JP2002186869A - Mechanical grinder and toner manufacturing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a mechanical grinder capable of efficiently grinding a powder raw material, capable of obtaining sharp particle size distribution, capable of arbitrarily controlling the surface shape of toner and suitably used in the production of toner. SOLUTION: In the mechanical grinder having at least a powder charging port 31 for charging coarsely ground matter in a grinding means for finely grinding the coarsely ground matter, a stator 310, a rotor 314 attached to at least central rotary shaft and a powder discharge port 302 for discharging the finely ground powder from the grinding means and constituted so that the stator includes the rotor and the rotor is arranged so as to have a predetermined gap between the surface of the stator and the surface of the rotor to form a grinding zone and the coarsely ground matter is ground in the grinding zone accompanied by the rotation of the rotor, the surface roughness of the grinding surface of the rotor is different from that of the grinding surface of the stator.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for producing a toner formed from a binder resin used for image formation by electrophotography and a method for producing a toner using the apparatus.

[0002]

2. Description of the Related Art In image forming methods such as electrophotography, electrostatography and electrostatic printing, a toner for developing an electrostatic image is used.

[0003] In general, a method for producing a toner for developing an electrostatic image includes a binder resin for fixing to a material to be transferred, various colorants for giving a color as a toner, and a charge control for giving a charge to particles. Agent as a raw material, or
In a so-called one-component developing method as disclosed in JP-A-42141 and JP-A-55-18656, in addition to these, various magnetic materials for imparting transportability and the like to the toner itself are used. In accordance with, for example, dry-mixing is performed by adding other additives such as a release agent and a fluidity-imparting agent, and then, after being melt-kneaded with a general-purpose kneading device such as a roll mill and an extruder, and cooled and solidified, The kneaded material is finely divided by various pulverizing devices such as a jet stream type pulverizer and a mechanical collision type pulverizer, and the obtained coarsely pulverized product is introduced into various air classifiers and classified to obtain a particle size required for toner. And a dry agent and a fluidizing agent and a lubricant are added as needed to obtain a toner to be used for image formation. In the case of a toner used in a two-component developing method, various magnetic carriers are mixed with the above-mentioned toner and then used for image formation.

As a pulverizing means, various pulverizing apparatuses are used. Among them, a pulverizing method using a jet air flow as shown in FIG. A collision-type airflow pulverizer is used.

[0005] A collision type air flow pulverizer using a high-pressure gas such as a jet gas stream conveys a powder material by a jet gas stream, injects the powder material from an outlet of the acceleration tube, and opposes the opening surface of the outlet of the acceleration tube. Then, the powder material is crushed by the impact force of the collision member.

For example, in the collision type air flow pulverizer shown in FIG. 5, an acceleration pipe 162 connected to a high pressure gas supply nozzle 161 is used.
A collision member 164 is provided opposite to the outlet 163 of the, and the high-pressure gas supplied to the acceleration pipe 162 sucks the powder raw material into the acceleration pipe 162 from the powder raw material supply port 165 communicated in the middle of the acceleration pipe 162. Then, the powder raw material is ejected together with the high-pressure gas to collide with the collision surface 166 of the collision member 164, crushed by the impact, and the crushed material is discharged from the crushed material discharge port 167.

However, the above-mentioned collision type air flow pulverizer produces a toner having a small particle diameter because the powder material is ejected together with the high-pressure gas to collide with the collision surface of the collision member and pulverize by the impact. Requires a lot of air. Therefore, power consumption is extremely large, and there is a problem in terms of energy cost.

In particular, in recent years, there has been a demand for energy saving of the apparatus in order to cope with environmental problems, and a mechanical collision type pulverizer which does not require a large amount of air and consumes less electric power instead of the conventional collision type air pulverizer. Is attracting attention.

For example, in the mechanical pulverizer shown in FIG. 1, a powder inlet for feeding coarsely pulverized material into a pulverizing means for finely pulverizing, a stator, and at least a central rotating shaft are attached. A rotor, having at least a powder discharge port for discharging the finely pulverized powder from the pulverizing means, the stator includes the rotor, and the surface of the stator and the rotor The rotor is arranged so as to have a predetermined gap from the surface to form a pulverizing zone. In the pulverizing zone, the coarsely pulverized material is pulverized as the rotor rotates.

[0010] Such a mechanical pulverizer consumes less electric power than a conventional impingement type air-flow pulverizer, and thus can cope with energy savings of a device which has recently been called out. Further, the shape of the toner pulverized by the mechanical pulverizer is rounded due to mechanical impact force, so that it is possible to cope with environmental problems such as cleanerlessness and reduction of waste toner amount.

However, in recent years, as the image quality and definition of copiers and printers have been improved, the performance required for the toner as a toner has become more severe, the particle size of the toner has been reduced, and the particle size distribution of the toner has been reduced. It is becoming increasingly demanded to have sharp particles which do not contain coarse particles and have few ultrafine powders. Further, with respect to the toner surface shape, further control of the toner surface shape is required in accordance with a demand for a high level of environmental stability.

[0012]

SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems, to efficiently pulverize powder raw materials, obtain a sharp particle size distribution, arbitrarily control the surface shape of the toner, An object of the present invention is to provide a mechanical pulverizer suitable for use in the production of toner.

It is a further object of the present invention to provide a method for producing a toner capable of obtaining a toner which solves the above problems.

It is an object of the present invention to control the surface shape of a toner in a mechanical pulverizer, so that it has good developability, transferability, and stable chargeability from the beginning even in a high temperature and high humidity environment, and has a long life. It is an object of the present invention to provide a method for producing a toner which can obtain a proper toner.

It is a further object of the present invention to control the surface shape of the toner in a mechanical pulverizer to obtain a toner having a high image density even at an early stage and after standing even under a high temperature and high humidity environment. An object of the present invention is to provide a method for producing a toner.

It is a further object of the present invention to provide a method for producing a toner capable of obtaining a toner having excellent durability on many sheets.

[0017]

SUMMARY OF THE INVENTION The present invention relates to a powder inlet for charging a coarsely pulverized material into a pulverizing means for finely pulverizing the same, a stator, and at least a rotor attached to a central rotating shaft. And a powder discharge port for discharging the finely pulverized powder from the pulverizing means, wherein the stator includes the rotor, and a surface of the stator and a surface of the rotor. The rotor is arranged so as to have a predetermined gap to form a pulverizing zone, and in the pulverizing zone, mechanical pulverization is performed so that coarsely pulverized material is pulverized with rotation of the rotor. The present invention relates to a mechanical crusher characterized in that the crushing surface of the rotor has a different surface roughness from the crushing surface of the stator.

Further, in the present invention, a mixture containing at least a binder resin and a colorant is melt-kneaded, the obtained kneaded product is cooled, the cooled product is roughly pulverized, and the coarsely pulverized product is finely pulverized by a pulverizing means. A finely pulverized product, and producing a toner having a weight average particle size of 4 to 12 μm from the obtained finely pulverized product. A powder inlet for charging, a stator,
At least a rotor attached to a central rotating shaft, and at least a powder discharge port for discharging finely pulverized powder from a pulverizing means, wherein the stator includes the rotor, The rotor is arranged so as to have a predetermined gap between the surface of the stator and the surface of the rotor to form a pulverizing zone. In the pulverizing zone, the coarsely pulverized material is pulverized with the rotation of the rotor. A mechanical pulverizer, wherein the surface roughness of the pulverized surface of the rotor and the surface roughness of the pulverized surface of the stator are differently pulverized by a mechanical pulverizer. The present invention relates to a method for producing a toner.

The inventor of the present invention has conducted intensive studies to solve the above-mentioned problems of the prior art, and as a result, the surface roughness of the crushing surfaces of the rotor and the stator in the mechanical crusher, and the crushing by the mechanical crusher. The inventors have found out that there is a relationship between the particle size distribution and the surface shape of the toner, and have derived the present invention having the above configuration.

That is, in a mechanical pulverizer, the surface roughness of a rotor having a large number of corrugated grooves formed on a surface which rotates at a high speed in a pulverization chamber and the surface roughness of a large number of corrugated grooves on the surface are increased. By setting the surface roughness to a mechanical pulverizer controlled to an appropriate state so that the surface roughness of the pulverized surface of the grooved stator is different, and by operating the mechanical pulverizer, excessive toner Prevents pulverization, obtains a toner having a sharp particle size distribution with a small amount of fine powder generated, and can arbitrarily control the surface shape of the toner. A long-lasting toner having stable chargeability can be obtained, and further, a toner having a high image density can be obtained from the beginning and even after standing, and further, a toner having excellent multi-sheet durability can be obtained. Find out what you can get It led to the present invention Te.

[0021]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail with reference to preferred embodiments.

First, raw materials of toner particles containing at least a binder resin and a colorant used in the present invention will be described.

[Wax] As the wax used in the present invention, various wax components conventionally known as a release agent can be used. For example, examples of the hydrocarbon wax include low-molecular-weight polyethylene, low-molecular-weight polypropylene, polyolefin copolymer, polyolefin wax, microcrystalline wax, paraffin wax, and aliphatic hydrocarbon-based wax such as Fischer-Tropsch wax.

As the wax having a functional group, an oxide of an aliphatic hydrocarbon wax such as polyethylene oxide wax; or a block copolymer thereof; a plant such as candelilla wax, carnauba wax, wood wax, jojoba wax, etc. Animal waxes such as beeswax, lanolin, and whale wax; mineral waxes such as ozokerite, ceresin, and petrolactam; waxes mainly containing aliphatic esters such as montanic acid ester wax and caster wax: deoxidized carnauba Examples thereof include those obtained by partially or entirely deoxidizing an aliphatic ester such as a wax.

Further, unsaturated straight-chain fatty acids such as palmitic acid, stearic acid, montanic acid, or long-chain alkyl carboxylic acids having a longer-chain alkyl group; unsaturated fatty acids such as brassic acid, eleostearic acid and barinaric acid ; Stearyl alcohol, eicosyl alcohol,
Saturated alcohols such as behenyl alcohol, kaunavir alcohol, seryl alcohol, melisyl alcohol, or alkyl alcohols having a longer chain alkyl group; polyhydric alcohols such as sorbitol; Aliphatic amides such as methylenebisstearic acid amide, ethylenebiscapric acid amide, ethylenebislauric acid amide, hexamethylenebisstearic acid amide; ethylenebisoleic acid amide, hexamethylenebisoleic acid amide, N, N Unsaturated fatty acid amides such as' -dioleyl adipamide, N, N'-dioleyl sebacamide; aromatic compounds such as m-xylene bisstearic acid amide and N, N'-distearyl isophthalic acid amide Bisamides; aliphatic metal salts such as calcium stearate, calcium laurate, zinc stearate, and magnesium stearate (commonly referred to as metallic soaps); partial esterified products of fatty acids such as behenic acid monoglyceride and polyhydric alcohols; Examples include a methyl ester compound having a hydroxyl group obtained by hydrogenating an oil or fat.

As the wax grafted with the vinyl monomer, there is a wax obtained by grafting an aliphatic hydrocarbon wax with a vinyl monomer such as styrene or acrylic acid.

Preferred waxes include polyolefins obtained by radical polymerization of olefins under high pressure;
A polyolefin obtained by purifying a low molecular weight by-product obtained during polymerization of a high molecular weight polyolefin; a polyolefin polymerized under a low pressure using a catalyst such as a Ziegler catalyst or a metallocene catalyst; a polyolefin polymerized using radiation, electromagnetic waves or light; paraffin wax , Microcrystalline wax, Fischer-Tropsch wax; synthetic hydrocarbon wax synthesized by the Zintall method, hydrocoll method, Aage method, etc .; synthetic wax using a compound having one carbon atom as a monomer; hydroxyl group, carboxyl group or ester group; A hydrocarbon wax having a functional group; a mixture of a hydrocarbon wax and a hydrocarbon wax having a functional group; styrene, maleic ester, acrylate, methacrylate, and maleic anhydride based on the wax. Waxes obtained by graft-modified with such vinyl monomers.

Further, these waxes may be obtained by sharpening the molecular weight distribution using a press sweating method, a solvent method, a recrystallization method, a vacuum distillation method, a supercritical gas extraction method or a liquid crystal deposition method, or a low molecular weight solid fatty acid. , Low molecular weight solid alcohol,
Low molecular weight solid compounds and those from which other impurities have been removed are also preferably used.

[Resin] As the binder resin used in the present invention, various resin compounds conventionally known as binder resins can be used.
Phenol resin, natural resin modified phenolic resin, natural resin modified maleic resin, acrylic resin, methacrylic resin, polyvinyl acetate, silicone resin, polyester resin, polyurethane, polyamide resin, furan resin, epoxy resin, xylene resin, polyvinyl butyral, terpene Resin, coumaroindene resin, petroleum resin and the like. Among them, vinyl resins and polyester resins are preferred in terms of chargeability and fixability.

Examples of the vinyl resin include styrene;
o-methylstyrene, m-methylstyrene, p-methylenestyrene, p-methoxystyrene, p-phenylstyrene, p-chlorostyrene, 3,4-dichlorostyrene, p-ethylstyrene, 2,4-dimethylstyrene,
such as pn-butylstyrene, p-tert-butylstyrene, pn-hexylstyrene, pn-octylstyrene, pn-nonylstyrene, pn-decylstyrene, pn-dodecylstyrene Styrene derivatives;
Ethylene unsaturated monoolefins such as ethylene, propylene, butylene, and isobutylene; unsaturated polyenes such as butadiene; vinyl halides such as vinyl chloride, vinylidene chloride, vinyl bromide, and vinyl fluoride; vinyl acetate, vinyl propionate , Vinyl esters such as vinyl benzoate; methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-butyl methacrylate;
Isobutyl methacrylate, n-octyl methacrylate,
Dodecyl methacrylate, 2-ethylhexyl methacrylate, stearyl methacrylate, phenyl methacrylate,
Α-methylene aliphatic monocarboxylic esters such as dimethylaminoethyl methacrylate and diethylaminoethyl methacrylate; methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, propyl acrylate, n-octyl acrylate Acrylates such as dodecyl acrylate, 2-ethylhexyl acrylate, stearyl acrylate, 2-chloroethyl acrylate and phenyl acrylate; vinyl ethers such as vinyl methyl ether, vinyl ethyl ether and vinyl isobutyl ether; vinyl methyl ketone ,
Vinyl ketones such as vinylhexyl ketone and methyl isopropenyl ketone; N-vinyl compounds such as N-vinylpyrrole, N-vinylcarbazole, N-vinylindole and N-vinylpyrrolidone; vinylnaphthalenes:
Acrylic acid or methacrylic acid derivatives such as acrylonitrile, methacrylonitrile, acrylamide; α, β
Esters of unsaturated acids, diesters of dibasic acids; acrylic acids such as acrylic acid, methacrylic acid, α-ethylacrylic acid, crotonic acid, cinnamic acid, vinyl acetic acid, isocrotonic acid, angelic acid and α- or β thereof -Alkyl derivatives; vinyl monomers such as fumaric acid, maleic acid, citraconic acid, alkenyl succinic acid, itaconic acid, mesaconic acid, dimethyl maleic acid, dimethyl fumaric acid and other unsaturated dicarboxylic acids and monoester derivatives or anhydrides thereof. The used polymer is mentioned. In the vinyl resin, the above-mentioned vinyl monomers are used alone or in combination of two or more. Among these, a combination of monomers that results in a styrene copolymer or a styrene-acrylic copolymer is preferred.

Further, the binder resin used in the present invention may be a polymer or a copolymer cross-linked with a cross-linkable monomer as exemplified below, if necessary.

As the crosslinkable monomer, a monomer having two or more crosslinkable unsaturated bonds can be used. As such a crosslinkable monomer, various monomers as shown below have been conventionally known, and can be suitably used for the toner of the present invention.

Examples of the crosslinkable monomer include aromatic divinyl compounds such as divinylbenzene and divinylnaphthalene; and diacrylate compounds linked by an alkyl chain such as ethylene glycol diacrylate and 1,3-butylene glycol. Diacrylate,
1,4-butanediol diacrylate, 1,5-pentanediol diacrylate, 1,6-hexanediol diacrylate, neopentyl glycol diacrylate, and those obtained by replacing the acrylate of the above compounds with methacrylate; ether bond Examples of the diacrylate compounds linked by an alkyl chain containing: diethylene glycol diacrylate, triethylene glycol diacrylate, tetraethylene glycol diacrylate, polyethylene glycol # 400 diacrylate, polyethylene glycol # 600 diacrylate, dipropylene glycol Diacrylates and acrylates of the above compounds in place of methacrylates; diacrylates linked by chains containing aromatic groups and ether linkages Examples of the compounds include polyoxyethylene (2) -2,2-bis (4-hydroxyphenyl) propane diacrylate, polyoxyethylene (4) -2,2-bis (4-hydroxyphenyl) propane diacrylate and The acrylates of the above compounds may be used in place of methacrylates; examples of polyester type diacrylates include the trade name MANDA
(Nippon Kayaku) and the like.

As the polyfunctional crosslinking agent, pentaerythritol triacrylate, trimethylolethane triacrylate, trimethylolpropane triacrylate, tetramethylolmethanetetraacrylate, oligoester acrylate, and acrylates of the above compounds replaced with methacrylate; Triallyl cyanurate, triallyl trimellitate and the like.

As the binder resin used in the present invention, the following polyester resins are also preferable. It is preferable that 45 to 55 mol% of the polyester resin is an alcohol component and 55 to 45 mol% is an acid component.

Examples of the alcohol component include ethylene glycol, propylene glycol, 1,3-butanediol, 1,4-butanediol, 2,3-butanediol, diethylene glycol, triethylene glycol,
1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, 2-ethyl-1,3-hexanediol, hydrogenated bisphenol A, the following (B)
A bisphenol derivative represented by the formula:

[0037]

Embedded image

(Wherein R represents an ethylene or propylene group, x and y are each an integer of 1 or more, and the average value of x + y is 2 to 10.) The diols represented by the formula (C) ;

[0039]

Embedded image Or polyhydric alcohols such as glycerin, sorbit, and sorbitan.

Preferred examples of the acid component include carboxylic acids. Examples of the divalent carboxylic acid include benzenedicarboxylic acids such as phthalic acid, terephthalic acid, isophthalic acid and phthalic anhydride or anhydrides thereof; Alkyl dicarboxylic acids such as succinic acid, adipic acid, sebacic acid, and azelaic acid or anhydrides thereof; unsaturated dicarboxylic acids such as fumaric acid, maleic acid, citraconic acid, and itaconic acid or anhydrides thereof; Examples of the carboxylic acid having a valency or higher include trimellitic acid, pyromellitic acid, benzophenonetetracarboxylic acid and anhydrides thereof.

The particularly preferred alcohol component of the polyester resin is a bisphenol derivative represented by the above formula (B), and the preferred acid component is phthalic acid, terephthalic acid, isophthalic acid or its anhydride, succinic acid, n-dodecenylsuccinic acid. Or dicarboxylic acids such as anhydrides, fumaric acid, maleic acid, and maleic anhydride; and trimellitic acids or tricarboxylic acids of anhydrides thereof. This is because a toner for fixing a heat roller using a polyester resin obtained from the acid component and the alcohol component as a binder resin has good fixability and excellent offset resistance.

[Magnetic Material] When the toner of the present invention is used as a magnetic toner, the magnetic material contained in the magnetic toner is not particularly limited as long as it is a generally used magnetic material, and examples thereof include magnetite, maghemite, and ferrite. Oxides, such as iron oxides and other metal oxides; F
e, metals such as Co, Ni, or these metals and Al, Co, Cu, Pb, Mg, Ni, Sn, Zn, S
b, Be, Bi, Cd, Ca, Mn, Se, Ti, W,
Alloys with metals such as V, and mixtures thereof.

Specifically, examples of the magnetic material include iron trioxide (Fe ₃ O ₄ ), iron sesquioxide (γ-Fe ₂ O ₃ ), yttrium iron oxide (Y ₃ Fe ₅ O ₁₂ ), and iron oxide. Cadmium (C
dFe ₂ O ₄ ), iron gadolinium oxide (Gd ₃ Fe)
₅ O ₁₂ ), iron oxide copper (CuFe ₂ O ₄ ), iron oxide lead (Pb
Fe ₁₂ O ₁₉ ), nickel iron oxide (NiFe ₂ O ₄ ), iron oxide niodymium (NdFe ₂ O ₃ ), barium oxide (BaF)
e ₁₂ O ₁₉ ), magnesium iron oxide (MgFe ₂ O ₄ ), lanthanum iron oxide (LaFeO ₃ ), iron powder (Fe), cobalt powder (Co), nickel powder (Ni) and the like. The above-mentioned magnetic materials are used alone or in combination of two or more. Particularly preferred magnetic materials are triiron tetroxide or γ-
It is a fine powder of iron sesquioxide.

These ferromagnetic materials have an average particle size of 0.05 to
At 2 μm, the magnetic properties at 795.8 kA / m applied are coercive force of 1.6 to 12.0 kA / m and saturation magnetization of 50 to 200 A
Those having m ² / kg (preferably 50 to 100 Am ² / kg) and residual magnetization of ^{2 to 20} Am ² / kg are preferable for use in the image forming method of the present invention, particularly, the electrophotographic image forming method.

Further, these magnetic materials are used as binder resin 100
It is preferable that the content is 60 to 200 parts by mass, more preferably 80 to 150 parts by mass with respect to parts by mass.

[Colorant] As described above, a magnetic material may be used as a colorant in the toner of the present invention, but a nonmagnetic colorant or the like may be used as another colorant. Such non-magnetic colorants include any suitable pigments or dyes. For example, examples of pigments include carbon black, aniline black, acetylene black, naphthol yellow, hansa yellow, rhodamine lake, vengar, phthalocyanine blue, and indanthrene blue. These have a good addition amount of 0.1 to 20 parts by mass, preferably 1 to 10 parts by mass, based on 100 parts by mass of the binder resin. Similarly, a dye is used, and a binder resin 10 is used.
0.1 to 20 parts by mass, preferably 0.3 to 0 parts by mass
The addition amount of 10 to 10 parts by mass is good.

As the colorant used in the present invention, a black colorant which is obtained by using carbon black, a magnetic substance, and a yellow / magenta / cyan colorant shown below as a black colorant is used.

As a yellow colorant, a condensed azo compound, an isoindolinone compound, an anthraquinone compound,
A compound represented by an azo metal complex, a methine compound or an allylamide compound is used. Specifically, C.I. I. Pigment Yellow 12, 13, 14, 15, 17, 6
2, 74, 83, 93, 94, 95, 97, 109, 1
10, 111, 120, 127, 128, 129, 14
7, 168, 174, 176, 180, 181, 191
Etc. are preferably used.

Examples of the magenta colorant include condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinones, quinacdrine compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds and perylene compounds. Specifically, C.I.
I. Pigment Red 2, 3, 5, 6, 7, 23, 4
8: 2, 48: 3, 48: 4, 57: 1, 81: 1, 1
44, 146, 166, 169, 177, 184, 18
5, 202, 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 can be used particularly preferably.

[Charge Control Agent] In the toner of the present invention, a charge control agent can be used if necessary in order to further stabilize the chargeability. The charge control agent is a binder resin 10
0.1 to 10 parts by mass, preferably 1 to 5 parts by mass per 0 parts by mass
It is preferable to use parts by mass in order to control the chargeability of the toner.

As the charge control agent, various types of charge control agents conventionally known can be used. Examples thereof include the following.

As a negative charge controlling agent for making the toner negatively chargeable, for example, an organometallic complex or a chelate compound is effective. Examples thereof include a monoazo metal complex, a metal complex of an aromatic hydroxycarboxylic acid, and a metal complex of an aromatic dicarboxylic acid. Others include aromatic hydroxycarboxylic acids, aromatic mono- and polycarboxylic acids and metal salts thereof, anhydrides thereof,
Or an ester thereof, or a phenol derivative of bisphenol. Preferred are monoazo metal compounds, wherein the substituent is an alkyl group,
Monoazo dyes synthesized from phenols and naphthols having halogen, nitro group, carbamoyl group, etc.
Metallic compounds of r, Co, and Fe are listed. Further, a metal compound of an aromatic carboxylic acid is also preferably used, and an alkyl group, a halogen, a nitro group or the like, benzene, naphthalene, anthracene, phenanthrene carboxylic acid,
Examples include hydroxycarboxylic acid and metal compounds of dicarboxylic acids.

Examples of the positive charge control agent that makes the toner positively chargeable include nigrosine, nigrosine derivatives, triphenylmethane compounds, and organic quaternary ammonium salts. For example, denatured products such as nigrosine and fatty acid metal salts, tributylbenzylammonium-1-hydroxy-4-naphthosulfonate, quaternary ammonium salts such as tetrabutylammonium tetrafluoroborate,
And onium salts such as phosphonium salts, which are analogs thereof, and their lake pigments, triphenylmethane dyes, and these lake pigments (as the lake-forming agent, phosphotungstic acid, phosphomolybdic acid, phosphotungsten molybdic acid, tannic acid) , Lauric acid, gallic acid, ferricyanide, ferrocyanide), metal salts of higher fatty acids; diorganotin oxides such as dibutyltin oxide, dioctyltin oxide, dicyclohexyltin oxide; dibutyltin borate, dioctyltin borate, dicyclohexyltin borate Diorganotin borates; these can be used alone or in combination of two or more.

[External Additives] As described above, the toner of the present invention generally contains, in addition to the toner particles, an external additive for adjusting the fluidity and chargeability of the toner. As such an external additive, a fluidity improver may be added to the toner of the present invention. The fluidity improver can be added to the toner particles to increase the fluidity before and after the addition. For example, fluororesin powder such as vinylidene fluoride fine powder; fine silica powder such as wet-process silica and dry-process silica, fine-powder titanium oxide, fine-powder alumina, and a silane compound, a titanium coupling agent, and a silicone oil. There is a treated fine powder or the like that has been subjected to the treatment.

The method for imparting hydrophobicity is provided by chemically treating an organic silicon compound or the like which reacts or physically adsorbs with fine powder.

Examples of the organosilicon compound include hexamethyldisilazane, trimethylsilane, trimethylchlorosilane, trimethylethoxysilane, dimethyldichlorosilane, methyltrichlorosilane, allyldimethylchlorosilane, allylphenyldichlorosilane, benzyldimethylchlorosilane, and bromomethtridimethyl. Chlorosilane,
α-chloroethyltrichlorosilane, β-chloroethyltrichlorosilane, chloromethyldimethylchlorosilane, triorganosilylmercaptan, trimethylsilylmercaptan, triorganosilyl acrylate, vinyldimethylacetoxysilane, dimethylethoxysilane, dimethyldimethoxysilane, diphenyldiethoxysilane, Hexamethyldisiloxane, 1,3-divinyltetramethyldisiloxane, 1,3-diphenyltetramethyldisiloxane and Si having 2 to 12 siloxane units per molecule and one for each terminal unit. And a dimethylpolysiloxane having a hydroxyl group bonded thereto. Further, a silicone oil such as dimethyl silicone oil may be used. These are used in one kind or in a mixture of two or more kinds.

As the particles having a particle size of 0.1 to 5.0 μm used in the present invention, inorganic fine particles, organic fine particles, and mixtures and composites thereof can be used. Specifically, strontium titanate, cerium oxide, aluminum oxide,
Examples include metal oxides such as magnesium oxide and the like, fluororesin powder, resin fine particles, and the like. Particularly, strontium titanate and cerium oxide are preferable in terms of charging characteristics.

[Charge Control Agent II] The toner of the present invention preferably contains a charge control agent.

The following compounds can be used to control the toner to be negatively charged.

Organic metal complexes and chelate compounds are effective, and examples thereof include monoazo metal complexes, acetylacetone metal complexes, aromatic hydroxycarboxylic acids, and metal complexes of aromatic dicarboxylic acids. Other examples include aromatic hydroxycarboxylic acids, aromatic mono- and polycarboxylic acids and their metal salts, anhydrides, esters, and phenol derivatives of bisphenol.

Among them, an azo metal complex represented by the following formula (1) is preferable.

[0063]

Embedded image [Wherein, M represents a coordination center metal, and Sc, Ti, V, C
r, Co, Ni, Mn or Fe. Ar
Is an aryl group, is an aryl group such as a phenyl group and a naphthyl group, and may have a substituent. Examples of the substituent in this case include a nitro group, a halogen group, a carboxyl group, an anilide group, an alkyl group having 1 to 18 carbon atoms, and an alkoxy group having 1 to 18 carbon atoms. X, X ', Y and Y' are -O-, -CO-, -NH-, -NR- (R is an alkyl group having 1 to 4 carbon atoms). C ⁺ represents a counter ion, and represents hydrogen, sodium, potassium, ammonium, aliphatic ammonium or a mixed ion thereof. ]

In particular, Fe or Cr is preferable as the central metal, halogen, an alkyl group or an anilide group is preferable as the substituent, and hydrogen or hydrogen is used as the counter ion.
Alkali metals, ammonium or aliphatic ammonium are preferred. A mixture of complex salts having different counter ions is also preferably used.

A basic organometallic complex represented by the following formula (2) is also preferable as a charge control agent imparting negative charge.

[0066]

Embedded image

The following compounds control the toner to be positively charged.

Modified nigrosine with nigrosine and fatty acid metal salts, etc .; tributylbenzylammonium-1-
Quaternary ammonium salts such as hydroxy-4-naphthosulfonate and tetrabutylammonium tetrafluoroborate, and onium salts such as phosphonium salts, which are analogs thereof, and lake pigments thereof; triphenylmethane dyes and lake pigments thereof (Examples of the lake-forming agent include phosphotungstic acid, phosphomolybdic acid, phosphotungsten molybdic acid, tannic acid, lauric acid, gallic acid, ferricyanide, ferrocyanide); metal salts of higher fatty acids; dibutyltin oxide, dioctyltin Diorganotin oxides such as oxide and dicyclohexyltin oxide; diorganotin borates such as dibutyltin borate, dioctyltin borate and dicyclohexyltin borate; guanidine compounds; imidazole Compounds, and the like. These can be used alone or in combination of two or more.

Among these, a triphenylmethane compound and a quaternary ammonium salt whose counter ion is not halogen are preferably used. The following equation (3)

[0070]

Embedded image [In the formula, R ₁ represents H or CH ₃ , and R ₂ and R ₃ represent a substituted or unsubstituted alkyl group (preferably C ₁ -C ₄ ). And a copolymer with a polymerizable monomer such as styrene, acrylate or methacrylate described above can be used as the positive charge control agent. In this case, the homopolymer and the copolymer have a function as a charge control agent and a function as (all or part of) a binder resin.

Particularly, the compound represented by the following formula (4) is preferable as the toner positive charge control agent of the present invention.

[0072]

Embedded image [Wherein, R ₁ , R ₂ , R ₃ , R ₄ , R ₅ and R ₆ may be the same or different from each other, and include a hydrogen atom, a substituted or unsubstituted alkyl group, or a substituted or unsubstituted alkyl group. Represents an aryl group. R ₇ , R ₈ and R ₉ may be the same or different from each other and represent a hydrogen atom, a halogen atom, an alkyl group or an alkoxy group. A ^- is a sulfate ion,
Anions such as nitrate ion, borate ion, phosphate ion, hydroxyl ion, organic sulfate ion, organic sulfonate ion, organic phosphate ion, carboxylate ion, organic borate ion and tetrafluoroborate are shown. ]

As a method for incorporating the charge control agent into the toner, there are a method of adding the charge control agent inside the toner particles and a method of externally adding the charge control agent. The use amount of these charge control agents is determined by the type of the binder resin, the presence or absence of other additives, the toner manufacturing method including the dispersion method, and is not limited to a specific one. Preferably it is used in the range of 0.1 to 10 parts by mass, more preferably 0.1 to 5 parts by mass, based on 100 parts by mass of the binder resin.

Next, a procedure for producing a toner by the method for producing a toner of the present invention using the above-described toner particle forming material and external additives will be described. First, in the raw material mixing step, a predetermined amount of at least a resin and a colorant are weighed and blended as the toner internal additive, and are mixed. Examples of the mixing device include a double-con mixer, a V-type mixer, a drum-type mixer, a super mixer, a Henschel mixer, and a Nauta mixer.

Further, the toner materials mixed and mixed as described above are melt-kneaded to melt the resins, and the colorant and the like are dispersed therein. In the melt kneading step, for example, a batch kneader such as a pressure kneader or a Banbury mixer or a continuous kneader can be used. In recent years, single-screw or twin-screw extruders have become the mainstream due to their superiority such as continuous production. For example, KTK-type twin-screw extruders manufactured by Kobe Steel, TEM-type twin-screw extruders manufactured by Toshiba Machine Co., Ltd. A twin screw extruder manufactured by Kay Kay Co., Ltd., a PCM type twin screw extruder manufactured by Ikegai Iron Works,
A bus kneader or the like is generally used. Furthermore,
The colored resin composition obtained by melt-kneading the toner raw material is rolled by two rolls or the like after melt-kneading, and then cooled through a cooling step of cooling with water cooling or the like.

The cooled product of the colored resin composition obtained as described above is then crushed to a desired particle size in a crushing step.
In the pulverization step, first, coarse pulverization is performed by a crusher, a hammer mill, a feather mill, or the like, and further finely pulverized by a mechanical pulverizer. In the pulverizing step, the toner is pulverized stepwise to a predetermined toner particle size. Further, after the pulverization, the toner is classified using a classifier such as an inertial classification type elbow jet, a centrifugal force classification type microplex, or a DS separator to obtain a toner having an average particle diameter of 4 to 12 μm. Among these, a multi-split airflow classifier is particularly preferred as the classifier.

As an example of a preferred multi-split air classifier, an apparatus of the type shown in FIG. 4 (cross-sectional view) will be illustrated and described as a specific example.

In FIG. 4, the side wall 22 and the G block 2
3 forms part of the classification chamber, the classification edge blocks 24 and 25 are provided with classification edges 17 and 18. The installation position of the G block 23 can be slid right and left. Further, the classification edges 17 and 18 correspond to the shaft 17a.
And 18a can be rotated, and the classification edge can be rotated to change the classification edge tip position.
Each of the classifying edge blocks 24 and 25 can be slid right and left, and accordingly, the respective knife-edge classifying edges 17 and 18 also slide right and left. The classification area 30 of the classification chamber 32 is divided into three by the classification edges 17 and 18.

Raw material supply port 40 for introducing raw material powder
At the rear end of the material supply nozzle 16, a high pressure air supply nozzle 41 and a material powder introduction nozzle 42 at the rear end of the material supply nozzle 16, and an opening in the classifying chamber 32. The nozzle 16 is provided on the right side of the side wall 22, and the Coanda block 26 is provided so as to draw a long elliptical arc in the extending direction of the lower tangent of the raw material supply nozzle 16.
The left block 27 of the classifying chamber 32 has a knife-edge type inlet edge 19 on the right side of the classifying chamber 32, and further, on the left side of the classifying chamber 32, there are provided inlet pipes 14 and 15 opening to the classifying chamber 32. It is. In addition, as shown in FIG.
4 and 15 are provided with a first gas introduction adjusting means 20, a second gas introduction adjusting means 21, such as a damper, and a static pressure gauge 28 and a static pressure gauge 29.

The positions of the classification edges 17 and 18, the G block 23 and the inlet edge 19 are adjusted according to the type of the toner to be classified and the desired particle size.

Further, on the upper surface of the classifying chamber 32, the outlets 11, 1 opening into the classifying chamber corresponding to the respective dividing areas.
2 and 13, and communication means such as a pipe is connected to the discharge ports 11, 12 and 13, and each of them may be provided with an opening / closing means such as a valve means.

The raw material supply nozzle 16 is composed of a right-angled cylinder and a pyramidal cylinder. The ratio of the inner diameter of the right-angled cylinder to the inner diameter of the narrowest part of the pyramidal cylinder is 20: 1 to 1: 1, preferably 10: 1. : 1
If the ratio is set to 2: 1 from, a good introduction speed can be obtained.

The classification operation in the multi-division classification region configured as described above is performed, for example, as follows. That is, the pressure in the classification chamber is reduced through at least one of the discharge ports 11, 12, and 13, and the air flow flowing by the reduced pressure and the high-pressure air supply nozzle 41 in the raw material supply nozzle 16 having an opening in the classification chamber are injected. Due to the ejector effect of the compressed air, the powder is jetted into the classifying chamber through the raw material supply nozzle 16 at a flow rate of preferably 10 to 350 m / sec, and dispersed.

The particles in the powder introduced into the classifying chamber move in a curved line due to the action of the Coanda block 26 and the action of gas such as air flowing in at that time. Depending on the particle size and the magnitude of the inertial force, large particles (coarse particles) are outside the airflow, ie, the first fraction outside the classification edge 18, and intermediate particles are the second fraction between the classification edges 18 and 17. , The small particles are classified into a third fraction inside the classification edge 17, the classified large particles are discharged from the outlet 11, the intermediate classified particles are discharged from the outlet 12, and the classified small particles are discharged. Are respectively discharged from the discharge ports 13.

In the above-described classification of the powder, the classification point is mainly determined by the edge tip positions of the classification edges 17 and 18 with respect to the lower end portion of the Coanda block 26 where the powder jumps into the classification chamber 32. Further, the classification point is affected by the suction flow rate of the classification airflow, the speed at which the powder is ejected from the raw material supply nozzle 16, and the like.

The multi-split airflow classifier described above is particularly effective for classifying toner or toner colored resin powder used in an image forming method by electrophotography.

Further, in the multi-split air classifier of the type shown in FIG. 4, a raw material supply nozzle, a raw material powder introduction nozzle, and a high pressure air supply nozzle are provided on the upper surface of the multi-split air flow classifier, and the classification edge is provided. Since the position of the classifying edge block provided with the classifier can be changed so that the shape of the classifying area can be changed, the classification accuracy can be remarkably improved as compared with the conventional airflow classifier.

The toner coarse powder generated by the classification in the classification step is returned to the pulverization step again and pulverized. The fine powder generated in the classification step may be returned to the toner raw material mixing step and reused.

Further, in the method for producing a toner of the present invention, inorganic fine particles having an average particle size of at least 50 nm or less are externally added to the toner obtained as described above. As a method of externally adding an external additive to the toner, a predetermined amount of the classified toner and various known external additives are blended, and a high-speed stirrer for applying a shearing force to powder such as a Henschel mixer or a super mixer is used. It is preferred that the mixture is used as an adder and stirred and mixed. At this time, heat is generated inside the external additive machine and aggregates are easily generated. Therefore, it is preferable to adjust the temperature by means such as cooling the periphery of the container of the external additive machine with water.

Next, a mechanical pulverizer used in the toner pulverization step of the present invention and a method for producing a toner using the mechanical pulverizer will be specifically described with reference to the drawings.

FIG. 1 shows an example of a toner particle pulverizing apparatus system incorporating a mechanical pulverizer used in the present invention.
FIG. 2 is a schematic sectional view taken along the line DD ′ in FIG. 1, and FIG. 3 is a perspective view of the rotor rotating at high speed in FIG.

In the mechanical pulverizer shown in FIG. 1, a high-speed machine comprising a casing 313, a jacket 316 in the casing 313 through which cooling water can pass, and a rotating body in the casing 313 attached to the central rotating shaft 312 is provided. A rotor 314 provided with a number of grooves on a rotating surface, a stator 310 provided with a number of grooves on a surface arranged at a constant interval on the outer periphery of the rotor 314, and
It comprises a raw material inlet 311 for introducing a raw material to be processed and a raw material outlet 302 for discharging powder after processing. The gap between the rotor 314 and the stator 310 is a crushing zone.

In the mechanical pulverizer configured as described above, when a predetermined amount of powder raw material is supplied from the quantitative feeder 315 shown in FIG. 1 to the raw material input port 311 of the mechanical pulverizer,
The particles are introduced into the crushing processing chamber, and a rotor 314 having a large number of corrugated grooves provided on a surface rotating at a high speed in the crushing processing chamber and a fixed member having a large number of corrugated grooves provided on the surface. The instantaneous crushing is caused by the generated shock between the child 310 and the numerous super-high-speed vortices generated behind the generated shock, and the high-frequency pressure vibration generated thereby. After that, it is discharged through the raw material discharge port 302. The air (toner) carrying the toner particles passes through the pulverization processing chamber and is discharged out of the system of the apparatus system through the raw material discharge port 302, the pipe 219, the collection cyclone 229, the bag filter 222, and the suction blower 224. Is done.

As such mechanical pulverization, for example,
P-type, M-type, E-type, R-type, and EX- of Hosokawa Micron Co., Ltd. pulverizer Inomaizer, Kawasaki Heavy Industries Co., Ltd. pulverizer Cryptolin, Turbo Kogyo Co., Ltd.
And RS-type.

A feature of the mechanical pulverizer of the present invention is that the surface roughness of the pulverized surface of the rotor is different from the surface roughness of the pulverized surface of the stator.

Further, the feature of the method for producing the toner of the present invention is that the surface roughness of the pulverized surface of the rotor in the mechanical pulverizer is
The purpose is to pulverize the toner using a mechanical pulverizer whose surface roughness is controlled to an appropriate state so that the surface roughness of the pulverized surface of the stator is different.

That is, as a result of the study by the present inventor, the relationship between the center line average roughness Ra of the crushing surface of the rotor and the center line average roughness Ra of the crushing surface of the stator in the mechanical crusher is expressed by the following equation. Stator crushing surface Ra <stator crushing surface Ra and stator crushing surface Ra
-Rotor grinding surface Ra ≧ 1.0 μm (more preferably, 1.
0 to 10.0 μm); the relationship between the maximum height Ry of the crushing surface of the rotor and the maximum height Ry of the crushing surface of the stator is
Rotor grinding surface Ry <stator grinding surface Ry, and stator grinding surface Ry−rotor grinding surface Ry ≧ 10.00 μm (more preferably 10.0 to 60.0 μm); The relationship between the ten-point average roughness Rz and the ten-point average roughness Rz of the crushed surface of the stator is as follows: rotor crushed surface Rz <stator crushed surface Rz, and stator crushed surface Rz-rotor crushed surface Rz
≧ 10.0 μm (more preferably 10.0 to 40.0
μm) is preferably satisfied.

Further, in the method for producing a toner according to the present invention, the center line average roughness Ra of the pulverized surface of the rotor is 2.0 μm.
m (more preferably 0.5 to 1.8 μm), a maximum height Ry of less than 25.0 μm (more preferably 3.0 to 24.8 μm), and a ten-point average roughness Rz of 20. Less than 0 μm (more preferably 2.0 to 19.8
μm), and the center line average roughness of the ground surface of the stator is Ra.
Is 2.0 μm or more (more preferably, 2.0 to 10.0
μm), the maximum height Ry is 25.0 μm or more (more preferably, 25.0 to 60.0 μm), and the ten-point average roughness Rz is 20.0 μm or more (more preferably, 20.mu.m).
0 to 40.0 μm).

That is, by setting the center line average roughness Ra, the maximum height Ry, and the ten-point average roughness Rz of the crushed surfaces of the rotor and the stator to the above values, excessive pulverization of the toner is prevented. It can sharpen the particle size distribution of the toner, reduce the amount of fine powder generated, and can arbitrarily control the surface shape of the toner, and have good developability, transferability, and stable chargeability from the beginning even under a high temperature and high humidity environment In addition, a long-life toner can be obtained, and a toner having a high image density can be obtained from the beginning and after standing, and further, a toner having excellent durability on many sheets can be obtained.

As a result of the investigations by the present inventors, it is considered that the particle size distribution and the surface shape of the toner depend on the surface roughness of the crushed surfaces of the rotor and the stator. It is considered that the influence of the surface roughness of the pulverized surface is large. In the present invention, the surface roughness of the grinding surface of the rotor,
By varying the surface roughness of the crushed surface of the stator, the surface shape of the toner can be arbitrarily controlled, and in the present invention, the surface roughness of the crushed surface of the rotor is lower than the surface roughness of the crushed surface of the stator. By setting, when the toner is introduced into a large number of corrugated grooves on the rotor surface and pulverized, the impact force on the toner can be reduced, so that excessive pulverization of the toner can be prevented and the amount of generated fine powder can be suppressed. It is believed that the particle size distribution of the toner can be sharpened.

In the present invention, regarding the surface treatment of the crushed surfaces of the rotor and the stator in the mechanical crusher, any one that can control the surface roughness of the crushed surfaces of the rotor and the stator within the above range can be used. It is not limited at all. Also, the shape of the rotor and the stator in the mechanical pulverizer is not limited at all.

Here, the value of each analysis parameter of the surface roughness is measured by a laser focus displacement meter L capable of non-contact measurement.
Measurement was performed using T-8100 (manufactured by Keyence Corporation) and surface shape measurement software Tres-Vale Lite (manufactured by Mitani Shoji Co., Ltd.). It was determined from the value. At this time, the reference length was set to 8 mm, the cutoff value was set to 0.8 mm, and the moving speed was set to 90 μm /
It was measured as sec.

In the analysis parameters of the surface roughness,
The "center line average roughness Ra" is obtained by extracting a portion of the reference length L from the roughness curve in the direction of the center line, setting the center line of the extracted portion as the X axis, and the direction of the vertical magnification as the Z axis. When the curve is represented by Z = f (x), it is determined by obtaining the following equation.

[0104]

(Equation 1)

The “maximum height Ry” is extracted from the roughness curve by a reference length in the direction of the average line, and the distance between the peak and the valley bottom of the extracted portion is determined by the direction of the longitudinal magnification of the roughness curve. To be determined. "Ten-point average roughness Rz" is a value obtained by extracting a reference length from the roughness curve in the direction of the average line and measuring the average length of the extracted portion in the direction of the vertical magnification from the highest peak to the fifth peak. It is determined by calculating the sum of the average of the absolute values of the peak elevations and the average of the absolute values of the valley bottom elevations from the lowest valley bottom to the fifth.

Further, in the method for producing a toner according to the present invention, the rotor and the stator are pulverized by a mechanical pulverizer in which the surface roughness of the pulverized surface is controlled, and a multi-divided airflow classification of the type shown in FIG. The specific surface area per unit volume Sb (m
² / cm ³ ) and the specific surface area St (m ² / c) per unit volume calculated from the weight average diameter assuming that the toner is a true sphere.
m ³ ) preferably satisfies Sb / St <1.8, and more preferably 1.25 ≦ Sb / St <1.
8 is preferably satisfied.

That is, the toner B crushed by the machine element crusher and classified by the multi-split airflow classifier of the type shown in FIG.
Specific surface area S per unit volume measured by ET method
b and weight average diameter (D4) assuming that the toner is a true sphere
Specific surface area St (St = 6)
/ D4) satisfies Sb / St <1.8 and further satisfies 1.25 ≦ Sb / St <1.8, so that good developability from the beginning even under a high temperature and high humidity environment can be achieved. A long-lasting toner having transferability and stable chargeability can be obtained. Further, a toner having a high image density can be obtained from the beginning and even after standing, and furthermore, it has excellent durability on many sheets. Can be obtained.

The specific surface area was measured according to the BET method using a specific surface area measuring apparatus, Autosorb 1 (manufactured by Yuasa Ionics Inc.), by adsorbing nitrogen gas on the sample surface, and calculating the specific surface area using the BET multipoint method.

The average particle size and the particle size distribution of the toner were measured by using a Coulter Counter TA-II or Coulter Multisizer (manufactured by Coulter Inc.).
An interface for outputting volume distribution (manufactured by Nikkaki) and a PC9801 personal computer (manufactured by NEC) were connected, and the electrolyte was 1% Na
Prepare a Cl aqueous solution. For example, ISOTON R-
II (manufactured by Coulter Scientific Japan)
Can be used. As a measuring method, the electrolytic solution 100
0.1 to 5 ml of a surfactant (preferably an alkylbenzene sulfonate) is added as a dispersing agent to 150 ml, 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 by an ultrasonic disperser, and a 2 μm
The volume and the number of the toner were measured to calculate the volume distribution and the number distribution. Then, the volume-based weight average particle diameter (D4: the median value of each channel is a representative value of the channel) obtained from the volume distribution according to the present invention, and the cumulative number of toner particles of 10.08 μm or more obtained from the volume distribution And the cumulative number of toner particles of 4.00 μm or less obtained from the number distribution. Here, the coarse powder is defined as 10.08 μm or more, and the fine powder is defined as 4.00 μm or less. In other words, a smaller value between 10.08 μm and 4.00 μm indicates a sharper particle size distribution, and a larger value indicates a broader particle size distribution.

Next, when the pulverized raw material is pulverized by a mechanical pulverizer in which the surface roughness of the pulverized surfaces of the rotor and the stator is controlled to the above condition, the cold air generating means 319 is used to pulverize the pulverized raw material together with the pulverized raw material. Preferably, cold air is blown into the mechanical pulverizer. Further, the temperature of the cold air is preferably 0 to -30 ° C. Further, as the internal cooling means of the mechanical crusher main body, the mechanical crusher preferably has a structure having a jacket structure 316, and it is preferable to pass cooling water (preferably, antifreeze such as ethylene glycol). Further, by the above-mentioned cooling air device and jacket structure, the room temperature T1 in the spiral chamber 212 communicating with the powder inlet in the mechanical pulverizer is 0 ° C. or lower, more preferably −5 to −15 ° C., and still more preferably −.
The temperature is preferably from 7 to -12 ° C from the viewpoint of toner productivity. The room temperature T1 of the vortex chamber in the crusher is 0 ° C. or lower, more preferably −5 to −15 ° C., and still more preferably −7 to −1.
By setting the temperature to 2 ° C., it is possible to suppress surface deterioration of the toner due to heat, and it is possible to efficiently pulverize the pulverized raw material. If the room temperature T1 of the spiral chamber in the pulverizer exceeds 0 ° C., it is not preferable from the viewpoint of toner productivity because the surface of the toner is liable to be deteriorated due to heat during the pulverization and the internal fusing is likely to occur.

As the refrigerant used in the cold air generating means 319, an alternative chlorofluorocarbon is preferable from the viewpoint of environmental problems on the whole earth.

As alternative Freon, R134a, R40
4A, R407c, R410A, R507A, R717
Among them, R404A is particularly preferable from the viewpoint of energy saving and safety.

The cooling water (preferably an antifreeze such as ethylene glycol) is supplied into the jacket from a cooling water supply port 317 and discharged from a cooling water discharge port 318.

Further, the finely pulverized product generated in the mechanical pulverizer passes through the rear chamber 320 of the mechanical pulverizer and is supplied to the powder outlet 3.
02 is discharged outside the machine. At this time, it is preferable that the room temperature T2 of the rear chamber 320 of the mechanical pulverizer is 30 to 60 ° C. from the viewpoint of toner productivity. Rear chamber 3 of mechanical crusher
By setting the room temperature T2 of 30 to 30 to 60 ° C., it is possible to suppress surface deterioration of the toner due to heat, and it is possible to efficiently pulverize the raw material. If the temperature T2 of the mechanical pulverizer is lower than 30 ° C., a short path may occur without being pulverized, which is not preferable in terms of toner performance. On the other hand, when the temperature is higher than 60 ° C., the toner may be excessively pulverized at the time of pulverization, and the surface of the toner may be deteriorated by heat or may be easily fused in the apparatus.

When the pulverized raw material is pulverized by the mechanical pulverizer, the room temperature T1 of the spiral chamber 212 of the mechanical pulverizer and the rear chamber 3 are reduced.
The temperature difference ΔT (T2−T1) of the room temperature T2 of 20 is preferably 30 to 80 ° C., more preferably 35 to 75 ° C., and even more preferably 37 to 72 ° C. from the viewpoint of toner productivity. . ΔT between the temperature T1 and the temperature T2 of the mechanical pulverizer is 30 to 80 ° C, more preferably 35 to 75 ° C, and still more preferably 37 to 72 ° C.
By doing so, the deterioration of the surface of the toner due to heat can be suppressed, and the pulverized raw material can be efficiently pulverized. ΔT between the temperature T1 and the temperature T2 of the mechanical pulverizer is 35.
If the temperature is lower than ° C, short paths may occur without being pulverized, which is not preferable in terms of toner performance. On the other hand, if the temperature is higher than 80 ° C., the toner may be excessively pulverized at the time of pulverization, and the surface of the toner may be deteriorated by heat or may be easily fused in the apparatus.

When the pulverized raw material is pulverized by a mechanical pulverizer, the glass point transfer (Tg) of the binder resin is 45 to 7
5 ° C, more preferably 55 to 65 ° C. Further, the room temperature T1 of the spiral chamber 212 of the mechanical pulverizer is expressed by:
It is preferable that the temperature is 0 ° C. or lower and 60 to 75 ° C. lower than Tg from the viewpoint of toner productivity. The room temperature T1 of the spiral chamber 212 of the mechanical crusher is 0 ° C. or less and Tg
By lowering the temperature by 60 to 75 ° C., deterioration of the surface of the toner due to heat can be suppressed, and the pulverized raw material can be efficiently pulverized. Also, the rear chamber 3 of the mechanical crusher
The room temperature T2 of 20 is 5 to 30 ° C. higher than Tg, and furthermore,
Preferably, it is lower by 10 to 20 ° C. By lowering the room temperature T2 of the rear chamber 320 of the mechanical pulverizer by 5 to 30 ° C., more preferably 10 to 20 ° C. below Tg, it is possible to suppress the surface deterioration of the toner due to heat, and to efficiently pulverize the raw material. can do.

In the present invention, the glass transition point Tg of the binder resin is determined by a differential thermal analyzer (DSC measurement device),
-7 (manufactured by PerkinElmer) under the following conditions. Sample: 5 to 20 mg, preferably 10 mg Temperature curve: temperature rise I (20 ° C. → 180 ° C., temperature rise rate 10 ° C.)
/ Min. ) Cooling I (180 ° C → 10 ° C, cooling rate 10 ° C / mi
n. ) Heating II (10 ° C → 180 ° C, heating rate 10 ° C / mi)
n. ) Tg measured at the temperature rise II is defined as a measured value. Measurement method: Put the sample in an aluminum pan and use an empty aluminum pan as a reference. The intersection of the line at the midpoint of the baseline before and after the endothermic peak appeared and the differential heat curve was defined as the glass transition point Tg.

The peripheral speed of the tip of the rotating rotor 314 is preferably 80 to 180 m / sec, more preferably 90 to 170 m / sec, and still more preferably 100 to 160 m / sec. It is preferable in terms of properties. Rotating rotor 314
Peripheral speed of 80 to 180 m / sec, more preferably 9
0 to 170 m / sec, more preferably 100 to 1
By setting the speed to 60 m / sec, insufficient pulverization of the toner and excessive pulverization can be suppressed, and the pulverized raw material can be efficiently pulverized. If the peripheral speed of the rotor is lower than 80 m / sec, it is not preferable in terms of toner performance because a short path is easily generated without being pulverized. Also, the rotor 314
When the peripheral speed is higher than 180 m / sec, the load on the apparatus itself is increased, and at the same time, the toner is excessively pulverized at the time of pulverization.

The minimum distance between the rotor 314 and the stator 310 is preferably 0.5 to 10.0 mm, more preferably 1.0 to 5.0 mm, and still more preferably 1.0 to 5.0 mm. It is preferably 3.0 mm. Rotor 3
0.5 to 10.0 m between the stator 14 and the stator 310
m, more preferably 1.0 to 5.0 mm, and still more preferably 1.0 to 3.0 mm, it is possible to suppress insufficient pulverization of the toner and excessive pulverization, and to pulverize the pulverized raw material efficiently. it can. If the distance between the rotor 314 and the stator 310 is larger than 10.0 mm, it is not preferable in terms of toner performance because a short path is easily generated without being pulverized. If the distance between the rotor 314 and the stator 310 is smaller than 0.5 mm, the load on the apparatus itself increases, and at the same time, the toner is over-pulverized at the time of pulverization, and the surface of the toner is likely to deteriorate due to heat and fuse in the apparatus. Therefore, it is not preferable from the viewpoint of toner productivity.

[0120]

Next, the present invention will be described more specifically with reference to examples and reference examples of the present invention.

Example 1 Binder resin 100 parts by mass (Styrene-butyl acrylate-butyl maleate half ester copolymer) (Tg 62 ° C., molecular weight: Mp 13000, Mn 6400, Mw 2400000) Magnetic iron oxide 90 parts by mass (average particle diameter 0.22 [mu] m, 795.8 kA / m characteristic Hc5.1kA / m in a magnetic ^{field, σs85.1Am 2 /kg,σr5.1Am 2 / kg)} · monoazo metal complex (negative charge control agent) 2 parts by weight 3 parts by mass of low molecular weight ethylene-propylene copolymer The above-mentioned formulation was mixed with a Henschel mixer (FM-75).
After mixing well with a mold and a Mitsui Miike Kakoki Co., Ltd.), the mixture was kneaded with a biaxial kneader (PCM-30, manufactured by Ikegai Iron Works Co., Ltd.) set at a temperature of 130 ° C. The obtained kneaded material was cooled and coarsely pulverized to 1 mm or less with a hammer mill to obtain a powder raw material (coarse pulverized material) which is a powder raw material for toner production.

The obtained powdery raw material was converted into a mechanical pulverizer 301 (Turbo Mill T250-RS manufactured by Turbo Kogyo Co., Ltd.) shown in FIG.
The mold was finely pulverized with a remodeling machine modified as follows, and the obtained finely pulverized product was classified by a multi-split airflow classifier 1 shown in FIG.

In this embodiment, the surface roughness of the crushing surface of the rotor 314 of the mechanical crusher 301 is determined by calculating the center line average roughness Ra =
1.2 μm, the maximum height Ry = 15.1 μm, the ten-point average roughness Rz = 10.4 μm, and the surface roughness of the crushed surface of the stator 310 was determined as the center line average roughness Ra = 6.2 μm. Maximum height Ry = 41.1 μm, ten-point average roughness Rz = 32.
The thickness was 5 μm. Therefore, the center line average roughness R
a-Rotor stator grinding surface center line average roughness Ra is 5.0μ
m, the stator grinding surface maximum height Ry-the rotor stator grinding surface maximum height Ry is 26.0 μm, the stator grinding surface ten-point average roughness Rz—the rotor stator grinding surface ten-point average Roughness R
z was 22.1 μm.

Further, the peripheral speed of the rotor 314 is set to 115 m /
s, the gap between the rotor 314 and the stator 310 is 1.5 mm,
The pulverization was performed at a pulverization supply amount of 15 kg / Hr.

At this time, the temperature of the cold air is -15 ° C., the temperature T1 of the swirl inside the mechanical crusher is -10 ° C., and the temperature T
2 was 48 ° C., and ΔT of T1 and T2 was 58 ° C. Further, Tg-T1 was 72 ° C. and Tg-T2 was 14 ° C. At this time, the finely pulverized product obtained by pulverization with the mechanical pulverizer 301 has a weight average diameter of 6.9 μm, 40% by number of particles having a particle diameter of 4.00 μm or less, and a particle diameter of 1%.
It had a sharp particle size distribution containing 2% by volume of particles of 0.08 μm or more.

Next, the finely pulverized product obtained by pulverization by the mechanical pulverizer 301 is introduced into the airflow type classifier 1 having the structure shown in FIG. .9
A μm toner was obtained.

The BET specific surface area per volume Sb of the obtained toner was 1.36 m ² / cm ³ , and the theoretical specific surface area St per volume was 0.87 m ² / cm ³ . Therefore, S
b / St was 1.56. This is a mechanical crusher 30
This is probably because the surface roughness of the crushed surfaces of the first rotor 314 and the stator 310 was appropriately controlled.

To 100 parts by mass of the toner, 1.0 part by mass of dry silica having a primary particle diameter of 12 nm, which had been subjected to hydrophobic treatment with hexamethyldisilazane and silicone oil, was added, followed by external addition and mixing with a Henschel mixer. The evaluation toner 1 was obtained.

Using this toner, an LBP manufactured by Canon
An image output test was carried out by mounting the apparatus on a -930 modified machine, and the image characteristics of the toner were evaluated in the following items.

<Evaluation-1> The evaluation toner is put in a developing device and left overnight (12 hours or more) in a room temperature and normal humidity room (23 ° C., 60%). After 1000 images have been printed, the image density is measured. Take out the developing unit and place it in a high-temperature, high-humidity
%) Overnight (12 hours). After returning the developing device to the room temperature and normal humidity chamber, 20 images are immediately output and the image density is measured in the same manner as the previous day. The last day image density and the first sheet image density are compared. The evaluation level is confirmed by the difference between the density of the 1000th sheet (last day before) and the density after standing (the smaller the value, the better). In this example, as shown in Table 2, the density difference was 0.010 or less. ◎: density difference of 0.010 or less ○: density difference of 0.011 to 0.029 ○ △: density difference of 0.030 to 0.050 Δ: density difference of 0.060 to 0.100 Δ ×: density difference of 0.110 × 0.150 ×: density difference 0.160 to 0.200 XX: density difference 0.210 or more

The in-machine fusion after the operation was completed was visually confirmed and judged according to the following criteria. In this embodiment,
After the operation was completed, an inspection inside the machine showed that no fusion had occurred to the rotor and the stator. ○: No in-machine fusion △: In-machine fusion is slightly observed, but practical is possible ×: In-machine fusion is remarkable and practical is not practical

Example 2 The surface roughness of the pulverized surface of the rotor 314 of the mechanical pulverizer 301 was calculated by measuring the center line average roughness Ra =
0.7 μm, the maximum height Ry = 4.0 μm, the ten-point average roughness Rz = 2.8 μm, and the surface roughness of the crushed surface of the stator 310 is calculated as follows: center line average roughness Ra = 3.1 μm, maximum height Sa Ry
= 27.7 μm and ten-point average roughness Rz = 25.0 μm, to obtain Evaluation Toner 2 in the same manner as in Example 1.

Therefore, the center line average roughness Ra of the stator ground surface is
-Rotor stator grinding surface center line average roughness Ra is 2.4 μm
The maximum height Ry of the crushed surface of the stator-the maximum height Ry of the crushed surface of the rotor is 27.7 μm, and the ten-point average roughness of the crushed surface of the stator Rz-the ten-point average roughness of the crushed surface of the rotor. Rz
Was 25.0 μm.

When the powder raw material was pulverized by a mechanical pulverizer, the temperature of the cold air was -15 ° C, the temperature T1 of the swirl chamber in the mechanical pulverizer was -10 ° C, the temperature T2 of the rear chamber was 47 ° C, and T1 and T
The ΔT of 2 was 57 ° C. Tg-T1 is 72
° C and Tg-T2 were 15 ° C. The finely pulverized product obtained by pulverization with the mechanical pulverizer 301 at this time has a weight average diameter of 6.8 μm, 42% by number of particles having a particle diameter of 4.00 μm or less, and a particle diameter of 10.08 μm. The particles had a sharp particle size distribution containing 2% by volume.

Next, the finely pulverized product obtained by pulverization by the mechanical pulverizer 301 is introduced into the air-flow type classifier 1 having the structure shown in FIG. .7
A μm toner was obtained.

The BET specific surface area per volume Sb of the obtained toner was 1.41 m ² / cm ³ , and the theoretical specific surface area St per volume was 0.90 m ² / cm ³ . Therefore, S
b / St was 1.58. This is a mechanical crusher 3
It is considered that the surface roughness of the crushed surfaces of the rotor 314 and the stator 310 of No. 01 was appropriately controlled.

The obtained toner was subjected to an external addition and mixing process in the same manner as in Example 1 to obtain Evaluation Toner 2. As a result, Table 2
As shown in Table 2, good results were obtained.

[0138] Inspection of the inside of the machine after the end of the operation revealed that no fusion occurred to the rotor and the stator.

Example 3 The surface roughness of the crushing surface of the rotor 314 of the mechanical crusher 301 was measured by calculating the center line average roughness Ra =
1.7 μm, the maximum height Ry = 23.3 μm, the ten-point average roughness = 18.8 μm, and the surface roughness of the ground surface of the stator 310 was determined as the center line average roughness Ra = 8.0 μm, the maximum height Ry
= Evaluation Toner 3 was obtained in the same manner as in Example 1, except that 54.3 µm and ten-point average roughness = 38.2 µm.

Accordingly, the center line average roughness Ra of the stator ground surface is
-Rotor stator grinding surface center line average roughness Ra is 6.3 μm
The maximum height Ry of the crushed surface of the stator−the maximum height Ry of the crushed surface of the rotor is 31.0 μm, and the ten-point average roughness of the crushed surface of the stator Rz−the ten-point average roughness of the crushed surface of the rotor Rz
Was 19.4 μm.

When the powder raw material was pulverized by a mechanical pulverizer, the cold air temperature was −15 ° C., the swirl chamber temperature T1 in the mechanical pulverizer was −10 ° C., the rear indoor temperature T2 was 48 ° C., and T1 and T
The ΔT of 2 was 58 ° C. Tg-T1 is 72
° C and Tg-T2 were 14 ° C. The finely pulverized product obtained by pulverization with the mechanical pulverizer 301 at this time has a weight average diameter of 6.9 μm, 41% by number of particles having a particle diameter of 4.00 μm or less, and a particle diameter of 10.08 μm. The particles had a sharp particle size distribution containing 4% by volume.

Next, the finely pulverized product obtained by pulverization by the mechanical pulverizer 301 is introduced into the airflow type classifier 1 having the structure shown in FIG. .8
A μm toner was obtained.

The BET specific surface area per volume Sb of the obtained toner was 1.39 m ² / cm ³ , and the theoretical specific surface area St per volume was 0.88 m ² / cm ³ . Therefore, S
b / St was 1.58. This is a mechanical crusher 3
It is considered that the surface roughness of the crushed surfaces of the rotor 314 and the stator 310 of No. 01 was appropriately controlled.

The obtained toner was subjected to an external addition and mixing process in the same manner as in Example 1 to obtain a toner 3 for evaluation. As a result, Table 2
As shown in Table 2, good results were obtained.

In addition, when the inside of the machine was inspected after the operation was completed, no fusion was found on the rotor and the stator.

Example 4 The surface roughness of the crushed surface of the rotor 314 of the mechanical crusher 301 was calculated by calculating the center line average roughness Ra =
3.1 μm, the maximum height Ry = 27.7 μm, the ten-point average roughness = 25.0 μm, and the surface roughness of the ground surface of the stator 310 was determined as the center line average roughness Ra = 1.2 μm, the maximum height. Ry
Evaluation toner 4 was obtained in the same manner as in Example 1, except that = 15.1 µm and ten-point average roughness = 10.4 µm.

Therefore, the center line average roughness Ra of the crushed surface of the stator is
-Rotor stator grinding surface center line average roughness Ra is -1.9μ
m, the maximum height Ry of the crushed surface of the stator-the maximum height Ry of the crushed surface of the rotor is -12.6 μm, and the average roughness Rz of the stator crushed surface is 10 points. The average roughness Rz was -14.6 μm.

When the powder raw material was pulverized by a mechanical pulverizer, the cold air temperature was −15 ° C., the swirl chamber temperature T1 in the mechanical pulverizer was −10 ° C., the rear indoor temperature T2 was 49 ° C., and T1 and T
The ΔT of 2 was 59 ° C. Tg-T1 is 72
° C and Tg-T2 were 13 ° C. The finely pulverized product obtained by pulverizing with the mechanical pulverizer 301 at this time has a weight average diameter of 7.1 μm, 50% by number of particles having a particle diameter of 4.00 μm or less, and a particle diameter of 10.08 μm The particles had a particle size distribution containing 5% by volume.

Next, the finely pulverized product obtained by the pulverization by the mechanical pulverizer 301 is introduced into the airflow type classifier 1 having the structure shown in FIG. .8
A μm toner was obtained.

The BET specific surface area per volume Sb of the obtained toner was 1.39 m ² / cm ³ , and the theoretical specific surface area St per volume was 0.88 m ² / cm ³ . Therefore, S
b / St was 1.58.

The obtained toner was subjected to an external addition and mixing process in the same manner as in Example 1 to obtain a toner 4 for evaluation. As a result, Table 2
The result as shown in FIG.

Further, when the inside of the machine was inspected after the operation was completed, no fusion was found on the rotor and the stator.

[0153]

[Table 1]

[0154]

[Table 2]

Example 5 Pulverization and classification were carried out in the same manner as in Example 1 except that the supply amount of the powdery raw material to the mechanical pulverizer was 20 kg / Hr, and the results shown in Tables 3 and 4 were obtained. Was.

Example 6 Pulverization and classification were carried out in the same manner as in Example 2 except that the supply amount of the powdery raw material to the mechanical pulverizer was 20 kg / Hr, and the results shown in Tables 3 and 4 were obtained. Was.

Example 7 Pulverization and classification were performed in the same manner as in Example 3 except that the supply amount of the powdery raw material to the mechanical pulverizer was 20 kg / Hr, and the results shown in Tables 3 and 4 were obtained. Was.

Example 8 Pulverization and classification were performed in the same manner as in Example 1 except that the supply amount of the powdery raw material to the mechanical pulverizer was 10 kg / Hr, and the results shown in Tables 3 and 4 were obtained. Was.

Example 9 Pulverization and classification were performed in the same manner as in Example 2 except that the supply amount of the powdery raw material to the mechanical pulverizer was 10 kg / Hr, and the results shown in Tables 3 and 4 were obtained. Was.

Example 10 Pulverization and classification were carried out in the same manner as in Example 3 except that the supply amount of the powdery raw material to the mechanical pulverizer was 10 kg / Hr, and the results shown in Tables 3 and 4 were obtained. Was.

[Embodiment 11] The surface roughness of the crushing surface of the rotor 314 of the mechanical crusher 301 was measured by calculating the center line average roughness Ra =
1.7 μm, the maximum height Ry = 23.3 μm, the ten-point average roughness = 18.8 μm, and the surface roughness of the ground surface of the stator 310 was determined as the center line average roughness Ra = 2.3 μm, the maximum height. Ry
= 27.7 μm and ten-point average roughness Rz = 25.0 μm, to obtain an evaluation toner 11 in the same manner as in Example 1.

Therefore, the center line average roughness Ra of the crushed surface of the stator is
-Rotor stator grinding surface center line average roughness Ra is 0.6 μm
The maximum height Ry of the crushed surface of the stator−the maximum height Ry of the crushed surface of the rotor is 4.4 μm, and the ten-point average roughness of the crushed surface of the stator Rz−the ten-point average roughness of the crushed surface of the rotor Rz was 6.2 μm.

When the powder raw material was pulverized by a mechanical pulverizer, the cold air temperature was −15 ° C., the swirl chamber temperature T1 in the mechanical pulverizer was −10 ° C., the rear room temperature T2 was 48 ° C., and T1 and T
The ΔT of 2 was 58 ° C. Tg-T1 is 72
° C and Tg-T2 were 14 ° C. The finely pulverized product obtained by pulverization with the mechanical pulverizer 301 at this time has a weight average diameter of 6.8 μm, 44% by number of particles having a particle diameter of 4.00 μm or less, and a particle diameter of 10.08 μm. The particles had a sharp particle size distribution containing 3% by volume.

Next, the finely pulverized product obtained by pulverization by the above-mentioned mechanical pulverizer 301 is introduced into an air-flow type classifier 1 having the structure shown in FIG. .8
A μm toner was obtained.

The BET specific surface area per volume Sb of the obtained toner was 1.02 m ² / cm ³ , and the theoretical specific surface area St per volume was 0.88 m ² / cm ³ . Therefore, S
b / St was 1.16.

The obtained toner was subjected to an external addition and mixing process in the same manner as in Example 1 to obtain a toner 11 for evaluation. As a result, the results as shown in Table 4 were obtained.

When the inside of the machine was inspected after the operation was completed, no fusion was found on the rotor and the stator.

[0168]

[Table 3]

[0169]

[Table 4]

[Reference Example 1] In this reference example, the surface roughness of the crushed surfaces of the rotor 314 and the stator 310 of the mechanical crusher 301 was determined by measuring the center line average roughness Ra = 1.2 μm and the maximum height R
Pulverization and classification were performed in the same manner as in Example 1 except that y = 15.1 μm and ten-point average roughness Rz = 10.4 μm, and the results shown in Table 5 were obtained.

[Reference Example 2] In this reference example, the surface roughness of the crushed surfaces of the rotor 314 and the stator 310 of the mechanical crusher 301 was determined by measuring the center line average roughness Ra = 0.7 μm and the maximum height R
Pulverization and classification were performed in the same manner as in Example 1 except that y = 4.0 μm and ten-point average roughness Rz = 2.8 μm, and the results shown in Table 5 were obtained.

REFERENCE EXAMPLE 3 In this reference example, the surface roughness of the crushed surfaces of the rotor 314 and the stator 310 of the mechanical crusher 301 was determined by measuring the center line average roughness Ra = 1.7 μm and the maximum height R
Pulverization and classification were performed in the same manner as in Example 1 except that y = 23.3 μm and ten-point average roughness Rz = 18.8 μm, and the results shown in Table 5 were obtained.

[0173]

[Table 5]

[0174]

As described above, according to the present invention, the surface roughness is controlled to an appropriate state so that the surface roughness of the grinding surface of the rotor and the surface roughness of the grinding surface of the stator are different. By crushing the toner using a mechanical crusher,
By controlling the impact during pulverization to an appropriate state, excessive pulverization of the toner can be prevented, the particle size distribution of the toner is sharp, the amount of generated fine powder can be reduced, and the surface shape of the toner can be arbitrarily controlled. The present invention provides a mechanical pulverizer and a toner manufacturing method capable of obtaining a long-life toner having good developability, transferability, and stable chargeability even from an early stage even in a high temperature and high humidity environment.

Further, by controlling the surface shape of the toner in the mechanical pulverizer, a method for producing a toner capable of obtaining a toner having a high image density from an early stage or even after standing in a high-temperature and high-humidity environment. Is provided.

Further, there is provided a method for producing a toner capable of obtaining a toner having excellent multi-sheet durability.

[Brief description of the drawings]

FIG. 1 is a schematic sectional view of an example of a mechanical pulverizer used in a pulverizing step of a toner of the present invention.

FIG. 2 is a schematic cross-sectional view taken along the line DD ′ in FIG.

FIG. 3 is a perspective view of the rotor shown in FIG. 1;

FIG. 4 is a schematic sectional view of a multi-split airflow classifier preferably used in the toner classifying step of the present invention.

FIG. 5 is a schematic sectional view of a conventional collision-type airflow pulverizer.

[Explanation of symbols]

 1: Multi-divider classifiers 11, 12, 13: Discharge outlets 1la, 12a, 13a: Discharge conduit 16: Raw material supply nozzle 18, 117, 118: Classification edge 19: Inlet edge 22, 23: Side wall 24, 25: Classification Edge block 26: Coanda block 27: Left block 30: Classification area 32: Classification chamber 40: Raw material supply port 41: High pressure air supply nozzle 42: Raw material powder introduction nozzle 161: High pressure gas supply nozzle 162: Acceleration tube 163: Acceleration Pipe outlet 164: collision member 165: powder material supply port 166: collision surface 167: pulverized material discharge port 168: pulverization chamber 212: spiral chamber 219: pipe 220: distributor 222: bag filter 224: suction blower 229: capture Cyclone 240: Raw material hopper 301: Mechanical crusher 302 Powder discharge port 310: Stator 311: Powder input port 312: Rotating shaft 313: Casing 314: Rotor 315: First metering device 316: Jacket 317: Cooling water supply port 318: Cooling water discharge port 319: Cold air Generation means 320: rear room

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme court ゛ (Reference) G03G 9/08 G03G 9/08 9/083 101 9/087 321 381 (72) Inventor Shinichi Iwata Tokyo 3-30-2 Shimomaruko, Ota-ku Canon Inc. F-term (reference) 2H005 AA02 AA15 AB04 EA03 EA05 EA07 EA10 4D063 FF12 FF14 FF21 GA10 GC05 GC19 GD02 GD03 GD04 GD12 GD22 GD24 4D067 EE34 GA20

Claims (42)

[Claims] 1. A powder inlet for charging a coarsely pulverized product into a pulverizing means for pulverizing a coarsely pulverized product, a stator, a rotor attached to at least a central rotating shaft, and a finely pulverized powder. At least a powder discharge port for discharging the powder from the pulverizing means, the stator includes the rotor, and the surface of the stator and the surface of the rotor have a predetermined gap. A crusher is arranged to form a crushing zone, and in a crushing zone, a mechanical crusher configured so that coarsely crushed material is finely crushed with rotation of the rotator; A mechanical pulverizer characterized in that the surface roughness of the pulverized surface is different from the surface roughness of the pulverized surface of the stator. 2. A center line average roughness Ra of a crushed surface of the rotor.
2. The mechanical crusher according to claim 1, wherein the center line average roughness Ra of the crushed surface of the stator satisfies the following condition. (Rotor center line average roughness Ra) <(stator center line average roughness Ra), and (stator center line average roughness Ra) − (rotor center line average roughness Ra) ≧ 1.0 μm 3. The center line average roughness Ra of the crushed surface of the rotor.
2. The mechanical crusher according to claim 1, wherein the center line average roughness Ra of the crushed surface of the stator satisfies the following condition. 1.0 μm ≦ (stator center line average roughness Ra) − (rotor center line average roughness Ra) ≦ 10.0 μm 4. The maximum height Ry of the crushing surface of the rotor and the maximum height Ry of the crushing surface of the stator satisfy the following conditions. A mechanical crusher according to any one of the above. (Rotor maximum height Ry) <(stator maximum height Ry), and (stator maximum height Ry) − (rotor maximum height Ry) ≧ 10.0 μm 5. The maximum height Ry of the crushing surface of the rotor and the maximum height Ry of the crushing surface of the stator satisfy the following condition. A mechanical crusher according to any one of the above. 10.0 μm ≦ (stator maximum height Ry) − (rotor maximum height Ry) ≦ 60.0 μm 6. A ten-point average roughness Rz of a crushed surface of the rotor.
The mechanical crusher according to any one of claims 1 to 5, wherein the ten-point average roughness Rz of the crushed surface of the stator satisfies the following condition. (Rotator ten-point average roughness R
z) <(stator ten-point average roughness Rz) and (stator ten-point average roughness Rz) − (rotor ten-point average roughness Rz) ≧ 1
0.0 μm 7. A ten-point average roughness Rz of a crushed surface of the rotor.
The mechanical crusher according to any one of claims 1 to 5, wherein the ten-point average roughness Rz of the crushed surface of the stator satisfies the following condition. 10.0 μm ≦ (stator ten-point average roughness Rz) − (rotor ten-point average roughness Rz) ≦ 40.0 μm 8. A mixture containing at least a binder resin and a colorant is melt-kneaded, the obtained kneaded product is cooled, the cooled product is roughly pulverized, and the coarsely pulverized product is finely pulverized by a pulverizing means. And a weight average particle diameter of 4 to 12
In the method for producing a toner for producing a μm toner, the pulverizing means is a mechanical pulverizer, and the mechanical pulverizer has Inlet, stator, at least a rotor attached to the central rotating shaft, at least having a powder outlet for discharging the finely pulverized powder from the pulverizing means,
The stator includes the rotor, and the rotor is arranged so as to have a predetermined gap between the surface of the stator and the surface of the rotor to form a grinding zone. A mechanical pulverizer configured to finely pulverize the coarsely pulverized material with the rotation of the rotor; and a surface roughness of a pulverized surface of the rotor and a surface roughness of a pulverized surface of the stator. A fine pulverization using a mechanical pulverizer having a different particle size. 9. A center line average roughness Ra of a crushed surface of the rotor.
9. The method according to claim 8, wherein the pulverized surface of the stator is finely pulverized by a mechanical pulverizer having a center line average roughness Ra satisfying the following condition. (Rotor center line average roughness Ra) <(stator center line average roughness Ra),
And (stator center line average roughness Ra) − (rotor center line average roughness Ra) ≧ 1.0 μm 10. A center line average roughness R of a grinding surface of the rotor.
The method for producing a toner according to claim 8, wherein a and a center line average roughness Ra of the crushed surface of the stator are finely crushed by a mechanical crusher satisfying the following conditions. 1.0 μm ≦ (stator center line average roughness Ra) − (rotor center line average roughness Ra) ≦ 10.0 μm 11. A maximum height Ry of a crushing surface of the rotor,
The method for producing a toner according to any one of claims 8 to 10, wherein the stator is pulverized with a mechanical pulverizer having a maximum height Ry of a pulverized surface satisfying the following conditions.
(Rotor maximum height Ry) <(stator maximum height Ry), and (stator maximum height Ry)-(rotor maximum height Ry)
≧ 10.0 μm 12. A maximum height Ry of a crushing surface of the rotor,
The method for producing a toner according to any one of claims 8 to 10, wherein the stator is pulverized with a mechanical pulverizer having a maximum height Ry of a pulverized surface satisfying the following conditions. 10.0 μm ≦ (stator maximum height Ry) − (rotor maximum height Ry) ≦ 60.0 μm 13. A ten-point average roughness Rz of a crushed surface of the rotor.
13. The toner according to claim 8, wherein the pulverized surface of the stator is finely pulverized by a mechanical pulverizer satisfying the following conditions. Production method. (Rotor ten-point average roughness Rz) <(stator ten-point average roughness Rz) and (stator ten-point average roughness Rz)-(rotor ten-point average roughness Rz) ≧ 10.0 μm 14. A ten-point average roughness Rz of a crushed surface of the rotor.
13. The toner according to claim 8, wherein the pulverized surface of the stator is finely pulverized by a mechanical pulverizer satisfying the following conditions. Production method. 10.0 μm ≦ (stator ten-point average roughness Rz) − (rotor ten-point average roughness Rz) ≦ 40.0 μm 15. A center line average roughness R of a grinding surface of the rotor.
15. The method according to claim 8, wherein a satisfies the following condition. Center line average roughness Ra <2.0 μm 16. A center line average roughness R of a crushed surface of the rotor.
15. The method according to claim 8, wherein a satisfies the following condition. 0.5 ≦ center line average roughness Ra ≦ 1.8 μm 17. The maximum height Ry of the grinding surface of the rotor is
17. The method according to claim 8, wherein the following conditions are satisfied. Maximum height Ry <25.0 μm 18. The maximum height Ry of the grinding surface of the rotor is
17. The method according to claim 8, wherein the following conditions are satisfied. 3.0 ≦ maximum height Ry ≦ 24.8 μm 19. A ten-point average roughness Rz of a crushed surface of the rotor.
Satisfies the following condition:
19. The method for producing a toner according to any one of the above items. Ten point average roughness Rz <20.0 μm 20. Ten-point average roughness Rz of a crushed surface of the rotor
Satisfies the following condition:
19. The method for producing a toner according to any one of the above items. 2.0 ≦ ten point average roughness Rz ≦ 19.8 μm 21. A center line average roughness R of a crushed surface of the stator.
21. The method according to claim 8, wherein a satisfies the following condition. Center line average roughness Ra ≧ 2.0 μm 22. A center line average roughness R of a crushed surface of the stator.
21. The method according to claim 8, wherein a satisfies the following condition. 2.0 ≦ center line average roughness Ra ≦ 10.0 μm 23. The maximum height Ry of the grinding surface of the stator is as follows:
The method for producing a toner according to any one of claims 8 to 22, wherein the following conditions are satisfied. Maximum height Ry ≧ 25.0 μm 24. The maximum height Ry of the grinding surface of the stator is
The method for producing a toner according to any one of claims 8 to 22, wherein the following conditions are satisfied. 25.0 ≦ maximum height Ry ≦ 60.0 μm 25. A ten-point average roughness Rz of a crushed surface of the stator.
Satisfies the following condition:
25. The method for producing a toner according to any one of the above items. Ten point average roughness Rz ≧ 20.0 μm 26. A ten-point average roughness Rz of a crushed surface of the stator.
Satisfies the following condition:
25. The method for producing a toner according to any one of the above items. 20.0 ≦ 10 point average roughness Rz ≦ 40.0 μm 27. The toner pulverized by the mechanical pulverizer has a specific surface area per unit volume Sb (m ² / cm ³ ) of the toner measured by the BET method, and the toner is assumed to be a true sphere. 28. The relationship of the specific surface area St (m ² / cm ³ ) per unit volume calculated from the weight average diameter of the above satisfies the following condition: Sb / St <1.8. 3. The method for producing a toner according to item 1. 28. The method for producing a toner according to claim 8, wherein the toner is a magnetic toner containing 60 to 200 parts by mass of a magnetic substance with respect to 100 parts by mass of a binder resin. . 29. The method for producing a toner according to claim 8, wherein the powder raw material is introduced into a mechanical pulverizer together with cold air. 30. The method according to claim 29, wherein the temperature of the cool air is 0 to −30.0 ° C. 31. The method for producing a toner according to claim 8, wherein the mechanical pulverizer includes a cooling unit for cooling the inside of the machine. 32. The production of a toner according to claim 8, wherein the mechanical pulverizer is provided with a jacket for cooling the inside of the machine, and pulverizes the powdery raw material while passing cooling water through the jacket. Method. 33. The toner production method according to claim 8, wherein the mechanical pulverizer has a swirl chamber communicating with the powder inlet, and the room temperature T1 of the swirl chamber is 0 ° C. or lower. Method. 34. The method according to claim 33, wherein the room temperature T1 of the spiral chamber of the mechanical pulverizer is -5 to -15 ° C. 35. The method for producing a toner according to claim 33, wherein the room temperature T1 of the spiral chamber of the mechanical pulverizer is a temperature of −7 to −12 ° C. 36. The finely pulverized product generated in the mechanical pulverizer is discharged from the powder discharge port through a rear chamber of the mechanical pulverizer to the outside of the machine, and the room temperature T2 of the rear chamber is 30 to 60 ° C. The method for producing a toner according to any one of claims 8 to 35, wherein 37. A temperature difference ΔT between the room temperature T2 and the room temperature T1.
(T2-T1) is 30 to 80 ° C.
7. The method for producing a toner according to any one of 6. 38. Temperature difference ΔT between room temperature T2 and room temperature T1
(T2-T1) is 35 to 75 ° C.
7. The method for producing a toner according to any one of 6. 39. Temperature difference ΔT between room temperature T2 and room temperature T1
(T2-T1) is 37 to 72 ° C.
7. The method for producing a toner according to any one of 6. 40. The glass transition point Tg of the binder resin is 45 to 75 ° C., and the room temperature T1 of the spiral chamber of the mechanical pulverizer is 0.
The method for producing a toner according to any one of claims 8 to 39, wherein the temperature is adjusted to be lower than or equal to 0C and lower by 60 to 75C than Tg. 41. The glass transition point Tg of the binder resin is 45 to 75 ° C., and the room temperature T2 of the rear chamber of the mechanical pulverizer is Tg.
The method for producing a toner according to any one of claims 8 to 40, wherein the temperature is adjusted so that the temperature is lower by 5 to 30 ° C. 42. A tip peripheral speed of a rotor is 80 to 180 m.
42. The method according to claim 8, wherein the minimum gap between the rotor and the stator is 0.5 to 10.0 mm.