KR101322920B1 - Method for Preparing Toner Comprising Suspension-Cohesion Polymerization Method - Google Patents

Abstract

The present invention relates to a method for producing a toner by a new suspension coagulation polymerization method. The suspension coagulation polymerization method of the present invention is prepared by dispersing and incorporating an initiator solution into the oil phase droplets by suspending agglomeration and association in the final stage of the assembling process. It is possible to minimize the disadvantage that the partially polymerized oil droplets stick to the wall of the stirring rod or the assembly tank during the assembly process, so that the manufacturing process is stable and the yield of the polymerization toner obtained in preparation for the input raw materials is generally suspended. Significantly higher than legal.

Description

Method for Preparing Toner Comprising Suspension-Cohesion Polymerization Method

The present invention relates to a manufacturing method of a toner using suspension coagulation polymerization method.

A toner for a laser printer and a multifunction apparatus is divided into pulverized toner and polymerized toner according to the production method. Pulverized toner is manufactured by dry mixing and mixing the polymerized resin and pigment, charge control agent and release agent to be distributed in toner particles, cooling by melt mixing, crushing finely by applying mechanical impact, and selecting the desired particle size and treating the surface. Manufacturing requires complex mechanical processes and requires a lot of energy. The toner produced in this manner is known to have poor developing properties and transferability because the pigment and release agent are highly likely to come out on the toner particle surface and have a morphology. In addition, since the distribution of the toner particle size during mechanical pulverization is broad, it is necessary to perform a screening operation for a desired particle size, so that the yield is low because the amount of toner to be produced is small compared with the amount of raw materials used. In order to solve the problem of such a pulverized toner, the development of a polymerized toner is in full swing.

The polymerized toner is mainly prepared by a suspension polymerization technique, in which an oil phase containing a monomer, a pigment, a charge controlling agent, a release agent and the like is dispersed in a water phase containing a suspension stabilizer by giving a mechanically high shear force to particles having a desired particle size Since a toner is manufactured by making a suspension and polymerized to produce a toner having a small energy consumption at the time of production and a particle diameter distribution of the toner is narrow so that only particles having a desired particle diameter are selected as in the case of a pulverized toner, Since the amount of toner to be produced is large in comparison with the amount of the raw material, the yield is higher than that of the pulverized toner production process. The polymerized toner thus produced has a spherical shape or a potato shape and has a narrow particle size distribution, and also has a superior performance because it can prevent the problem of pulverized toner in which the pigment and the release agent come out to the toner particle surface.

On the other hand, Korean Patent Publication Nos. 10-2011-0046376, 10-2011-0097668, 10-2011-00113051, and 10-2010-0034305 disclose a manufacturing method of a toner using a polymerization method.

Recently, with the spread of digital devices, the spread of high-quality high-speed color laser printers has been rapidly increasing, so the necessity of developing and distributing high-quality polymerized toner is also rapidly increasing. However, in general, the process of manufacturing polymerized toner by suspension polymerization method has the disadvantage of partially polymerized oil droplets sticking to the wall of the stirring rod or assembly tank when the polymerization process proceeds during oil droplet assembly. Not only that, but also due to this problem, the yield of the polymerization toner obtained is low compared to the amount of the input raw materials. Therefore, a new method of producing a polymerized toner that can stably operate easily and easily controls the production process is not only high yield of polymerized toner obtained by overcoming the above disadvantages of the general process of polymerized toner by the suspension polymerization method, but also effective in controlling the manufacturing process. need.

Numerous papers and patent documents are referenced and cited throughout this specification. The disclosures of the cited papers and patent documents are incorporated herein by reference in their entirety to better understand the state of the art to which the present invention pertains and the content of the present invention.

The inventors of the present invention minimize the unnecessary polymerization of the oil phase droplets during the oil phase droplet assembly process of the general suspension polymerization process by controlling the timing of the initiator injection, thereby partially polymerizing the oil phase droplets on the wall of the stirring rod or the assembly tank. Efforts have been made to develop an improved process for producing polymerized toner that can prevent sticking disadvantages. As a result, a primary particle granulation suspension is prepared using an oil phase containing no initiator, and the initiator solution is added thereto to prepare a final particle granulation suspension through suspension agglomeration and association. By minimizing the polymerization reaction, it is possible to prevent the disadvantage that the partially polymerized oil droplets stick to the wall of the stirring rod or the assembly tank, and the yield of the polymerization toner obtained in proportion to the amount of raw materials added is high. The present invention was completed by confirming that it is easy.

It is therefore an object of the present invention to provide a method for producing a polymerized toner by suspension coagulation polymerization.

The objects and advantages of the present invention will become more apparent from the following detailed description of the invention, claims and drawings.

According to one aspect of the present invention, there is provided a toner manufacturing method comprising the steps of: (a) preparing a water phase comprising distilled water and a suspension stabilizer; (b) preparing an oil phase comprising at least one monomer, colorant, charge control agent, crosslinker and wax; (c) dissolving the initiator in one monomer to prepare an initiator solution; (d) adding the prepared aqueous phase and the oil phase to the oil phase droplet granulator and stirring to prepare a primary particle granulation suspension in which the oil phase droplets are dispersed; (e) After adding the initiator solution prepared in step (c) to the primary particle granulation suspension prepared in step (d), stirring at a high speed to produce ultra-suspended particles, and then the ultra-suspended particles Preparing a final particle granulation suspension by stirring at low speed so as to produce final suspended particles through suspension agglomeration and association again; (f) warming and polymerizing the final granulation suspension prepared in step (e) in a reactor to form toner particles.

Hereinafter, the production method of the present invention will be described in detail in each step.

Step (a): Water (distilled water containing a suspension stabilizer, and phase )

In the toner manufacturing method of the present invention, first, distilled water and a suspension stabilizer are added to an aqueous reservoir equipped with a stirrer capable of raising a temperature to prepare an aqueous phase.

As the suspension stabilizer used for the preparation of the aqueous phase in the method of the present invention, an organic suspension stabilizer, an inorganic suspension stabilizer or a cellulose-based water-soluble resin is used. The organic suspension stabilizer may be selected from the group consisting of polyvinyl alcohol, polyacrylic acid salts, polyethylene glycol, polyvinyl pyrrolidone, polyacrylamide, and tertiary phosphates, but is not limited thereto. The inorganic suspension stabilizer may be at least one selected from the group consisting of polyvalent metal salts of phosphoric acid such as calcium phosphate, magnesium phosphate, aluminum phosphate and zinc phosphate, carbonates such as calcium carbonate and magnesium carbonate, inorganic salts such as calcium sulfate and barium sulfate, calcium hydroxide, Silica, bentonite, and alumina, but the present invention is not limited thereto. The cellulose water-soluble resin may be selected from the group consisting of methyl cellulose, hydroxyethyl cellulose, and hydroxypropyl methyl cellulose, but is not limited thereto.

The content of the suspension stabilizer is preferably 0.1 to 10 parts by weight based on 100 parts by weight of distilled water.

The distilled water and the suspension stabilizer are poured into a water reservoir and heated to a temperature of, for example, 60 to 80 ° C to prepare a water phase. During the preparation of the aqueous phase, the suspension stabilizer is sufficiently dissolved in distilled water in parallel with heating and stirring.

Step (b): oil comprising one or more monomers , colorants, charge control agents , crosslinkers and waxes phase )

In step (b) an oil phase is prepared comprising at least one monomer, colorant, charge control agent, crosslinker and wax. That is, in the method of the present invention, an oil phase containing only the initiator and all other toner particle components is prepared and used.

In the present invention, the monomer contained in the oil phase is selected from among aromatic vinyl monomers, acrylate monomers and methacrylate monomers. The monomer may be selected from, for example, styrene, monochlorostyrene, methylstyrene, dimethylstyrene, acrylate, methacrylate, methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, But are not limited to, acrylate, ethyl methacrylate, propyl methacrylate, butyl methacrylate, or 2-ethylhexyl methacrylate. The content of the monomer is not limited, but it is preferably within the range of 50-97 parts by weight based on 100 parts by weight of the oil phase. If the content of the monomer is less than 50 parts by weight, the function required for the toner can not be sufficiently exhibited. If the amount is more than 97 parts by weight, the viscosity is too high and it is difficult to obtain a polymerized toner having a uniform particle diameter.

In the present invention, the colorant may be selected from, for example, yellow, magenta, cyan, and black pigments, but is not limited thereto. As the yellow colorant, condensed nitrogen compounds, isoindolinone compounds, atrazine compounds, azo metal complexes, or allyl imide compounds are used. Specifically, C.I. Pigment Yellow 12, 13, 14, 17, 62, 74, 83, 93, 94, 95, 109, 110, 111, 128, 129, 147, 168, 180 and the like can be used. The magenta colorant may be a condensed nitrogen compound, an anthraquin, a quinacridone compound, a base dye rate compound, a naphthol compound, a benzoimidazole compound, a thioindigo compound, or a perylene compound. Specifically, C.I. Pigment Red 2, 3, 5, 6, 7, 23, 48: 2, 48: 3, 48: 4, 57: 1, 81: 1, 122, 144, 146, 166, 169, 177, 184, 185, 202, 206, 220, 221, or 254 may be used. The cyan colorant may be a copper phthalocyanine compound or its derivative, an anthraquinone compound, or a base dye rate compound. Specifically, C.I. Pigment Blue 1, 7, 15, 15: 1, 15: 2, 15: 3, 15: 4, 60, 62, 66 or the like can be used. Carbon black may be used as the black pigment. The colorant may be used alone or in admixture of two or more thereof, and is selected in consideration of color, saturation, lightness, weather resistance, dispersibility in toner, and the like. The content of the colorant is preferably 0.1 to 20 parts by weight based on 100 parts by weight of the oil phase.

The charge phase of the present invention may contain a charge control agent. The charge control agent is selected from the group consisting of salicylic acid, dibutylsalicylic acid, naphthoic acid, dicarboxylic acid, aluminum dibutylsalicylic acid compound, zinc dibutylsalicylic acid compound, zirconium dibutylsalicylic acid compound, chromic dibutylsalicylic acid compound, nigrosine compound, quaternary ammonium salt , Imidazole compounds may be used, but are not limited thereto.

A crosslinking agent may be added to the oil phase of the present invention, and for example, divinylbenzene, trimethylolpropane triacrylate, pentaerythritol triacrylate, or pentaerythritol tetraacrylate may be used, but the present invention is not limited thereto.

Wax may be added to the oil phase of the present invention. For example, polyethylene wax, polypropylene wax, silicone wax, paraffin wax, ester wax, carnauba wax and metallocene wax may be used. But is not limited thereto. The content of the wax is not particularly limited, but is preferably 0.1 to 30 parts by weight based on 100 parts by weight of the oil phase.

A pigment dispersant may be added to the oil phase of the present invention. The pigment dispersant is selected depending on the characteristics of the pigment and the monomer. It can be used to increase the dispersing effect of the pigment by using a chemical compound having affinity to the pigment and the monomer.

Step (c): in one monomer Dissolving the initiator to prepare an initiator solution

An initiator solution is prepared by dissolving the initiator in one of the monomers of the one or more monomers constituting the toner particles. If an initiator solution is prepared by selecting only one monomer of one or more monomers constituting the toner, the initiator solution can be prepared in a simple and stable manner in a more simple and stable manner than in the case of dissolving the initiator in two or more monomers. In the present invention, the polymerization of the oil phase droplets preferably proceeds from the reaction of the radicals produced by the initiator with the monomers. Polymerization initiators usable in the process of the present invention include, but are not limited to, azo compounds, peroxides, redox initiators, and the like, for example, 4,4-azobis (4-cyanogilacetic acid), Dimethyl-2,2'-azobis (2-methylpropionate), 2,2-azobis (2-amidinopropane) dihydrochloride, 2,2-azobis-2-methyl-N-1,1 -Bis (hydroxymethyl) -2-hydroxyethylpropioamide, 2,2'-azobis (2,4-dimethylvaleronitrile), 2,2'-azobisisobutyronitrile, 1,1 Azo compounds such as' -azobis (1-cyclohexanecarbonitrile); But are not limited to, methyl ethylperoxide, di-t-butyl peroxide, acetyl peroxide, dicumyl peroxide, lauroyl peroxide, benzoyl peroxide, Peroxides such as oxy dicarbonate and di-t-butyl peroxyisophthalate; Persulfates such as potassium persulfate and ammonium persulfate, but are not limited thereto.

The content of the initiator is preferably 0.1 to 5 parts by weight based on 100 parts by weight of the monomer. If the content of the initiator is less than 0.1 part by weight based on 100 parts by weight of the monomer, the effect of initiating polymerization is insufficient, and if it exceeds 5 parts by weight, the molecular weight of the polymerized polymer becomes small, It is not desirable.

Step (d): the step of producing the above-prepared aqueous phase and yusangreul a stirred and then added to W emulsion dispersion had a primary particle suspension assembly to the oil phase droplet granulator

The aqueous phase is added and mixed with an oil phase containing no initiator, and the mixture is stirred to prepare a primary particle granulated suspension in which oil phase droplets are dispersed. Since the primary particle granulation suspension preparation process proceeds without the initiator in the oil phase droplet, the polymerization does not proceed, and the next step makes the process of containing the initiator in the oil phase droplet easier.

Step (e): The initiator prepared in step (c) is added to the primary particle granulation suspension prepared in step (d). In one yongaekreul then suspended ultrafine particles are to be created at a high speed stirring, and this standing, the ultra-fine particles are suspended are aggregated again suspended Preparing a final particle granulation suspension by stirring at low speed so that the final suspended particles are made through the association process.

In the present invention, the preparation of the final particle granulation suspension is performed by mixing the primary granulation suspension and the initiator solution followed by high speed stirring and low speed stirring to prepare the final particle granulation suspension. That is, the initiator solution prepared in step (c) is added to the primary particle granulation suspension prepared in step (d), and ultrafine suspended particles composed of oil phase particles and initiator solution oil phase particles which do not contain an initiator are The final particle granulation suspension is prepared by stirring at high speed to make, and then at low speed to produce the initiator-containing oily droplet suspension particles through the process of suspending and associating the ultrafine suspended particles again.

In the present invention, the ultrafine suspended particles mean particles having a size of 1 μm or less, and the final suspended particles mean particles having an average particle diameter of 1-10 μm.

The term "high speed" in the present invention may vary depending on the stirrer, but refers to a stirring speed at which ultrafine suspended particles having a size of 1 μm or less may be made, and the term "low speed" may vary depending on the stirrer. However, the ultra-suspended particles having a size of 1 μm or less are suspended and aggregated again to mean a stirring speed at which final suspended particles having an average particle size of 1 to 10 μm may be made.

According to one specific embodiment of the invention, when stirring using a conventional homogenizer, the high speed is at least 3,000 rpm, more preferably at least 4,000 rpm, even more preferably at least 5,000 rpm. Further, it is preferable that the low speed is adjusted to 500 rpm or less, more preferably 1,000 rpm or less, and still more preferably 2,000 rpm or less.

Step (f): warming and polymerizing the suspension prepared in step (e) in a reactor to form toner particles

The final particle granulated suspension prepared in step (e) is stirred at a constant stirring speed in a reactor connected to a cooling capacitor and reacted under a nitrogen atmosphere to form toner particles.

According to one preferred embodiment of the present invention, when the main component of the monomer contained in the oil phase is a styrene monomer, the final particle granulation suspension is put into a reactor connected to the cooling capacitor and then reacted while maintaining a stirring speed of 100 to 500 rpm under a nitrogen atmosphere After the first polymerization at a temperature of 50 to 80 ℃ for 2 to 24 hours, the polymerization is finally polymerized to complete the polymerization reaction for 2 to 12 hours at a reaction temperature of 75 to 95 ℃ to form toner particles.

Typically, after step (f), a step of separating, drying, and surface treating the toner particles is further included. After the toner particles formed through the cleaning process and the filtering process are separated and dried in a vacuum oven at 30 to 40 캜 for more than 24 hours, a final polymerized toner capable of processing the surface of the toner particles so as to prevent the toner particles from adhering to each other, Obtain the product.

The average particle diameter of the toner produced by the above method of the present invention is preferably 1-10 m.

The present invention relates to a method for producing a toner by a new suspension coagulation polymerization method. The suspension coagulation polymerization method of the present invention is prepared by dispersing and incorporating an initiator solution into the oil phase droplets by suspending agglomeration and association in the final stage of the assembling process. It can be minimized. In addition, it is possible to prevent the disadvantage that oil droplets partially polymerized during the assembly process stick to the wall of the stirring rod or the assembly tank, so that the manufacturing process is stable and the yield of the polymerization toner obtained in comparison with the raw materials added is higher than that of the general suspension polymerization method. Significantly higher.

1 is a view showing a polymerization toner manufacturing process by a conventional suspension polymerization method. As shown in FIG. 1, the prepared aqueous and oil phases are mixed and stirred to form a final granulated suspension, which is then polymerized to form toner particles. Subsequently, the final polymerization toner is prepared by performing a cleaning process and a drying process for removing a suspension stabilizer that may be stuck to the surface of the toner particles, and surface treating the toner particles so as not to stick to each other during use. In the conventional suspension polymerization method, in order to effectively disperse and melt all the components in the process of preparing an oil phase containing all of the toner particle components, stirring is required above the melting temperature of the component having the highest melting temperature. The reaction is advanced in advance, making it difficult to effectively control the final particle granulation suspension preparation process. Therefore, it is difficult to optimize the processing conditions such as stirring temperature and time, and there is a disadvantage in that the yield of the polymerization toner obtained compared to the amount of the input raw materials is low.
2 is a view showing a polymerization toner production process by the suspension coagulation polymerization method of the present invention. As shown in FIG. 2, the prepared aqueous phase and the oil phase containing no initiator are mixed and stirred to form a primary particle granulation suspension, and then an initiator solution prepared by dissolving an initiator in a monomer is added thereto to suspend aggregation and association. To prepare a final particle granulation suspension containing an initiator in the oil phase droplets, which are then polymerized to form toner particles. Subsequently, the polymerized toner product is completed by treating the surface so that the toner particles do not stick together while being used through a washing process and a drying process to remove the suspension stabilizer that may be attached to the surface of the toner particles.
3 is a view showing the preparation of the final granulated suspension by suspension agglomeration of the present invention. After preparing the primary particle granulation suspension composed of oil-free particles containing no initiator, the initiator solution was added and stirred at a high speed to produce ultra-suspended particles composed of initiator-excluded oil particles and initiator solution oil particles having a size of 1 μm or less. Subsequently, the final particle granulation suspension is prepared by stirring at a low speed so that the ultra-suspended particles are suspended and aggregated again to form suspended particles composed of initiator-containing oil droplets having an average particle size of 1-10 μm.

Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for describing the present invention in more detail and that the scope of the present invention is not limited by these embodiments in accordance with the gist of the present invention .

Example

Example  One : Suspension Condensation Polymerization  Used Of the polymerized toner  Produce

A polymerized toner was prepared by the suspension coagulation polymerization method of the present invention. First, 300 g of distilled water and 8 g of polyvinyl chloride (PVA, molecular weight 20,000, Junsei Co., Ltd.) as a suspending stabilizer were added to a 500 ml water reservoir (duran) equipped with a stirrer, and the temperature of the reservoir was increased. Stirring slowly at 65 ° C. to sufficiently dissolve the suspension stabilizer to prepare a water phase.

Styrene (Junsei) 16.0 g, n-butyl acrylate (Junsei) 8.00 g, carbon black (Mogul-L, Cabot) 2.24 g, charge control agent (Bontron E-84, Orient Chemical Co., Ltd.) 0.32 g , 0.64 g of suspension stabilizer (PVA, molecular weight 20,000, quasi-same company) and 0.20 g of crosslinking agent (divinylbenzene, Aldrich) were dispersed and mixed at room temperature for 6 hours using a ball mill (KMC-T2 from KOREA CO., LTD.) An oily mixture was prepared. 1.60 parts by weight of paraffin wax (Pelemol BB, Phoenix Chemical Co., Ltd.) was added to the primary oil mixture, followed by stirring for 4 hours in a water bath at 65 ° C. to prepare an oil phase containing no initiator.

The above-mentioned water phase and oil phase were put into an oil phase droplet granulator (Duran) and a homogenizer (Premix, Mark II) was used to form an oil phase droplet by stirring shear force with stirring at a speed of 5,000 rpm at 65 ° C. for 3 minutes. To prepare a primary particle granulation suspension.

8.00 g of styrene (Jansei Co.) and 1.00 g of a polymerization initiator (2,2'-azobis (2,4-dimethylvaleronitrile, Wako Chemical Co., Ltd.) were mixed to prepare an initiator solution separately, and then the prepared primary particles were assembled. After the suspension was put into a granulator containing suspension, it was stirred for 3 minutes at a high speed of 10,000 rpm at 65 ° C. to make ultra-suspended particles having a size of 1 μm or less, and then ultra-suspended with a slow stirring for 3 minutes at a low speed of 500 rpm. The final particle granulation suspension was prepared by allowing the final particles to be granulated into an oily droplet having an average particle size of 1-10 μm containing an initiator by the process of resuspending and associating the particles.

The final granulated suspension prepared above was maintained at a constant stirring speed (100 rpm) in a reactor connected to a cooling capacitor (Duran), and was first polymerized at a reaction temperature of 65 ° C. for 6 hours under a nitrogen atmosphere, followed by a reaction temperature of 75. Toner particles were prepared by finally polymerizing at 3 ° C. for 3 hours to completely terminate the polymerization.

The prepared final toner particles were thoroughly washed with a mixture of water and ethanol and filtered to remove the suspension stabilizer, and dried in a vacuum oven at 40 ° C. for 24 hours, and the toner particles were not entangled with each other. The surface of the particles was treated with silica (Aerosil R972 by Degussa) to prepare a polymerized toner.

In the suspension coagulation polymerization method of the present invention, an initiator solution is added to the final stage of the assembly process to uniformly disperse and contain the initiator in the oil droplets by suspension coagulation and association. The polymerization reaction can be minimized, and the oil droplets partially polymerized in the assembly step can be prevented from adhering to the wall of the stirring rod or the assembly tank. Thus, the polymerization toner can be produced in a high yield of 97% by a stable manufacturing process. Could. The average particle diameter of the prepared polymerized toner was 4.49 µm, and the particle size distribution coefficient (CV) was 35.8, which is narrow, and thus the particle size distribution was preferable.

Comparative Example  1: conventional Suspension polymerization  Used Of the polymerized toner  Produce

For comparison with Example 1, a polymerized toner was prepared by using a general suspension polymerization method. 300 g of distilled water and 8 g of polyvinyl chloride (PVA, molecular weight 20,000, Junsei Co., Ltd.) as a suspending stabilizer were added to a 500 ml water reservoir (Duran) equipped with a stirrer and stirred while gradually raising the temperature to 65 ° C. The suspension stabilizer was sufficiently dissolved to prepare an aqueous phase.

24 g of styrene (Junsei), 8.00 g of n-butyl acrylate (Jansei), 2.24 g of carbon black (Mogul-L, Cabot), 0.32 g of charge control agent (Bontron E-84, Orient Chemical Co., Ltd.) , By dispersing and mixing 0.64 g of suspension stabilizer (PVA, molecular weight 20,000, Junsei Co., Ltd.) and 0.20 g of crosslinking agent (Divinylbenzene, Aldrich Co., Ltd.) at a room temperature for 6 hours using a ball mill (KMC-T2 from KOREA CO., LTD.) An oily mixture was prepared. To this primary oil mixture, 1.60 g of paraffin wax (Pelemol BB, Phoenix Chemical Co., Ltd.) was added, followed by stirring in a water bath at 65 ° C. for 4 hours to fully dissolve, followed by polymerization initiator (2,2'-azobis (2,4- 1.00 g of dimethylvaleronitrile, Wako Chemical Co., Ltd. was added and stirred for 3 minutes to prepare an oil phase.

1-10 μm by stirring shear force while putting the prepared water phase and oil phase in the oil phase droplet granulator (Duran) and stirring for 3 minutes at a speed of 7,000 rpm at 65 ° C. using a homogenizer (Mark II). Final particle granulation suspensions were prepared by forming oily droplets having an average particle diameter of size.

The final granulated suspension prepared above was first polymerized at a reaction temperature of 65 ° C. for 6 hours under a nitrogen atmosphere while maintaining a constant stirring speed (100 rpm) in a reactor connected to a cooling capacitor (Duran), followed by a reaction temperature of 75 ° C. The toner particles were finally prepared by polymerizing finally for 3 hours to completely terminate the polymerization reaction. The final toner particles were thoroughly washed with a mixture of water and ethanol and filtered to remove suspension stabilizers. The toner particles were dried in a vacuum oven at 40 ° C. for 24 hours, and the toner particles were not entangled with each other. Was treated with silica (Aerosil R972 from Degussa) to prepare a polymerized toner.

After the paraffin wax is dissolved, an initiator is added and mixed to prepare an oil phase, the oil phase is transferred to a granulator, and the oil phase droplets which are partially polymerized due to the early polymerization reaction during the final granulation suspension production process are partially polymerized. The production process was not stable due to the problem of sticking to the stirring rod or the wall of the assembly tank, and the yield of the polymerization toner was 51% because the raw materials were lost. The average particle size of the prepared polymerized toner was 5.11 µm, and the particle size distribution coefficient (CV) was 45.7, which was wider than that of the toner prepared in Example 1.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the same is by way of illustration and example only and is not to be construed as limiting the scope of the present invention. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (6)

A process for preparing a polymerized toner comprising the following steps:
(a) preparing a water phase comprising distilled water and a suspension stabilizer;
(b) preparing an oil phase comprising at least one monomer, colorant, charge control agent, crosslinker and wax;
(c) dissolving the initiator in one monomer to prepare an initiator solution;
(d) adding the prepared aqueous phase and the oil phase to the oil phase droplet granulator and stirring to prepare a primary particle granulation suspension in which the oil phase droplets are dispersed;
(e) After adding the initiator solution prepared in step (c) to the primary particle granulation suspension prepared in step (d), stirring at a high speed to produce ultra-suspended particles, and then the ultra-suspended particles Preparing a final particle granulation suspension by stirring at low speed so as to produce final suspended particles through suspension agglomeration and association again;
(f) warming and polymerizing the final granulation suspension prepared in step (e) in a reactor to form toner particles.
The method of claim 1, wherein the suspension stabilizer in step (a) is an organic suspension stabilizer or an inorganic suspension stabilizer.
The method of claim 1, wherein the monomer in step (b) is at least one selected from aromatic vinyl monomers, acrylate monomers and methacrylate monomers.
The method of claim 1, wherein the ultra-suspended particles in the step (e) is a particle having a size of less than 1μm, the final suspended particles are particles having a particle size of 1-10μm average particle diameter Way.
The method of claim 1, wherein the high speed stirring in step (e) is 5,000 rpm or more, and the low speed stirring is 2,000 rpm or less.
The method of claim 1, wherein the average particle diameter of the polymerized toner particles prepared in the step (f) is 1-10μm.

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