JPH0862892A - Toner for electrostatic charge image developer and its production - Google Patents

Abstract

PURPOSE: To provide a toner showing good dispersion of a coloring agent or release agent in a resin and having stable electrification property without causing fog, to suppress cutting in the chains of resin molecules of the fine powder component produced by classification and separation of a toner which is passed twice a kneading process, and to obtain a toner having excellent offset performance. CONSTITUTION: This toner for an electrostatic charge image developer is obtd. by kneading a compsn. comprising at least a resin, coloring agent, release agent and fine powder obtd. by classification and separation of a toner. The kneading machine is provided with at least two supply ports 4, 6 for the source material. A compsn. having 0.30 to 0.70g/cm<3> static bulk density in the compsn. above described is supplied through the first source material supply port 4 on the most upstream side the kneading machine. A compsn. containing at least the fine powder produced by classification and separation of a toner and having 0.02 to 0.30g/cm<3> static bulk density is supplied through the source material supply port 6 in the more downstream side than the first supply port Theme compsns. thus supplied are kneaded to obtain the toner.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an electrostatic charge image developing toner used in electrophotography, electrostatic recording, electrostatic printing and the like, and more particularly to a method for producing the same.

[0002]

2. Description of the Related Art Conventionally, in the electrophotographic method, an electrostatic latent image is usually formed on a latent electrostatic image bearing member made of a photoconductive photosensitive member by charging and exposure, and then the electrostatic latent image is formed in a resin. The toner image obtained by adding a colorant and the like to form fine particles is developed, and the obtained toner image is transferred and fixed on a support such as transfer paper to form a visible image. On the other hand, the photoconductor after the transfer is destaticized, and the toner remaining on the photoconductor without being transferred is cleaned and then used for forming the next image.

Conventionally, as a method for producing the toner for developing an electrostatic image, a colorant, a resin, a release agent, and the like as a toner composition are preliminarily prepared except for a polymerized toner synthesized in one shot by a polymerization reaction. It comprises three steps of a mixing step, a melt-kneading step of kneading a preliminary mixture, and a crushing / classifying step of crushing and classifying to a desired toner particle size after melt-kneading.

In order to maintain various performances and qualities required of the toner, it is particularly required in the toner manufacturing process to improve the dispersibility of the additive in the resin and optimize the molecular chain cleavage ratio of the resin. In order to improve the dispersibility of the additive in the resin, a method has been attempted in which the operating conditions of the mixer in the pre-mixing step and the operating conditions of the kneading machine in the kneading step are changed to find an appropriate condition.
On the other hand, changing the screw shape of the kneading machine has been studied in order to optimize the resin molecular chain cleavage ratio.

For example, in JP-A-54-118250, a magnetic toner is prepared by kneading a magnetic material with a resin having a low melting point or a brittle resin, and then kneading the resin with a resin having a higher melting point than the resin at a temperature higher than the melting point of the high melting resin. A method has been proposed. Kohei
In the 3-86224 publication, the kneading paddle is divided into the feed screw and the kneading part in the kneading machine screw design,
It is proposed that the kneading part should be provided in two or more places and that the length of the kneading part on the discharge side should be designed to be 20% or more and 50% or less with respect to the entire length of the paddle. Further, in JP-A-3-149567, from the viewpoint of improving production efficiency,
From the inlet side of the barrel (length L) of the kneading machine, a mixed raw material containing 10 to 50% by weight of the additive in the resin is supplied from a supply port provided within a position of 0.3 L to 0.3 L to 0.9 L. A manufacturing method has been proposed in which a mixed raw material having an additive amount of 20% by weight or less in a resin is supplied from a supply port provided at a position and simultaneously taken out from a discharge port.

On the other hand, a method of producing a toner by reusing fine powder toner components (fine powder separated and classified) generated during toner classification has been studied. For example, in Japanese Patent Application Laid-Open No. 4-39671, a color toner composition composed of a binder resin having a weight average molecular weight of 40,000 or less and a flushing pigment is classified and separated, and the fine powder is reused as a part or all of a toner manufacturing raw material. Is proposed. Japanese Patent Application Laid-Open No. 4-50864 proposes to add fine powder having a volume average particle diameter of 2 to 15 μm and mechanically mix it with a toner component in the mechanical mixing step.

However, in the technique described in JP-A-54-118250, in order to simultaneously satisfy the contradictory conditions of reliable exposure of the magnetic material on the toner surface and improvement of fixing property,
There is a problem that the manufacturing efficiency is lowered because the kneading step is essential. In addition, in the technology described in Japanese Patent Laid-Open No. 3-86224
The dye and pigment and the charge control agent are uniformly dispersed in the resin as it passes through the kneading zone once, but the kneaded material stays in the zone because the kneading zone on the discharge side is long and excessive shearing force is applied. The temperature rises due to frictional heat, which makes temperature control difficult, and at the same time molecular chain scission of the resin, which is the main component, occurs, which has drawbacks in terms of production stability and toner fixing performance. Further, in the technique described in Japanese Patent Laid-Open No. 3-149567, the production efficiency is improved by setting the number of times of toner kneading to one, but the shearing force received during kneading is different between the resin forming the masterbatch and the remaining resin, and stable. It is difficult to secure good fixing performance. Further, in the techniques described in JP-A-4-39671 and JP-A-4-50864, the usual kneading step is premised, and since the toner fine powder is contained, the bulk of the toner composition becomes large, and the preliminary kneading step is performed before the kneading step. It is essential to provide a mixing process.

[0008]

SUMMARY OF THE INVENTION The present invention is directed to the efficient production of toner without the above problems.

From the viewpoint of ensuring good dispersibility of the toner composition and simplifying the toner manufacturing process and saving labor, the present inventors have adopted a method of supplying each toner composition in the melt-kneading process of the toner manufacturing process. It was thought that the pre-mixing step could be omitted if the uniformity of the toner composition in the resin could be secured by devising it. Paying attention to the difference in particle size between toner compositions, which is an obstacle to achieving the uniformity of toner compositions, that is, the difference in static bulk density. It was found that if a colorant having a low density was successively supplied to the molten main raw material, the colorant could be easily kneaded into the resin, and as a result of intensive studies, the present invention was accomplished.

An object of the present invention is to provide a toner in which a colorant and a release agent are well dispersed in a resin, the chargeability is stable, and there is no fog, and at the same time, the toner is classified and separated by passing through a kneading step twice. An object of the present invention is to provide a toner having excellent offset performance in order to suppress breakage of resin molecular chains of fine powder components.

A second object of the present invention is to distinguish the method of feeding the toner composition to the extruder according to the static bulk density of each toner composition in the melt-kneading process using a twin-screw extruder. Another object of the present invention is to provide a method for producing a toner in which a premixing step is substantially omitted, and a toner produced by using the toner production method.

[0012]

The object of the present invention can be achieved by adopting any one of the following configurations.

(1) In a toner for an electrostatic image developer obtained by kneading a composition comprising at least a resin, a colorant, a release agent and a toner classification / separation fine powder, a kneader has at least two raw material supply ports. In the above composition, the composition having a static bulk density of 0.30 to 0.70 g / cm ³ is supplied from the first raw material supply port provided on the most upstream side of the kneader, and at least the toner classification is performed. Static bulk density including separated fine powder is 0.
A toner for an electrostatic image developer characterized in that the composition of 02 to 0.30 g / cm ³ is supplied and kneaded from a raw material supply port provided on the downstream side of the first raw material supply port of the kneader. .

(2) At least 2 compositions containing at least a resin, a colorant, a release agent, and a toner classifying and separating fine powder.
In the method for producing a toner for an electrostatic image developer, which comprises kneading with a twin-screw extruder, the twin-screw extruder has at least two or more raw material supply ports in the barrel length direction,
Static bulk density consisting of at least resin and release agent is 0.30-0.
70 g / cm ³ of composition was supplied from a first raw material supply port provided on the most upstream side of the extruder, and at least a colorant,
The static bulk density consisting of fine powder separated and classified by toner is 0.02-0.30 g /
A method for producing a toner for an electrostatic charge image developer, comprising supplying a composition having a volume of cm ³ to a raw material supply port provided on the downstream side of a first raw material supply port of an extruder and kneading the mixture.

(3) In a toner for an electrostatic image developer, which is produced through a step of kneading a composition comprising at least a resin, a colorant, a release agent, and toner classification and separation fine powder using a twin-screw extruder, The twin-screw extruder has at least two or more raw material supply ports in the length direction of the barrel, and has a static bulk density of 0.30 to 0.70 g including at least a resin and a release agent.
/ Cm ³ of the composition is supplied from a first raw material supply port provided on the most upstream side of the extruder, and has a static bulk density of 0.02 to 0.30 g / cm ³ composed of at least a colorant and toner classification / separation fine powder.
^A toner for an electrostatic image developer, which comprises the step of supplying the composition of ³ from a raw material supply port provided on the downstream side of the first raw material supply port of an extruder and kneading the mixture.

The present invention will be described with reference to typical manufacturing process examples.
In the melt-kneading step, a twin-screw extruder having a plurality of raw material supply ports along the barrel length direction is used as a kneader, and a static bulk density of at least a resin and a mold release agent is used.
0.30 to 0.70 g / cm ³ of composition is supplied from the first raw material supply port provided on the most upstream side of the extruder, and has a static bulk density of at least 0.02 to 0.30 consisting of a colorant and toner classification / separation fine powder.
The composition of g / cm ³ is supplied from at least one raw material supply port provided on the downstream side of the first raw material supply port of the extruder and kneaded to obtain a colorant and a release agent in the toner. It was found that the dispersion uniformity of the resin, etc. is not impaired.

The toner manufacturing method of the present invention comprises a resin, a colorant,
A twin screw provided with at least two raw material supply ports along a barrel length direction as a kneading machine when producing a toner containing a release agent, a toner classifying and separating fine powder, and optionally other additives. It is characterized by using an extruder.

In the present invention, the static bulk density of each toner composition is a Kawakita static bulk density measuring instrument (manufactured by Seishin Enterprise Co., Ltd.) IH.
Using a -2000 type, each toner composition was supplied onto 48 mesh, vibrated, and put into a 20 cm ³ container, and the weight thereof was measured.
The static bulk density was calculated as the quotient of the weight and the container volume of 20 cm ³ .

The softening point is the flow tester CFT-500.
(Manufactured by Shimadzu Corporation), while heating a 1 cm ³ sample at a heating rate of 6 ° C./min, apply a load of 20 kg / cm ³ from the plunger to push out a nozzle with a diameter of 1 mm and a length of 1 mm. And draw a curve (softening flow curve) between the plunger drop and temperature of the flow tester,
It is a temperature corresponding to h / 2 when the height of the curve is h.

Regarding the dispersion state of the composition in the toner, the plate-shaped toner molded product discharged from the discharge port of the twin-screw extruder and cooled and rolled was taken out, sliced with a microtome and observed with a polarizing microscope.

The number average particle size of the resin, colorant, etc. was visually measured by a scanning electron microscope.

[0022]

The present invention will be described in detail below.

The toner and the toner manufacturing method of the present invention are a toner manufactured by using a specific kneader and a toner manufacturing method. A toner manufacturing apparatus having a toner kneader used in the present invention is shown in FIGS. In FIG. 1, 1 is a hopper for charging a toner composition such as a resin and a release agent having a bulk density of 0.30 to 0.70 g / cm ³ , and 2 is a static bulk density of a colorant, a toner classification and separation fine powder 0.02 to 0.30 g / cm ^3. Toner composition charging hopper, 3 is a feeder, 4 is a first raw material supply port, 5 is a side feeder, 6 is a second raw material supply port, 7 is a kneader motor, 8 is a speed reducer, 9 is a deaeration vent, 10 Is a discharge port, and 11 is a kneading zone. Typically, a twin screw extruder is used to supply these first raw material supply port 4, second raw material supply port 6, kneading motor 7, speed reducer 8, degassing vent 9, and discharge port. It is composed of 10 and a plurality of kneading zones 11. 13 is a rolling roller for cooling, 14 is a cooling belt, 15 is a crusher, and 16 is a classifier, which is characterized by not having a premixing step. 2 is a type having two sets of feeders to the first raw material supply port with respect to FIG. 1, FIG. 3 is a type with one set of side feeders and raw material supply ports added to FIG. 1, and 12 is a third raw material. It is a supply port. FIG. 4 is a type having two sets of feeders to the first raw material supply port in contrast to FIG. However, the number of raw material supply ports installed on the discharge port side of the first raw material supply port is at least one and may be plural.

The eleven kneading zones are preferably arranged on the discharge side of each raw material supply port, and the first, second and third kneading zones corresponding to the first, second and third raw material supply ports are provided. It is preferable that the first kneading zone and the second and third kneading zone are shorter than the first kneading zone from the viewpoint of suppressing the breakage of the resin molecular chain. The temperature of each kneading zone is preferably set within a temperature range of softening point + 20 ° C. to softening point −40 ° C. with respect to the softening point of the resin as the main component, and is not necessarily set to the same temperature. When kneading is performed at a temperature exceeding the softening point + 20 ° C, the melt viscosity of the resin is excessively lowered, the shearing force at the time of kneading is reduced, and the dispersion state of the colorant, the release agent, etc. is deteriorated. On the other hand, when kneading at a temperature lower than the softening point of −40 ° C., the melt viscosity of the resin is high, the shearing force at the time of kneading is high, the molecular chain breakage of the resin occurs, and the fixing performance of the toner deteriorates.

The feed rates of the raw materials fed from the feeders 3 and 5 and the side feeder are not particularly limited, but the concentrations of the respective components in the toner discharged from the discharge port are the same at the beginning and at the end of the discharged material. It is essential to control the feed rate.

The toner manufacturing method will be described with reference to FIG. The toner raw material containing a resin as a main component, which is charged from the first raw material supply port No. 4, is melt-kneaded in the first kneading zone, and advances to the left-hand direction discharge port side 10 in a molten state. On the other hand, a colorant is charged from the second raw material supply port 6 and melted and kneaded in the second kneading zone, and further, the toner classification separation fine powder is charged to the molten resin component from the third raw material supply port 12, and the third knee is supplied. The toner composition is further melt-kneaded in the bonding zone, and then the toner composition is discharged from the discharge port 10. The discharged toner composition was further pulverized by a pulverizer 15 so as to have a required particle size after cooling, and classified by a dispenser 16, and the volume average particle size of the toner was adjusted to about 5 to 20 μm. Obtain colored particles. The cooling rolling roller 13 is usually 1 to 10 in order to effectively cool the sufficiently kneaded toner raw material composition.
Rolled to a thickness of cm and made into a plate, and further cooling belt 14
Is an apparatus that cools and solidifies this plate-shaped material to about room temperature so that it can be efficiently crushed. From the viewpoint of ensuring the fluidity of the toner, inorganic fine particles such as silica and titanium oxide are added to the colored particles as external additives to finally obtain toner particles.

In the toner manufacturing method of the present invention, when a plurality of raw material compositions for toner are simultaneously supplied from the same raw material supply port, the feed screw for melt kneading does not bite well, and the composition is poorly dispersed in the obtained toner. Easier to do. From the viewpoint of improving this dispersibility, two or more sets of feeders 3 are provided as in the toner manufacturing apparatus shown in FIGS.
Although it is possible to separately supply each of the toner raw material compositions, the difference in static bulk density between the toner compositions is 0.20 g /
When it is ³ cm ³ or more, there is no effect of improving the dispersibility even if different feeders are used, and it cannot withstand use as a toner, and the difference in static bulk density between toner compositions that can be supplied from the same raw material supply port is 0.20. It is less than g / cm ³ .

For example, when a resin, a coloring agent, a release agent, and a toner classification / separation fine powder are simultaneously supplied from the first supply port, the colorant, the toner classification / separation fine powder, etc. have a small static bulk density and a large amount of air is taken in. At times, the shearing force is not evenly applied, resulting in poor dispersion of the colorant and the release agent in the obtained toner.

The resin used in the present invention is not particularly limited, and examples thereof include polyester resin, styrene-alkyl acrylate resin, styrene-alkyl methacrylate resin, styrene-butadiene resin, styrene-acrylonitrile resin, styrene. -Acrylic-polyester resin, styrene-acrylic-crystalline polyester graft resin, polyurethane resin, epoxy resin, silicone resin, polyvinyl chloride, polyamide, polyvinyl butyral, rosin, modified rosin, phenol resin, xylene resin and the like. The static bulk density of the resin varies depending on the synthesis method, but in general, in the solution polymerization method, the bulk polymerization method, etc., the synthesized resin is pulverized in advance and the number average particle diameter is adjusted to about 0.1 to 2 mm and subjected to the kneading step. The number average particle diameter in the case of the suspension polymerization method, the emulsion polymerization method or the like is about 0.1 to 1 mm. The static bulk density of the resin having these number average particle diameters is 0.50 to 0.
It is about 70 g / cm ³ .

In addition to the resin, the colored particles contain components such as a colorant, a charge control agent and a release agent, if necessary. The addition amount is not particularly limited, but is preferably 1 part to 50 parts each.

The colorant is not particularly limited, and various conventionally known materials can be used. For example, carbon black such as furnace black, lamp black, channel black and thermal black, C.I. I. Pigment Blue 15: 3, C.I. I. Pigment Blue 15, C.I. I. Pigment Blue 15: 6, C.I. I. Pigment Blue 68, C.I.
I. Pigment Red 48-3, C.I. I. Pigment red
122, C.I. I. Pigment Red 212, C.I. I. Pigment Red 57-1, C.I. I. Pigment Yellow 17, C.I.
I. Pigment Yellow 81, C.I. I. Pigment Yellow 154 and the like, nigrosine dye, monoazo dye, anthraquinone dye, xanthene dye and the like, and mixtures thereof can be used. The number average primary particle diameter of these colorants is about 5 to 400 nm, and their static bulk density is
It is about 0.10 to 0.20 g / cm ³ .

As the releasing agent, a low molecular weight polyethylene having a number average molecular weight (the number average molecular weight indicates a polystyrene molecular weight conversion value in high temperature GPC) of 1500 to 5000, a low molecular weight polypropylene, a low molecular weight polyethylene-polypropylene copolymer, etc. Polyolefin wax, or high-melting paraffin wax such as microwax or Fischer-Tropsch wax, or ester wax such as fatty acid lower alcohol ester, fatty acid higher alcohol ester, fatty acid polyhydric alcohol ester, or amide wax, alone or in combination. Can be used. The static bulk density of these release agents is about 0.30 to 0.55 g / cm ³ .

A charge control agent may be used as another component.

Toner classification and separation fine powder refers to components having a volume average particle size of 5 μm or less, which are separated in the classification step, and the static bulk density of these fine powders is about 0.15 to 0.30 g / cm ³ .

Any external additive can be used as long as it can improve the fluidity of the toner, and silica, alumina, titanium oxide, barium titanate, magnesium titanate, calcium titanate, strontium titanate, zinc oxide, and oxides can be used. Inorganic fine particles such as chromium, cerium oxide, antimony trioxide and zirconium oxide can be mentioned, and these may be subjected to a hydrophobic treatment.

[0036]

EXAMPLES The present invention will be further described below with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples. In addition, "part" represents a weight part.

Preparation of toner classification separation fine powder (toner classification separation fine powder a) Resin: styrene acrylic resin (softening point 125 ° C. static bulk density 0.58 g / cm ³ ) 100 parts Colorant: carbon black furnace black (number average primary Particle size 20 nm Static bulk density 0.17 g / cm ³ ) 10 parts Release agent; Low molecular weight polypropylene (Static bulk density 0.48 g / cm ³ ) 5 parts Using the toner manufacturing apparatus shown in FIG. 5 parts of the molding agent are fed through separate feeders from the first raw material supply port 4 at a constant rate of 6.7 kg / hr., The screw rotation speed is 220 rpm, and the first kneading zone temperature is 120 ° C.
And kneading, 10 parts of the colorant is quantitatively supplied from the second raw material supply port 6 at a rate of 0.3 kg / hr., The second kneading zone temperature is set to 120 ° C., melted and kneaded, and then cooled. The powder was pulverized and classified to obtain colored particles A having a volume average particle diameter of 8 μm. At this time, particles having a volume average particle diameter of 4.5 μm, which are collected as fine powder at the time of classification, are referred to as toner classification / separation fine powder a. The dispersed state of the colorant and the release agent in the resin of the colored particles A was almost uniform.

(Toner classification and separation fine powder b) Resin: Polyester resin (Softening point 138 ° C. static bulk density 0.60 g / cm ³ ) 100 parts Colorant: Furnace black (number average primary particle diameter 16 nm, static bulk density 0.15 g / cm ³ ) 8 parts Release agent; low molecular weight polyethylene (static bulk density 0.51 g / cm ³ ) 4 parts Using the toner manufacturing apparatus shown in FIG. 2, separate 100 parts of the above resin and 4 parts of the release agent into separate feeders. Through the first raw material supply port 4 at a constant rate of 6.5 kg / hr., The screw rotation speed is 150 rpm, and the first kneading zone temperature is 145 ° C.
To knead, and 8 parts of colorant from the second raw material supply port
The mixture was supplied at a rate of 0.2 kg / hr., The second kneading zone temperature was set to 130 ° C., melted and kneaded, and then cooled, pulverized and classified to obtain colored particles B having a volume average particle diameter of 8 μm. . At this time, particles having a volume average particle diameter of 4.8 μm, which are collected as fine powder during classification, are referred to as toner classification fine powder b. The dispersed state of the colorant and the release agent in the resin of the colored particles B was almost uniform.

(Toner classification and separation fine powder c) Resin; Polyester resin (Softening point 119 ° C. Static bulk density 0.63 g / cm ³ ) 100 parts Colorant; C.I. I. Pigment Red 122 (number average particle size 100 nm, static bulk density 0.17 g / cm ³ ) 7 parts Using the toner manufacturing apparatus shown in FIG. 1, 100 parts of the above resin is supplied from the first raw material supply port 4 to 7 parts of the colorant. 2 From the raw material supply port, quantitatively supply at a rate of 5.7 kg / hr., 0.4 kg / hr.
After kneading with the screw rotation speed set to 200 rpm and the first and second kneading zone temperatures set to 130 ° C, cooling, pulverization,
Coloring was performed to obtain colored particles C having a volume average particle diameter of 9 μm. At this time, the volume average particle size of 4.6 μm recovered as fine powder during classification.
The particles are designated as toner classification fine powder c. The dispersibility of the pigment in the resin of the colored particles C was substantially uniform.

(Toner classification and separation fine powder d) Resin; Styrene acrylic resin (Softening point 115 ° C. Static bulk density 0.58 g / cm ³ ) 100 parts Colorant; C.I. I. Pigment Blue 15: 3 (number average particle size 60 nm, static bulk density 0.13 g / cm ³ ) 3 parts Release agent; low molecular weight polypropylene (static bulk density 0.50 g / cm ³ ) 4 parts Using the toner manufacturing apparatus shown in FIG. Then, 100 parts of the resin and 4 parts of the release agent are quantitatively supplied from the first raw material supply port at a rate of 6.3 kg / hr. Through separate feeders, the screw rotation speed is 180 rpm, and the first kneading zone temperature is Knead at 120 ℃, 3 parts colorant 0.2kg from the second raw material supply port
After quantitatively supplying the mixture at a rate of / hr., Setting the second kneading zone temperature at 130 ° C., melt-kneading, cooling, pulverizing and classifying, colored particles D having a volume average particle diameter of 8 μm were obtained. At this time, the volume average particle size recovered as fine powder during classification was 4.8 μm.
The particles are designated as toner classification fine powder d. The dispersed state of the pigment and the release agent in the resin of the colored particles D was almost uniform.

Example 1 Resin: Styrene acrylic resin (softening point 125 ° C. static bulk density 0.58 g / cm ³ ) 100 parts Colorant: furnace black (number average primary particle diameter 20 nm static bulk density 0.17 g / cm ³ ) 10 parts Release agent; Low molecular weight polypropylene (static bulk density 0.48 g / cm ³ ) 5 parts Classification separation fine powder; Fine powder a (static bulk density 0.22 g / cm ³ ) 30 parts The toner manufacturing apparatus shown in FIG. Using 100 parts of the resin and 5 parts of the releasing agent, a fixed amount of 5.1 kg / hr. In total is supplied from the first raw material supply port through separate feeders, the screw rotation speed is 220 rpm, and the first kneading zone. The temperature is set to 120 ° C and kneading is performed, and 10 parts of the colorant is added from the second raw material supply port to 0.
A fixed amount is supplied at a rate of 5 kg / hr., The second kneading zone temperature is set to 120 ° C., and kneading is further performed, and 30 parts of fine powder a is further supplied at a constant rate of 1.4 kg / hr. From the third raw material supply port. After the temperature of 3 kneading zones was set to 140 ° C., the mixture was melt-kneaded, cooled, pulverized and classified to obtain colored particles having a volume average particle diameter of 8 μm. Further, 0.4 part of hydrophobic silica and 0.4 part of titanium oxide were added to the colored particles to obtain toner E of the present invention. The dispersed state of the colorant and the release agent in the resin of the colored particles E was almost uniform.

This toner E is used as a copying machine U-BI manufactured by Konica Corporation.
X1017 (equipped with a fluorine resin coated heat roller, no roller cleaning mechanism, modified fixing roller setting temperature variable type)
Heat roller linear velocity of 130mm / sec, linear pressure of 0.80kg / cm
When the offset performance was evaluated by setting the value to 1, the offset phenomenon did not occur up to 220 ° C.

Further, this toner E is used as a copying machine manufactured by Konica Corporation.
As a result of performing an actual copy evaluation using U-BIX 3135, the change in the charge amount with time was small, and fog did not occur up to 40,000 copies.

Example 2 Resin: Polyester resin (softening point 138 ° C. static bulk density 0.60 g / cm ³ ) 100 parts Colorant: furnace black (number average primary particle diameter 16 nm static bulk density 0.15 / cm ³ ) 8 parts Release agent: Low molecular weight polyethylene (static bulk density 0.51 g / cm ³ ) 4 parts Classification separation fine powder; Fine powder b (static bulk density 0.19 g / cm ³ ) 25 parts Using the toner manufacturing apparatus shown in FIG. , 100 parts of the above resin and 4 parts of the release agent are supplied at a constant rate of 5.1 kg / hr. From the first raw material supply port 4 through separate feeders, the screw rotation speed is 150 rpm, and the first kneading zone temperature is 145 ° C
And kneading, 8 parts of the colorant is fed from the second raw material supply port 6 at a rate of 0.4 kg / hr., The second kneading zone temperature is set to 130 ° C., and the fine powder b30 is added. Part is quantitatively supplied from the third raw material supply port 12 at a rate of 1.2 kg / hr.
After the temperature of the third kneading zone is set to 150 ° C and the mixture is melt-kneaded, it is cooled, pulverized and classified to have a volume average particle diameter of 8μ.
m colored particles were obtained. Further, 1.1 parts of hydrophobic silica was added to the colored particles to obtain toner F of the present invention. The dispersed state of the colorant and the release agent in the resin of this toner F was substantially uniform.

This toner F is used as a copying machine U-BI manufactured by Konica Corporation.
X1017 (equipped with a fluorine resin coated heat roller, no roller cleaning mechanism, modified fixing roller setting temperature variable type)
Heat roller linear velocity of 130mm / sec, linear pressure of 0.80kg / cm
As a result of performing offset performance evaluation with setting to, the offset phenomenon did not occur up to 230 ° C.

Further, this toner F is used as a copying machine manufactured by Konica Corporation.
As a result of performing an actual copy evaluation using U-BIX 3135, the change in the charge amount with time was small, and fog did not occur up to 40,000 copies.

Example 3 Resin: Polyester resin (softening point 119 ° C. static bulk density 0.63 g / cm ³ ) 100 parts Colorant; C.I. I. Pigment Red 122 (number average particle size 100 nm, static bulk density 0.17 g / cm ³ ) 7 parts Classification separation fine powder; Fine powder c (static bulk density 0.27 g / cc) 35 parts Using the toner manufacturing apparatus shown in FIG. Resin 100 parts from the first raw material supply port 4, colorant 7 parts from the second raw material supply port 6, fine powder c35 parts from the third raw material supply port 4.3 kg / h
It is supplied at a constant rate of r., 0.3 kg / hr., 1.5 kg / hr., the screw rotation speed is 200 rpm, the first and second kneading zone temperatures are 130 ° C, and the third kneading zone temperature is 135 ° C. After kneading, the mixture was cooled, pulverized, and classified to obtain colored particles having a volume average particle diameter of 9 μm. Further, 0.6 part of hydrophobic silica and 0.2 part of hydrophobic alumina were added to the colored particles to obtain toner G of the present invention. The dispersibility of the pigment in the resin of this toner G was substantially uniform.

This toner G is used as a copying machine U-BI manufactured by Konica Corporation.
X 1017 (equipped with fluororesin coated heat roller, silicone oil application device, modified fixing roller temperature setting type)
Heat roller linear velocity of 130mm / sec, linear pressure of 0.80kg / cm
When the offset performance was evaluated by setting to, the offset phenomenon did not occur up to 200 ° C.

Further, this toner G was evaluated for actual copying using a full-color electrophotographic copying machine konica 9028 manufactured by Konica Corporation. As a result, the change in charge amount over time was small and fog did not occur up to 40,000 copies. .

Example 4 Resin: Styrene acrylic resin (softening point 115 ° C., static bulk density 0.58 g / cm ³ ) 100 parts Colorant; C.I. I. Pigment Blue 15: 3 (number average particle diameter 60 nm, static bulk density 0.13 g / cm ³ ).
3 parts Release agent; Low molecular weight polypropylene (static bulk density 0.50 g / cm ³ ) 4 parts Classification separation fine powder; Fine powder d (static bulk density 0.22 g / cm ³ ) 40 parts Using the toner manufacturing apparatus shown in FIG. , 100 parts of the resin and 4 parts of the mold release agent are fed at a rate of 4.6 kg / hr. From the first raw material supply port 4 through separate feeders, the screw rotation speed is 180 rpm, and the first kneading zone temperature is Knead at 120 ℃, 3 parts of colorant from the second raw material supply port 6 to 0.
A fixed amount is supplied at a rate of 1 kg / hr., The second kneading zone temperature is set to 130 ° C. and kneading is performed, and a fine powder d is supplied at a constant rate of 1.8 kg / hr. 3 After setting the kneading zone temperature to 135 ° C and melting and kneading,
The particles were cooled, pulverized, and classified to obtain colored particles having a volume average particle diameter of 9 μm. Further, 0.9 part of hydrophobic silica was added to the colored particles to obtain toner H of the present invention. The dispersed state of the pigment and the release agent in the resin of this toner H was almost uniform.

This toner H is used as a copying machine U-BI manufactured by Konica Corporation.
X 1017 (equipped with fluorine resin coated heat roller, no roller cleaning mechanism, modified fixing roller setting temperature variable type)
Heat roller linear velocity of 130mm / sec, linear pressure of 0.80kg / cm
When the offset performance was evaluated by setting to, the offset phenomenon did not occur up to 200 ° C.

Further, this toner H was evaluated for actual copying using a full-color electrophotographic copying machine konica 9028 manufactured by Konica Corporation. As a result, the change in the charge amount with time was small and fog did not occur up to 40,000 copies. .

Comparative Example 1 Comparative Example 1 Resin: Styrene acrylic resin (softening point 125 ° C. static bulk density 0.58 g / cm ³ ) 100 parts Colorant: furnace black (number average primary particle size 20 nm static bulk density) 0.17 g / cm ³ ) 10 parts Release agent; Low molecular weight polypropylene (static bulk density 0.48 g / cm ³ ) 5 parts Classification and separation fine powder; Fine powder a (static bulk density 0.22 g / cm ³ ) 30 parts Using a toner manufacturing apparatus, 100 parts of the resin, 10 parts of the colorant, 5 parts of the release agent, and 30 parts of the fine powder for classification and separation were collectively supplied from the first raw material supply port 4 through the same feeder at 7.0 kg.
/ Rpm is supplied at a constant rate and the screw rotation speed is 200 rp
m, the temperature of the first and second kneading zones was set to 120 ° C., and the mixture was melt-kneaded, then cooled, pulverized and classified to obtain colored particles having a volume average particle diameter of 9 μm. Further, 0.8 part of hydrophobic silica was added to the colored particles to obtain a comparative toner I. In this toner I, colorant aggregates were observed and the dispersion state was non-uniform.

This toner I is a copy machine U-BI manufactured by Konica Corporation.
X 1017 (equipped with fluorine resin coated heat roller, modified fixing roller setting temperature variable type) heat roller linear velocity of 130 mm /
As a result of performing offset performance evaluation with the line pressure set to 0.80 kg / cm for 2 seconds, the offset phenomenon occurred at 170 ° C.

Further, this toner I is used as a copying machine manufactured by Konica Corporation.
As a result of evaluation of actual images using U-BIX 3135, the amount of electrification was drastically decreased and fogging on the image was serious after 1000 copies and it was not practical.

Comparative Example 2 Resin: Styrene acrylic resin (softening point 125 ° C. static bulk density 0.58 g / cm ³ ) 100 parts Colorant: furnace black (number average primary particle diameter 20 nm static bulk density 0.17 g / cm ³ ) 10 parts Release agent; Low molecular weight polypropylene (static bulk density 0.48 g / cm ³ ) 5 parts Classification separation fine powder; Fine powder a (static bulk density 0.22 g / cm ³ ) 30 parts The toner manufacturing apparatus shown in FIG. Using 100 parts of the above resin and 30 parts of fine powder for classification and separation, a fixed amount is supplied through a separate feeder from the first raw material supply port 4 at a total speed of 6.3 kg / hr., The screw rotation speed is 200 rpm, and the first kneading zone. Kneading is performed by setting the temperature to 120 ° C, and 10 parts of the colorant is quantitatively supplied from the second raw material supply port 6 at a rate of 0.5 kg / hr., And the second kneading zone temperature is set to 120 ° C and kneading is performed. , Release agent 5
Part of the third raw material supply port 12 at a rate of 0.25 kg / hr., The third kneading zone temperature is set to 130 ° C., and the mixture is melt-kneaded, followed by cooling, pulverizing, and classifying to obtain volume average particles. Colored particles having a diameter of 9 μm were obtained. Further, 0.8 part of hydrophobic silica was added to the colored particles to obtain comparative toner J. In this toner J, an agglomerate of a release agent was observed and the dispersion state was non-uniform.

This toner J is a copying machine U-BI manufactured by Konica Corporation.
X 1017 (equipped with fluorine resin coated heat roller, modified fixing roller setting temperature variable type) heat roller linear velocity of 130 mm /
As a result of performing offset performance evaluation with the line pressure set to 0.80 kg / cm for 2 seconds, the offset phenomenon occurred at 160 ° C.

Further, this toner J is a copying machine manufactured by Konica Corporation.
As a result of performing an actual shooting evaluation using U-BIX 3135, the fixing cleaning member was heavily soiled and could not be put to practical use.

Comparative Example 3 Resin: Styrene acrylic resin (softening point 115 ° C., static bulk density 0.58 g / cm ³ ) 100 parts Colorant; C.I. I. Pigment Blue 15: 3 (number average particle size 60 nm, static bulk density 0.13 g / cm ³ ) 3 parts Release agent; low molecular weight polypropylene (static bulk density 0.50 g / cm ³ ) 4 parts Classification separation fine powder; Fine powder d (static) Bulk density 0.22 g / cm ³ ) 40 parts Using the toner manufacturing apparatus shown in FIG. 4, 100 parts of the resin and 3 parts of the colorant are fed by separate feeders to the first raw material supply port 4
To 4.6 kg / hr. At a constant rate, kneading with the screw rotation speed set to 180 rpm and the first kneading zone temperature set to 120 ° C., and 4 parts of the release agent from the second raw material supply port 6 to 0.1 k
It is supplied at a constant rate of g / hr., the second kneading zone temperature is set at 130 ° C. and kneaded, and the fine powder d is supplied at a constant rate of 1.8 kg / hr. from the third raw material supply port. After the kneading zone temperature was set to 135 ° C. and the mixture was melt-kneaded, it was cooled, pulverized and classified to obtain colored particles having a volume average particle diameter of 9 μm. Further, 0.9 part of hydrophobic silica was added to the colored particles to obtain Toner K of the present invention. Aggregates were observed in the pigment in the resin of this toner K, and the dispersed particle diameter of the pigment was not uniform.

This toner K is used as a copying machine U-BI manufactured by Konica Corporation.
Offset performance of X1017 (equipped with fluorine-coated heat roller, no roller cleaning mechanism, modified fixing roller setting temperature variable type) heat roller linear velocity of 130 mm / sec and linear pressure of 0.80 kg / cm The offset phenomenon occurred at 180 ° C.

Further, this toner K was evaluated for actual copying using a full-color electrophotographic copying machine Konica 9028 manufactured by Konica Corporation. As a result, after 10,000 copies, the charge amount began to decrease and fog was generated on the image. It wasn't practical.

[0062]

EFFECTS OF THE INVENTION According to the toner manufacturing method, a toner composition such as a resin, a colorant, a release agent, and a toner classification / separation fine powder can be prepared in a resin such as a colorant or a release agent without requiring a preliminary mixing step. Good dispersibility can be ensured, and by omitting the preliminary mixing step, the manufacturing process can be simplified, the manufacturing efficiency can be increased, and the toner manufacturing cost can be significantly reduced.

On the other hand, the simultaneous inclusion of the toner classification and separation fine powder suppresses the breakage of the molecular chain during kneading and can maintain the offset performance. Therefore, since the toner manufactured by the toner manufacturing method has excellent dispersibility of the colorant and the release agent,
Not only the uniformity of the charge amount is ensured, but also the fixing performance is excellent and the developer has long-term durability.

[Brief description of drawings]

FIG. 1 is a schematic diagram of a toner manufacturing apparatus having a kneading machine of the present invention.

FIG. 2 is a schematic diagram of a toner manufacturing apparatus having a kneading machine of the present invention.

FIG. 3 is a schematic diagram of a toner manufacturing apparatus having a kneader of the present invention.

FIG. 4 is a schematic view of a toner manufacturing apparatus having the kneading machine of the present invention.

[Explanation of symbols]

1 Shizukasa density 0.30~0.70g / cm ³ of the toner composition of the toner composition input hopper 2 Shizukasa density 0.02~0.30g / cm ³ charging hopper 3 feeder 4 first raw material supply port 5 side feeder 6 second raw material supply mouth

Claims (3)

[Claims] 1. A toner for an electrostatic charge image developer obtained by kneading a composition comprising at least a resin, a colorant, a release agent and a toner classification and separation fine powder, wherein the kneading machine has at least two or more raw material supply ports. In the above composition, a composition having a static bulk density of 0.30 to 0.70 g / cm ³ is supplied from a first raw material supply port provided on the most upstream side of the kneader, and at least toner classification separation is performed. Static bulk density including fine powder is 0.02-0.30
A toner for an electrostatic image developer, characterized in that the composition of g / cm ³ is supplied and kneaded from a raw material supply port provided on the downstream side of the first raw material supply port of the kneader. 2. A toner for an electrostatic charge image developer produced through a step of kneading a composition comprising at least a resin, a colorant, a release agent and a toner classification and separation fine powder using a twin-screw extruder, The twin-screw extruder has at least two or more raw material supply ports in the barrel length direction, and a composition having at least a static bulk density of 0.30 to 0.70 g / cm ³ comprising a resin and a mold release agent is used for the extruder. The first raw material for the extruder is a composition having a static bulk density of 0.02 to 0.30 g / cm ³ which is supplied from a first raw material supply port provided on the most upstream side of A toner for an electrostatic image developer, which is characterized in that it is supplied from a raw material supply port provided on the downstream side of the supply port and kneaded. 3. A method for producing a toner for an electrostatic image developer, which comprises kneading a composition comprising at least a resin, a colorant, a release agent, and fine powder for toner classification and separation using at least a twin-screw extruder. The machine has at least two or more raw material supply ports in the length direction of the barrel, and the static bulk density of at least resin and mold release agent is 0.30 to 0.70 g / cm.
The composition of ³ is supplied from the first raw material supply port provided on the most upstream side of the extruder, and has a static bulk density of 0.02 to 0.30 g / cm ³ including at least a colorant and a toner classification / separation fine powder. Is supplied from a raw material supply port provided on the downstream side of the first raw material supply port of the extruder, and kneading is performed.