JP2002086089A - Apparatus for producing toner, method for cleaning the apparatus, and method for producing toner - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for easily cleaning a toner production apparatus in a short time without damaging the apparatus while dispensing with post treatments such as the recovery of the cleaner used, and taking care of the health and sanitary of the worker. SOLUTION: There is provided a method for cleaning an apparatus for producing a polymerization process toner having colored polymer particles obtained by polymerizing a polymerizable monomer composition having at least a polymerizable monomer and a colorant in the presence of a polymerization initiator, which comprises allowing sublimable solid pellets to collide at a high speed against that surface of the apparatus which is to be cleaned to remove the adherent matter therefrom.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] 1. Field of the Invention [0002] The present invention relates to an apparatus for producing a toner for visualizing a latent image, a method for cleaning the apparatus, and a method for producing the toner.

[0002]

2. Description of the Prior Art Electrophotography is disclosed in U.S. Pat. No. 2,297,6.
As described in, for example, JP-A-91, a number of methods are known. Generally, a photoconductor made of a photoconductive substance is used, and an electric latent image is formed on the photoconductor by various means. Then, the latent image is developed using toner to form a visible image, and if necessary, the toner image is transferred to a transfer material such as paper. Alternatively, a printed matter is obtained.

As a method of developing using a toner or a method of fixing a toner image, various methods have been conventionally proposed, and a method suitable for each image forming process is adopted.

Conventionally, as a toner used for these purposes, a coloring agent such as a dye and a pigment is generally melt-mixed in a thermoplastic resin, uniformly dispersed, and then pulverized by a pulverizer to classify the pulverized material. A toner having a desired particle size has been produced by classification with a machine.

[0005] Although this method can produce fairly good toners, it does have certain limitations, namely the choice of toner materials. For example, the resin colorant dispersion is brittle enough,
It must be able to be comminuted in an economically feasible production equipment. However, when the resin colorant dispersion is made brittle to satisfy these requirements, the particle size range of the particles formed when the nuclear dispersion is actually finely pulverized at a high speed tends to be widened, and in particular, a relatively large proportion. There is a problem that the fine particles are contained therein. Further, such a highly brittle material is liable to be further pulverized or powdered when used for development in a copying machine or the like.

Further, in this method, it is difficult to completely and uniformly disperse solid fine particles such as a colorant in a resin.
Depending on the degree of the dispersion, it may cause an increase in fog during image formation, a decrease in the image density, or a poor color mixture or transparency. Therefore, sufficient attention must be paid to the dispersion of the colorant. Further, exposure of the coloring agent to the fracture surface of the pulverized particles may cause a change in development characteristics.

On the other hand, in order to overcome the problems of the toner caused by these pulverization methods, Japanese Patent Publication Nos.
JP-A-3-10799 and JP-A-51-14895 have proposed various polymerization toners, including suspension polymerization toners, and methods for producing the same. For example, in a suspension polymerization toner, a polymerizable monomer, a colorant and a polymerization initiator, and if necessary, a crosslinking agent, a charge control agent, and other additives are uniformly dissolved or dispersed to prepare a monomer composition. After that, this monomer composition is dispersed in a continuous phase containing a dispersion stabilizer, for example, an aqueous phase using a suitable stirrer to form colored monomer particles and simultaneously carry out a polymerization reaction. ,
A colored polymer particle having a desired particle size is obtained. An acid or an alkali is added to the obtained suspension containing the colored polymer particles to solubilize the dispersion stabilizer in the aqueous phase, and then washed,
Dehydration and drying are performed to obtain desired toner particles.

According to this method, since no pulverizing step is included, the toner does not need to be brittle, a soft material can be used as a resin, and the colorant is not exposed on the particle surface. There is an advantage that a toner having a uniform triboelectric charging property can be obtained. Further, since the particle size distribution of the obtained toner is relatively sharp, even if the classification step is omitted or the classification is performed, the toner can be obtained in a high yield, so that energy is saved, time is shortened, and the process yield is improved. Great cost reduction effect. Further, since a large amount of a low softening point substance can be included in the toner as a release agent, there is an advantage that the obtained toner has excellent offset resistance.

As described above, a polymerized toner having excellent characteristics in which a soft material can be used as a resin, however, there is a problem that the soft resin is easily adhered and fused in a manufacturing apparatus due to the use of the soft resin. Have been. In addition, since the liquid monomer composition is handled in the initial stage of the process, some liquid deposits which are not observed in the pulverized toner are also generated.

[0010] Even with the conventional pulverization method toner, adhered matter and fused matter have been generated in the manufacturing apparatus. Since the deposit is a dry powder, it is easy to suction by a vacuum cleaner or the like, and the suction is the most suitable cleaning method. Further, since the fused material produced by the pulverized toner is solid and brittle, peeling by the blast method was effective. In particular, since the fused material generated from the collision plate in the pulverizing step is firmly fused, a cleaning method having a strong peeling force such as sand blast was effective. In addition, Japanese Patent Application Laid-Open
As disclosed in JP-A-319634 and JP-A-10-319638, washing with a sublimable solid pellet such as dry ice is also being studied, but a relatively high pressure of about 300 to 1000 kPa is required to peel off a strong fusion product. It was necessary to clean using compressed gas.

However, as described above, since the deposits generated by the polymerization toner are soft or liquid, suction cleaning with a vacuum cleaner or the like is not suitable. In many cases, the apparatus for producing a polymerized toner also treats the surface to be cleaned with glass lining, fluorine coating, or the like as an adhesion preventing means. Since these treated surfaces are vulnerable to impact, it was not possible to use sandblasting or a powerful blasting means using sublimable solid pellets using a compressed gas having a relative pressure of about 300 to 1000 kPa. In addition, even when the surface to be cleaned is not treated, when a compressed gas having a relative pressure of about 300 to 1000 kPa is blown, the soft and liquid deposits are scattered, and there is no cleaning effect such as reattaching to another surface to be cleaned. There was also.

[0012] Therefore, it has been common practice to manually clean the deposits on the polymerized toner production apparatus using an organic solvent. However, although cleaning with a solvent is excellent in detergency, it has problems in treatment of waste liquid and health and hygiene of workers.

On the other hand, as described above, although a sharper particle size distribution can be obtained in the polymerization method than in the pulverization method, further reduction due to miniaturization of copying machines, printers and the like, and an increase in equipment restrictions due to personalization. It has been considered difficult to omit the classification step in order to meet the demand for sharpening the particle size distribution.

Further, since the toner obtained by this polymerization method obtains particles in an aqueous phase, a certain amount of water accompanies the toner particles after polymerization.

In the state with the water, the chargeability required for the toner particles is naturally lost, and the cohesiveness of the particles becomes extremely high, so that the toner particles required for classification can hardly be dispersed. Would.

Therefore, in order to remove water to a satisfactory extent, it has been necessary to remove water by drying in a subsequent step.

Conventionally, as described above, as a method for producing a polymerized toner, a drying step and a classification step are required after the polymerization. However, these two steps are difficult to carry out continuously, and usually are separated. Has been done in the process. Then, for example, when flash drying is selected as the drying means, the material once dispersed during drying is aggregated again before the next classification step, and the classification efficiency is reduced.

In addition, after many separate steps, the amount of adhesion and the like also increases, resulting in a decrease in product yield. That is, there is a problem that a load is extremely involved in production efficiency and production cost.

[0019]

SUMMARY OF THE INVENTION An object of the present invention is to provide an apparatus for producing a polymerized toner which can be easily cleaned in a short time, does not require a post-process such as recovery of a detergent, and damages the apparatus. It is an object of the present invention to provide a cleaning method that does not require the use of the same and also takes into consideration the health and hygiene of workers.

It is another object of the present invention to save energy, improve production efficiency, and reduce production costs by shortening the toner production process by the polymerization method or by providing a production method that does not degrade the performance of the product. It is another object of the present invention to provide a method for producing a toner which can reduce the amount of toner.

[0021]

The present invention provides a colored polymer obtained by polymerizing a polymerizable monomer composition containing at least a polymerizable monomer and a colorant in the presence of a polymerization initiator. The present invention relates to a method for producing a polymerized toner having coalesced particles, wherein a sublimable solid pellet is collided at a high speed to remove deposits on a surface to be cleaned of the production apparatus.

Further, the present invention has colored polymer particles obtained by polymerizing a polymerizable monomer composition containing at least a polymerizable monomer and a colorant in the presence of a polymerization initiator. The present invention relates to an apparatus for producing a toner, characterized in that the apparatus for producing a polymerized toner is provided with a cleaning device for colliding sublimable solid pellets at high speed to remove deposits on the surface to be cleaned of the production device.

Further, according to the present invention, a polymerizable monomer composition containing at least a polymerizable monomer and a colorant is polymerized in an aqueous dispersion medium to produce colored polymer particles.
Washing and dried, the weight average diameter of 3 to 10 [mu] m, variation in number distribution represented by the following formula Factor _{A A = S n / D 1} × 100 ( where standard deviation of S _n is a number distribution, D ₁ is the number Wet colored polymer particles having an average particle size of less than 40% are obtained, dispersed in a hot air stream while continuously supplying the particles, and continuously dispersed while being sent in parallel with the hot air stream. And to classify the toner.

In the following description, the invention of the cleaning method of the toner production apparatus and the invention of the toner production apparatus will be referred to as "Invention 1", and the invention of the toner production method will be referred to as "Invention 2".

[0025]

DESCRIPTION OF THE PREFERRED EMBODIMENTS (I) First, the present invention 1 will be described in detail.

The apparatus for producing the polymerized toner to be cleaned by the method of the present invention 1 is not particularly limited, as long as it is generally used in the production step of the polymerized toner. Examples of the apparatus for producing a polymerized toner include a dispersing apparatus, a mixing apparatus, a dissolving apparatus, a granulating apparatus, a reaction apparatus, a distillation apparatus, a sieving apparatus, a filtration apparatus, a drying apparatus, a classification apparatus, and piping associated therewith. In such an apparatus for producing a polymerized toner, for example, a polymerizable monomer, a crosslinking agent, a chain transfer agent, a resin, a low softening point substance, a colorant, a charge control agent, a polymerization initiator, An agent, a releasing agent, a fluidizing agent, or the like, or a mixture or a reactant thereof adheres as an adhered substance and a fused substance.

In the toner according to the first aspect of the present invention, in order to faithfully develop finer latent image dots for higher image quality, the toner was also measured with a finer particle size, specifically, a Coulter counter. The present invention provides a toner having a weight average diameter of 4 to 8 μm and a coefficient of variation A of the number distribution of 35% or less.
Most preferred as a toner used for

In the case of a toner having a weight average diameter of less than 4 μm, a large amount of untransferred toner is generated on a photoreceptor or an intermediate transfer member due to poor transfer efficiency, which causes non-uniform unevenness of an image due to fog or poor transfer. It is not preferable as the toner used in the first invention. The toner has a weight average diameter of 8 μm.
When the ratio is more than 35%, fusing to a member is likely to occur, and when the variation coefficient A of the number distribution of the toner exceeds 35%, the tendency is further increased, which causes a problem.

[0029] Here, the variation coefficient A of the number _{distribution, A = S n / D 1} × 100 ( where, S _n is the standard deviation of the number distribution, D ₁ is the number average particle diameter) calculated by the equation, the particle size Represents the spread of the distribution.

As the low softening point substance used in the toner according to the first aspect of the present invention, a compound having a main maximum peak value of 40 to 90 ° C. measured according to ASTM D3418-8 is preferable. If the maximum peak is less than 40 ° C., the self-cohesive force of the low softening point substance becomes weak, and as a result, the hot offset resistance becomes weak, which is not preferable for a full color toner. On the other hand, when the maximum peak exceeds 90 ° C., the fixing temperature becomes high, and it becomes difficult to appropriately smooth the surface of the fixed image, which is not preferable from the viewpoint of color mixing. Furthermore, in the case of obtaining a toner by a direct polymerization method, when the temperature of the maximum peak value is high due to granulation and polymerization in an aqueous system, a substance having a low softening point mainly precipitates during granulation and hinders a suspension system. Therefore, it is not preferable.

For the measurement of the temperature of the maximum peak value, for example, DSC-7 manufactured by Perkin Elmer Co., Ltd. is used. The temperature correction of the device detection unit uses the melting points of indium and zinc, and the heat quantity correction uses the heat of fusion of indium. For the sample, an aluminum pan is used, an empty pan is set as a control, and measurement is performed at a heating rate of 10 ° C./min.

Specifically, paraffin wax, polyolefin wax, Fischer-Tropsch wax,
Amide waxes, higher fatty acids, ester waxes and their derivatives or their graft / block compounds can be used.

The ester wax preferably used in the present invention preferably has a hardness of 0.5 to 5.0.
The hardness of the ester wax is 5mm in diameter and 5mm in thickness.
This is a value obtained by measuring a Vickers hardness using a dynamic ultra-fine hardness tester (DUH-200) manufactured by Shimadzu Corporation after preparing a cylindrical sample having a diameter of mm. The measurement conditions are
After displacing 10 μm under the condition of a load speed of 9.67 mm / sec with a load of 0.5 g and holding it for 15 seconds, the resulting dent shape is measured to determine Vickers hardness. The hardness of the ester wax preferably used in the present invention 1 is 0.5-5.
Indicates a value of 0. A low softening point substance having a hardness of less than 0.5 has a large dependence on the pressure and process speed of the fixing device, and tends to exhibit insufficient high-temperature offset resistance. Since the stability is poor and the self-cohesive force of the release agent itself is small, similarly, the high-temperature offset resistance tends to be insufficient.

In recent years, the need for full-color double-sided images has also increased. When forming a double-sided image, the toner image formed on the transfer paper first on the front side is used even when the image is formed on the rear side. Therefore, it is necessary to sufficiently consider the high-temperature offset resistance of the toner. Therefore, in the present invention 1, it is necessary to add a large amount of a low softening point substance. Specifically, it is preferable to add a low softening point substance to the toner in an amount of 5 to 40% by mass. Addition of less than 5% by mass does not show sufficient high-temperature offset resistance, and the image on the back surface tends to show an offset phenomenon during fixing of a double-sided image. On the other hand, when it exceeds 40% by mass, coalescence of toner particles tends to occur during granulation, and a toner having a wide particle size distribution is easily formed, which is not suitable for the present invention 1.

The method for producing the toner particles of the present invention 1 is described in JP-B-36-10231 and JP-A-59-5.
No. 3,856, JP-A-59-61842, a method of directly producing a toner using a suspension polymerization method, an aqueous organic solvent which is soluble in a monomer and insoluble in a polymer obtained. It is possible to produce the toner using an emulsion polymerization method typified by a dispersion polymerization method of directly producing a toner using a method or a soap-free polymerization method of producing a toner by directly polymerizing in the presence of a water-soluble polar polymerization initiator. .

However, in the dispersion polymerization method,
The resulting toner shows a very sharp particle size distribution,
From the viewpoint of narrow selection of materials to be used and the use of organic solvents in terms of treatment of waste solvents and flammability of the solvents, the production apparatus is complicated and easily complicated. Emulsion polymerization methods typified by soap-free polymerization are effective because the particle size distribution of the toner is relatively uniform, but when the used emulsifier and initiator terminals are present on the surface of the toner particles, the environmental characteristics are likely to deteriorate.

In the present invention 1, a suspension polymerization method under normal pressure or under pressure is particularly preferable, in which a fine particle toner having a sharp particle size distribution and a particle size of 4 to 8 μm can be obtained relatively easily. A so-called seed polymerization method in which a monomer is further adsorbed on the polymer particles once obtained and then polymerized using a polymerization initiator can also be suitably used in the present invention 1.

Further, from the viewpoint of fixability, it is necessary to incorporate a large amount of the low softening point substance into the toner, so that it is necessary to include the low softening point substance in the outer shell resin. As a specific method for encapsulating the low softening point substance, the polarity of the material in the aqueous medium is set to be smaller for the low softening point substance than for the main monomer, and a small amount of a large polar resin or monomer is used. By adding it, a toner having a so-called core-shell structure in which a low softening point substance is coated with an outer shell resin can be obtained. To control the particle size distribution and the particle size of the toner, a method of changing the type and amount of a poorly water-soluble inorganic salt or a dispersant that acts as a protective colloid, and mechanical device conditions, such as the peripheral speed of the rotor, the number of passes, and stirring By controlling the stirring conditions such as the shape of the blades, the shape of the container, or the concentration of the solid content in the aqueous solution, the predetermined toner of the present invention 1 can be obtained.

The polymerizable monomers that can be used in the above-mentioned polymerized toner include styrene-based monomers such as styrene, o (m-, p-) methylstyrene and m (p-)-ethylstyrene; Methyl acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, octyl (meth) acrylate, dodecyl (meth) acrylate, stearyl (meth) acrylate, (meth) acrylic acid (Meth) acrylate monomers such as behenyl, 2-ethylhexyl (meth) acrylate, dimethylaminoethyl (meth) acrylate, and diethylaminoethyl (meth) acrylate; butadiene, isoprene, cyclohexene, (meth) acrylonitrile And vinyl monomers such as acrylic acid amide are preferably used. These can be used alone or generally in the published Polymer Handbook, 2nd edition III-P 139-192 (John
The monomers are appropriately mixed and used so that the theoretical glass temperature (Tg) described in Wiley & Sons) is 40 to 75 ° C. If the theoretical glass transition temperature is lower than 40 ° C., problems arise in terms of the storage stability of the toner and the durability stability of the developer. In this case, the color mixture of each color toner is insufficient and the color reproducibility is poor, and the transparency of the OHP image is remarkably reduced, which is not preferable from the viewpoint of high image quality.

In the present invention 1, it is particularly preferable to add a polar resin in addition to the outer shell resin in order to encapsulate the low softening point substance in the outer shell resin. As the polar resin used in the present invention 1, a copolymer of styrene and (meth) acrylic acid, a maleic acid copolymer, a saturated polyester resin, and an epoxy resin are preferably used. It is particularly preferable that the polar resin does not contain an unsaturated group capable of reacting with a shell resin or a monomer in the molecule. When a polar resin having an unsaturated group is contained, a cross-linking reaction occurs with the monomer forming the outer shell resin layer, and as a full-color toner, it becomes extremely high in molecular weight and disadvantageous for color mixing of four-color toner, which is not preferable. .

The colorant used in the present invention 1 is a black colorant that is toned to black using carbon black, a magnetic substance, and the following yellow / magenta / cyan colorants.

Examples of yellow colorants include condensed azo compounds, isoindolinone compounds, anthraquinone compounds,
Compounds represented by azo metal complexes, methine compounds and allylamide compounds are used. Specifically, C.I. I. Pigment Yellow 12, 13, 14, 15, 17, 6
2, 74, 83, 93, 94, 95, 109, 110,
111, 128, 129, 147, 168 and the like are preferably used. Condensed azo compounds, magenta colorants,
Diketopyrrolopyrrole compounds, anthraquinones, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds,
A perylene compound is used. Specifically, C.I. I. Pigment Red 2, 3, 5, 6, 7, 23, 48: 2,
48: 3, 48: 4, 57: 1, 81: 1, 144, 1
46, 166, 169, 177, 184, 185, 20
2, 206, 220, 221, 254 are particularly preferred.

As the cyan coloring agent, copper phthalocyanine compounds and derivatives thereof, anthraquinone compounds, basic dye lake compounds and the like can be used. Specifically, C.I. I.
Pigment Blue 1, 7, 15, 15: 1, 15: 2,
15: 3, 15: 4, 60, 62, 66, etc. can be particularly preferably used.

These colorants can be used alone or as a mixture or in the form of a solid solution. The colorant of the present invention 1 is selected from the viewpoints of hue angle, saturation, brightness, weather resistance, OHP transparency, and dispersibility in toner. The colorant is used in an amount of 1 to 20 parts by mass per 100 parts by mass of the resin. When a magnetic material is used as a black colorant,
Unlike other colorants, 40 to 1 with respect to 100 parts by mass of resin
Used by adding 50 parts by mass.

As the charge control agent used in the present invention 1, a known charge control agent can be used, but a charge control agent which is colorless, has a high toner charging speed and can stably maintain a constant charge amount is preferable. Further, in the case where a direct polymerization method is used in the present invention, a charge control agent having no polymerization inhibitory property and having no solubilized substance in an aqueous system is particularly preferable. Specific compounds include metal compounds of salicylic acid, naphthoic acid, and dicarboxylic acid, polymer compounds having sulfonic acid and carboxylic acid in the side chain, boron compounds, urea compounds, silicon compounds, and carricks arenes as negative compounds. As the positive system, a quaternary ammonium salt, a high molecular compound having the quaternary ammonium salt in a side chain, a guanidine compound, an imidazole compound and the like are preferably used. The charge control agent is preferably used in an amount of 0.5 to 10 parts by mass based on 100 parts by mass of the resin. However, in the present invention 1, the addition of the charge control agent is not essential, and in the case of using the two-component developing method, the non-magnetic one-component blade coating developing method utilizing the triboelectric charging with the carrier is used. It is not always necessary to include a charge control agent in the toner by positively utilizing the triboelectric charging with the blade member and the sleeve member.

Examples of the polymerization initiator that can be used in the polymerization toner according to the present invention include 2,2′-azobis-
(2,4-dimethylvaleronitrile), 2,2′-azobisisobutyronitrile, 1,1′-azobis (cyclohexane-1-carbonitrile), 2,2′-azobis-4-methoxy-2, Azo or diazo polymerization initiators such as 4-dimethylvaleronitrile and azobisisobutyronitrile; peroxides such as benzoyl peroxide, methyl ethyl ketone peroxide, diisopropyl peroxycarbonate, cumene hydroperoxide, 2,4-dichlorobenzoyl peroxide and lauroyl peroxide; An oxide polymerization initiator is used. The amount of the polymerization initiator varies depending on the desired degree of polymerization, but is generally used in an amount of 0.5 to 20% by mass based on the monomer. The type of the polymerization initiator varies slightly depending on the polymerization method, but is used alone or in combination with reference to the 10-hour half-life temperature.

In order to control the degree of polymerization, a known crosslinking agent, chain transfer agent, polymerization inhibitor and the like can be further added and used.

In the polymerized toner according to the first aspect of the present invention, in particular, when suspension polymerization using a dispersant is used, the dispersant used is an inorganic compound such as tricalcium phosphate, magnesium phosphate, aluminum phosphate, or phosphoric acid. Zinc, calcium carbonate, magnesium carbonate, calcium hydroxide,
Examples include magnesium hydroxide, aluminum hydroxide, calcium metasilicate, calcium sulfate, barium sulfate, bentonite, silica, and alumina. As the organic compound, polyvinyl alcohol, gelatin, methylcellulose, methylhydroxypropylcellulose, ethylcellulose, sodium salts of carboxymethylcellulose, polyacrylic acid and its salts, starch and the like can be used by dispersing them in an aqueous phase. It is preferable to use 0.2 to 20 parts by mass of these stabilizers based on 100 parts by mass of the polymerizable monomer.

When an inorganic compound is used among these stabilizers, a commercially available one may be used as it is, but the inorganic compound may be formed in a dispersion medium in order to obtain fine particles. For example, in the case of tricalcium phosphate, an aqueous sodium phosphate solution and an aqueous calcium chloride solution may be mixed under high stirring.

Further, in order to finely disperse these stabilizers, 0.001 to 0.1% by mass per 100 parts by mass of the polymerizable monomer.
One part by weight of a surfactant may be used. This is to promote the expected action of the dispersion stabilizer, and specific examples thereof include sodium dodecylbenzene sulfate, sodium tetradecyl sulfate, sodium pentadecyl sulfate, sodium octyl sulfate, sodium oleate,
Examples include sodium laurate, potassium stearate, calcium oleate and the like.

In the method for producing the polymerized toner according to the first aspect of the present invention, the toner can be specifically produced by the following production method.

That is, a releasing agent comprising a low softening point substance, a colorant, a charge control agent, a polymerization initiator and other additives are added to the polymerizable monomer, and the mixture is uniformly dissolved by a homogenizer, an ultrasonic disperser or the like. Or, the polymerizable monomer composition was dispersed,
It is dispersed in an aqueous phase containing a dispersion stabilizer using a conventional stirrer, homomixer, homogenizer or the like. Preferably, the agitation speed and time are adjusted so that the monomer droplets have the desired size of the toner particles, and granulation is performed. Thereafter, by the action of the dispersion stabilizer, stirring may be performed to such an extent that the particle state is maintained and the particles are prevented from settling. The polymerization is preferably performed at a polymerization temperature of 40 ° C. or higher, generally 50 to 90 ° C. Further, the temperature may be raised in the latter half of the polymerization reaction, and further, in order to remove unreacted polymerizable monomers and by-products which cause odor at the time of fixing the toner, the second half of the reaction, or the end of the reaction. Later, a part of the aqueous medium may be distilled off. After completion of the reaction, the generated toner particles are collected by washing and filtration, and dried. The toner particles after drying are supplied to an image forming apparatus with an external additive such as a fluidizing agent added as necessary.

In the suspension polymerization method, it is usually preferable to use 300 to 3000 parts by mass of water as a dispersion medium with respect to 100 parts by mass of the monomer system.

The water content of the toner of the present invention 1 was measured as follows. A sample of 0.5 ± 0.1 g is measured by a trace moisture measuring device (AQ-6 Hiranuma Sangyo Co., Ltd.). Hydranal Aqualite RS was used as a titration reagent.
Heating of the sample is performed by connecting the AQ-6 with the interface through an automatic moisture vaporizer (SE-24 Hiranuma Sangyo Co., Ltd .;
0 ℃ setting, performed in N ₂ gas 0.25 l / min setting).

Further, the particle size distribution of the toner can be measured by various methods. In the present invention 1, the particle size distribution was measured using a Coulter counter.

As a measuring device, a Coulter counter TA-II type (manufactured by Coulter Inc.) is used, and an interface (manufactured by Nikkaki) for outputting a number average distribution and a volume average distribution, and a PC 9801 personal computer (NE)
C), and a 1% aqueous NaCl solution is prepared as the electrolyte using primary sodium chloride.

The measuring method is as follows.
In 150 ml, 0.1 to 5 ml of a surfactant, preferably an alkylbenzene sulfonate, is added as a dispersant, and 2 to 20 mg of a measurement sample is further added. The electrolytic solution in which the sample was suspended was subjected to a dispersion treatment for about 1 to 3 minutes with an ultrasonic disperser, and the Coulter Counter TA-II was used, and a 100 μm aperture was used as an aperture. The particle size distribution is measured and various values are determined therefrom.

The above is the production process of the polymerized toner. It is necessary to clean each production apparatus after completing the production of a series of the polymerized toner. Image forming devices such as copiers are available in a variety of lineups, from low-speed machines to high-speed machines, from inexpensive low-resolution machines to expensive but high-resolution machines, and analog and digital machines. It is necessary to prepare many types. Further, in recent years, full-color copying machines and printers have been promoted, and opportunities for producing color toners have been increasing. In the case of full color, it is necessary to prepare four color toners per model. For example, there are four colors of yellow toner, magenta toner, cyan toner and black toner.

As described above, in order to produce various types of toners corresponding to various types of image forming apparatuses and four types of color toners of each type corresponding to full color, an apparatus for producing a polymerization toner dedicated to each prescription is prepared. That is not economic. Therefore, it is common to manufacture several types of toners with one polymerization toner manufacturing apparatus.

However, if different types of toners are mixed in the polymerization toner manufacturing apparatus, the image characteristics may be adversely affected. In particular, the mixing of positive toner for positive development (used for analog machines) and negative toner for reversal development (used for digital machines) and the mixing of different color toners in full-color toner when using a negatively charged photoreceptor Reproducibility is impaired, causing serious defects.

Further, even in the case of continuous production of the same prescription, the accumulation of deposits in the apparatus increases due to the continuous production and the manufacturing conditions change, resulting in the production of defective products. If it is significant, the production itself may be difficult such as blockage of a pipeline.

As a means for extending the time of continuous production due to the accumulation of the deposits, a material or a surface treatment that is difficult to adhere to the adhered surface of the inside of the apparatus for producing the polymerized toner is often used. Specifically, glass lining, fluorine coating, etc. are performed, but these treatments only have the effect of delaying the initial adhesion and have no effect on the deposition phenomenon where the adhered substances adhere to each other, so it is a complete solution. I couldn't.

Accordingly, it is necessary to clean the apparatus for producing the polymerized toner, and in many cases, thorough cleaning is required to prevent the above-mentioned contamination. The deposits on the polymerized toner manufacturing apparatus are in a wet state because they contain liquid such as moisture or a polymerizable monomer, unlike the deposits on the pulverized toner manufacturing apparatus. It is difficult to suck a wet attached matter with a vacuum cleaner or the like, and even if it can be sucked, it will damage equipment such as a vacuum cleaner, so that suction cleaning is not suitable. In addition, as described above, the adhered surface of the polymerization toner manufacturing apparatus is often coated with glass lining, fluorine, or a coating, and sandblast or blast of a relatively high-pressure sublimable solid pellet is adhered. Not suitable as it will damage the surface. In addition, immersion or hand wiping with a solvent is a reliable method with a high cleaning effect,
This method was not preferable because of problems in terms of safety and health of workers and disposal of waste liquid.

Therefore, it is suitable to remove the deposits by colliding sublimable solids at a relatively low pressure for washing the deposits in the apparatus for producing a polymerized toner. Any sublimable solid pellets that can be used at this time may be used as long as they sublimate at room temperature. However, if the density is not sufficient, sufficient kinetic energy cannot be obtained, so that effective washing cannot be performed. Those having a density at −79 ° C. of 1.3 g / cm ³ or more, especially 1.5
g / cm ³ or more is desirable. For example, dry ice or the like is easily available and suitable.

As described above, since the present invention 1 is suitable for cleaning the attached matter in a wet state, a liquid substance reaction vessel such as a mixing vessel, a granulation vessel, a reaction vessel, a distillation vessel and the like, and a space between these vessels. It is particularly effective for cleaning the connecting pipe.

The shape of the sublimable solid pellet used as a cleaning agent in the present invention 1 is not particularly limited. For example, the shape may be a sphere, a column, a cuboid, or a block. And the like obtained by cutting and pulverizing a sublimable solid such as.

The particle size of the sublimable solid pellets is not particularly limited, and can be appropriately selected according to the type and size of the adhered substance, the type and size of the apparatus for producing the polymerized toner, and the like. . Preferably, it is 0.1 to 10 mm, more preferably 0.5 to 5 mm. From the viewpoint of preventing sublimable solid pellets from sublimating during transportation,
The sublimable solid pellets preferably have a particle size of 0.1 mm or more. On the other hand, the particle diameter of the sublimable solid pellets is preferably 10 mm or less from the viewpoint of preventing the washing performance per unit mass of the sublimable solid pellets from decreasing. When a certain mass of the sublimable solid pellets is jetted, as the particle size increases, the ratio of the area of the sublimable solid pellets colliding with the surface to be cleaned (the area to be cleaned per unit mass of the sublimable solid pellets) decreases, In addition, since the tip of the sublimable solid pellet collides with and causes the attached matter to peel off, the remaining portion is not involved in the detachment of the attached matter, so that the proportion of the sublimable solid pellet that does not directly collide with the attached matter increases. Also,
By using small sublimable solid pellets having a particle size of 10 mm or less, it is possible to effectively clean even very fine parts that are difficult to wash by hand.

The injection amount of the sublimable solid pellet group is not particularly limited, and is appropriately set depending on the type and size of the attached matter. For example, when the injection is performed using a nozzle, the injection amount is 10 per nozzle. -100 kg / Hr is preferable, and 20-90 kg / Hr is particularly preferable. 10 kg / Hr or more is preferable from the viewpoint of detergency, and 100 kg / Hr or less is preferable from the viewpoint of economy.

The compressed gas for spraying the sublimable solid pellets is not particularly limited, but includes, for example, gas such as air and nitrogen.

The pressure of the compressed gas is preferably from 100 to 300 kPa in terms of relative pressure when the surface to be cleaned of the apparatus for producing a polymerized toner is protected by glass lining, fluorine coating or the like. At less than 100 kPa, there is no cleaning effect,
If the pressure exceeds 0 kPa, the surface to be cleaned is damaged.

The case where the surface to be cleaned is a metal surface without protection is not limited to this, and the pressure of the compressed gas is not particularly limited. The pressure is appropriately set depending on the type, size, and the like. For example, when a nozzle is used, the pressure is preferably 100 to 1000 kPa from the viewpoint of impact force and economy.

The air volume is not particularly limited, and is appropriately set depending on the type of the adhered substance, the mode of the adhered substance, and the type and size of the apparatus for producing the polymerized toner.
8.0 m ³ / min. The method of spraying the sublimable solid pellets is not particularly limited as long as the sublimable solid pellets are directly sprayed on the surface to be cleaned by the compressed gas. A method of spraying a group may be used.
The shape of the nozzle is not particularly limited, and can be appropriately selected and used according to the surface to be cleaned. For example, there are circular and polygonal cross sections.

The nozzle diameter of the nozzle is not particularly limited, and can be appropriately selected depending on the size and shape of the surface to be cleaned. Preferably it is 5 to 30 mm, more preferably 5 to 20 mm. A nozzle having a nozzle diameter of 5 mm or more is preferable from the viewpoint of preventing the nozzle from being clogged by the sublimable solid pellets and reducing the pressure loss at the time of injection. On the other hand, the nozzle diameter is preferably 30 mm or less from the viewpoint of preventing a decrease in the cleaning power due to a decrease in the linear velocity of the sublimable solid pellet flow and a decrease in kinetic energy. The number of nozzles is not particularly limited, and one or more nozzles can be set arbitrarily.

The apparatus for injecting the sublimable solid pellets is not particularly limited, but is preferably a structure capable of guiding the sublimable solid pellets to the surface to be cleaned and capable of adjusting the gas pressure, air volume and the like. For example, there is an apparatus schematically shown in FIG. 1 or FIG.

A hopper 1 for storing sublimable solid pellets shown in FIG. 1 is provided with a supply valve (for example, a rotary valve) 2 below the hopper 1.
Sublimable solid pellets are supplied into the gas pressurized by the compressor 3 and the like, and are injected from the hose 4 and the nozzle 5. Further, as shown in FIG. 2, the gas pressurized by the compressor 9 is jetted by the compressed gas supply hose 8 and the nozzle 10, and the suction force generated by the sublimation solid pellet transfer hose 7 and the hopper 6 through the suction nozzle 11. The sublimable solid pellets inside are sucked and injected from the nozzle 10 together with the compressed gas.

The sublimable solid pellets sprayed in this way are directly sprayed on the surface to be cleaned by directing the nozzle toward the surface to be cleaned, and are guided to the position where the deposits are attached.

The attached matter is the impact due to the collision of the sublimable solid pellets at a high pressure, the impact of the high pressure gas for injecting the sublimable solid pellets, and the rapid volume due to the sublimation of the collided sublimable solid pellets. Due to the expansion, it is removed from the surface to be cleaned. Due to the difference in the coefficient of thermal expansion between the surface to be cleaned and the adhered substance, which is formed when cooled rapidly by the sprayed sublimable solid pellets, the adhered substance is easily peeled off from the surface to be cleaned, and the adhered substance is easily removed. It is removed from the surface to be cleaned. By such a washing action by the sublimable solid pellets, the deposits can be efficiently removed.

The time required for cleaning depends on the kind of the adhered substance, the manner of the adhered substance, the presence / absence of surface treatment of the surface to be cleaned, the desired degree of cleanliness of the surface to be cleaned, and the like, and is not particularly limited.
At the time of cleaning, the polymerization toner manufacturing apparatus may be in an operating state or a stopped state. When washing in a stopped state, the apparatus may be disassembled and sprayed with sublimable solid pellets, or may be sprayed while the apparatus is assembled.

In any case, the cleaning device and the production device for the polymerized toner may be independent or integrated. However, in order to improve workability, especially when cleaning is performed during operation, the cleaning device and the production device must be integrated. Is preferred. FIG. 3 shows an example of a case where the production device for the polymerized toner and the cleaning device are integrated. FIG.
Medium, polymerizable monomer, colorant, charge control agent, polar resin,
A mixing container 12 and a mixing stirrer 13 in which a release agent and the like are dissolved and dispersed and a polymerization initiator is added to form a polymerizable monomer composition; ion-exchanged water and a dispersant such as sodium phosphate and calcium chloride in advance A granulating container 14 and a granulating stirrer 15 for granulating the polymerizable monomer composition by charging the polymerizable monomer prepared above to prepare an aqueous medium obtained by stirring A reaction vessel 16 and a reaction stirrer 17 for performing a polymerization reaction by stirring the polymerizable monomer composition after completion of the above with a paddle stirring blade or the like; a distillation vessel 18 capable of depressurizing to distill off residual monomers and the like if necessary; A stirrer 19 is shown. The pressure in the reaction vessel can be reduced, the remaining monomers and the like are distilled off in the reaction vessel, and the distillation vessel 18 and the distillation stirrer 19 may be omitted.

FIG. 1 or FIG. 2 is attached to each container used in the apparatus for producing a polymerized toner as described above, and to a pipe portion connecting the containers.
It is possible to integrally mount a cleaning device as shown by. In FIG. 3, typically, a washing device as shown in FIG.
Although the washing apparatus as shown in FIG. 2 is integrated with the distillation vessel 6 and the distillation vessel 18, the present invention is not limited to the combination shown in FIG. 3, but can be applied to all vessels and piping sections. Can be implemented.

The sublimable solid pellets used for cleaning the apparatus for producing a polymerized toner are sublimed and released as a gas into the atmosphere, so that there is no need to collect them. Further, the sublimable solid pellets as a cleaning agent are softer than metal, and do not damage the surface to be cleaned when the surface to be cleaned is metal. In the present invention 1, in order to spray the sublimable solid pellets directly on the surface to be cleaned to which the adhered substance is adhered by a guiding means such as a nozzle,
Even when the surface to be cleaned is hot, there is no need to cool the equipment,
Energy for cooling is not required, and there is no cooling waiting time, so that the operation time of the apparatus is increased.

Since the cleaning time is greatly reduced by the above effects, the operation rate of the apparatus is increased, and the productivity is improved.
Furthermore, since no organic solvent is used, safety is high in terms of hygiene.

(II) Next, the present invention 2 will be described in detail. The present inventors have conducted intensive studies and polymerized a polymerizable monomer composition containing at least a polymerizable monomer and a colorant in an aqueous dispersion medium to produce colored polymer particles. Thereafter, washing and dehydration are performed, and the obtained weight average diameter is 3 to 10 μm.
m, the coefficient of variation A of the number distribution is less than 40%, and the wet colored polymer particles having a water content of preferably 40% or less are dispersed while being continuously supplied into hot air particles, and a wind classifier is more preferable. Can perform the drying process and the classification process at the same time by performing continuous classification using a wind-type classifier equipped with adjustable movable parts. It has been found that the process can be shortened without lowering the performance of.

Further, since the classification point can be adjusted by adjusting the movable portion provided in the classifier itself, in the process of sending the wet colored polymer particles before classification in a co-current with a hot air flow,
In other words, in the process of affecting the removal of water from the wet colored polymer particles, the necessity of adjusting and changing the flow rate, flow rate, and the like is reduced, the toner particles having a stable water content, and having a predetermined particle size range. Can be provided.

Hereinafter, the present invention 2 will be described in more detail.

In the method for producing a toner according to the second aspect of the present invention,
In order to increase the drying efficiency when the wet colored polymer particles are sent in parallel with the hot air flow, make sure that the particles are single particles as much as possible during classification, that is, to increase the classification rate. It is preferable that the crushing is performed.

In the method for producing a toner according to the second aspect of the present invention,
After polymerizing the polymerizable monomer composition to produce colored polymer particles, washing, dehydrating the obtained colored polymer particles,
The obtained wet-colored polymer particles are used as a raw material. When the wet-colored polymer particles are used as a raw material, such wet-colored polymer particles have a water content of 40% or less from the viewpoint of fluidity as a powder. Preferably, there is. Further, it is more preferably at most 30%. The `` moisture content '' here refers to the moisture content based on moisture content, that is, the ratio of the water mass to the total mass (sum of the dry toner mass and the water mass),
It was determined by a weight loss method at 105 ° C.

The toner particles having such a water content are as follows:
Although it can be easily obtained by ordinary solid-liquid separation means (for example, filtration), preliminary drying may be performed to obtain such a water content.

In the present invention, an example of an apparatus for dispersing such a raw material (wet particles) in a powder stream in a hot air stream and classifying the raw material (wet particles) while maintaining the dispersed state while sending it in parallel with the high-speed hot air stream. For example, there is an apparatus in which a classifier is installed after a loop-type pipe (drying pipe) as shown in FIG. 4, but the apparatus is not particularly limited.

In the system shown in FIG. 4 for simultaneously performing drying and classification, first, compressed air heated to a predetermined temperature in a hot air generator 42 is discharged at a supersonic speed in an air flow dispersing unit 43.
The raw material supplied from the raw material supply device 46 is dispersed and dried instantaneously (0.5 to several tens of seconds) in the loop type pipe 44. By setting the airflow outlet 45 inside the loop-type airflow drying tube, the particles in the aggregated state and those dispersed and close to a single particle are easily classified by the Coanda effect, and the airflow outlet 45 is converted into a single particle. Those in a close state are classified into a predetermined particle size distribution by the classification part A while maintaining the dispersion state as it is.

In the classifying section A, it is preferable to use a classifier using wind power, preferably a wind classifier having an adjustable movable part. Specifically, as an example, FIG.
It is more preferable to use a classifier of the embodiment shown in FIGS.

The classifier shown in FIG. 5 is a device for classifying fine particles and coarse particles by using a difference in inertial force. First, particles sent while maintaining a state of being dispersed in a cocurrent with a hot air flow are It enters from the supply port 50, turns the guide cone 51 to a stable concentration state, the fine powder passes through the classification zone 52 according to the air flow, and is discharged out of the apparatus through the exhaust port 54, and the coarse powder is classified according to the inertia force and classified into the classification cone 53. , And is guided to the coarse powder discharge port 56.

The classifying cone 53 can be adjusted vertically, that is, the classifying point can be moved by adjusting the distance from the guide cone.

Also, by taking in secondary air from 55, it is possible to increase the dispersing power in the classification zone and increase the classification efficiency.

Further, just before entering the supply port, it is also possible to supply new air to the apparatus by further introducing air to increase the dispersion.

If the main purpose is to cut coarse powder, the powder collected through a cyclone or the like through the exhaust port is collected and collected.
If the main purpose is to use and cut the fine powder, it is possible to select the collecting position according to the purpose so as to collect and use the powder discharged from the coarse powder outlet.

The classifier shown in FIG. 6 is a device that performs classification by balancing centrifugal force due to rotation of the rotor 58 and suction force from a fan.

First, the particles sent from the supply port 57 while maintaining the state of being dispersed in the co-current with the hot air flow are classified by the rotor 58 under the action of the centrifugal force and the suction force from the blower.

Since the fine powder is more strongly affected by the suction force than the centrifugal force, the fine powder passes through the inside of the rotor together with the airflow, and is discharged from the airflow delivery pipe 59 to the outside of the apparatus.

On the other hand, the coarse powder is more strongly affected by the centrifugal force than the suction force, and is guided from the coarse powder discharge port 61 to the outlet through the inner wall of the apparatus.

The rotation speed of the rotor 58 can be adjusted. By adjusting the rotation speed, the centrifugal force and the suction force are balanced, and the classification point is moved.

Also, as with the apparatus shown in FIG. 5, by taking in secondary air from the secondary air intake 60, it is possible to increase the dispersion force in the apparatus and increase the classification efficiency.
Immediately before entering the supply port, it is also possible to introduce new air so as to further increase the dispersion and feed it into the apparatus.

Further, as in FIG. 5, if the main purpose is to cut coarse powder, if the main purpose is to collect and use the powder that has exited the air flow delivery pipe 59 and collected by a cyclone, etc. , Collecting the powder discharged from the coarse powder discharge port 61
It is possible to select the target particles according to the position to be collected so as to be used.

In the second embodiment of the present invention, there is a possibility that the apparatus alone shown in FIGS. 5 and 6 may be limited to only coarse powder cutting or fine powder cutting. Therefore, the same classifiers shown in FIGS. Alternatively, it is also possible to combine different classifiers, connect them in series, cut fine powder and coarse powder at the same time, and completely omit the classification, which is a process separated in the subsequent process.

The classifier used in the present invention is, specifically, a Micron classifier (manufactured by Seishin Enterprise Co., Ltd.), a DS classifier (manufactured by Nippon Pneumatic Co., Ltd.), a micron separator (manufactured by Hosokawa Micron Corporation), D-plex. A classifier (manufactured by Hosokawa Micron Corporation) may be used, but the present invention is not limited thereto.

Next, in order to faithfully develop finer latent image dots for higher image quality, the toner used in the present invention 2 has a finer particle diameter, specifically, measured with a Coulter counter. Weight average diameter of 3 to 10 μm
Is most preferred as the toner used in the present invention. In the case of a toner having a weight average diameter of less than 3 μm, the cohesive force becomes too strong, so that the number of particles that do not disperse even in a high-speed hot air flow increases, and not only the drying efficiency is reduced, but also the classification ability in the classification section is significantly reduced. . Further, due to poor transfer efficiency, a large amount of untransferred toner is generated on the photoreceptor or the intermediate transfer member, which causes non-uniform unevenness of an image due to fog and poor transfer, which is not preferable as the toner used in the present invention 2. On the other hand, when the weight average diameter of the toner exceeds 10 μm, fusion to members tends to occur, and as a result,
Image characteristics are degraded.

In addition to the necessity of the particle size distribution, in addition to the number average diameter, the spread of the particle size distribution greatly contributes to image reproducibility particularly in the transfer process. When the above coefficient of variation is more than 40%, development is performed well even if the particle size is in the range of 3 to 10 μm, but halftone reproduction is particularly caused by scattering at the time of transfer and the presence of untransferred toner. Sexuality is reduced. If the coefficient of variation exceeds 40%, not only does the load at the classification portion increase, but also, especially when there are many particles on the coarse powder side, the classification yield is significantly reduced.

In the production method of the present invention 2, a polymerized toner obtained by polymerizing a polymerizable monomer is used as a raw material. The constituent materials (polymerizable monomer, release agent, colorant, charge control agent, polymerization initiator, and the like) of the polymerization toner, polymerization method and polymerization conditions are the same as those of the first embodiment of the present invention.

The water content of the toner of the present invention 2 was measured by a MA40 electronic moisture meter (manufactured by Sartorius).
Determined by the weight loss method at ℃.

[0110]

Hereinafter, the present invention will be described in more detail with reference to specific production methods, but the present invention is not limited thereto.

(I) Invention 1: <Example 1> 15.0 parts by mass of ion-exchanged water and 0.1 M-Na ₃ were placed in a granulation vessel having a jacket for temperature control.
After charging 14.4 parts by mass of PO ₄ and heating to 60 ° C.,
The mixture was stirred at 5000 rpm using a Claremix stirrer (manufactured by M Technique). 1.0M-C
2.18 parts by mass of aCl ₂ aqueous solution was added, and Ca ₃ (P
An aqueous medium containing O ₄ ) ₂ was obtained. On the other hand, (monomer)-5.28 parts by mass of styrene-1.12 parts by mass of n-butyl acrylate (colorant)-C.I. I. Pigment Blue 15: 3 0.5 parts by mass (charge control agent) ・ Metal salicylate compound 0.08 parts by mass (polar resin) ・ Saturated polyester 0.3 parts by mass (acid value 10 mgKOH / g, peak molecular weight: 7500) 1.0 part by mass of ester wax (melting point 70 ° C.) The above-mentioned materials are put into a mixing vessel (with a stirrer) having a jacket for temperature control, heated to 60 ° C., and uniformly dissolved.
Dispersed. The mixing container was made of metal, and the surface to be cleaned was not subjected to surface treatment. In addition, polymerization initiator 2,
2'-azobis (2,4-dimethylvaleronitrile)
0.3 parts by mass was dissolved to prepare a polymerizable monomer composition.

The above-mentioned polymerizable monomer composition was put into the above-mentioned aqueous medium, and the mixture was stirred at 60 ° C. under an N ₂ atmosphere at 5000 rpm (the peripheral speed of the tip of the blade: 2).
(4.9 m / s), and the polymerizable monomer composition was granulated. Thereafter, the polymerizable monomer composition after the granulation was transferred to a reaction vessel having a jacket for temperature control, and stirred with a paddle stirring blade. The reaction vessel is made of metal,
No surface treatment was performed on the surface to be cleaned. The reaction was carried out for 5 hours while adjusting the liquid temperature to 60 ° C. while stirring with a paddle stirring blade. Thereafter, the liquid temperature was raised to 80 ° C.,
The polymerization reaction was carried out for an hour.

After completion of the polymerization reaction, residual monomers were distilled off under reduced pressure. After cooling, hydrochloric acid was added to dissolve calcium phosphate, followed by filtration and washing with water to obtain wet colored particles A. The water content of the wet colored particles A is 30%, and the styrene content is 50%.
It was 0 ppm. The water content was measured by Karl Fischer titration, and the styrene content was measured by gas chromatography.

The wet colored particles A are charged into a fluidized bed drier,
Drying was performed. The drying time was 3 hours, and when the water content and the styrene content were measured, the water content was 0.1% and the styrene content was 100 ppm. When the particle size distribution of the obtained dry toner was measured by a Coulter counter, the weight average particle size was 6.5 μm, and the coefficient of variation was 30%.

The trial operation of the toner was completed as described above, and two workers performed disassembly and cleaning operations of the apparatus for producing the polymerized toner used in the trial production, that is, the granulating container, the mixing container, and the reaction container.

In the cleaning method, dry ice was sprayed on the surface to be cleaned using compressed air of 300 kPa. The cleaning property was good, there was no damage on the adhered surface, and the cleaning operation was completed in 6 hours.

<Comparative Example 1> Using the same apparatus for producing a polymerized toner as in Example 1, a polymerized toner similar to that of Example 1 was experimentally produced.

The washing was performed using an organic solvent. Parts with complex shapes are removed and immersed. Deposits were removed. Although the cleaning performance was good, the cleaning operation required 18 hours with the addition of 2 hours waiting for cooling, and the productivity was greatly reduced.

<Example 2> Using the same apparatus for producing a polymerized toner as in Example 1, a polymerized toner similar to that of Example 1 was experimentally produced.

The same cleaning method as in Example 1 was adopted except that the pressure of the compressed air used was 400 kPa. The cleaning performance was better than that of Example 1, and the cleaning operation was completed in 5 hours. However, since a part of the wet state scattered around and it took 1 hour for cleaning, the total cleaning time was less than that of Example 1. Same as 1.

Example 3 A polymerized toner similar to that of Example 1 was experimentally produced using the same apparatus for producing a polymerized toner as in Example 1 except that the surface to be cleaned of the mixing container was coated with fluorine.

When the cleaning conditions were set to 300 kPa, which is the same as in Example 1, the cleaning performance was better than that of Example 1, and the cleaning operation was completed in 5 hours and 30 minutes, and there was no damage on the fluorine-coated surface.

Reference Example 1 Using the same polymerization toner production apparatus as in Example 3, a polymerization toner similar to that of Example 3 was produced. The same cleaning method as in Example 3 was adopted except that the pressure of the compressed air used was 400 kPa.

The cleaning performance was better than that of Example 3. The cleaning operation was completed in 4 hours and 30 minutes, but a part of the fluorine-coated surface was damaged.

<Example 4> A polymerized toner similar to that of Example 1 was experimentally produced using the same apparatus for producing a polymerized toner as in Example 1 except that the surface to be cleaned of the reaction vessel was provided with glass lining.

When the cleaning conditions were set to 300 kPa, which is the same as in Example 1, the cleaning performance was better than that in Example 1, the cleaning operation was completed in 5 hours, and there was no damage on the glass lining surface.

Reference Example 2 Using the same polymerization toner production apparatus as in Example 4, a polymerization toner similar to that in Example 4 was produced. The same cleaning method as in Example 4 was adopted except that the pressure of the used compressed air was 1000 kPa.

The cleaning performance was better than that of Example 4. The cleaning operation was completed in 3 hours, but a part of the glass lining surface was damaged.

(II) Invention 2: <Example 5> 0.1 mol /
The mixture was charged with 450 parts by mass of an aqueous solution of Na ₃ PO ₄ littor and charged with 60 parts by weight.
After warming to ° C, the mixture was stirred at 3500 rpm using CLEARMIX (manufactured by M Technique Co., Ltd.). To this, 68 parts by mass of a 1.0 mol / liter CaCl ₂ aqueous solution was added to obtain an aqueous medium containing Ca ₃ (PO ₄ ) ₂ .

On the other hand, the dispersoid system includes: 162 parts by mass of styrene monomer; 38 parts by mass of n-butyl acrylate; I. Pigment Red 122 10 parts by mass-Saturated polyester 20 parts by mass-Metal salicylate compound 3 parts by mass-Paraffin wax 25 parts by mass. I. Pigment Red 122, 100 parts by mass of a metal salicylate compound and a styrene monomer are dispersed for 3 hours using an attritor (manufactured by Mitsui Miike Kakoki Co., Ltd.)
A colorant dispersion was obtained. Next, the rest of the above formulation was added to the colorant dispersion, heated to 60 ° C., and dissolved and mixed for 30 minutes. Into this, 10 parts by mass of 2,2′-azobis (2,4-dimethylvaleronitrile) as a polymerization initiator was dissolved to prepare a polymerizable monomer composition.

The above polymerizable monomer composition was charged into the aqueous dispersion medium and granulated for 15 minutes while maintaining the rotation speed. Then, the stirrer was changed from a high-speed stirrer to a propeller stirring blade, the internal temperature was raised to 80 ° C., and polymerization was performed at 50 revolutions / minute.
Continued for hours. Next, the internal temperature is 80 ° C. and the internal pressure of the apparatus is 47.
The distillation was performed for 4 hours under the condition of 3 kPa. After polymerization,
Cool the slurry, add dilute hydrochloric acid and add Ca ₃ (PO ₄ ) ₂
Was dissolved, filtered, washed with water, and then crushed to obtain wet colored polymer particles having a water content of 25%.

At this point, the weight-average particle diameter of the wet colored polymer particles was 7.8 μm, 25% by number of particles having a particle diameter of 4 μm or less, and the coefficient of variation was 35%.

The obtained wet-colored polymer particles were obtained by using FIG.
(The classifier A uses a classifier shown in FIG. 5). The operating conditions were as follows: air at 80 ° C. was blown at 600 m ³ / hr, and the wet colored polymer particles
It was fed continuously at 0 kg / hr to dry and remove fines.

After completion of the operation, the water content of the toner particles was 0.3
%, The weight average particle diameter was 8.2 μm, the number of particles having a particle diameter of 4 μm or less was 12% by number, and the variation coefficient was 25%. The yield of the toner particles after the operation was 93%.

<Example 6> Except that the classifying unit uses a classifier shown in Fig. 6, the same wet colored polymer particles as in Example 5 were charged into the apparatus under the same operating conditions as those in Example 5, and drying and fine powder were removed.

After completion of the operation, the water content of the toner particles was 0.2
%, The weight average particle diameter was 8.05 μm, particles having a particle diameter of 4 μm or less were 13% by number, and the variation coefficient was 24%. Also,
The yield of the toner particles after the operation was 92%.

Example 7 A wet colored polymer particle after washing, dehydration and crushing had a water content of 8%, and the wet colored polymer particle was continuously supplied at 50 kg / hr.
The same wet colored polymer particles and the same operating conditions as in Example 5 were charged into the same apparatus as in Example 5 to dry and remove fine powder.

At the end of the operation, the toner particles had a water content of 0.2%, a weight average particle size of 8.25 μm, and a particle size of 4 μm.
The following particles were 13% by number, and the coefficient of variation was 23%.
Further, the yield of the toner particles after the operation was 92%.

Example 8 The water content of the wet-colored polymer particles after washing, dehydration and crushing was 45%, and the wet-colored polymer particles were continuously supplied at a rate of 17 kg / hr. Except for the supply, the same wet colored polymer particles as in Example 5 were introduced into the same apparatus as in Example 5 under the same operating conditions as in Example 5 to dry and remove fine powder.

At the end of the operation, the water content of the toner particles was 0.3%, the weight average particle size was 8.0 μm, and the particle size was 4%.
The number of particles having a particle size of μm or less was 14% by number, and the coefficient of variation was 25%. The yield of the toner particles after the operation was 90%.

<Comparative Example 2> The wet colored polymer particles obtained in the same manner as in Example 5 until washing, dehydration and crushing were mixed with a continuous instantaneous flash dryer (flash dryer FJD-4:
(Manufactured by Seishin Enterprise Co., Ltd.). As operating conditions, air at 80 ° C. was blown at 600 m ³ / hr,
The wet colored polymer particles were continuously supplied at a rate of 30 kg / hr and dried. At this point, the water content of the toner particles was 0.3%.

Thereafter, the steps were separated and classified using a micron separator (manufactured by Hosokawa Micron Corporation). At the end of the classification, the weight average particle size of the toner particles was 7.9 μm, the number of particles having a particle size of 4 μm or less was 20% by number, and the variation coefficient was 32%. Further, the yield of the classified toner particles was 80%.

The separation of the drying and classification steps not only complicates the steps but also reduces the yield of toner particles.

<Comparative Example 3> The wet colored polymer particles after washing, dehydration and crushing had a water content of 25% and a weight average particle size of 8.1.
The wet colored polymer particles obtained in the same manner as in Example 5 were operated under the same operating conditions as in Example 5, except that 50% by number of particles having a particle size of 4 μm or less and a coefficient of variation of 55%. The mixture was placed in the same apparatus as in Example 5, and dried and fine powder was removed.

At the end of the operation, the water content of the toner particles was 0.4%, the weight average particle size was 8.6 μm, and the particle size was 4 μm.
The following particles were 38 number%, and the coefficient of variation was 46%.
The yield of the toner particles after the operation was 78%.

Since the coefficient of variation was large, the yield of toner particles was significantly reduced.

[0147]

As described above, according to the first aspect of the present invention, the cleaning time of the apparatus for producing a polymerized toner is greatly reduced, and cooling of the apparatus for producing a polymerized toner is not required.
The operation rate of the device is greatly increased, and the productivity is improved. Further, low labor and low cost are realized. Further, it is not necessary to provide a post-process such as collecting sublimable solid pellets of the cleaning agent.

According to the second aspect of the present invention, the production process of the toner by the polymerization method is shortened, and at the same time, the continuous processes of drying and classification are performed efficiently so as not to lower the performance of the toner particles, thereby saving energy and improving production efficiency. It is possible to provide a method for producing a toner which realizes improvement in production and reduction in production cost.

[Brief description of the drawings]

FIG. 1 is a view schematically showing an apparatus for injecting a sublimable solid pellet group, which is preferably used in the cleaning method of the present invention 1. FIG.

FIG. 2 is a diagram schematically showing an apparatus for injecting a sublimable solid pellet group, which is preferably used in the cleaning method of the present invention 1.

FIG. 3 is a diagram illustrating an example of a case where a polymer toner production apparatus and a cleaning apparatus are preferably used in the cleaning method of the first embodiment of the present invention;

FIG. 4 shows a state in which the wet colored polymer particles obtained by the polymerization method used in the present invention 2 are dispersed while being continuously supplied into a hot air stream, and are kept in a dispersed state while being sent in parallel with the hot air stream. This is an example of a system for continuously performing classification.

FIG. 5 is an example of a classifier and a classification system used in a classification section A of FIG. 4;

FIG. 6 is an example of a classifier and a classification system used in a classification section A of FIG.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Hopper 2 Valve 3 Compressor 4 Hose 5 Nozzle 6 Hopper 7 Sublimation solid pellet conveyance hose 8 Compressed gas supply hose 9 Compressor 10 Nozzle 11 Suction nozzle 12 Mixing container 13 Mixing stirrer 14 Granulating container 15 Granulating stirrer 16 Reaction container 17 Reaction Stirrer 18 Distillation Vessel 19 Distilling Stirrer 41 Discharge Blower 42 Airflow Heating Device 43 Airflow Dispersion Unit 44 Airflow Drying Tube 45 Airflow Extraction Unit 46 Sample Supply Device 47 Cyclone 48 Bag Filter 49 Discharge Blower 50 Supply Port (Sample + Hot Airflow) ) 51 Guide cone 52 Classification zone 53 Classification cone 54 Exhaust port 55 Secondary air intake 56 Coarse powder (or product) discharge 57 Supply port 58 Rotor 59 Air flow delivery pipe 60 Secondary air intake 61 Coarse powder (or product) Outlet 62 B Motor shaft 63 motor

Continuation of the front page (72) Inventor Hitoshi Kanda 3-30-2 Shimomaruko, Ota-ku, Tokyo Inside Canon Inc. (72) Inventor Yoshinori Tsuji 3-30-2 Shimomaruko, Ota-ku, Tokyo Inside Canon Inc. F term (reference) 2H005 AB03 AB06 EA05 3B116 AA47 BB21 BB88

Claims (17)

[Claims] 1. Production of a polymerized toner having colored polymer particles obtained by polymerizing a polymerizable monomer composition containing at least a polymerizable monomer and a colorant in the presence of a polymerization initiator. A cleaning method for a toner manufacturing apparatus, wherein a sublimable solid pellet is collided at a high speed in an apparatus to remove an adhered substance on a surface to be cleaned of the manufacturing apparatus. 2. The method according to claim 1, wherein the sublimable solid is dry ice. 3. The method for cleaning a toner manufacturing apparatus according to claim 1, wherein the surface to be cleaned is a glass lining. 4. The method for cleaning a toner manufacturing apparatus according to claim 1, wherein the surface to be cleaned is a fluorine coat. 5. The cleaning method for a toner manufacturing apparatus according to claim 1, wherein the means for causing the sublimable solid pellets to collide with the surface to be cleaned at a high speed is spraying with a compressed gas. 6. The method according to claim 5, wherein the pressure of the compressed gas is 100 to 300 kPa in relative pressure. 7. The method for cleaning a toner production apparatus according to claim 1, wherein the method for producing the polymerized toner produced by the toner production apparatus is a suspension polymerization method. 8. Production of a polymerized toner having colored polymer particles obtained by polymerizing a polymerizable monomer composition containing at least a polymerizable monomer and a colorant in the presence of a polymerization initiator. An apparatus for producing a toner, characterized in that the apparatus is provided with a cleaning device for colliding sublimable solid pellets at high speed to remove deposits on a surface to be cleaned of the production device. 9. The apparatus according to claim 8, wherein the sublimable solid is dry ice. 10. The apparatus for producing a toner according to claim 8, wherein the surface to be cleaned is a glass lining. 11. The apparatus according to claim 8, wherein the surface to be cleaned is a fluorine coat. 12. The apparatus according to claim 8, wherein the means for causing the sublimable solid pellets to collide with the surface to be cleaned at a high speed is spraying with a compressed gas. 13. The toner manufacturing apparatus according to claim 12, wherein the pressure of the compressed gas is 100 to 300 kPa in relative pressure. 14. The apparatus for producing a toner according to claim 8, wherein the method for producing the polymerized toner produced by the toner production apparatus is a suspension polymerization method. 15. A polymerizable monomer composition containing at least a polymerizable monomer and a colorant is polymerized in an aqueous dispersion medium to produce colored polymer particles, which are then washed and dehydrated. ,
A weight average diameter of 3 to 10 [mu] m, variation in number distribution represented by the following formula Factor _{A A = S n / D 1} × 100 ( where, S _n is the standard deviation of the number distribution, D ₁ is an average particle diameter number) is Wet colored polymer particles having a particle size of less than 40% are obtained, dispersed in a hot air stream while continuously supplying the particles, and continuously classified while maintaining a dispersed state while being sent in parallel with the hot air stream. A method for producing a toner. 16. The method for producing a toner according to claim 15, wherein the classification uses an air classifier. 17. The method according to claim 15, wherein the water content of the wet colored polymer particles after washing and dehydration is 40% or less.
Or a method for producing a toner according to item 16.