JPH0534971A - Production of electrostatic latent image developing toner - Google Patents

Abstract

PURPOSE:To easily produce an electrostatic latent image developing toner without its composition being fluctuated and excellent in charge stability and flowability by fixing the surface-treating fine particles or forming a film of the particles on the surface of a toner core grain consisting essentially of resin. CONSTITUTION:A rotary member 20 provided in a treating chamber 10 is rotated, the toner core grain consisting essentially of resin and surface-treating fine particles are mixed in the chamber 10 by a high-speed air current to uniformly disperse and deposit the particles on the surface of the toner core grain, and then the mixing is accelerated to fix the particles or form a film of the particles on the surface of the toner core grain.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an electrostatic latent image developing toner used for developing an electrostatic latent image in an image forming apparatus such as a copying machine or a printer, and more particularly to a resin. The present invention relates to a method for producing a toner for electrostatic latent image development, in which fine particles for surface treatment are fixed and / or film-formed on the surface of toner core particles as a component.

[0002]

2. Description of the Related Art Conventionally, in image forming apparatuses such as copying machines and printers, various toners have been used as developers for developing electrostatic latent images formed on photoconductors.

In recent years, in the image forming apparatus as described above, there is a demand for higher quality images to be formed, and accordingly, as the toner used for development, toner having a small particle size is used. It came to be considered.

Here, when manufacturing a toner having such a small particle diameter, it is difficult to uniformly disperse additives such as a charge control agent in the toner, and therefore the charge stability of the obtained toner is improved. However, there is a problem that the formed image is fogged or the toner is scattered and the inside of the image forming apparatus is soiled with the toner.

For this reason, in recent years, Japanese Patent Laid-Open No. 63-
As disclosed in Japanese Patent No. 85756 and Japanese Patent Laid-Open No. 63-244056, fine particles for surface treatment such as a coloring agent and a charge control agent are mainly used for impact force on the surface of toner core particles containing a resin as a main component. Immobilization or film formation using mechanical and thermal energy has been studied.

Here, when the fine particles for surface treatment such as the coloring agent and the charge control agent are fixed or formed into a film on the surface of the toner core particles as described above, the fine particles for surface treatment are directly subjected to an impact force. When the particles are fixed or formed into a film on the surface of the toner core particles by the main mechanical and thermal energy, the fine particles for surface treatment are not sufficiently dispersed on the surface of the toner core particles and are solidified. There are problems that the composition of the toner that is fixed or formed into a film varies, the chargeability of the toner becomes unstable, and the fluidity of the toner becomes poor.

Therefore, in the past, when fixing and / or forming a film of fine particles for surface treatment such as a coloring agent and a charge control agent on the surface of the toner core particle as described above, the toner core is generally used. After the particles and the fine particles for surface treatment are mixed using a mixer such as a V-type mixer, an automatic mortar, a Henschel mixer, the mixture is mechanomill (Okada Seiko Co., Ltd.), Ongmill (Hosokawa Micron Co., Ltd.),
Processing was performed using a processing device such as a hybridization system (manufactured by Nara Machinery Co., Ltd.) so that the fine particles for surface treatment were fixed and / or formed into a film on the surface of the toner core particles.

However, when the toner for developing an electrostatic latent image is manufactured in this manner, a step of mixing the toner core particles and the fine particles for surface treatment with a mixer as described above, In this way, the mixture of the toner core particles and the fine particles for surface treatment is treated by a treatment device to fix the fine particles for surface treatment on the surface of the toner core particles and / or form a film. Requires two steps,
There was a problem that productivity deteriorated.

[0009]

SUMMARY OF THE INVENTION The present invention is directed to a copying machine,
In an image forming apparatus such as a printer, it is an object to solve the above problems in the toner for developing an electrostatic latent image used for developing an electrostatic latent image.

That is, according to the present invention, when the fine particles for surface treatment such as the coloring agent and the charge control agent are fixed and / or formed into a film on the surface of the toner core particles containing the resin as a main component, this treatment is The fine powder for the surface treatment is fixed and / or formed into a film in a state of being uniformly dispersed on the surface of the toner core particles, so that the composition of the toner varies. It is an object of the present invention to obtain a toner for developing an electrostatic latent image excellent in charging stability and fluidity.

[0011]

According to the present invention, in order to solve the above-mentioned problems, at least toner core particles containing a resin as a main component and fine particles for surface treatment are provided in the treatment chamber. After rotating the provided rotating member and mixing in a high-speed air stream, fine particles for surface treatment are uniformly dispersed and attached to the surface of the toner core particles, and then the toner core particles and the fine particles for surface treatment are separated. The mixing conditions were strengthened so that the fine particles for surface treatment adhering to the surface of the toner core particles were fixed and / or formed into a film on the surface of the toner core particles.

The toner core particles used for producing the electrostatic latent image developing toner in the present invention are as follows.
Generally, those obtained by the kneading-grinding method used for producing toner and those obtained by various methods such as wet granulation can be used.

When the wet granulation method is used, any known method may be used, and a suspension polymerization method or an emulsion polymerization method may be used. A granulation method that does not involve a polymerization process such as a turbidity method may be used.

In the case of the suspension polymerization method, a polymerization composition containing a polymerizable monomer capable of forming a resin component, a polymerization initiator, and other additives such as a colorant in an aqueous medium is used. It is suspended in and polymerized to be granulated.

Further, in the case of the emulsion polymerization method, it is preferable to use the method known as the seed polymerization method because a general emulsion polymerization has a good particle size distribution but only extremely fine particles can be obtained. That is, a part of the polymerizable monomer and a polymerization initiator are added to an aqueous medium obtained by adding an aqueous medium or an emulsifier, and the mixture is stirred and emulsified. It is preferable to obtain such particles, and perform the polymerization in the droplets of the polymerizable monomer using these particles as seeds. In this case, the polymerization may be carried out in the droplets of the polymerizable monomer containing an additive such as a colorant.

Further, as a wet granulation method including other polymerization processes, a toner-free core particle can be prepared by a soap-free emulsion polymerization method, a microcapsule method (interfacial polymerization method, in-situ polymerization method, etc.), a non-aqueous dispersion polymerization method, etc. May be manufactured.

On the other hand, in the case of the suspension method, an additive such as a colorant is mixed with the resin component and melted or dissolved and dispersed in an appropriate organic solvent, and this is suspended in an aqueous medium for granulation. To do.

The liquid medium used in the above wet granulation method depends on the type of resin or polymerizable monomer contained in the toner composition, but is generally as follows. Something is used. First, among wet granulation methods including a polymerization process, water and a water / organic solvent mixture can be used in the suspension polymerization method, emulsion polymerization method, soap-free emulsion polymerization method, microcapsule method and the like. The organic solvent used here may be any one having a high affinity for water, for example, alcohols such as methanol, ethanol, propanol, butanol, ethylene glycol monomethyl ether, Ether alcohols such as ethylene glycol monoethyl ether, ethers such as tetrahydrofuran and dimethoxyethane are used,
These may be used as one kind or a mixture of two or more kinds.

Further, as a liquid medium used in the non-aqueous dispersion polymerization method among the wet granulation methods including the polymerization process, it exhibits solubility with respect to the monomers used but solubility with respect to the polymer produced. Any organic solvent may be used as long as it does not show.

Examples of such an organic solvent include, in addition to the above-mentioned organic solvents, aliphatic hydrocarbons such as pentane, hexane, octane, xylene, benzene, toluene and other alkylbenzenes, aromatic naphtha and other aromatic hydrocarbons. It is possible to use various organic solvents such as hydrocarbons, ketones, and ester-based organic solvents. These organic solvents may be used alone or in admixture of two or more, or may be used in admixture with water. It is appropriately selected and used accordingly.

In the wet granulation method that does not involve a polymerization process, any liquid medium may be used as long as it does not dissolve the resin used for the toner core particles. For example, the organic solvent as described above, Water / organic solvent mixture as well as water are used. The organic solvents may be used alone or in combination of two or more.

When the toner core particles are granulated in a wet process using the liquid medium as described above, the average particle size is usually 1 to 15 μm, preferably 2 to 10 μm. To do. Incidentally, when the toner core particles are granulated in the wet method as described above, it is easy to adjust those having a uniform particle size distribution such that the toner core particles are contained in an average particle size of ± 25% in an amount of 30% or more. Become.

The resin used for the toner core particles may be any resin as long as it is generally used as a binder used in the production of toner, for example polystyrene. Thermoplastic resin such as resin, poly (meth) acrylic resin, polyolefin resin, polyamide resin, polycarbonate resin, polyether resin, polysulfone resin, polyester resin, epoxy resin, butadiene resin, or A thermosetting resin such as a urea resin, a urethane resin, a urea resin or an epoxy resin, or a copolymer, block polymer, graft polymer or polymer blend of these can be used. The above-mentioned resin is not limited to a resin in a complete polymer state such as a thermoplastic resin, and it is possible to use a resin containing an oligomer or a prepolymer such as a thermosetting resin and a crosslinking agent. It is possible.

When the toner for developing an electrostatic charge image used in the high speed system of the present invention is manufactured, it is necessary to fix the toner on a transfer paper or the like in a short time or to improve the separability from the fixing roller. Therefore, as a resin constituting the toner core particles, a styrene monomer, a (meth) acrylic monomer, a homopolymer or a copolymer polymer synthesized from a (meth) acrylate monomer,
Alternatively, it is preferable to use a polyester resin.

In such a resin, the number average molecular weight Mn and the weight average molecular weight Mw are 1000 ≦.
Mn ≦ 10000, 20 ≦ Mw / Mn ≦ 70, and regarding the number average molecular weight Mn, 2,000 ≦ Mn ≦
It is desirable to use that which is 7,000.

When this electrostatic image developing toner is used as an oilless fixing toner, the resin constituting the toner core particles has a glass transition point of 55 to 80 ° C. and a softening point of 80 to 150 ° C. Further, it is desirable to use the one containing 5 to 20% by weight of the gelling component.

Further, when a translucent color toner for full color is manufactured in the present invention, it is preferable to use a polyester resin as a resin constituting the toner core particles.

Here, the polyester resin constituting the toner core particles in the translucent color toner has a glass transition temperature of 55 to 70 ° C. and a softening point of 80 to 150 ° C.
It is desirable to use a linear polyester having a number average molecular weight Mn of 2000 to 15,000 and a molecular weight distribution (Mw / Mn) of 3 or less.

Further, linear urethane-modified polyester obtained by reacting the above linear polyester resin with diisocyanate can also be used.

Here, the linear urethane-modified polyester is a linear polyester resin 1 composed of a dicarboxylic acid and a diol, having a number average molecular weight Mn of 2000 to 15,000, an oxidation of 5 or less, and a terminal group substantially having a hydroxyl group.
A linear urethane-modified polyester resin obtained by reacting 0.3 to 0.95 mol of diisocyanate with respect to mol, and having a glass transition temperature of 40 to 80.
A material whose main component is one whose oxidation is 5 ° C. or less is used.

Further, the above linear polyester is modified with a styrene-based, acrylic-based, aminoacrylic-based monomer or the like by a method such as grafting or block polymerization to obtain the same glass transition temperature, softening point, and the like as the linear urethane-modified polyester. Those having a molecular weight characteristic can also be preferably used.

In the toner core particles, a colorant, a charge control agent, an offset preventing agent, etc. may be added in addition to the resin as described above.

On the other hand, as the fine particles for surface treatment mixed with the toner core particles, various coloring agents, charge control agents,
A fluidizing agent, an abrasive, a magnetic powder, an anti-offset agent, a resin fine particle and the like can be used alone or in combination, and generally, the average particle diameter thereof is 1/5 or less, preferably 1/10 of the toner core particle. Hereinafter, it is more preferable to use fine particles of 1/20 or less.

When the surface-treating fine particles are added to the toner core particles, if the amount of addition is too small, the surface-treating fine particles are uniformly treated on the surface of the toner core particles. On the other hand, while the effect of the fine particles for surface treatment is reduced, if the addition amount is too large, not all of the fine particles for surface treatment adhere to the toner core particles, but these exist alone to form particles. Therefore, 0.01 to 50 parts by weight, preferably 0.1 to 30 parts by weight, of such fine particles for surface treatment is usually added to 100 parts by weight of the toner core particles.

Here, as the colorant used as the fine particles for surface treatment, various organic or inorganic pigments and dyes of various colors as described below can be used.

First, as the black pigment, carbon black, copper oxide, manganese dioxide, aniline black, activated carbon, non-magnetic ferrite, magnetic ferrite, magnetite or the like can be used.

The yellow pigments include yellow lead, zinc yellow,
Cadmium yellow, yellow iron oxide, mineral fast yellow, nickel titanium yellow, navels yellow, naphthol yellow S, bunzer yellow G, bunzer yellow 10G, benzidine yellow G, benzidine yellow GR, quinoline yellow rake, permanent yellow NCG, tartrazine rake. Etc. can be used.

As the orange pigment, red yellow lead, molybdenum orange, permanent orange GTR, pyrazolone orange, vulcan orange, induslen brilliant orange RK, benzidine orange G, induslen brilliant orange GK and the like can be used.

The red pigments include red iron oxide, cadmium red, red lead, mercury sulfide, cadmium, permanent red 4R, resole red, pyrazolone red,
Watching red, calcium salt, lake red C,
Lake Red D, Brilliant Carmine 6B, Eosin Lake, Rhodamine Lake B, Alizarin Lake, Brilliant Carmine 3B and the like can be used.

Further, as the purple pigment, manganese purple, fast violet B, netyl violet lake, etc. can be used.

As the blue pigment, navy blue, cobalt blue, alkali blue lake, Victoria blue lake, phthalocyanine blue, metal-free phthalocyanine blue, phthalocyanine blue partially chlorinated compound, fast sky blue, induslen blue BC, etc. should be used. You can

As the green pigment, chrome green, chrome oxide, pigment green B, malachite green lake, final yellow green G and the like can be used.

As the white pigment, zinc white, titanium oxide, antimony white, zinc sulfide and the like can be used.

As the extender pigment, barite powder, barium carbonate, clay, silica, white carbon, talc, alumina white or the like can be used.

Various dyes such as basic, acidic, disperse and direct dyes include nigrosine, methylene blue,
Rose bengal, quinoline yellow, ultramarine blue, etc. can be used.

When using these colorants as fine particles for surface treatment, these colorants may be used alone or in combination.

When these colorants are mixed with the toner core particles as fine particles for surface treatment, if the amount of the colorant is too large, the fixing property of the toner is deteriorated, while the amount of the colorant is too small. Since the desired image density cannot be obtained, the amount of these colorants including the colorant contained in the toner core particles as described above is 1 to 20 with respect to 100 parts by weight of the resin in the toner. Parts by weight, preferably 2 to 10 parts by weight.

Further, in the present invention, when the above-mentioned translucent color toner is manufactured, as the fine particles for the surface treatment, a colorant composed of pigments or dyes of various colors as described below is used. You can

Here, as the yellow pigment used for the translucent color toner, C.I. I. 10316 (Naphthol Yellow S), C.I. I. 11710 (Hansa Yellow 10
G), C.I. I. 11660 (Hansa Yellow 5G),
C. I. 11670 (Hansa Yellow 3G), C.I. I.
11680 (Hansa Yellow G), C.I. I. 11730
(Hansa Yellow GR), C.I. I. 11735 (Hansa Yellow A), C.I. I. 11740 (Hansa Yellow R
N), C.I. I. 12710 (Hansa Yellow R), C.I.
I. 12720 (Pigment Yellow L), C.I. I. Two
1090 (benzidine yellow), C.I. I. 21095
(Benzidine Yellow G), C.I. I. 21100 (Benzidine Yellow GR), C.I. I. 20040 (Permanent Yellow NCG), C.I. I. 21220 (Vulcan Fast Yellow 5), C.I. I. 21135 (Vulcan Fast Yellow R) or the like can be used.

As the red pigment for the translucent color toner, C.I. I. 12055 (Stalin I), C.I.
I. 12075 (permanent orange), C.I. I. 1
2175 (Resor Fast Orange 3GL), C.I.
I. 12305 (Permanent Orange GTR), C.I.
I. 11725 (Hansa Yellow 3R), C.I. I. 21
165 (Vulcan Fast Orange GG), C.I. I. Two
1110 (benzidine orange G), C.I. I. 1212
0 (Permanent Red 4R), C.I. I. 1270 (Para Red), C.I. I. 12085 (Fire Red), C.I. I. 12315 (Brilliant Fast Scarlet), C.I. I. 12310 (Permanent Red F2R), C.I. I. 12335 (Permanent Red F
4R), C.I. I. 12440 (Permanent Red FR
L), C.I. I. 12460 (Permanent Red FRL
L), C.I. I. 12420 (Permanent Red F4R
H), C.I. I. 12450 (Light Fast Red Toner B), C.I. I. 12490 (Permanent Carmine FB), C.I. I. 15850 (Brilliant Carmine 6
B) and the like can be used.

As the blue pigment for the translucent color toner, C.I. I. 74100 (metal-free phthalocyanine blue), C.I. I. 74160 (phthalocyanine blue), C.I. I. 74180 (Fast Sky Blue) or the like can be used.

When these colorants for light-transmitting color toners are used as fine particles for surface treatment, they can be used alone or in combination as in the case of ordinary colorants, or in combination. The amount is 1 to 10 parts by weight, preferably 2 parts by weight, including 100 parts by weight of the resin in the toner, including the colorant contained in the toner core particles as described above.
~ 5 parts by weight.

When an offset preventive agent is used as the above-mentioned fine particles for surface treatment, as such an offset preventive agent, various waxes, particularly low molecular weight polypropylene, polyethylene, or polyolefins such as oxidized polypropylene and polyethylene are used. A system wax is preferably used.

When a charge control agent is used as the above-mentioned fine particles for surface treatment, examples of the positive charge control agent include azine compound Nigrosine base EX and Bontron N-01, 02, 04, 05, 07, 09. , 1
0,13 (manufactured by Orient Chemical Industry Co., Ltd.), oil black (manufactured by Chuo Synthetic Chemical Industry Co., Ltd.), quaternary ammonium salt P-5
1, polyamine compound P-52, Sudan Chief Schwarz BB (solvent black 3: C.I. No. 26)
150), Fetschwartz HBN (C.I. No. 2)
6150), Brilliant Spirits Schwarz TN
(Manufactured by Farben Fabriken Bayer Co., Ltd.), alkoxylated amines, alkylamides, molybdic acid chelate pigments, imidazole compounds, etc. can be used.
On the other hand, as the negative charge control agent, for example, chromium complex salt type azo dye S-32, 33, 34, 35, 37, 38, 4
0,44 (manufactured by Orient Chemical Industry Co., Ltd.), Eisenspiro Black TRH, BHH (manufactured by Hodogaya Chemical Co., Ltd.), Kayaset Black T-22,004 (manufactured by Nippon Kayaku Co., Ltd.), copper phthalocyanine dye S-39 (Orient Chemistry) Industrial Co., Ltd.), chromium complex salt E-81, 82 (Orient Chemical Co., Ltd.), zinc complex salt E-84 (Orient Chemical Co., Ltd.), aluminum complex salt E-86 (Orient Chemical Co., Ltd.), etc. You can

When these charge control agents are mixed as fine particles for surface treatment with the toner core particles, if the amount is too large, the charge amount of the toner becomes unstable and the fixing property of the toner deteriorates. On the other hand, if the amount is too small, the desired charge amount cannot be obtained. Therefore, the amount of these charge control agents, including the charge control agent contained in the toner core particles as described above, is 0.01 to 10 parts by weight, preferably 0.1 to 5 parts by weight, relative to 100 parts by weight of the resin in 1.

When a fluidizing agent is used as the above-mentioned fine particles for surface treatment, silica, aluminum oxide, titanium oxide, magnesium fluoride or the like can be used alone or in combination.

When non-magnetic inorganic fine particles are used as the fine particles for surface treatment, for example, silicon carbide, boron carbide, titanium carbide, zirconium carbide, hafnium carbide, vanadium dicarbide, tantalum carbide, niobium carbide, carbonized Various carbides such as tungsten, chromium carbide, molybdenum carbide, calcium carbide, diamond carbon random; various nitrides such as boron nitride, titanium nitride, zirconium nitride; boride such as zirconium boride; iron oxide, chromium oxide, oxidation Various oxides such as titanium, calcium oxide, magnesium oxide, zinc oxide, copper oxide, aluminum oxide, silica, colloidal silica and hydrophobic silica; sulfides such as molybdenum disulfide; fluorides such as magnesium fluoride and carbon fluoride Compound; Aluminum stearate, Steari Calcium, zinc stearate, various metal soaps such as magnesium stearate: talc, can be used various non-magnetic inorganic fine particles of bentonite. In addition, it is desirable that these fine particles be subjected to a hydrophobizing treatment before use.

When organic fine particles are used as the above-mentioned fine particles for surface treatment, for example, a wet polymerization method such as an emulsion polymerization method, a soap-free emulsion polymerization method or a non-aqueous dispersion polymerization method,
Various organic fine particles such as styrene-based, (meth) acrylic-based, benzoguanamine, melamine, Teflon, silicon, polyethylene and polypropylene which are granulated by a vapor phase method can be used.

When magnetic fine particles are used as the above-mentioned fine particles for surface treatment, for example, metals exhibiting ferromagnetism such as cobalt, iron and nickel, aluminum, cobalt, iron, lead, magnesium, nickel, zinc, Antimony, beryllium, bismuth, cadmium, calcium,
It is possible to use alloys of metals such as manganese, selenium, titanium, tungsten, vanadium, mixtures thereof, and fine particles of known magnetic materials such as oxides and fired bodies (ferrite).

Then, the toner core particles containing the above resin as a main component and the above-mentioned fine particles for surface treatment are mixed to uniformly disperse the fine particles for surface treatment on the surfaces of the toner core particles. 1 is used to fix the fine particles for surface treatment attached to the surface of the toner core particles to the surface of the toner core particles and / or to form a film, using a processing apparatus as shown in FIG. can do.

Here, in the processing apparatus shown in FIG.
Inside the processing chamber 10 in which the stator 13 having the jacket 12 is attached to the inner peripheral surface of the casing 11,
The rotary member 20 in which the blade 22 is provided on the rotary plate 21 is provided.

Then, the toner core particles and the fine particles for surface treatment as described above are supplied from the raw material supply chute 14 into the processing chamber 10, and the rotating member 20 is rotated in the processing chamber 10. By the high-speed airflow generated by the above, the toner core particles and the fine particles for surface treatment supplied as described above are passed between the rotating plate 21 provided with the blade 22 and the stator 13, and the toner core particles and the surface are processed. The processing fine particles are mixed and mechanical and thermal shocks are applied, and the toner core particles and the surface processing fine particles in the processing chamber 10 are circulated through the circulation port 15 provided in the processing chamber 10. This processing chamber 1
0 and the raw material supply chute 14 for communicating with each other
It was made to lead to the inside of the processing chamber 10 many times through.

The toner core particles and the fine particles for surface treatment thus supplied into the processing chamber 10 are fed to the blade 22.
The toner core particles and the fine particles for surface treatment are mixed many times between the rotary plate 21 provided with and the stator 13 to disperse the fine particles for surface treatment on the surface of the toner core particles. And uniformly attach it to the rotary member 20.
The rotation speed and the like are changed so that the fine particles for surface treatment adhering to the surface of the toner core particles are fixed and / or formed into a film on the surface of the toner core particles.

Here, when the toner core particles and the fine particles for surface treatment are mixed by using the above-mentioned processing apparatus, the fine particles for surface treatment are dispersed and uniformly adhered to the surface of the toner core particles. Generally, the temperature of the processing chamber 10 is set to 5 to 40 ° C., and the peripheral speed of the tip of the blade 22 attached to the rotating plate 21 is set to 10 to 50 m / se.
The rotating member 20 is rotated so as to be c, and this treatment is performed for 1 to 5 minutes.

Further, after the fine particles for surface treatment are adhered to the surface of the toner core particles in this manner, the fine particles for surface treatment are fixed and / or film-formed on the surface of the toner core particles. Usually, the temperature of the processing chamber 10 is set to 5 to 60 ° C., and the peripheral speed of the tip of the blade 22 attached to the rotating plate 21 is 30 to 100 m / se.
The rotating member 20 is rotated so as to be c, and this treatment is performed for 1 to 20 minutes.

[0066]

In the present invention, when the toner for developing an electrostatic latent image is manufactured, the rotating member is rotated in the processing chamber for processing at least the toner core particles containing the resin as the main component and the fine particles for the surface treatment. The toner core particles and the fine particles for surface treatment are mixed in this processing chamber in a high-speed air stream to disperse the fine particles for surface treatment on the surface of the toner core particles to uniformly adhere them, and then mixed in the processing chamber. Since the conditions are strengthened so that the fine particles for surface treatment adhering to the surface of the toner core particles are fixed and / or formed into a film on the surface of the toner core particles, the toner core particles and the fine particles for surface treatment are And the immobilization of the fine particles for surface treatment on the surface of the toner core particles and / or film formation can be continuously performed in a series of steps.

Further, after the fine particles for surface treatment are dispersed on the surface of the toner core particles as described above and uniformly attached,
Since the fine particles for surface treatment are fixed and / or formed into a film on the surface of the toner core particles, the fine particles for surface treatment are uniformly dispersed on the surface of the toner core particles. The toner is fixed and / or formed into a film on the surface, the composition of the manufactured toner is eliminated, and a toner for electrostatic latent image development having excellent charging stability and fluidity can be obtained. ..

[0068]

EXAMPLES Hereinafter, a method for manufacturing a toner for developing an electrostatic latent image according to an example of the present invention will be specifically described, and
It is revealed that the electrostatic latent image developing toner manufactured by the manufacturing method according to the embodiment of the present invention is superior to the electrostatic latent image developing toner manufactured by the manufacturing method of the comparative example. ..

Example 1 In this example, the toner core particles A produced as follows were used.

Here, in producing the toner core particles A, 100 parts by weight of a styrene monomer, 35 parts by weight of n-butyl methacrylate, 5 parts by weight of methacrylic acid and 2,2-azobis- (2,4-). Dimethyl valeronitrile) 0.5 part by weight, low molecular weight polypropylene (manufactured by Sanyo Kasei Kogyo KK, Viscole 605P) 3 parts by weight, and carbon black (Mitsubishi Kasei Kogyo KK, MA # 8) 8 parts by weight by a sand stirrer. A polymerization composition was prepared by mixing.

Then, this polymerization composition was put into an aqueous solution of gum arabic having a concentration of 3%, and these were rotated with a stirrer (TK Auto Homomixer manufactured by Tokushu Kika Kogyo Co., Ltd.) at a rotation speed of 40.
While stirring at 00 rpm, a polymerization reaction was carried out at a temperature of 60 ° C. for 6 hours, and then the rotation speed of the agitator was set to 2000 rp.
m, and the temperature is raised to 85 ° C. to agglomerate the polymerized particles with each other.
50 by sticking to the surface of fine particles of μm or more and melting
Aggregate to about 1 μm to 1 mm, dry it to 100
Aggregates of about μm to 2 mm were obtained.

Next, this aggregate was pulverized by a jet mill and further classified by wind to produce toner core particles A having an average particle diameter of 6 μm.

In this embodiment, 100 parts by weight of the toner core particles A produced as described above are composed of a zinc complex salt compound (E-84, manufactured by Orient Chemical Industry Co., Ltd.) as fine particles for surface treatment. A charge control agent was added in an amount of 0.5 part by weight, and these particles were treated using the treatment apparatus (hybridization system NHS-3 type manufactured by Nara Machinery Co., Ltd.) as shown in FIG.

Here, in treating these particles by the above-mentioned treatment apparatus, first, these particles are fed into the treatment chamber 10 through the raw material feeding chute 14 and at the tip of the blade 22 attached to the rotary plate 21. The rotating member 20 is rotated at a peripheral speed of 40 m / sec to allow these particles to pass between the rotating plate 21 provided with the blade 22 and the stator 13, and the circulation path 16 described above. While circulating through 1
A mixing process was performed for a minute.

After the mixing process is performed as described above, the peripheral speed of the tip of the blade 22 is continuously set at 80 m / m.
The rotating member 20 is rotated so that the time becomes sec, and the particles are mixed as described above to allow the particles to pass between the rotating plate 21 provided with the blade 22 and the stator 13, and the circulation path. The charge control agent was fixed on the surface of the toner core particle A by performing a treatment for 5 minutes while circulating through 16 to produce a black toner having an average particle diameter of 6 μm.

(Example 2) In this example, the toner core particles B produced as described below were used.

In the production of the toner core particles B, in the production of the toner core particles A in the above-mentioned Example 1, no low molecular weight polypropylene (manufactured by Sanyo Kasei Kogyo Co., Ltd., Viscole 605P) was added. A toner core particle B having an average particle diameter of 6 μm was manufactured in the same manner as the toner core particle A.

In this example, 100 parts by weight of the toner core particles B produced as described above were used as a fine particle for surface treatment, and a chromium complex salt type dye (manufactured by Hodogaya Chemical Co., Ltd., Eisenspirone) was used. Black TRH)
And 0.5 parts by weight of a fluidizing agent composed of hydrophobic titanium oxide (T-805, manufactured by Degussa), and the particles were mixed with those in Example 1 above. By the same treatment, a black toner having an average particle diameter of 6 μm was manufactured.

(Example 3) In this example, the same toner core particles B as in Example 2 were used.
Then, with respect to 100 parts by weight of the toner core particles B, 1.5 parts by weight of a charge control agent composed of a quaternary ammonium salt compound (P-51 manufactured by Orient Chemical Industry Co., Ltd.) as a fine particle for surface treatment, and a hydrophobic agent. 1.0 part by weight of a superplasticizer made of water-soluble silica (R-974, manufactured by Nippon Aerosil Co., Ltd.) was added, and these particles were treated in the same manner as in Example 1 above to give an average particle size of 6 μm. Black toner was produced.

(Example 4) In this example, the toner core particles C produced as follows were used.

In producing the toner core particles C, 100 parts by weight of styrene-n-butyl methacrylate resin (softening point: 108 ° C., glass transition point: 52 ° C.),
Carbon black (Mitsubishi Kasei Co., Ltd., MA # 8) 10
3 parts by weight of low-molecular-weight polypropylene (manufactured by Sanyo Kasei Kogyo Co., Ltd., VISCOL 605P) were thoroughly mixed in a ball mill, and then kneaded by a three-roll mill heated to 140 ° C. The kneaded product was left to cool, coarsely pulverized with a feather mill, finely pulverized with a jet mill, and then air-classified to obtain a toner having an average particle size of 8 μm. Core particles C were produced.

In this example, 100 parts by weight of the toner core particles C produced as described above were used as surface-treating fine particles of a chromium complex salt type azo dye (Orient Chemical Co., Ltd., S-34). 1.0 part by weight of a charge control agent, and titanium oxide (Taika Co., MT-
0.5 parts by weight of a fluidizing agent consisting of 600 BS),
These particles were treated in the same manner as in Example 1 above to produce a black toner having an average particle size of 8 μm.

(Example 5) In this example, the toner core particles D produced as described below were used.

In producing the toner core particles D, in the production of the toner core particles C in the above-mentioned Example 4, instead of the styrene-n-butylmethacrylate resin, a polyelter resin (Tafton NE-38 manufactured by Kao Corporation) was used.
2) was used, and otherwise the same as in the case of the toner core particles C, and the toner core particles D having an average particle diameter of 7.5 μm were produced.

In this example, 100 parts by weight of the toner core particles D produced as described above were used as the fine particles for surface treatment, and the quaternary ammonium salt (produced by Orient Chemical Industry Co., Ltd., P -51) 1.0 parts by weight of a charge control agent and a fluidizing agent 0.3 comprising the above hydrophobic silica (R-974 manufactured by Nippon Aerosil Co., Ltd.).
Parts by weight and the above-mentioned hydrophobic titanium oxide (manufactured by Degussa, T-
0.5 part by weight of a fluidizing agent of 805) was added, and these particles were treated in the same manner as in Example 1 above to obtain a black toner having an average particle size of 7.5 μm.

(Comparative Example 1) In this comparative example, the same toner core particles A as in Example 1 were used. Then, with respect to 100 parts by weight of the toner core particles A, 0.5 parts by weight of a charge control agent composed of the chromium complex salt type dye (Hodogaya Chemical Co., Ltd., Eisenspiron Black TRH) as fine particles for surface treatment. In addition, these particles were processed using the same processing apparatus (manufactured by Nara Machinery Co., Ltd., hybridization system NHS-3 type) as in Example 1 above.

Here, in this comparative example, a step of rotating the rotating member 20 at a low speed to mix the toner core particles A and the fine particles for the surface treatment when performing the processing using the above-mentioned processing apparatus Omitted, the above blade 2
The rotating member 20 was rotated so that the peripheral speed of the two tips was 80 m / sec, and these particles were treated for 5 minutes to produce a black toner having an average particle size of 6 μm.

Comparative Example 2 In this comparative example, the same toner core particles B as in Example 2 were used. Then, with respect to 100 parts by weight of the toner core particles B, 1.0 part by weight of a charge control agent composed of the quaternary ammonium salt (P-51 manufactured by Orient Chemical Co., Ltd.) as fine particles for surface treatment, 1.0 part by weight of a fluidizing agent made of the above-mentioned hydrophobic silica (manufactured by Nippon Aerosil Co., Ltd., R-974) was added, and these particles were treated in the same manner as in Comparative Example 1 above to give an average particle size of A black toner having a size of 6 μm was manufactured.

(Comparative Example 3) In this comparative example, the same toner core particles C as those in Example 4 were used. Then, with respect to 100 parts by weight of the toner core particles C, as the fine particles for surface treatment, the above-mentioned chrome complex salt type azo dye (Hodogaya Chemical Co., Ltd., Aizenspirone Black TR) was used.
H) and 0.5 parts by weight of a charge control agent and 0.5 parts by weight of a fluidizing agent made of the above-mentioned hydrophobic titanium oxide (T-805 manufactured by Degussa Co.) were added, and these particles were added to the above Comparative Example. 1
In the same manner as in the above case, a black toner having an average particle diameter of 8 μm was manufactured.

Next, Example 1 produced as described above
5 to 5 and Comparative Examples 1 to 3, the average charge amount [μC / g], the poorly charged toner amount [wt%], and the toner scattering amount are examined, and the fog of the formed image is evaluated. did.

In the evaluation of the toners of Examples 1 to 5 and Comparative Examples 1 to 3, colloidal silica (R-972, manufactured by Nippon Aerosil Co., Ltd.) was used for 100 parts by weight of each toner. 0.2 part by weight was added and post-treated.

In making these evaluations,
Each of the toners of Examples 1 to 5 and Comparative Examples 1 to 3 was mixed with a binder type carrier produced as described below, and evaluated.

Here, as the binder type carrier, a polyester resin (NE-111 manufactured by Kao Corporation) is used.
0) 100 parts by weight and inorganic magnetic powder (manufactured by Toda Kogyo Co., EP
T-1000) 500 parts by weight and carbon black (MA # 8 manufactured by Mitsubishi Kasei Co., Ltd.) 2 parts by weight were thoroughly mixed, pulverized, and then set to 180 ° C. for the cylinder part and 170 ° C. for the cylinder head part. Binder having an average particle diameter of 55 μm obtained by melt-kneading using an extrusion kneader, cooling and roughly crushing this kneaded product, finely crushing with a jet mill, and further classifying with a wind classifier. A mold carrier was used.

The above Examples 1-5 and Comparative Examples 1-3
In measuring the average particle size of each toner and the average particle size of the carrier in (1), a laser diffraction type particle size distribution measuring device (manufactured by Shimadzu Corporation, SALD-1100) was used.

When the charge amount and the poorly charged toner amount of each of the toners of Examples 1 to 5 and Comparative Examples 1 to 3 are measured using the binder type carrier described above, the amount of each toner is 2 g of each toner described above. 2 careers
8 g was added, and these were put in a plastic bottle of 50 cc and rotated at 120 rpm for 10 minutes on a rotary rack.

Then, 3 g of the developer containing each toner thus adjusted was weighed with a precision balance, and the amount of electrification and the amount of poorly electrified toner of each toner were measured using the apparatus shown in FIG.

Here, in measuring the charge amount of each toner and the amount of poorly charged toner by using the apparatus shown in FIG. 2, each developer measured as described above is evenly distributed over the entire surface of the conductive sleeve 1. And put it so that
The rotation speed of the magnet roll 2 provided in the conductive sleeve 1 was set to 100 rpm.

Then, a bias voltage of 0 to 10 KV is sequentially applied from the bias power source 3, the conductive sleeve 1 is rotated for 5 seconds, and the potential Vm at the cylindrical electrode 4 at the time when the conductive sleeve 1 is stopped is read. At the same time, the weight of the toner attached to the cylindrical electrode 4 from the conductive sleeve 1 was measured by a precision balance to obtain the average charge amount [μC / g] of each toner, and the results are shown in Table 1 below. ..

Further, the results of the above measurements are totaled to measure the charge amount distribution of each toner contained in the developer. Based on this charge amount distribution, the average charge amount [μC / G], the amount of toner having a charge amount of ⅕ or less was determined, and the value is shown in Table 1 below as the amount of poorly charged toner [wt%].

The above Examples 1 to 5 and Comparative Examples 1 to 1
In examining the amount of scattering in each toner of No. 3, the developer containing each toner of Examples 1 to 5 and Comparative Examples 1 to 3 was used in the same manner as in the case of measuring the average charge amount [μC / g]. It was adjusted.

When examining the amount of scattering in each toner, a digital dust meter P5H2 type (manufactured by Shibata Chemical Co., Ltd.) was used, and this dust meter was measured at 10c from a magnet roll.
The developer containing the respective toners adjusted as described above is set on the magnet rolls at a distance of m.
After setting g, this magnet roll is 2000 rp
The amount of each toner that generated dust when rotated at m was read by the above dust meter, and the count number per minute [cpm] was obtained.

When the count number per minute thus obtained is 300 cpm or less, it is indicated by ◯, and 500 cp.
Table 1 below shows Δ when m or less and x when more than 500 cpm.

In the evaluation of fogging of the formed image, the above carrier was used for each of the toners of Examples 1 to 5 and Comparative Examples 1 to 3 as toner / carrier =
Mixing to give a weight ratio of 5/95, Examples 1-5
A two-component developer using each toner of Comparative Examples 1 to 3 was prepared.

Then, Examples 1, 2, 4 and Comparative Example 1,
For the developer using each toner of No. 3, the fixing device of the commercially available copying machine (EP-570Z manufactured by Minolta Camera Co., Ltd.) improved to the oil coating system is used.
For the developers using the toners of Examples 3 and 5 and Comparative Example 2, commercially available copying machines (EP manufactured by Minolta Camera Co., EP
-8600) was used.

Then, using these copying machines, a printing durability test of 100,000 sheets was conducted using a chart having a black ratio of 6%, and formed at the initial, 10,000, and 100,000 sheet tests. The fogging of the images was evaluated.

Here, in the evaluation of image fogging, ◯ is good, Δ is feasible with some fog but practically usable, and x is practically problematic. It was shown to.

[0107]

[Table 1]

As is clear from this result, when the toners of Examples 1 to 5 are used, the amount of defectively charged toner is significantly smaller than that when the toners of Comparative Examples 1 to 3 are used. As a result, the amount of toner scattering and fog in the formed image were reduced.

[0109]

As described above in detail, according to the present invention, at the time of producing the electrostatic latent image developing toner, at least the toner core particles containing the resin as the main component and the fine particles for the surface treatment are treated. By rotating the rotating member in the chamber, the toner core particles and the fine particles for surface treatment are mixed in a high-speed airflow in this processing chamber, and the fine particles for surface treatment are dispersed and uniformly attached to the surface of the toner core particles. After that, the mixing conditions in the processing chamber are strengthened so that the fine particles for surface treatment adhered to the surface of the toner core particles as described above are fixed and / or formed into a film on the surface of the toner core particles. Therefore, the mixing of the toner core particles and the fine particles for surface treatment and the fixing of the fine particles for surface treatment on the surface of the toner core particles and / or the formation of a film can be continuously performed in a series of steps. In comparison with the conventional method in which the mixing of the toner core particles and the fine particles for surface treatment and the fixing and / or film formation of the fine particles for surface treatment on the surface of the toner core particles are separately performed, The productivity of the toner for developing an electrostatic latent image is remarkably improved.

In the present invention, the fine particles for surface treatment are dispersed and evenly adhered to the surface of the toner core particles as described above, and then the fine particles for surface treatment are fixed on the surface of the toner core particles. Since the fine particles for surface treatment are uniformly dispersed on the surface of the toner core particles, the fine particles for surface treatment are fixed and / or formed into a film. As a result, there is no variation in the composition of the manufactured toner, and an electrostatic latent image developing toner having excellent charging stability and fluidity can be obtained.

[Brief description of drawings]

FIG. 1 shows an example of a processing apparatus used for processing toner core particles containing a resin as a main component and fine particles for surface treatment in producing an electrostatic latent image developing toner in the present invention. It is a schematic explanatory drawing.

FIG. 2 is a schematic view of an apparatus used to measure the charge amount of toner.

[Explanation of symbols]

 10 Processing chamber 20 Rotating member 30 Adhesion suppressing means

Claims (1)

[Claims] 1. Toner core particles containing at least a resin-based toner core particle and fine particles for surface treatment are mixed in a processing chamber by rotating a rotary member provided in the processing chamber in a high-speed air stream. After the fine particles for surface treatment are uniformly dispersed and adhered to the surface of the toner, the mixing condition of the toner core particles and the fine particles for surface treatment is strengthened, and the surface treatment particles adhered on the surface of the toner core particles are treated. The method for producing a toner for developing an electrostatic latent image, wherein the fine particles of 1) are fixed and / or formed into a film on the surface of toner core particles.