JPH063835A - Method for manufacturing electrophotographic photoreceptor - Google Patents

Abstract

(57) [Summary] [Object] The present invention is a method for producing an electrophotographic photosensitive member, by which an electrophotographic photosensitive member having excellent image characteristics can be obtained. [Structure] In a method of manufacturing an electrophotographic photosensitive member in which a photosensitive layer is provided on a conductive support, an aluminum drum having an aqueous anodic oxide film formed on the surface thereof is used as a conductive support and contains a surfactant. This is a method for producing an electrophotographic photosensitive member in which washing is performed with hot water at a temperature of 30 to 90 ° C., and then the drum is immersed and washed with pure water at a temperature of 30 to 90 ° C.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing an electrophotographic photosensitive member, and more particularly to a method for manufacturing an electrophotographic photosensitive member having excellent image characteristics.

[0002]

2. Description of the Related Art An electrophotographic photosensitive member has a structure in which a photosensitive layer is vacuum-deposited or coated on a conductive support and is used in copying machines, printers and the like. The support used for the electrophotographic photosensitive member may be any one as long as it has conductivity, but the most commonly used one is a metal drum (hereinafter referred to as a blank tube). The raw tube is a metal formed into a drum shape by impact molding, extrusion processing, drawing processing, or the like, and the surface may be further subjected to ironing processing or cutting processing. On the surface of such a raw pipe, metal powder generated in the process of raw pipe processing, dust and dust from the surrounding environment, oil used during processing, rust prevention of the surface when storing the raw pipe after processing The oil etc. applied to is adhered. Since these deposits adversely affect the image characteristics and electrophotographic properties of the electrophotographic photoreceptor after forming the photosensitive layer on the tube, it is necessary to remove these deposits in the manufacturing process of the electrophotographic photoreceptor. The tube is being cleaned. As the method for cleaning the raw tube, there are non-contact cleaning methods such as jet cleaning method, ultrasonic cleaning method, immersion cleaning method, steam cleaning method, etc., and contact cleaning method in which a brush, waste cloth, etc. are pressed against the surface of the raw tube. It is being appreciated. Methanol, ethanol, ethylene glycol, 1,3-butadiol, methylene chloride, CFC113, etc. were used for these cleaning solutions. However, under the present circumstances, these organic solvents have drawbacks in hygiene, cost and environment.

[0003]

The present invention provides a method for producing an electrophotographic photosensitive member having excellent image characteristics.

[0004]

The conductive support used in the present invention is an aluminum-based shell (hereinafter referred to as an alumite shell) having an aqueous anodic oxide film formed on its surface. To form an aqueous anodic oxide film on the surface of an aluminum tube, completely remove the dust, dust, oil, etc. adhering to the tube, and then conduct the conductivity in an aqueous solution of oxalic acid, sulfuric acid, etc. A method in which electrolysis is performed using a transparent support (aluminum-based tube) as an anode. As a result, an anodic oxide film is formed on the surface of the aluminum-based tube, and an alumite tube can be obtained. A water-soluble liquid is used to form the anodic oxide film, so no oily substance will adhere to the surface of the alumite tube, and the surface of the alumite tube does not rust unlike the aluminum tube. Therefore, it is not necessary to apply oil for rust prevention on the surface.
Therefore, after the alumite tube is processed, most of the substances that adhere to the surface of the alumite tube until the formation of the photosensitive layer are dust, dust, or water-soluble substances. However, they have found that it is effective to use a surfactant as a cleaning method for stains that are difficult to remove by washing with water alone, and have reached the present invention. As the surfactant used in the present invention, anionic, cationic, nonionic, amphoteric surfactants generally used for cleaning can be used. For example, as an anion system, carboxylate, sulfonate, sulfate ester,
Phosphate ester salt type, etc., cationic amine compounds such as aliphatic amine salt, aliphatic quaternary ammonium salt, heterocyclic compound quaternary salt type, etc. Nonionic compounds such as ether type, ether ester type, ester type, nitrogen-containing type, etc. As the amphoteric system, betaine type, aminocarboxylic acid type, imidazoline derivative type and the like are used, but the surfactant used is not limited to these, and it is also possible to use several kinds thereof in combination.

In the course of further studies using the above-mentioned surfactant, a washing process including passing a bath containing the surfactant in the washing process with pure water has a negative effect on the image characteristics after the formation of the photosensitive layer. It was found that it greatly affects and gives good image characteristics. The bath containing the surfactant may be equipped with a device capable of ultrasonic cleaning or brush cleaning, and it is also possible to perform cleaning with a combination thereof. The surfactant adhering to the drum is then washed several times with a shower rinse or an intermediate washing tank, and then the drum is moved to a warm pure water washing tank. It is preferable that the pure water is sufficiently filtered and passes through an ion-exchange resin-based tank to maintain the conductivity of 3 μS / cm or less.

The photosensitive layer is formed after cleaning the alumite tube with pure water. Examples of the charge generating agent used in the photosensitive layer include phthalocyanine pigments such as metal phthalocyanine and metal-free phthalocyanine, monoazo dyes and disazo dyes. Azo dyes such as, indigo pigments, quinacridone pigments, indanthrene pigments, xanthene dyes, benzimidazole pigments, perylene pigments,
Dye / pigment such as squaric menane dye, eutectic complex formed from pyrylium salt dye and polycarbonate resin, electron donating substance such as polyvinylcarbazole and TN
Examples of the charge transfer complex include an electron accepting substance such as F, and it is particularly preferable to use a phthalocyanine pigment. Examples of the charge transfer agent used in the photosensitive layer include:
Examples thereof include hydrazone-based compounds, styryl-based compounds, pyrazoline-based compounds, oxazole-based compounds, and thiazole-based compounds, but it is particularly preferable to use one or more hydrazone-based compounds and styryl-based compounds. The photosensitive layer according to the invention may contain a known sensitizer. Also,
If necessary, a surfactant, a plasticizer, an antioxidant, an ultraviolet absorber, a dispersion aid, an anti-settling agent and the like can be appropriately used. Further, the photoreceptor of the present invention has a structure in which a charge generating agent and a charge transporting agent are provided on the alumite tube in the same layer, which is usually referred to as a single-layer type photoreceptor, or mainly contains a charge generating agent. It is possible to have a structure generally called a laminated type photoreceptor, which is formed by laminating one layer and a second layer mainly containing a charge transfer agent on an alumite tube. In the case of a laminated type photoreceptor, which of the charge generation layer and the charge transport layer is to be the upper layer is determined by whether the chargeability is positive or negative. In general, when negatively charged, it is advantageous in terms of characteristics that the charge transport layer is an upper layer.

Examples of the present invention will be described below, but the present invention is not limited to the following examples. Less than,
In the examples, "parts" in the examples means parts by weight.

Example 1 An alumite tube was ultrasonically cleaned using an aqueous solution of 2 parts of sodium dodecylbenzenesulfonate in 100 parts of warm water at 40 ° C. Then, after washing with a water brush, the surfactant is preliminarily washed in a shower rinse tank, and ultrasonic rinse is washed in an intermediate cleaning tank of pure water.
After soaking in pure water with a conductivity of 1.5 μS / cm at 3 ° C and pulling it up, 3 parts of τ-type metal-free phthalocyanine as a charge generating agent and a vinyl chloride-vinyl acetate co-weighing are added to an alumite tube that has been dried with warm air. Combined resin (trade name VM manufactured by Union Carbide)
A coating liquid prepared by dispersing 3 parts of CH) together with 94 parts of tetrahydrofuran in a ball mill for 2 hours was applied and dried at 100 ° C. for 2 hours to form a 0.25 μm charge generation layer. Next, 1-benzyl-1,2,3,4-as a charge transport agent
Tetrahydroquinoline-6-carboxaldehyde-
A solution prepared by dissolving 10 parts of 1 ', 1'-diphenylhydrazone and 10 parts of a polyester resin (manufactured by Toyobo Co., Ltd., BYRON 200) in 100 parts of methylene chloride was applied onto the charge generation layer and dried to form a 15 μm charge transport layer. did. When the electrophotographic photosensitive drum was visually observed, coating cissing did not occur. Next, this photoconductor was attached to an electrophotographic copying machine having a corona charger, an exposure part, a transfer charging part, a charge removal exposure part and a cleaner. When the dark portion potential of this copying machine was set to -650 V and the light portion potential was set to -150 V, the obtained image was evaluated, and it was an excellent image without black spots and streaks.

[0008]

Example 2 Brush-contact cleaning was performed using an aqueous solution of 1 part of dialkylsulfosuccinic acid ester salt in 100 parts of warm water at 40 ° C., and then the surface-active agent was preliminarily washed in a shower rinse tank and purified water was used. Ultrasonic rinsing in the intermediate cleaning tank, and immersing in pure water with a conductivity of 1.5 μS / cm at 83 ° C.
After pulling up, a photoconductor similar to that of Example 1 was prepared in an anodized aluminum tube which was dried with warm air. Visual observation of this electrophotographic photosensitive drum revealed that coating cissing did not occur. Next, when the same image evaluation as in Example 1 was performed, it was an excellent image without black spots and streaks.

[0009]

Example 3 After dipping and washing with an aqueous solution containing 2 parts of dioctadecyl-dimethylammonium bromide in 100 parts of warm water at 50 ° C., washing with a water brush was performed,
Pre-clean the surface-active agent in the shower rinse tank, ultrasonic rinse in the intermediate cleaning tank of pure water, immerse it in pure water with a conductivity of 1.5 μS / cm at 83 ° C, pull it up, and then dry it with warm air. A photoconductor similar to that of Example 1 was prepared in the anodized alumite tube. Visual observation of this electrophotographic photosensitive drum revealed that coating cissing did not occur. Next, when the same image evaluation as in Example 1 was performed, it was an excellent image without black spots and streaks.

[0010]

Example 4 Immersion ultrasonic cleaning was performed using an aqueous solution containing 2 parts of polyoxyethylene monododecyl ether in 100 parts of warm water at 35 ° C., followed by water brush contact cleaning and a surfactant in a shower rinse tank. Was pre-cleaned, ultrasonic rinse cleaning was performed in a pure water intermediate cleaning tank, and the conductivity was 1.5μ at 83 ° C.
After immersing in S / cm pure water, pulling it up, and then drying with warm air, a photoreceptor similar to that of Example 1 was prepared. Visual observation of this electrophotographic photosensitive drum revealed that coating cissing did not occur. Next, when the same image evaluation as in Example 1 was performed, it was an excellent image without black spots and streaks.

[0011]

Example 5 Immersion ultrasonic cleaning and brush cleaning were performed using an aqueous solution containing 100 parts of hot water at 60 ° C. and 1 part of TEGO-Betaine, a carboxybetaine-type surfactant, Goldschmidt, followed by water brush contact. Cleaning, pre-cleaning the surfactant in a shower rinse tank, ultrasonic rinse cleaning in an intermediate cleaning tank of pure water, immersing in pure water with a conductivity of 1.5 μS / cm at 83 ° C, pulling it up, then warm air A photoconductor similar to that of Example 1 was prepared on the dried alumite tube. Visual observation of this electrophotographic photosensitive drum revealed that coating cissing did not occur. Next, when the same image evaluation as in Example 1 was performed, it was an excellent image without black spots and streaks.

[0012]

Example 6 Immersion ultrasonic cleaning and brush cleaning were carried out using an aqueous solution containing 100 parts of warm water at 45 ° C. and 1 part of TEGO-Betaine, a carboxybetaine type surfactant, from Goldschmidt, followed by water brush contact. Cleaning, pre-cleaning the surfactant in a shower rinse tank, ultrasonic rinse cleaning in an intermediate cleaning tank of pure water, dipping in pure water with a conductivity of 1.5 μS / cm at 83 ° C, pulling it up, then warm air A photoconductor similar to that of Example 1 was prepared on the dried alumite tube. Visual observation of this electrophotographic photosensitive drum revealed that coating cissing did not occur. Next, when the same image evaluation as in Example 1 was performed, it was an excellent image without black spots and streaks.

[0013]

[Comparative Example 1] An aluminum tube (no anodized film formed on the surface of the tube) was heated to 55 ° C and the electric conductivity was 1.5μ.
Brush contact cleaning and ultrasonic rinsing cleaning using S / cm pure water, immersing in pure water with a conductivity of 1.5 μS / cm at 83 ° C, pulling up, and suction drying with hot air. A photoconductor similar to that in Example 1 was produced in the raw tube. When this electrophotographic photosensitive drum was visually observed, coating cissing occurred. Next, when the same image evaluation as in Example 1 was performed, it was an image with black spots. A photoconductor similar to that of the example was manufactured on the tube.

[0014]

[Comparative Example 2] Brush cleaning was carried out using an aqueous solution containing 2 parts of sodium dodecylbenzene sulfonate in 100 parts of water at 15 ° C, and after the water brush cleaning, the same cleaning and drying as in Example 1 was carried out. A photoconductor similar to that in Example 1 was produced on the alumite tube. When this electrophotographic photosensitive drum was visually observed, coating cissing occurred. Next, when the same image evaluation as that of the example was performed, it was an image with black spots and streaks.

[0015]

Comparative Example 3 An alumite tube was ultrasonically cleaned using an aqueous solution containing 2 parts of sodium dodecylbenzenesulfonate in 100 parts of water at 40 ° C. Next, after performing water brush contact cleaning, pre-cleaning the surfactant in the shower rinse tank, and ultrasonic rinse cleaning in the pure water intermediate cleaning tank,
After immersing in pure water having a conductivity of 1.5 μS / cm at 25 ° C., pulling it up, and drying it with warm air, a photoreceptor similar to that of Example 1 was prepared. When this electrophotographic photosensitive drum was visually observed, coating cissing occurred. Next, when the same image evaluation as that of the example was performed, it was an image with black spots and streaks.

[0016]

INDUSTRIAL APPLICABILITY In a method for producing an electrophotographic photoreceptor in which a photosensitive layer is provided on a conductive support, an aluminum drum having an aqueous anodic oxide film formed on the surface thereof is used as a conductive support, and a surfactant is used. It is possible to obtain an electrophotographic photosensitive member having excellent image characteristics by washing with contained hot water having a temperature of 30 to 90 ° C. and then dipping and washing the drum with pure water having a temperature of 30 to 90 ° C.

 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Toshio Nishimura 2-3-13 Kyobashi, Chuo-ku, Tokyo Within Toyo Inki Manufacturing Co., Ltd. (72) Yoshiyuki Onai 2-3-13 Kyobashi, Chuo-ku, Tokyo No. Toyo Inki Manufacturing Co., Ltd. (72) Inventor Toshio Seta 2-33 Kyobashi, Chuo-ku, Tokyo Toyo Inki Manufacturing Co., Ltd.

Claims (1)

[Claims] 1. A method for producing an electrophotographic photosensitive member comprising a photosensitive layer provided on a conductive support, wherein an aluminum drum having an aqueous anodic oxide film formed on the surface is used as the conductive support, and a surfactant is used. A method for producing an electrophotographic photosensitive member, comprising: washing the drum with warm water having a temperature of 30 to 90 ° C., and then washing the drum with warm pure water having a temperature of 30 to 90 ° C.