JPS6211860A - Preparation of electrophotographic zinc oxide particles - Google Patents

Preparation of electrophotographic zinc oxide particles

Info

Publication number
JPS6211860A
JPS6211860A JP15165385A JP15165385A JPS6211860A JP S6211860 A JPS6211860 A JP S6211860A JP 15165385 A JP15165385 A JP 15165385A JP 15165385 A JP15165385 A JP 15165385A JP S6211860 A JPS6211860 A JP S6211860A
Authority
JP
Japan
Prior art keywords
zinc oxide
particles
oxide particles
oxide powder
powder
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.)
Pending
Application number
JP15165385A
Other languages
Japanese (ja)
Inventor
Kenichi Yasuda
謙一 安田
Tatsuo Yazaki
矢崎 達雄
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.)
HAKUSUI KAGAKU KOGYO KK
Original Assignee
HAKUSUI KAGAKU KOGYO KK
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 HAKUSUI KAGAKU KOGYO KK filed Critical HAKUSUI KAGAKU KOGYO KK
Priority to JP15165385A priority Critical patent/JPS6211860A/en
Publication of JPS6211860A publication Critical patent/JPS6211860A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02Charge-receiving layers
    • G03G5/04Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G03G5/087Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and being incorporated in an organic bonding material
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02Charge-receiving layers
    • G03G5/04Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G03G5/082Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and not being incorporated in a bonding material, e.g. vacuum deposited

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

PURPOSE:To prevent agglomeration of zinc oxide particles in an insulating resin solution by pulverizing their compressed blocks obtained by compressing the zinc oxide powder with a pressure of 20-150kg/cm<2>, and burning the obtained particles of <=2.0mm diameter at a temperature of 200-600 deg.C. CONSTITUTION:The zinc oxide powder is compressed with a pressure of 20-150kg/cm<2>, pulverizing the compressed product to <=2.0mm particle diameter, and burning the obtained particles at a temperature of 200-600 deg.C to obtain the intended electrophotographic zinc powder. To compress the zinc oxide powder, an optional compressor, such as a hydraulic press used for molding mozaic tiles, can be used, and the compressed blocks may be pulverized by an optional method, and the intended particles can be obtained by passing the pulverized product through a sieving step. To burn the compressed blocks, a rotary kiln can be used, and particle density is, generally, 0.6-1.5g/cm<3>, and preferably, 0.7-1.2g/cm<3>.

Description

【発明の詳細な説明】 本発明は電子写真用感光体に用いる改良された酸化亜鉛
粒子の製造法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improved method for producing zinc oxide particles for use in electrophotographic photoreceptors.

従来より電子写真に用いられる酸化亜鉛感光体は、導電
処理を施した紙、プラスチックフィルム等の支持体上に
、酸化亜鉛粉末および絶縁性樹脂を主成分とする厚さ約
1OJLの光導電層を塗布す・  ることによって作ら
れている。
Zinc oxide photoreceptors conventionally used in electrophotography consist of a photoconductive layer with a thickness of about 1 OJL mainly composed of zinc oxide powder and an insulating resin on a support such as paper or plastic film that has been subjected to conductive treatment. It is made by applying.

上記光導電層を形成するため従来から使用されている酸
化亜鉛粉末はIIi、以下、より一般的には0.2〜0
.5川の粒径の粉末であり、絶縁性樹脂としてはシリコ
ーン樹脂、アクリル樹脂、アルキッド樹脂等が使用され
ている。
The zinc oxide powder conventionally used to form the photoconductive layer is IIi, hereinafter more generally 0.2 to 0.
.. It is a powder with a particle size of 5 mm, and silicone resin, acrylic resin, alkyd resin, etc. are used as the insulating resin.

光導電層を形成するに当たっては絶縁性樹脂の有機溶剤
溶液に、重量比で酸化亜鉛粉末対絶縁性樹脂の割合が約
4〜7:lとなるように酸化亜鉛粉末を分散させ、この
分散液を支持体に塗布することによって製造している。
To form the photoconductive layer, zinc oxide powder is dispersed in an organic solvent solution of an insulating resin so that the weight ratio of zinc oxide powder to insulating resin is approximately 4 to 7:l, and this dispersion is It is manufactured by coating a support with:

酸化亜鉛感光体をオフセット印刷用または転写原板に使
用して印刷する場合、印刷枚数として少なくとも300
0枚、好ましくは5000枚以上の印刷ができる耐性を
有することが要求されているが、上述した如き従来の光
導電層を塗布した酸化亜鉛感光体は、光導電層の表面硬
度が充分でないため摩耗し易く、印刷時の地の汚れや、
画像不鮮明を生する原因となっている。その原因は種々
考えられるが、その一つば、酸化亜鉛感光体−1−に潜
像または顕像を形成した光導電層の結合剤たる絶縁性樹
脂が印刷または転写を繰返すうちに摩耗されて、離脱ま
たは剥離を起こし、更には醇化亜鉛粉末自体も脱落して
画像を不鮮明にしたり、あるいは醇化亜鉛が露出し、こ
こに現像液もしくはトナーが付着し、印刷された画面を
汚したりするためである。
When printing using a zinc oxide photoreceptor for offset printing or as a transfer plate, the number of printed sheets is at least 300.
However, the conventional zinc oxide photoreceptor coated with a photoconductive layer as described above does not have sufficient surface hardness. Easy to wear, dirt on the background during printing,
This causes the image to become unclear. There are various possible causes for this, but one of them is that the insulating resin, which is the binder of the photoconductive layer that formed the latent or developed image on the zinc oxide photoreceptor-1, is worn out during repeated printing or transfer. This is because the zinc chloride powder may detach or peel off, and the zinc chloride powder itself may fall off, making the image unclear, or the zinc chloride may be exposed, and the developer or toner may adhere to it, staining the printed screen. .

このため光導電層の表面硬度を向上させる一つの手段と
して、絶縁性樹脂として硬質樹脂例えばポリエステル樹
脂を使用する方法も考えられるが、この方法を採用する
と光導電層の光感度の低下を生じたり、あるいは光導電
層の可撓性が劣るようになり、光導電層に亀裂を生じ易
く、斑を生ずるので好ましくない。
For this reason, one possible method for improving the surface hardness of the photoconductive layer is to use a hard resin, such as polyester resin, as the insulating resin, but this method may result in a decrease in the photosensitivity of the photoconductive layer. Otherwise, the flexibility of the photoconductive layer becomes poor, and the photoconductive layer is likely to crack and cause unevenness, which is undesirable.

従来の光導電層を作るための酸化亜鉛粉末−絶縁性樹脂
分散液を作るに当たって、酸化亜鉛粉末を絶縁性樹脂溶
液に分散させると、酸化亜鉛粉末は単一粉末粒子として
挙動せず、凝集して凝集体を形成し、この凝集体は分散
液を支持体に塗布・乾燥した場合にもそのままの形で存
在する。この凝集体は凝集力が比較的弱くしかもその中
に微細な空洞を有しているため、感光体を印刷に使用し
たとき、絶縁樹脂の摩耗と共に酸化亜鉛圧縮体も摩擦力
により破壊されて脱落または陥没し、上述した欠点を生
ずる。
When making a conventional zinc oxide powder-insulating resin dispersion for making a photoconductive layer, when zinc oxide powder is dispersed in an insulating resin solution, the zinc oxide powder does not behave as a single powder particle but aggregates. The dispersion liquid forms aggregates, and these aggregates remain as they are even when the dispersion is applied to a support and dried. This aggregate has a relatively weak cohesive force and has minute cavities within it, so when the photoreceptor is used for printing, the zinc oxide compressed body is destroyed by frictional force and falls off when the insulating resin is worn. Or it may cave in, causing the above-mentioned drawbacks.

本発明は−I−述した欠点に鑑みてなされたものであり
、その目的は、従来の酸化亜鉛粉末および絶縁性樹脂を
用いた光導電層を有する感光体の欠点を解消し、表面硬
度のすぐれた感光体を提供することのできる酸化亜鉛粒
子の製造法を提供することにある。
The present invention has been made in view of the drawbacks mentioned above, and its purpose is to eliminate the drawbacks of the conventional photoreceptor having a photoconductive layer using zinc oxide powder and an insulating resin, and to reduce the surface hardness. An object of the present invention is to provide a method for producing zinc oxide particles that can provide an excellent photoreceptor.

本発明は酸化亜鉛粉末を20〜150 Kg/ cm2
の圧力で圧縮し、圧縮体を破砕することにより得られる
粒径2.0)以下の粒子を200〜600 ’0で焼成
することからなる電子写真用酸化亜鉛粒子の製造法にあ
る。
The present invention uses zinc oxide powder at a rate of 20 to 150 Kg/cm2.
The present invention provides a method for producing zinc oxide particles for electrophotography, which comprises firing particles having a particle size of 2.0 or less obtained by compressing the compressed body at a pressure of 2.0 to 600.

本発明で使用する酸化亜鉛粉末としては、従来より電子
写真用光導電層の形成に使用されている耐化拒鉛粉末を
使用することができる。
As the zinc oxide powder used in the present invention, a hardened lead-resistant powder that has been conventionally used for forming photoconductive layers for electrophotography can be used.

酸化亜鉛粉末を圧縮して圧縮体を作るには任意の圧縮機
例えばモザイクタイル素地成型用油圧プレスを使用でき
る。酸化亜鉛粉末を圧縮するに当たっては20 Kg/
 cm2−150 Kg/ cm2 、好ましくは40
Kg/Cm2〜100Kg/Cm2の圧力を採用するの
がよく、20 Kg/ cm2 より小さい圧力では、
続いて圧縮体を破砕して得られる粒子の結合力が充分で
なく、焼成工程で粒子が更に破砕されることがあり、ま
たこれを用いて形成される光導電層の表面硬度が充分で
なくなり好ましくない。
Any compressor, such as a hydraulic press for forming mosaic tile substrates, can be used to compress the zinc oxide powder to form a compressed body. When compressing zinc oxide powder, 20 kg/
cm2-150 Kg/cm2, preferably 40
It is better to adopt a pressure between Kg/Cm2 and 100Kg/Cm2, and at a pressure lower than 20 Kg/cm2,
Subsequently, the bonding force of the particles obtained by crushing the compressed body is not sufficient, and the particles may be further crushed in the baking process, and the surface hardness of the photoconductive layer formed using the particles may not be sufficient. Undesirable.

また圧力が150 Kg/ cm2 を超えると、光導
電層の光感度を低下させることがあり好ましくない。
Moreover, if the pressure exceeds 150 Kg/cm2, the photosensitivity of the photoconductive layer may be lowered, which is not preferable.

またあまり大きすぎると圧縮体の破砕に手間がかかり、
また圧縮機の性能からも不必要に大にするのは実用的で
ない。
Also, if it is too large, it will take a lot of effort to crush the compressed body.
In addition, it is not practical to make the compressor unnecessarily large in terms of its performance.

本発明によれば−L述した如く圧縮して得られた酸化亜
鉛圧縮体を破砕する。破砕に当たっては圧縮体を任意の
方法で破砕した後部工程を通すことによって達成でき、
篩手段としては回転ふるい、一平面ふるい等が用いられ
るが、より好ましいのは振動ふるいである。別法として
、酸化亜鉛粉末を上記圧力を付与しうるよう調整した二
本ロールの二、プに導入して圧縮するこよにより、酸化
亜鉛粒子の圧縮と破砕を同時に行なうこともできる。
According to the present invention, the zinc oxide compressed body obtained by compression as described above is crushed. Crushing can be achieved by passing the compressed body through a rear process of crushing it by any method,
As the sieving means, a rotating sieve, a single plane sieve, etc. can be used, but a vibrating sieve is more preferable. Alternatively, the zinc oxide particles can be compressed and crushed at the same time by introducing the zinc oxide powder into two rolls of two rolls adjusted to apply the above-mentioned pressure and compressing the powder.

破砕して得られた酸化亜鉛粒子は要すれば篩分けして粗
粒物を除去し、粒径2.0mm以下好ましくは0.3 
mm 〜1.0 mmの粒子とする。
If necessary, the zinc oxide particles obtained by crushing are sieved to remove coarse particles, and the particle size is 2.0 mm or less, preferably 0.3 mm.
The particle size is 1.0 mm to 1.0 mm.

本発明ではこの粒子を200〜600℃より好ましくは
200〜4. O0℃で焼成することによって、感光体
構成材としての感度を高めると共に硬度を高める。20
0℃以下でも未焼成粒子に比べ感度の向上は認められる
が感光体の硬度が充分でなく、又600℃以下になると
、酸化亜鉛粒子と絶縁性樹脂との分散に時間を要すると
共に帯電4位の低下が起こり、画像濃度がうすくなる。
In the present invention, the particles are heated at a temperature of 200 to 600°C, preferably 200 to 4.0°C. By firing at 00° C., the sensitivity and hardness of the photoreceptor component are increased. 20
Sensitivity is improved compared to unfired particles even below 0°C, but the hardness of the photoreceptor is not sufficient, and below 600°C, it takes time to disperse the zinc oxide particles and the insulating resin, and the electrification level increases. This causes a decrease in image density, resulting in a decrease in image density.

又焼成に当たってはロータリーキルン、トンネルキルン
、マツフル炉など通常用いられる焼成炉を使用すること
が出来る。これらの粒子は一般に0.6〜1.5 g/
am3好ましくは0.7〜1.2 g / cm”の嵩
密度を有する。
Further, for firing, a commonly used firing furnace such as a rotary kiln, tunnel kiln, Matsufuru furnace, etc. can be used. These particles are generally 0.6-1.5 g/
am3 preferably has a bulk density of 0.7-1.2 g/cm''.

尚焼成粒子の粒径が2.0 mmを超えると酸化亜鉛粒
子の分散液を製造するとき、その分散に長時間を要し好
ましくない。粒径の下限には厳密な規制はない。また製
造された酸化亜鉛粒子は、一つの尺度として、次の方法
で測定して2.0〜10.0g特に3.0〜6.0gの
硬さを有するものが好ましい。
If the particle size of the fired particles exceeds 2.0 mm, it will take a long time to disperse when producing a dispersion of zinc oxide particles, which is not preferable. There is no strict regulation on the lower limit of particle size. The produced zinc oxide particles preferably have a hardness of 2.0 to 10.0 g, particularly 3.0 to 6.0 g, as measured by the following method.

この範囲であるど、本発明による酸化亜鉛粒子を用いて
作った感光体の表面硬度が良好で、耐摩耗性を改良する
ことができることが分かった。硬さの測定は次の如くし
て行なった。即ち直径0.84mm(20メツシユ) 
〜1.7 mm (10メツシユ)ノ粒子をとり、惑星
(読みとり限度)を0.5 gに設定したバネ式秤量機
を乗せて粒子を圧縮し、粒子がくずれたときの表示重量
を硬さの表示とした。
It has been found that within this range, the surface hardness of the photoreceptor made using the zinc oxide particles according to the present invention is good and the wear resistance can be improved. The hardness was measured as follows. That is, the diameter is 0.84 mm (20 meshes)
Take ~1.7 mm (10 mesh) particles, compress the particles using a spring-type weighing machine with a planet (reading limit) set to 0.5 g, and calculate the displayed weight when the particles collapse as hardness. It was displayed as follows.

本発明で製造した上記粒度の焼成酸化亜鉛粒子を用いる
と、前述した従来の酸化亜鉛粉末を用いた場合と異なり
、表面硬度のすぐれた光導電層を形成することができる
When the calcined zinc oxide particles having the above-mentioned particle size produced according to the present invention are used, a photoconductive layer with excellent surface hardness can be formed, unlike the case where the conventional zinc oxide powder described above is used.

本発明方法で製造した酸化亜鉛粒子は従来より知られて
いる通常の方法で絶縁性樹脂の有機溶剤溶液に分散させ
て公知の支持体に塗布し、乾燥することにより電子写真
用感光体とすることができる。
The zinc oxide particles produced by the method of the present invention are dispersed in an organic solvent solution of an insulating resin by a conventionally known method, applied to a known support, and dried to form an electrophotographic photoreceptor. be able to.

以下に実施例および参考例をあげて本発明を説明する。The present invention will be explained below with reference to Examples and Reference Examples.

実施例 通常の電子写真用の粒径0.2〜0.5pの酸化亜鉛粉
末をモザイクタイル素地用油圧プレスを用い、80 K
g/ cm2に圧縮し、形成された圧縮体を次いで振動
ふるいで破砕しつつ篩分けし、粒径1mm以下の酸化亜
鉛粒子500gを得た。この酸化亜鉛粒子を200℃、
300℃、400’0゜500℃及び600℃で各々1
時間焼成し、焼成された酸化亜鉛粒子を得た。
Example Zinc oxide powder with a particle size of 0.2 to 0.5p for ordinary electrophotography was heated at 80 K using a hydraulic press for mosaic tile substrates.
g/cm2, and the formed compressed body was then crushed and sieved using a vibrating sieve to obtain 500 g of zinc oxide particles with a particle size of 1 mm or less. These zinc oxide particles were heated at 200°C.
1 at 300°C, 400'0°, 500°C and 600°C, respectively.
It was fired for a period of time to obtain fired zinc oxide particles.

参考例 上記実施例で作った各焼成酸化亜鉛粒子を用い、下記の
処方の酸化亜鉛分散液を作った。
Reference Example Using each of the calcined zinc oxide particles prepared in the above examples, a zinc oxide dispersion having the following formulation was prepared.

焼成酸化亜鉛粒子          35.0gアク
リル樹脂LR−637 (三菱レーヨン社製、商品名)     17.5gブ
ロムフェノールブルー1%メタノール溶液0.5cc トルエン               80cc上記
各成分をボールミルで4時間分散させて分散液を製造し
た。裏面を高分子導電剤(ダウケミカル社製ECR−7
7)で導電処理した紙の表面に、上記分散液を塗布し、
100℃で5分間乾燥し、酸化亜鉛感光紙を作った。塗
布量は22g/、2 (固形分)とした。
Calcined zinc oxide particles 35.0 g Acrylic resin LR-637 (manufactured by Mitsubishi Rayon Co., Ltd., trade name) 17.5 g Bromophenol blue 1% methanol solution 0.5 cc Toluene 80 cc The above components were dispersed in a ball mill for 4 hours to prepare a dispersion liquid. Manufactured. The back side is coated with a polymer conductive agent (ECR-7 manufactured by Dow Chemical Company).
Applying the above dispersion to the surface of the paper treated with conductivity in 7),
It was dried at 100° C. for 5 minutes to produce zinc oxide photosensitive paper. The coating amount was 22 g/.2 (solid content).

比較例として、上記分散液に用いた焼成酸化亜鉛粒子の
代りに、通常の光導電性酸化亜鉛粉末及び焼成を行なわ
ない酸化亜鉛粒子(圧wj成形後、破砕・篩分けしたも
の) 35.0gを用いて、同様に酸化亜鉛感光紙を作
った。塗布量は同じく22g/m2(固形分)とした。
As a comparative example, instead of the calcined zinc oxide particles used in the above dispersion, 35.0 g of ordinary photoconductive zinc oxide powder and zinc oxide particles that were not calcined (crushed and sieved after pressure wj molding) were used. Zinc oxide photosensitive paper was similarly made using The coating amount was also 22 g/m2 (solid content).

これらの感光紙の特性は次のとおりであった。The properties of these photosensitive papers were as follows.

(以 下 余 白) 上記表のデータから明らかな如く、本発明の方法で作っ
た焼成酸化亜鉛粒子を用いて作った感光紙は、従来例で
ある比較例に示す様に通常の光導電性粉末及び未焼成粒
子に比し、感度及び感光層の硬度が向上している。この
ためこれらはオフセット印刷用原版および転写用原版等
の電子写真用感光体としてすぐれている。
(Margin below) As is clear from the data in the table above, the photosensitive paper made using the calcined zinc oxide particles made by the method of the present invention has a normal photoconductivity as shown in the comparative example, which is a conventional example. Compared to powder and unfired particles, the sensitivity and hardness of the photosensitive layer are improved. For this reason, these are excellent as photoreceptors for electrophotography such as original plates for offset printing and original plates for transfer.

Claims (3)

【特許請求の範囲】[Claims] (1)酸化亜鉛粉末を20〜150Kg/cm^2の圧
力で圧縮し、圧縮体を破砕することにより得られる粒径
2.0mm以下の粒子を200〜600℃で焼成するこ
とを特徴とする電子写真用酸化亜鉛粒子の製造法。
(1) Particles with a particle size of 2.0 mm or less obtained by compressing zinc oxide powder at a pressure of 20 to 150 kg/cm^2 and crushing the compressed body are fired at 200 to 600°C. A method for producing zinc oxide particles for electrophotography.
(2)酸化亜鉛粒子が少なくとも0.6g /cm^3
の嵩密度を有する特許請求の範囲第1項記載の製造法。
(2) Zinc oxide particles of at least 0.6 g/cm^3
The manufacturing method according to claim 1, having a bulk density of .
(3)酸化亜鉛粒子が2.0〜10.0gの荷重で破砕
される硬さを有する特許請求の範囲第1項又は第2項記
載の製造法。
(3) The manufacturing method according to claim 1 or 2, wherein the zinc oxide particles have a hardness that can be crushed under a load of 2.0 to 10.0 g.
JP15165385A 1985-07-10 1985-07-10 Preparation of electrophotographic zinc oxide particles Pending JPS6211860A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP15165385A JPS6211860A (en) 1985-07-10 1985-07-10 Preparation of electrophotographic zinc oxide particles

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP15165385A JPS6211860A (en) 1985-07-10 1985-07-10 Preparation of electrophotographic zinc oxide particles

Publications (1)

Publication Number Publication Date
JPS6211860A true JPS6211860A (en) 1987-01-20

Family

ID=15523276

Family Applications (1)

Application Number Title Priority Date Filing Date
JP15165385A Pending JPS6211860A (en) 1985-07-10 1985-07-10 Preparation of electrophotographic zinc oxide particles

Country Status (1)

Country Link
JP (1) JPS6211860A (en)

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