JPS6116126B2 - - Google Patents
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- Publication number
- JPS6116126B2 JPS6116126B2 JP5962180A JP5962180A JPS6116126B2 JP S6116126 B2 JPS6116126 B2 JP S6116126B2 JP 5962180 A JP5962180 A JP 5962180A JP 5962180 A JP5962180 A JP 5962180A JP S6116126 B2 JPS6116126 B2 JP S6116126B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- weight
- white
- metal oxide
- coating layer
- 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
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- 239000000843 powder Substances 0.000 claims description 34
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000011247 coating layer Substances 0.000 claims description 15
- 150000004706 metal oxides Chemical class 0.000 claims description 13
- 229910001361 White metal Inorganic materials 0.000 claims description 11
- 239000010969 white metal Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 5
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 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
- 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
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000010410 layer Substances 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- 229910006404 SnO 2 Inorganic materials 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 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
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 235000014692 zinc oxide Nutrition 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000007788 liquid 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
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
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紛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. be.
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紛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）紛末は、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に均一なも
のを安定的に製造することが難しく、さらによう
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よい、すなわち高抵
抗をもつものでよいことから、前記導電層は、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で構成されているが、こ
れら白色の電解質には、大気中および紙中の水分
を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 completely white color and is unstable in production. It is difficult to stably produce a homogeneous product, 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 electrically conductive thermal paper,
Since the conductive layer need only have low conductivity, that is, high resistance, the conductive layer is composed of an inorganic electrolyte such as ammonium sulfate or ammonium chloride, or an organic electrolyte. Since the electrolyte has the property of adsorbing moisture in the air and paper, this adsorbed moisture changes the resistance of the conductive layer, making it difficult to ensure stable conductivity. It had some points.
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紛末を、品質および毒
性上の問題なく、コスト安く製造すべく研究を行
なつた結果、白色金属酸化物紛末を加熱水中に分
散させたものからなる加熱懸濁液に、アセトンに
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、アセトンは加熱水と接触すること
によつて瞬時に蒸発し、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）が前記金属酸化物紛末の表面上
に均等に析出し、しかもこの結果得られた複合紛
末は、白色を呈すると共に、良好な導電性を有
し、かつ吸湿性がなく、品質的に安定したもので
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 research to produce a suitable powder at a low cost and without quality or toxicity problems, a heated suspension consisting of a white metal oxide powder dispersed in heated water was mixed with acetone. When a solution consisting of tin chloride (hereinafter referred to as SnCl4 ) and antimony chloride (hereinafter referred to as SbCl3 ) is added, acetone evaporates instantly by contacting the heated water, and at the same time hydrolysis occurs. As a result, tin oxide (hereinafter referred to as SnO 2 ) in which antimony (Sb) is uniformly dissolved is precipitated evenly on the surface of the metal oxide powder, and the resulting composite powder has a white color. They found that it has good conductivity, no hygroscopicity, and is stable in quality.
したがつて、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
積を有する白色金属酸化物紛末を加熱水中に分散
させたものからなる加熱懸濁液に、アセトンに78
〜783ｇ／のSnCl4と0.085〜212ｇ／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、前記白色金属酸化物紛末の表面を、Sb：0.1
〜20重量％を含有し、残りが実質的にSnO2から
なる組成を有し、かつ全体割合で５〜67重量％を
占める被覆層で被覆したものからなる白色金属酸
化物紛末を製造することに特徴を有するものであ
る。 Therefore, the present invention has been made based on the above findings, and provides a heated suspension comprising white metal oxide powder having a specific surface area of 1 to 10 m 2 /g dispersed in heated water. liquid, acetone 78
~783g/ SnCl4 and 0.085~212g/ SbCl3
By adding a solution consisting of dissolved Sb: 0.1, the surface of the white metal oxide powder was
~20% by weight, with the remainder essentially consisting of SnO2 , and coated with a coating layer having a total proportion of 5 to 67% by weight. It has particular characteristics.
つぎに、この発明の白色導電性複合紛末の製造
法において、白色金属酸化物紛末の比表面積、ア
セトン中のSnCl4およびSbCl3の含有量、さらに
被覆層のSb含有量および全体割合を上記の通り
に限定した理由を説明する。 Next, in the method for producing a white conductive composite powder of the present invention, the specific surface area of the white metal oxide powder, the content of SnCl 4 and SbCl 3 in acetone, and the Sb content and overall proportion of the coating layer are determined. The reason for the above limitations will be explained.
(a) 白色金属酸化物紛末の比表面積
１m2／ｇ未満の比表面積では、白色金属酸化物
紛末自体の粒度が粗くなつて、例えば複写用紙の
導電性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
えた細かくなりすぎると、白色金属酸化物紛末の
凝集力が強くなつて、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 white metal oxide powder When the specific surface area is less than 1 m 2 /g, the particle size of the white metal oxide powder itself becomes coarse, and when used for forming conductivity on copy paper, for example, the paper surface becomes rough. If the powder becomes too fine with a specific surface area of more than 10 m 2 /g, the cohesive force of the white metal oxide powder will become stronger and it will be difficult to disperse it uniformly in heated water. Therefore, the specific surface area is 1
~10m 2 /g.
(b) アセトン中の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、金属酸化物紛末の
表面上にSnO2が析出する速度が遅くなりすぎ、
所定の被覆層を形成するのに長時間を要するよう
になつて効率的でなく、一方783ｇ／を越えて
含有させると、白色金属酸化物紛末表面上への
SnO2の析出が不均一になつて望ましくないこと
から、その含有量を78〜783ｇ／と定めた。(b) Content of SnCl 4 in acetone If the content is less than 78 g/
The content of SnCl 4 is too low, the rate of precipitation of SnO 2 on the surface of metal oxide powder is too slow,
It takes a long time to form a predetermined coating layer, making it inefficient. On the other hand, if the content exceeds 783 g/powder, it will cause a layer to form on the surface of the white metal oxide powder.
Since the precipitation of SnO 2 becomes uneven, which is undesirable, the content was determined to be 78 to 783 g/.
(c) アセトン中のSbCl3の含有量
その含有量が0.085ｇ／未満では、被覆層を
構成するSnO2中に0.1重量％以上のSbを含有させ
ることはできず、一方212ｇ／を越えて含有さ
せると、被覆層中のSb含有量が20重量％を越え
て高くなることから、その含有量を0.085〜212
ｇ／と定めた。(c) Content of SbCl 3 in acetone If the content is less than 0.085 g/, it is impossible to contain more than 0.1% by weight of Sb in the SnO 2 constituting the coating layer, whereas if the content exceeds 212 g/ If Sb is included, the Sb content in the coating layer will exceed 20% by weight, so the content should be increased from 0.085 to 212% by weight.
g/.
(d) 被覆層のSb含有量
その含有量が0.1重量％未満では、所望の良好
な導電性を確保することができず、一方20重量％
を越えて含有させると、白色が失なわれて青味を
帯びるようになることから、その含有量を0.1〜
20重量％と定めた。(d) Sb content in the coating layer If the content is less than 0.1% by weight, the desired good conductivity cannot be secured;
If it is added in excess of
It was set at 20% by weight.
(e) 被覆層の全体割合
全体割合で５重量％未満の被覆層では、良好な
導電性を確保することができず、一方同67重量％
を越えて被覆させてめ、より一層の導電性向上効
果がないばかりか、剥離現象を起すようになるこ
とから、被覆層の全体割合を５〜67重量％と定め
た。(e) Total proportion of the coating layer If the total proportion of the coating layer is less than 5% by weight, good conductivity cannot be ensured;
If the coating layer exceeds 50% by weight, not only will there be no further improvement in conductivity, but also a peeling phenomenon will occur. Therefore, the total proportion of the coating layer was set at 5 to 67% by weight.
なお、この発明における白色金属酸化物紛末と
しては、白色性があり、かつ低価で、顔料性のす
ぐれたものであれば何でもよいが、特にチタニア
（TiO2）、シリカ（SiO2）、アルミナ（Al2O3）、亜
鉛白（ZnO）、ジルコニア（ZrO2）、マグネシア
（MgO）、および粘土などが望ましい。 The white metal oxide powder used in the present invention may be any powder as long as it is white, inexpensive, and has excellent pigment properties, but titania (TiO 2 ), silica (SiO 2 ), Desirable materials include alumina (Al 2 O 3 ), zinc white (ZnO), zirconia (ZrO 2 ), magnesia (MgO), and clay.
つぎに、この発明を実施例により説明する。 Next, the present invention will be explained by examples.
実施例 １
５m2／ｇの比表面積を有する白色SiO2紛末：
100ｇを水：1000c.c.に加え、温度：90℃に加熱保
持し、撹拌を加えて前記SiO2紛末が均一に分散
した加熱懸濁液とした状態を保持しながら、アセ
トン：300c.c.にSnCl4：86.5ｇ／とSbCl3：10.4
ｇ／を溶解したものからなる溶液を２時間かけ
てゆつくりと注入することによつて、前記SiO2
紛末表面上に、Sb含有SnO2からなる被覆層を析
出形成せしめ、ついで、これを別し、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時間保持の加熱処理を施すことによつ
て本発明複合紛末を製造した。Example 1 White SiO 2 powder with a specific surface area of 5 m 2 /g:
Add 100 g to 1000 c.c. of water, heat and maintain the temperature at 90°C, stir to form a heated suspension in which the SiO 2 powder is uniformly dispersed, and add 300 c.c. of acetone. c. SnCl 4 : 86.5g/and SbCl 3 : 10.4
The SiO 2
A coating layer made of Sb-containing SnO 2 is deposited on the powder surface, and then this is separated and washed.
In air and temperature to further improve crystallinity:
The composite powder of the present invention was produced by heat treatment at 500°C for 2 hours.
この結果得られた本発明複合紛末は、全体割合
で67重量％のSiO2紛末の表面が、Sb：10重量％
を含有し、残りが綬質的にSnO2からなる同33重
量％の被覆層で被覆されたものからなり、かつ白
色を呈すると共に、比抵抗：420Ω・cmを有する
導電性の良好なものであつた。 In the composite powder of the present invention obtained as a result, the surface of the SiO 2 powder with a total proportion of 67% by weight is Sb: 10% by weight.
, and the rest is coated with a 33% by weight coating layer consisting of SnO2 , and is white in color and has good conductivity with a specific resistance of 420 Ω cm. It was hot.
実施例 ２
３m2／ｇの比表面積を有するTiO2紛末：100ｇ
を水：1000c.c.に加え、温度：90℃に加熱保持し、
かつ撹拌を加えて前記TiO2紛末が均一に分散し
た加熱懸濁液とした状態を保持しながら、アセト
ン：500c.c.にSnCl4：173ｇ／とSbCl3：9.81ｇ／
を溶解したものからなる溶液を３時間かけてゆ
つくりと加えて、前記TiO2紛末の表面上に、Sb
含有SnO2からなる被覆層を析出形成せしめ、引
続いて実施例１におけると同一の条件にて処理す
ることによつて本発明複合紛末を製造した。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℃,
While stirring to maintain a heated suspension in which the TiO 2 powder was uniformly dispersed, SnCl 4 : 173 g/ and SbCl 3 : 9.81 g/ were added to acetone: 500 c.c.
A solution consisting of dissolved Sb was slowly added over a period of 3 hours, and Sb
A composite powder of the present invention was produced by depositing a coating layer containing SnO 2 and subsequently treating it under the same conditions as in Example 1.
この結果得られた本発明複合紛末は、実質的に
坦体たるTiO2紛末：50重量％と、Sb：５重量
％、SnO2：残りからなる組成を有する被覆層：
50重量％とから構成された白色を呈するものであ
り、しかも比抵抗：140Ω・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 a coating layer having a composition consisting essentially of TiO 2 powder as a carrier: 50% by weight, Sb: 5% by weight, and SnO 2 : the remainder.
It was white in color and had good electrical conductivity with a specific resistance of 140 Ω·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紛末は、良好
な導電性ときわめて鮮明な白色を有するので、複
写用紙の導電層形成用材料として、また帯電防止
用プラスチツク材やゴム材などの充填材などとし
て使用した場合にきわめてすぐれた特性を発揮す
るのである。 As mentioned above, according to the present invention, the non-toxic and non-hygroscopic composite powder of stable quality has good conductivity and a very clear white color, so it can be used as a material for forming a conductive layer of copy paper. It also exhibits excellent properties when used as a filler for antistatic plastic materials and rubber materials.
Claims (1)
化物紛末を加熱水中に分散させたものからなる加
熱懸濁液に、アセトン78〜783ｇ／の塩化錫と
0.085〜212ｇ／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、前記白色
金属酸化物紛末の表面に、アンチモン：0.1〜20
重量％を含有し、残りが実質的に酸化錫からなる
被覆層を全体割合で５〜67重量％の量、析出形成
せしめることを特徴とする白色導電性複合紛末の
製造法。1 A heated suspension consisting of a white metal 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 acetone and tin chloride.
By adding a solution consisting of 0.085 to 212 g of antimony chloride dissolved therein, 0.1 to 20 g of antimony is added to the surface of the white metal oxide powder.
% by weight, with the remainder substantially consisting of tin oxide, by precipitating a coating layer in a total amount of 5 to 67% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5962180A JPS56156604A (en) | 1980-05-06 | 1980-05-06 | Method of producing white color conductive composite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5962180A JPS56156604A (en) | 1980-05-06 | 1980-05-06 | Method of producing white color conductive composite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS56156604A JPS56156604A (en) | 1981-12-03 |
| JPS6116126B2 true JPS6116126B2 (en) | 1986-04-28 |
Family
ID=13118489
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5962180A Granted JPS56156604A (en) | 1980-05-06 | 1980-05-06 | Method of producing white color conductive composite powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS56156604A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0351424B2 (en) * | 1989-05-26 | 1991-08-06 | Haruchika Seimitsu Kk | |
| JPH0611282B2 (en) * | 1989-08-17 | 1994-02-16 | 株式会社赤土製作所 | Sick bed |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5552371B2 (en) * | 2010-05-31 | 2014-07-16 | 三菱マテリアル株式会社 | White conductive powder and method for producing the same |
-
1980
- 1980-05-06 JP JP5962180A patent/JPS56156604A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0351424B2 (en) * | 1989-05-26 | 1991-08-06 | Haruchika Seimitsu Kk | |
| JPH0611282B2 (en) * | 1989-08-17 | 1994-02-16 | 株式会社赤土製作所 | Sick bed |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS56156604A (en) | 1981-12-03 |
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