10 m 2 /g.
A heated suspension consisting of TiO 2 powder dispersed in heated water was added with 78 to 783 g/g of TiO2 powder in ethanol.
By adding a solution consisting of SnCl 4 and 0.085 to 8.59 g/SbCl 3 dissolved in the
A white conductive composite powder is formed by coating the surface of TiO 2 powder with a coating layer containing 0.1 to less than 1% by weight of Sb, and the remainder substantially consisting of SnO 2 with a total proportion of 5 to 67% by weight. It is characterized by its manufacturing.
つぎに、この発明の白色導電性複合粉末および
その製造法に関し、上記の通り数値限定した理由
を説明する。 Next, regarding the white conductive composite powder of the present invention and its manufacturing method, the reason for limiting the numerical values as described above will be explained.
(a) TiO2粉末の比表面積
１m2／ｇ末満の比表面積では、TiO2粉末自体
の粘度が粗くなつて、例えば複写用紙の導電層形
成に使用した場合、紙面の平滑さが失なわれるよ
うになり、一方比表面積が10m2／ｇを越えて細か
くなりすぎると、TiO2粉末の凝集力が強くな
り、加熱水中に均一に分散させることが困難にな
ることから、その比表面積を１〜10m2／ｇと定め
た。(a) Specific surface area of TiO 2 powder When the specific surface area is less than 1 m 2 /g, the viscosity of the TiO 2 powder itself becomes rough, and when used, for example, to form a conductive layer on copy paper, the paper surface may lose its smoothness. On the other hand, if the specific surface area exceeds 10 m 2 /g and becomes too fine, the cohesive force of the TiO 2 powder becomes strong and it becomes difficult to disperse it uniformly in heated water. It was determined to be 1 to 10 m 2 /g.
(b) 被覆層のSb含有量
その含有量が0.1％末満では、被覆層との関係
において所望の良好な導電性を確保することがで
きず、一方、１％以上の含有は、特にきびしい白
色度を要求される場合望ましくないことから、そ
の含有量を0.1〜１％未満と定めた。(b) Sb content in the coating layer If the Sb content is less than 0.1%, the desired good conductivity cannot be secured in relation to the coating layer, while if the content is 1% or more, the Sb content is particularly severe. Since it is undesirable when whiteness is required, its content is set at 0.1 to less than 1%.
(c) 被覆層の全体割合
その全体割合が５％未満では、Sb含有量との
関係において所望の良好な導電性を確保すること
ができず、一方67％を越えて被覆しても導電性に
より一段の改善がみられず、むしろ剥離現象が発
生するようになることから、その全体割合を５〜
67％と定めた。(c) Total ratio of the coating layer If the total ratio is less than 5%, it is not possible to secure the desired good conductivity in relation to the Sb content, while on the other hand, even if the coating layer exceeds 67%, the conductivity will not be maintained. However, since no further improvement was observed, and rather a peeling phenomenon started to occur, the overall ratio was reduced to 5 to 5.
It was set at 67%.
(d) エタノール中のSnCl4の含有量
その含有量が78ｇ／未満では、実質的に
SnCl4の含有量が少なすぎて、TiO2粉末表面上へ
のSnO2の析出速度が遅くなり、長時間の処理時
間を必要とするようになつて効率的でなく、一方
783ｇ／を越えて含有させると、TiO2粉末表面
上へのSnO2の析出が不均一になり、均一な層厚
の被覆層を形成することができなくなることか
ら、その含有量を78〜783ｇ／と定めた。(d) Content of SnCl4 in ethanol If the content is less than 78g/
If the content of SnCl 4 is too low, the precipitation rate of SnO 2 on the TiO 2 powder surface will be slow, requiring a long processing time, which is not efficient;
If the content exceeds 783g, the precipitation of SnO2 on the surface of the TiO2 powder will become uneven, making it impossible to form a coating layer with a uniform thickness. / determined.
(e) エタノール中のSbCl3の含有量
SnCl4含有量との相対関係において、その有量
が0.085ｇ／未満では、被覆層のSb含有が0.1％
未満となり、一方8.59ｇ／を越えて含有させる
と、被覆層のSb含有量が１％以上になることか
ら、その含有量を0.085〜8.59ｇ／と定めた。(e) Content of SbCl 3 in ethanol In relation to the content of SnCl 4 , if the amount is less than 0.085g/, the Sb content of the coating layer is 0.1%.
On the other hand, if the content exceeds 8.59 g/, the Sb content of the coating layer becomes 1% or more, so the content was determined to be 0.085 to 8.59 g/.
ついで、この発明を実施例により具体的に説明
する。 Next, the present invention will be specifically explained with reference to Examples.
実施例 １
５m2／ｇの比表面積を有するTiO2粉末：100ｇ
を水：1000c.c.に加え、温度：90℃に加熱保持し、
撹拌を加えることによつて、前記TiO2粉末が均
一に分散した加熱懸濁液を調製し、この加熱懸濁
液に、エタノール：350c.c.にSnCl4：86.5ｇ，
SbCl3：0.852ｇを溶解したものからなる溶液を２
時間かけてゆつくり注入して、前記TiO2粉末表
面上にSb含有のSnO2からなる被覆層を析出形成
せしめ、引続いてろ別し、洗浄し、さらに結晶性
を向上させるために空気中、温度500℃に２時間
保持することによつて本発明複合粉末を製造し
た。Example 1 TiO 2 powder with a specific surface area of 5 m 2 /g: 100 g
Add to water: 1000c.c., heat and maintain at temperature: 90℃,
By adding stirring, a heated suspension in which the TiO 2 powder was uniformly dispersed was prepared, and to this heated suspension, ethanol: 350 c.c., SnCl 4 : 86.5 g,
A solution consisting of 0.852g of SbCl 3 dissolved in 2
By slowly injecting the TiO 2 powder over a period of time, a coating layer of Sb-containing SnO 2 is precipitated on the surface of the TiO 2 powder, followed by filtering, washing, and further injecting in air to improve crystallinity. The composite powder of the present invention was produced by maintaining the temperature at 500°C for 2 hours.
この結果得られた本発明複合粉末は、Sb：0.9
重量％を含有し、残りが実質的にSnO2からな
り、かつ全体割合で33％を占める白色の被覆層を
有し、しかも比抵抗：530Ω・cmを有する導電性
の良好なものであつた。 The composite powder of the present invention obtained as a result has Sb: 0.9
% by weight, with the remainder essentially consisting of SnO 2 , and had a white coating layer accounting for 33% of the total percentage, and had good conductivity with a specific resistance of 530 Ω cm. .
実施例 ２
３m2／ｇの比表面積を有するTiO2粉末：100ｇ
を水：1000c.c.に加え、温度：90℃に加熱保持し、
撹拌を加えることによつて、前記TiO2粉末が均
一に分散した加熱懸濁液を調製し、この加熱懸濁
液に、エタノール：120c.c.に、SnCl4：34.6ｇ，
SbCl3：0.189ｇを溶解したものからなる溶液を
1.5時間かけてゆつくり滴下し、以後実施例１に
おけると同一の操作および条件により本発明複合
粉末を製造した。Example 2 TiO 2 powder with a specific surface area of 3 m 2 /g: 100 g
Add to water: 1000c.c., heat and maintain at temperature: 90℃,
By adding stirring, a heated suspension in which the TiO 2 powder was uniformly dispersed was prepared, and to this heated suspension, ethanol: 120 c.c., SnCl 4 : 34.6 g,
SbCl 3 : A solution consisting of 0.189g dissolved
The mixture was slowly added dropwise over 1.5 hours, and the composite powder of the present invention was produced using the same operations and conditions as in Example 1.
この結果得られた本発明複合粉末は、Sb：0.5
重量％を含有し、残りが実質的にSnO2からな
り、かつ全体割合で17％を占める白色の被覆層を
有し、しかも比抵抗：：2.5KΩ．cmを有する導
電性の良好なものであつた。 The composite powder of the present invention obtained as a result has Sb: 0.5
% by weight, the remainder essentially consisting of SnO 2 , and has a white coating layer that accounts for 17% of the total proportion, and has a specific resistance of: 2.5KΩ. It had good conductivity with cm.
実施例 ３
３m2／ｇの比表面積を有するTiO2粉末：100ｇ
を水：1000c.c.に加え、温度：90℃に加熱保持し、
撹拌を加えることによつて加熱懸濁液を調製し
た。ついで別途用意した、SbCl3：0.188ｇ，
0.943ｇ，および1.70ｇのそれぞれをSnCl4：173
ｇと共にエタノール：600c.c.に溶解したものから
なる３種の溶液を、前記加熱懸濁液に別個に３時
間かけてゆつくり注入することによつてエタノー
ルの蒸発と加水分解反応を行なわしめて、前記
TiO2粉末表面上にSb含有SnO2からなる被覆層を
析出形成せしめ、以後実施例１におけると同一の
条件および操作にて本発明複合粉末を製造した。Example 3 TiO 2 powder with a specific surface area of 3 m 2 /g: 100 g
Add to water: 1000c.c., heat and maintain at temperature: 90℃,
A heated suspension was prepared by adding stirring. Next, separately prepared SbCl 3 : 0.188g,
0.943g and 1.70g each of SnCl4 :173
Ethanol: Evaporation and hydrolysis reaction were carried out by slowly injecting three kinds of solutions consisting of g and 600 c.c. of ethanol into the heated suspension separately over a period of 3 hours. , said
A coating layer made of Sb-containing SnO 2 was deposited on the surface of the TiO 2 powder, and the composite powder of the present invention was produced under the same conditions and operations as in Example 1.
この結果得られた本発明複合粉末は、それぞれ
Sb：0.1重量％，0.5重量％，および0.9重量％を
含有し、実質的に残りがSnO2からなり、しかも
いずれも全体割合で50％を占める白色の被覆層を
有し、比抵抗もそれぞれ500Ω・cm，350Ω・cm，
および150Ω・cmを有する導電性の良好なもので
あつた。 The resulting composite powders of the present invention are each
Contains Sb: 0.1% by weight, 0.5% by weight, and 0.9% by weight, with the remainder essentially consisting of SnO 2 , and each has a white coating layer that accounts for 50% of the total percentage, and each has a specific resistance. 500Ω・cm, 350Ω・cm,
It had good electrical conductivity and had a resistance of 150Ω·cm.
上述のように、この発明によれば、毒性および
吸湿性のない、安定した品質の複合粉末を簡単な
操作でコスト安く製造することができ、しかもこ
の結果得られた複合粉末は良好な導電性と所望の
白色を有することから、特に複写用紙の導電層形
成に使用するのに適し、また帯電防止用プラスチ
ツク材やゴム材などの充填材として使用すること
もできるのである。 As described above, according to the present invention, a non-toxic and non-hygroscopic composite powder of stable quality can be produced with simple operations at a low cost, and the resulting composite powder has good conductivity. Because it has a desired white color, it is particularly suitable for use in forming a conductive layer on copy paper, and can also be used as a filler for antistatic plastic materials, rubber materials, and the like.
Claims (1)
粉末を加熱水中に分散させたものからなる加熱懸
濁液に、エタノールに78〜783ｇ／の塩化錫と
0.085〜8.59ｇ／の塩化アンチモンを溶解した
ものからなる溶液を加えることによつて、前記酸
化チタン粉末の表面に、アンチモン：0.1〜１重
量％末満を含有し、残りが実質的に酸化錫からな
る被覆層を析出形成せしめることを特徴とする白
色導電性複合粉末の製造法。1 A heated suspension consisting of titanium oxide powder having a specific surface area of 1 to 10 m 2 /g dispersed in heated water was mixed with 78 to 783 g of tin chloride in ethanol.
By adding a solution consisting of 0.085 to 8.59 g of antimony chloride dissolved therein, the surface of the titanium oxide powder contains 0.1 to 1% by weight of antimony, and the remainder is substantially tin oxide. 1. A method for producing a white conductive composite powder, which comprises depositing a coating layer consisting of:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1621680A JPS56114215A (en) | 1980-02-13 | 1980-02-13 | White conductive composite powder and method of manufacturing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1621680A JPS56114215A (en) | 1980-02-13 | 1980-02-13 | White conductive composite powder and method of manufacturing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS56114215A JPS56114215A (en) | 1981-09-08 |
| JPS6139685B2 true JPS6139685B2 (en) | 1986-09-05 |
Family
ID=11910322
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1621680A Granted JPS56114215A (en) | 1980-02-13 | 1980-02-13 | White conductive composite powder and method of manufacturing same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS56114215A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0791398B2 (en) * | 1987-04-23 | 1995-10-04 | 三菱化学株式会社 | Conductive stretched polyolefin film |
-
1980
- 1980-02-13 JP JP1621680A patent/JPS56114215A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS56114215A (en) | 1981-09-08 |
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