Treatment method using a cyclone device

Abstract

To provide a processing method using a cyclone device which has high separation performance and can be operated for a long time.SOLUTION: A processing method is provided, for processing a processing object using a cyclone device 9, the cyclone device has: a container 1 that is installed almost vertically; and inlet piping 4 that is connected from an almost horizontal direction to an almost tangential direction of the container and supplies the processing object into the container. The container has an almost circular form in a horizontal cross section including the inlet piping. The cyclone device has a swirling space (i) in which the processing object supplied from the inlet piping swirls, and a second space (ii) outside the swirling space and at a position near the inlet piping. At least a part of the processing object swirling in the swirling space joins with a processing object that is newly supplied from the inlet piping after having gone through the second space.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a method for treating an object using a cyclone device, a method for producing powder using this method, and a method for producing toner for developing electrostatic images used in electrophotographic image formation using this method. [Background technology]

[0002] In recent years, the quality requirements in various industries have become stricter, and the performance required for cyclone devices used to remove coarse particles from materials being treated in manufacturing processes has also become more advanced.Cyclone devices are required to improve the yield of the product and separation capacity. To address the above-mentioned issues, for example, Patent Documents 1 and 2 disclose cyclone devices that have a structure such as a baffle plate in the inlet pipe. This increases the swirling force by suppressing collisions between the material swirling inside the container of the cyclone device and new material being supplied from the inlet pipe, thereby improving separation performance. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Special Publication No. 60-12914 [Patent Document 2] Special Publication No. 2-60385 Summary of the Invention [Problem to be solved by the invention]

[0004] However, in the above-described cyclone device, the materials to be treated swirling inside the container collide with the baffle plates, and the materials to be treated merge with new materials supplied from the inlet pipe, preventing the effect of increasing the swirling force from being fully achieved. Another problem is that materials adhere to the baffle plates, preventing long-term operation. Therefore, a treatment method using a cyclone device that further increases the swirling force, improves separation performance, and reduces adhesion, allowing long-term operation. An object of the present invention is to provide a method for treating an object using a cyclone device that solves the above-mentioned problems, a method for producing powder using this treatment method, and a method for producing toner using this treatment method. [Means for solving the problem]

[0005] As a result of extensive research into improving the yield, the present inventors have found the following method. That is, the present invention is a method for treating an object to be treated using a cyclone device, The cyclone device comprises: a vessel that is installed in a substantially vertical direction; and an inlet pipe connected to the container in a substantially horizontal direction and in a substantially tangential direction, for supplying the material to be treated into the container; the vessel is generally circular in horizontal cross section including the inlet pipe; The cyclone device comprises: (i) a swirling space in which the material to be treated supplied from the inlet pipe swirls; (ii) a second space located outside the swirl space and adjacent to the inlet pipe; and At least a portion of the material to be treated swirling in the swirling space passes through the second space and then merges with material to be treated newly supplied from the inlet pipe. The present invention relates to a method for treating an object to be treated, characterized in that: The present invention also relates to a method for producing powder, which comprises using the above-described treatment method. Furthermore, the present invention provides a method for producing a toner, comprising: The manufacturing method comprises: a granulation step of forming toner particle precursors in an aqueous medium to obtain a dispersion containing the toner particle precursors; a coarse particle removal step of removing coarse particles from the dispersion using a cyclone device; a drying step of filtering the toner particle precursor from the dispersion and drying the filtered toner particle precursor; and The cyclone device comprises: a vessel that is installed in a substantially vertical direction; and an inlet pipe connected to the container in a substantially horizontal direction and in a substantially tangential direction, for supplying the dispersion liquid into the container; the vessel is generally circular in horizontal cross section including the inlet pipe; The cyclone device comprises: (i) a swirling space in which the dispersion liquid supplied from the inlet pipe swirls; (ii) a second space located outside the swirl space and adjacent to the inlet pipe; and At least a part of the dispersion swirling in the swirling space passes through the second space and then merges with the dispersion newly supplied from the inlet pipe. The present invention relates to a method for producing a toner. [Effects of the Invention]

[0006] The present invention provides a processing method using a cyclone device that has excellent separation performance and can be operated for a long time.Furthermore, it provides a method for producing a powder and a toner in which coarse particles are reduced using the processing method of the present invention. [Brief explanation of the drawings]

[0007] [Figure 1] 1 is a schematic diagram showing an example of a cyclone device according to the present invention. [Figure 2] 2 is a schematic diagram showing dimensions of various parts of the cyclone device according to the present invention. FIG. [Figure 3] 1 is a schematic diagram showing the spatial location of a cyclone device according to the present invention; [Figure 4]FIG. 4 is a schematic diagram showing another example of a cyclone device according to the present invention. [Figure 5] FIG. 4 is a schematic diagram showing another example of a cyclone device according to the present invention. [Figure 6] FIG. 1 is a schematic diagram of a cyclone device used in Comparative Example 1. [Figure 7] FIG. 10 is a schematic diagram of a cyclone device used in Comparative Example 5. DETAILED DESCRIPTION OF THE INVENTION

[0008] <Cyclone device> The features of the cyclone device used in the present invention will be described below with reference to the drawings. Fig. 1 shows an example of a cyclone device according to the present invention, Fig. 2 shows the dimensions of various parts of the cyclone device, Fig. 3 shows the spatial position of the cyclone device, and Figs. 4 and 5 are schematic diagrams showing other examples of cyclone devices according to the present invention. A cyclone device 9 according to the present invention has a container 1 installed in a substantially vertical direction, and an inlet pipe 4 connected to the container in a substantially horizontal and substantially tangential direction and for supplying material to be treated into the container, and the container 1 is substantially circular in horizontal cross section including the inlet pipe 4, as shown in Fig. 1(B).

[0009] Furthermore, the cyclone device 9 (i) a swirling space 11 in which the material to be treated supplied from the inlet pipe 4 swirls; (ii) a second space 12 located outside the swirling space 11 and adjacent to the inlet pipe 4; and At least a part of the material to be treated swirling in the swirling space 11 passes through the second space 12 and then joins with new material to be treated that is supplied from the inlet pipe 4 .

[0010] Here, inlet pipe 4 is a pipe that supplies the liquid to be treated to cyclone device 9. Meanwhile, outlet pipe 5 is connected to the center of bottom plate 3, coarse particle discharge pipe 6 is connected near the lower part of the side of container 1, and coarse particle discharge pipe valve 7 is installed on the coarse particle discharge pipe immediately adjacent to the container. Furthermore, inlet pipe 4 shown in Figure 1 is the inner pipe of a double pipe structure, and has second space 12, which is the space between the inner pipe and the outer pipe.

[0011] Although the reason why the effects of the present invention are exhibited is not entirely clear, the present inventors believe that it is as follows.

[0012] When the container 1 is approximately circular in the horizontal cross section including the inlet pipe 4, the liquid to be treated supplied from the inlet pipe swirls smoothly within the container, improving separation performance. If the container is not approximately circular in the horizontal cross section including the inlet pipe, the liquid to be treated supplied from the inlet pipe will not swirl smoothly within the container due to turbulence, etc., resulting in reduced separation performance.

[0013] Furthermore, the cyclone device 9 according to the present invention has a second space 12 located outside the swirling space 11 and close to the inlet pipe 4. The swirling space is the shaded area in FIG. 3(B), and the second space is the shaded area in FIG. 3(C). With this configuration, a portion of the material swirling in the swirling space 11 passes through the second space 12 and then merges with new material supplied from the inlet pipe 4. At this time, the two flows are aligned, increasing the swirling force and improving separation capacity. If the cyclone device did not have the second space, the material swirling in the swirling space would collide with the new material supplied from the inlet pipe, generating turbulence and reducing the swirling force and separation capacity.

[0014] In the present invention, in the horizontal cross section of the cyclone device 9 where the area of ​​the second space 12 is maximum, the area of ​​the second space is preferably 5.6% to 15.2% of the area of ​​the swirling space 11. If it is 5.6% or more, a sufficient amount of the materials swirling in the swirling space can be ensured to pass through the second space, leading to improved swirling force, i.e., improved separation performance. If it is 15.2% or less, the materials do not stagnate in the second space and merge with new materials supplied from the inlet pipe, leading to improved swirling force, i.e., improved separation performance.

[0015] The area of ​​the second space 12 was determined as the area outside the container 1, on the secondary side of the inlet pipe primary flange portion 13, and where the inlet pipe 4 was not present, when viewed horizontally near the inlet pipe 4.

[0016] In the present invention, if the inlet pipe 4 is the inner pipe of the double pipe structure, when a part of the material to be treated that has swirled in the swirling space 11 passes through the second space 12 and then joins with new material to be treated that is supplied from the inlet pipe, the materials can join from many directions surrounding the inlet pipe. This is preferable because it leads to an improvement in the swirling force, i.e., an improvement in separation performance.

[0017] Furthermore, if the inlet pipe 4 is tilted downward by 0° to 15° with respect to the horizontal direction (θ in FIG. 2(B)), when the material to be treated swirls in the swirling space 11 and comes close to the inlet pipe 4, part of it enters the second space 12, and part of it continues to swirl downward in the swirling space to an extent that it will not collide with new material to be treated supplied from the inlet pipe 4. This is therefore preferable as it leads to an improvement in the swirling force, i.e., an improvement in separation performance.

[0018] Furthermore, in the present invention, if the inlet pipe 4 is the inner pipe of a double-pipe structure and is tilted downward at an angle of 0° to 15° relative to the horizontal, the outer pipe of the double-pipe structure can be connected to the horizontal direction of the cyclone device container, and the inlet pipe, which is the inner pipe of the double-pipe structure, can be tilted downward. Therefore, the space vertically below the inlet pipe has a gradient in width relative to the direction of travel of the treated material. This is preferable because it increases the momentum of the treated material after passing through the second space when it joins with the treated material entering from the inlet pipe, improving the swirling force and, therefore, the separation performance.

[0019] In the present invention, if the container 1 is an approximately cylindrical shape extending in an approximately vertical direction, the container has an inner diameter that is the same both above and below the vertical direction of the container, and therefore the swirling force can be maintained the same both above and below the container, leading to improved separation performance, which is preferable.

[0020] It is also preferable that an inlet pipe 4 is connected to the top of the container 1 and an outlet pipe 5 for the treated material obtained by the method for treating the material is connected to the bottom of the container 1, because the material swirls within the container and a product is obtained that is separated from coarse particles. Furthermore, it is also preferable that a discharge pipe 6 for the coarse particles is connected near the bottom of the side of the container 1, because coarse particles that accumulate during operation can be easily discharged outside the container.

[0021] In the present invention, it is preferable to have a cylindrical filter 8 inside the vessel 1, since this allows for the material to be treated and coarse particles to be separated appropriately. It is also preferable for the cylindrical filter to be either a punched mesh or a wedge wire screen, since this allows for the liquid to be treated and coarse particles to be separated appropriately.

[0022] <Toner manufacturing method> The present invention relates to a method for treating an object using a cyclone device having the above-described configuration, and can be applied to the production of powder or toner. As an example, the use of the present invention in a method for producing toner will be described below.

[0023] (Toner constituent materials) The binder resin may be a styrene-acrylic copolymer.

[0024] The styrene-acrylic copolymer is a copolymer of a styrene-based monomer and an acrylic-based monomer (acrylic acid or methacrylic acid and their alkyl esters).

[0025] Here, the styrene-acrylic copolymer may be contained in the binder resin in a state constituted only of the styrene-acrylic copolymer, or may be contained in the binder resin in the state of a block copolymer, a graft copolymer, or a mixture thereof with other polymers.

[0026] The content of the styrene acrylic polymer in the binder resin is 50% by mass or more, and preferably 80% by mass or more and 100% by mass or less.

[0027] When the binder resin contains a styrene-acrylic copolymer, the developing characteristics and durability of the toner are improved.

[0028] As the binder resin, in addition to the styrene-acrylic copolymer, known resins or polymers used in toners can be used.

[0029] Examples of the styrene-based monomer include the following:

[0030] Styrene, α-methylstyrene, β-methylstyrene, o-methylstyrene, m-methylstyrene, p-methylstyrene, 2,4-dimethylstyrene, divinylbenzene, etc.

[0031] The styrene monomers may be used alone or in combination of two or more selected from these.

[0032] Examples of the acrylic monomer include the following.

[0033] acrylic acid alkyl esters such as methyl acrylate, ethyl acrylate, n-propyl acrylate, isopropyl acrylate, n-butyl acrylate, isobutyl acrylate, tert-butyl acrylate, n-amyl acrylate, n-hexyl acrylate, 2-ethylhexyl acrylate, n-octyl acrylate, n-nonyl acrylate, n-decyl acrylate, and n-dodecyl acrylate; methacrylic acid alkyl esters such as methyl methacrylate, ethyl methacrylate, n-propyl methacrylate, isopropyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, tert-butyl methacrylate, n-amyl methacrylate, n-hexyl methacrylate, 2-ethylhexyl methacrylate, n-octyl methacrylate, n-nonyl methacrylate, n-decyl methacrylate, and n-dodecyl methacrylate; acrylic acid diesters such as diethylene glycol diacrylate, triethylene glycol diacrylate, tetraethylene glycol diacrylate, polyethylene glycol diacrylate, and 1,6-hexanediol diacrylate; Acrylic acid, methacrylic acid, etc.

[0034] The acrylic monomers may be used alone or in combination of two or more selected from these.

[0035] The glass transition temperature (Tg) of the binder resin can be adjusted to a desired range by adjusting the polymerization ratio of the styrene-based monomer and the acrylic-based monomer.

[0036] Specifically, the polymerization ratio of the styrene-based monomer to the acrylic monomer (styrene-based monomer:acrylic monomer) is preferably 65:35 to 100:0, and more preferably 70:30 to 85:15, on a mass basis.

[0037] The glass transition temperature (Tg) of the binder resin is preferably 25°C or higher and 65°C or lower.

[0038] As the polymerization initiator used in producing the toner particles, various types such as peroxide-based polymerization initiators and azo-based polymerization initiators can be used.

[0039] Examples of organic peroxide polymerization initiators include peroxyesters, peroxydicarbonates, dialkyl peroxides, peroxyketals, ketone peroxides, hydroperoxides, and diacyl peroxides.

[0040] Specific examples of organic peroxide polymerization initiators include peroxyesters such as t-butyl peroxyacetate, t-butyl peroxypivalate, t-butyl peroxyisobutyrate, t-hexyl peroxyacetate, t-hexyl peroxypivalate, t-hexyl peroxyisobutyrate, t-butyl peroxyisopropyl monocarbonate, and t-butyl peroxy 2-ethylhexyl monocarbonate; Examples include diacyl peroxides such as benzoyl peroxide; peroxydicarbonates such as diisopropyl peroxydicarbonate; peroxyketals such as 1,1-di-t-hexylperoxycyclohexane; dialkyl peroxides such as di-t-butyl peroxide; and others such as t-butylperoxyallyl monocarbonate.

[0041] Examples of inorganic peroxide polymerization initiators include persulfates and hydrogen peroxide.

[0042] Examples of azo polymerization initiators include 2,2'-azobis-(2,4-dimethylvaleronitrile), 2,2'-azobisisobutyronitrile, 1,1'-azobis(cyclohexane-1-carbonitrile), 2,2'-azobis-4-methoxy-2,4-dimethylvaleronitrile, azobisisobutyronitrile, and dimethyl-2,2'-azobis(2-methylpropionate).

[0043] If necessary, two or more of these polymerization initiators can be used simultaneously.

[0044] The amount of the polymerization initiator used is preferably 0.10 parts by mass or more and 20.0 parts by mass or less relative to 100.0 parts by mass of the polymerizable monomer.

[0045] The toner particles may also contain a polar resin.

[0046] Examples of polar resins include polyester resins, etc. By using a polyester resin as the polar resin, the lubricity of the resin itself can be expected when the resin is unevenly distributed on the surface of the toner particles to form a shell.

[0047] The polyester resin may be a condensation polymer of an alcohol monomer and a carboxylic acid monomer.

[0048] The alcohol monomers include the following:

[0049] Alkylene oxide adducts of bisphenol A such as polyoxypropylene(2.2)-2,2-bis(4-hydroxyphenyl)propane, polyoxypropylene(3.3)-2,2-bis(4-hydroxyphenyl)propane, polyoxyethylene(2.0)-2,2-bis(4-hydroxyphenyl)propane, polyoxypropylene(2.0)-polyoxyethylene(2.0)-2,2-bis(4-hydroxyphenyl)propane, and polyoxypropylene(6)-2,2-bis(4-hydroxyphenyl)propane; ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, neopentyl glycol, 1,4-butenediol, 1,5-pentanediol, 1,6-hexanediol, 1,4-cyclohexanedimethanol, dipropylene glycol, polyethylene glycol, polypropylene glycol, polytetramethylene glycol, bisphenol A, hydrogenated bisphenol A, sorbitol, 1,2,3,6-hexanetetrol, 1,4-sorbitan, pentaerythritol, dipentaerythritol, tripentaerythritol, 1,2,4-butanetriol, 1,2,5-pentanetriol, glycerol, 2-methylpropanetriol, 2-methyl-1,2,4-butanetriol, trimethylolethane, trimethylolpropane, 1,3,5-trihydroxymethylbenzene.

[0050] On the other hand, examples of the carboxylic acid monomer include the following.

[0051] Aromatic dicarboxylic acids or their anhydrides such as phthalic acid, isophthalic acid, and terephthalic acid; alkyl dicarboxylic acids or their anhydrides such as succinic acid, adipic acid, sebacic acid, and azelaic acid; succinic acid or its anhydrides substituted with an alkyl or alkenyl group having 6 to 18 carbon atoms; unsaturated dicarboxylic acids or their anhydrides such as fumaric acid, maleic acid, and citraconic acid.

[0052] In addition, the following monomers can also be used:

[0053] Polyhydric alcohols such as sorbitol, sorbitan, and oxyalkylene ether of novolac type phenolic resin; polycarboxylic acids such as trimellitic acid, pyromellitic acid, benzophenonetetracarboxylic acid, and anhydrides thereof.

[0054] The toner particles may contain a colorant, such as any of various conventionally known dyes and pigments.

[0055] Examples of black colorants include carbon black, magnetic materials, and those toned to black using the yellow, magenta, and cyan colorants described below.

[0056] Examples of yellow colorants include monoazo compounds, disazo compounds, condensed azo compounds, isoindolinone compounds, anthraquinone compounds, azo metal complexes, methine compounds, and allylamide compounds.

[0057] Specific examples include CI Pigment Yellow 74, 93, 95, 109, 111, 128, 155, 174, 180, and 185.

[0058] Examples of magenta colorants include monoazo compounds, condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinone compounds, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds, and perylene compounds.

[0059] Specific examples include CI Pigment Red 2, 3, 5, 6, 7, 23, 48:2, 48:3, 48:4, 57:1, 81:1, 122, 144, 146, 150, 166, 169, 177, 184, 185, 202, 206, 220, 221, 238, 254, 269, and CI Pigment Violet 19.

[0060] Examples of cyan colorants include copper phthalocyanine compounds and derivatives thereof, anthraquinone compounds, and basic dye lake compounds.

[0061] Specific examples include CI Pigment Blue 1, 7, 15, 15:1, 15:2, 15:3, 15:4, 60, 62, and 66.

[0062] The toner can be used as a magnetic toner by incorporating a magnetic material into the toner particles, which can also serve as a colorant.

[0063] Examples of the magnetic material include iron oxides such as magnetite, hematite, and ferrite; metals such as iron, cobalt, and nickel, and alloys and mixtures thereof of these metals with metals such as aluminum, cobalt, copper, lead, magnesium, tin, zinc, antimony, beryllium, bismuth, cadmium, calcium, manganese, selenium, titanium, tungsten, and vanadium.

[0064] The colorant may be selected from the viewpoints of hue angle, saturation, brightness, lightfastness, OHP transparency, and dispersibility in toner particles. The colorants may be used alone or in combination, or in the form of a solid solution.

[0065] The content of the colorant is preferably 1.0 part by mass or more and 20.0 parts by mass or less with respect to 100.0 parts by mass of the binder resin or the polymerizable monomer that forms the binder resin.

[0066] The wax used in the present invention is not particularly limited, and any known wax can be used. However, the wax should have a solubility parameter SPw of 8.40 (cal / cm 3 ) 1 / 2 More than 9.00(cal / cm 3 ) 1 / 2 It is preferable that:

[0067] From the viewpoint of compatibility with the styrene-acrylic copolymer contained in the binder resin, the wax is preferably an ester wax, which is a condensate of an alcohol component and a carboxylic acid component.

[0068] In the present invention, the wax is not particularly limited as long as it satisfies the above relationship, but from the viewpoints of compatibility with the styrene-acrylic copolymer contained in the binder resin and releasability during fixing, ester wax is preferred. Furthermore, monofunctional or difunctional ester wax is preferred because it has better plasticity.

[0069] Examples of the monofunctional or difunctional ester wax include an ester of a monohydric or dihydric linear saturated alcohol and a monohydric linear saturated fatty acid, or an ester of a monohydric or dihydric linear saturated fatty acid and a monohydric linear saturated alcohol.

[0070] As the monohydric linear saturated alcohol, an alcohol having 6 to 24 carbon atoms is used, and examples thereof include, but are not limited to, the following compounds: hexanol, heptanol, octanol, nonyl alcohol, decanol, lauryl alcohol, myristyl alcohol, palmityl alcohol, stearyl alcohol, and behenyl alcohol.

[0071] As the dihydric linear saturated alcohol, a diol having 6 to 24 carbon atoms is used, and examples thereof include, but are not limited to, the following compounds: 1,6-hexanediol, 1,7-heptanediol, 1,8-octanediol, 1,9-nonanediol, 1,10-decanediol, 1,12-dodecanediol, 1,14-tetradecanediol, 1,16-hexadecanediol, 1,18-octadecanediol, 1,20-icosanediol, 1,22-docosanediol, and 1,24-tetracosanediol.

[0072] The monovalent straight-chain saturated fatty acid has 8 to 24 carbon atoms, and includes, but is not limited to, the following compounds: hexanoic acid, octylic acid, nonylic acid, decanoic acid, dodecanoic acid, lauric acid, myristic acid, palmitic acid, stearic acid, and behenic acid.

[0073] As the divalent linear saturated fatty acid, a dicarboxylic acid having 8 to 24 carbon atoms is used, and examples thereof include, but are not limited to, the following compounds: suberic acid, sebacic acid, dodecanedioic acid, tetradecanedioic acid, hexadecanedioic acid, octadecanedioic acid, icosane diacid, docosane diacid, and tetracosane diacid.

[0074] The wax is preferably used in an amount of 1.0 part by mass or more and 30.0 parts by mass or less per 100.0 parts by mass of the binder resin.

[0075] The toner particles may further contain a hydrocarbon wax in addition to the ester wax.

[0076] Examples of hydrocarbon waxes include aliphatic hydrocarbon waxes such as low-molecular-weight polyethylene, low-molecular-weight polypropylene, microcrystalline wax, paraffin wax, and Fischer-Tropsch wax; oxides of aliphatic hydrocarbon waxes such as oxidized polyethylene wax or block copolymers thereof; and waxes obtained by grafting aliphatic hydrocarbon waxes with vinyl monomers such as styrene and acrylic acid.

[0077] The content of the hydrocarbon wax is preferably 0.5 parts by mass or more and 5.0 parts by mass or less with respect to 100 parts by mass of the binder resin.

[0078] The melting point of the ester wax and hydrocarbon wax is preferably 30° C. or higher and 130° C. or lower, and more preferably 60° C. or higher and 100° C. or lower. By exhibiting such thermal properties, it becomes easier to ensure that the resulting toner has both low-temperature fixability and heat-resistant storage stability.

[0079] The toner particles may contain a charge control agent. Examples of the charge control agent include the following.

[0080] Organic metal compounds, chelate compounds, monoazo metal compounds, acetylacetone metal compounds, urea derivatives, metal-containing salicylic acid compounds, metal-containing naphthoic acid compounds, quaternary ammonium salts, calixarenes, silicon compounds, non-metal carboxylic acid compounds and their derivatives, sulfonic acid resins having sulfonic acid groups, sulfonate salt groups, or sulfonate ester groups.

[0081] Specifically, the following may be mentioned as negative charge control agents.

[0082] Metal compounds of aromatic carboxylic acids such as salicylic acid, alkylsalicylic acid, dialkylsalicylic acid, naphthoic acid, and dicarboxylic acids; polymers or copolymers having a sulfonic acid group, a sulfonate salt group, or a sulfonate ester group; metal salts or metal complexes of azo dyes or azo pigments; boron compounds, silicon compounds, calixarenes, etc.

[0083] On the other hand, examples of the charge control agent for positive charging include the following.

[0084] Quaternary ammonium salts, polymeric compounds having quaternary ammonium salts in the side chains; guanidine compounds; nigrosine compounds; imidazole compounds, etc.

[0085] Of these, negative charge control agents are often used.

[0086] Furthermore, examples of the polymer or copolymer having a sulfonic acid group, sulfonate salt group, or sulfonate ester group include homopolymers of sulfonic acid group-containing vinyl monomers typified by styrenesulfonic acid, 2-acrylamido-2-methylpropanesulfonic acid, 2-methacrylamido-2-methylpropanesulfonic acid, vinylsulfonic acid, and methacrylsulfonic acid, and copolymers of the sulfonic acid group-containing vinyl monomers with other vinyl monomers.

[0087] The content of the charge control agent is preferably 0.01 parts by mass or more and 20.0 parts by mass or less, and more preferably 0.1 parts by mass or more and 10.0 parts by mass or less, relative to 100.0 parts by mass of the binder resin or the polymerizable monomer that forms the binder resin.

[0088] From the viewpoint of improving image quality, it is preferable that the toner contains an external additive added to the toner particles.

[0089] Examples of external additives include inorganic fine particles such as silica fine particles, titanium oxide fine particles, and aluminum oxide fine particles.

[0090] The inorganic fine particles are preferably hydrophobized with a hydrophobizing agent such as a silane coupling agent, silicone oil, or a mixture thereof.

[0091] The content of the external additive is preferably 0.1 parts by mass or more and 5.0 parts by mass or less, and more preferably 0.1 parts by mass or more and 3.0 parts by mass or less, relative to 100.0 parts by mass of the toner particles.

[0092] Methods for producing toner particles include a solution suspension method, an emulsion aggregation method, and a suspension polymerization method. Below, a method for producing toner particles by a suspension polymerization method will be described step by step.

[0093] The suspension polymerization method is a production method in which particles of a polymerizable monomer composition containing a polymerizable monomer and a colorant are formed in an aqueous medium, and the polymerizable monomer contained in the particles of the polymerizable monomer composition is polymerized to obtain toner particles.

[0094] (Preparation step of polymerizable monomer composition) A polymerizable monomer composition containing a polymerizable monomer and a colorant is prepared. The colorant may be dispersed in advance in the polymerizable monomer using a medium stirring mill or the like and then mixed with the other components, or the colorant may be dispersed after all the components have been mixed.

[0095] (granulation process) A polymerizable monomer composition is added to an aqueous medium containing an inorganic dispersion stabilizer, and granulated by dispersing to obtain a polymerizable monomer composition dispersion. The granulation process can be carried out, for example, in a vertical stirring tank equipped with a high-shear stirrer. The high-shear stirrer is not particularly limited, but commercially available stirrers such as a High Shear Mixer (manufactured by IKA Corporation), a TK Homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.), a TK Filmix (manufactured by Tokushu Kika Kogyo Co., Ltd.), and a Clearmix (manufactured by M Technique Co., Ltd.) can be used.

[0096] Examples of inorganic dispersion stabilizers include carbonates such as barium carbonate, calcium carbonate, and magnesium carbonate; metal phosphates such as aluminum phosphate, magnesium phosphate, calcium phosphate, barium phosphate, and zinc phosphate; sulfates such as barium sulfate and calcium sulfate; and metal hydroxides such as calcium hydroxide, aluminum hydroxide, magnesium hydroxide, and ferric hydroxide. These can be used alone or in combination of two or more. These function as dispersion stabilizers when present as poorly water-soluble inorganic fine particles in an aqueous medium.

[0097] (Reaction step) The polymerizable monomer in the polymerizable monomer composition dispersion obtained as described above is polymerized to obtain a dispersion of toner particle precursors. In the reaction step of the present invention, a general stirring tank capable of controlling the temperature can be used.

[0098] The polymerization temperature is 40° C. or higher, and generally 50 to 90° C. The polymerization temperature may be constant throughout, but may be increased in the latter half of the polymerization step in order to obtain a desired molecular weight distribution.

[0099] Any stirring blade may be used for stirring as long as it can suspend the polymerizable monomer composition dispersion without stagnation and maintain a uniform temperature in the tank. Examples of the stirring blade or stirring means include common stirring blades such as paddle blades, inclined paddle blades, triple swept blades, propeller blades, disk turbine blades, helical ribbon blades, and anchor blades, as well as "Fullzone" (manufactured by Kobe Steel Pantech Co., Ltd.), "Twinstar" (manufactured by Kobe Steel Pantech Co., Ltd.), "Maxblend" (manufactured by Sumitomo Heavy Industries, Ltd.), "Supermix" (manufactured by Satake Chemical Machinery Co., Ltd.), and "Hi-F Mixer" (manufactured by Soken Chemical & Engineering Co., Ltd.).

[0100] (Coarse particle removal process) When polymerizing polymerizable monomers to obtain toner particles in a reaction process, a considerable amount of non-standard particles called coarse particles (coarse particles) are generated. These coarse particles may clog equipment in subsequent processes or may be mixed into products, causing quality problems. Therefore, the cyclone device or the like according to the present invention is used to separate and remove coarse particles from a dispersion of toner particles.

[0101] (Washing process, solid-liquid separation process) To remove the dispersion stabilizer adhering to the toner particle surface, the toner particle dispersion is treated with an acid or alkali. After this, the polymer particles are separated (filtered) from the liquid phase using a typical solid-liquid separation method, but the toner particles are washed again with water to completely remove the acid or alkali and the dispersion stabilizer components dissolved in it. This washing process is repeated several times, and after sufficient washing, wet toner particles are obtained by solid-liquid separation again.

[0102] (drying process) The obtained wet toner particles are dried to remove the contained water and aqueous medium.

[0103] As a drying method generally used in the drying step, various drying methods such as vacuum drying, fluidized bed drying, and air flow drying can be used.

[0104] (Classification process) After drying, the toner particles are classified using an air classifier or the like to obtain the desired particle size distribution.

[0105] (External addition process) Toner can be obtained by mixing external additives with toner particles for the purpose of imparting various properties to the toner particles. [Example]

[0106] Hereinafter, the present invention will be described in more detail based on a process for producing a toner by a suspension polymerization method as a specific example of the present invention, but the present invention is not limited to this example.

[0107] Example 1 Dispersion medium (aqueous medium): 14 parts by mass of sodium phosphate and 4.5 parts by mass of 10% hydrochloric acid were added to 1,000 parts by mass of ion-exchanged water in a reaction vessel, and the mixture was kept at 65°C for 60 minutes while purging with N2. An aqueous calcium chloride solution prepared by dissolving 7.8 parts by mass of calcium chloride in 10 parts by mass of ion-exchanged water was added all at once while stirring at 12,000 rpm using a TK homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.) to prepare an aqueous medium containing a dispersion stabilizer.

[0108] Polymerizable monomer composition: Styrene 70 parts by weight Carbon black (manufactured by Orion Engineered Carbons, product name "Printex35") 7 parts by weight Charge control agent (Orient Co., Ltd.: Bontron E-89) 0.25 parts by weight The above materials were placed in an Attritor disperser (Mitsui Miike Chemical Engineering Co., Ltd.), and further dispersed using zirconia particles with a diameter of 1.7 mm at 220 rpm for 5 hours to obtain a composition.

[0109] The composition comprises: Styrene 20 parts by mass n-Butyl acrylate 20 parts by mass ·Polar resin 10 parts by mass (A saturated polyester resin obtained by the condensation polymerization reaction of 2 moles of propylene oxide adduct of bisphenol A with terephthalic acid and isophthalic acid; weight average molecular weight: 13,000, acid value: 8 mgKOH / g, glass transition temperature: 74°C) Fischer-Tropsch wax (manufactured by Schumann Sasol, trade name "C80": melting point 83.0°C) 9 parts by mass Added.

[0110] The above materials were kept at 65°C in a separate container and uniformly dissolved and dispersed at 500 rpm using a TK Homomixer (manufactured by Tokushu Kika Kogyo Co., Ltd.) to prepare a polymerizable monomer composition by dissolving 10.0 parts by mass of a polymerization initiator, t-hexyl peroxypivalate (manufactured by NOF Corporation, trade name "Perhexyl PV", molecular weight: 202, 10-hour half-life temperature: 53.2°C).

[0111] The polymerizable monomer composition was added to the aqueous medium in the granulation tank, and stirred at 10,000 rpm for 5 minutes in a TK homomixer under N purging at 65°C, and granulated at pH 5.2. The mixture was then transferred to a polymerization tank, where the polymerization process was carried out at 70°C for 4 hours while stirring with a paddle impeller at 30 rpm. The tank temperature was then raised to 90°C and further operation was carried out.

[0112] After the polymerization reaction was completed, 25,000 kg of a dispersion of toner particles was obtained, which was then transferred to a pre-treatment tank.

[0113] (coarse grain removal) The dispersion of toner particles was transferred by a pump, passed through the cyclone device shown in Figure 1, and then transferred to a tank (not shown) after treatment to remove coarse particles. Details are as follows.

[0114] A punched metal round hole with a diameter of 10 mm was installed at the inlet of the post-treatment tank. The pump frequency was adjusted so that the flow rate of the treated liquid was 12,000 kg / h. The cyclone inlet pipe 4 was connected along the tangent of the casing of the cyclone device in vessel 1 (Figure 1(B)).

[0115] The cyclone device had an approximately cylindrical container 1, with an inner diameter a of the container a = 0.3556 m, an outer diameter b of the filter = 0.130 m, a container height c = 1.300 m, a length d of the inlet pipe and the outer pipe of the double pipe = 0.300 m, a length f from the inside of the top plate to the top of the inner surface of the inlet pipe = 0.150 m, and a filter height of 1.300 m.

[0116] An outlet pipe 5 was connected to the center of the bottom plate 3, a coarse particle discharge pipe 6 was connected near the bottom of the side of the container 1, and a coarse particle discharge pipe valve 7 was installed on the coarse particle discharge pipe immediately adjacent to the container. The filter 8 used was a punched metal filter with a 10 mm round hole and an opening rate of 50%.

[0117] The inlet pipe 4 is the inner pipe of a double-pipe structure, and has a second space 12 between the inner pipe and the outer pipe 10. The outer pipe has a nominal diameter (outer diameter) of 150A, and the inner pipe, i.e., the inlet pipe, has a nominal diameter (outer diameter) of 65A. Furthermore, at the flange portion 13 on the primary side of the inlet pipe, the inner pipe of the double pipe is installed at the center in the vertical direction and the farthest from the center of the cyclone device vessel in the horizontal direction relative to the outer pipe. Furthermore, the most secondary side of the inner pipe is installed in a position overlapping on the circumference of the circle that forms the outer wall of the vessel. Furthermore, like the inlet pipe, the inner pipe is connected tangentially to the cyclone device casing (Figure 1(B)).

[0118] In this case, the ratio of the area of ​​the second space to the area of ​​the swirling space 11 in the horizontal cross section of the cyclone device where the area of ​​the second space is maximum was calculated to be 11.0%. In addition, the downward inclination angle θ of the inlet pipe relative to the horizontal direction was set to 5°.

[0119] The pump was operated for 1 hour, and 25,000 kg of the treated liquid from the pre-treatment tank was passed through the cyclone. After that, the top plate 2 of the cyclone device was opened, the filter 8 was removed, and its mass W1 (kg) was measured. The mass W0 (kg) of the filter before operation was measured, and the mass W2 attached to the filter was calculated using equation (1). W1-W0=W2 Formula (1)

[0120] When the filter was removed, the second space was checked and found to be wet with toner particle dispersion. Since it was dry before operation, this suggests that toner particle dispersion had passed through the second space.

[0121] After the treatment, the coarse particles remaining in the round hole with a diameter of 10 mm in the punched metal placed at the entrance of the tank were collected and designated as the passing mass W3.

[0122] <Examples 2 to 8, Example 10, Example 12> Coarse particle removal from a toner particle dispersion was carried out using the same manufacturing method as in Example 1, except for changing the conditions as shown in Table 1. When the filter was removed, the second space was checked and found to be wet with the toner particle dispersion. Since it was dry before operation, this suggests that the toner particle dispersion had passed through the second space.

[0123] Example 9 Coarse particles were removed from the toner particle dispersion using the same manufacturing method as in Example 1, except that the structure near the inlet pipe was changed to a non-double pipe structure as shown in Figure 4. When the second space was checked after removing the filter, it was confirmed to be wet with the toner particle dispersion. Since it was dry before operation, this suggests that the toner particle dispersion had passed through the second space.

[0124] Example 11 Coarse particles were removed from the toner particle dispersion using the same manufacturing method as in Example 1, except that the cyclone device was replaced with the conical container 1 shown in Figure 5. When the filter was removed, the second space was checked and found to be wet with the toner particle dispersion. Since it was dry before operation, this suggested that the toner particle dispersion had passed through the second space.

[0125] <Comparative Examples 1 and 2> Coarse particles were removed from a toner particle dispersion liquid using the same manufacturing method as in Example 1, except that the cyclone device had a rectangular parallelepiped upper container portion 14 and a cylindrical lower container portion 15, as shown in Fig. 6. In this case, the rectangular parallelepiped portion was square in a horizontal plane, and the length of one side was the same as the diameter of the cylindrical portion at the bottom of the container.

[0126] <Comparative Example 3> 7, removal of coarse particles from a toner particle dispersion was carried out using the same manufacturing method as in Comparative Example 2, except that a baffle plate 16 was installed in the inlet pipe 4. The length of the baffle plate (from the outer wall of the container to the tip) was set to 0.060 m, a length that would not collide with the filter.

[0127] [Table 1]

[0128] The cyclone devices of each Example and Comparative Example were evaluated for filter adhesion (adhesion amount W2) and cyclone passage (passage amount W3) based on the values ​​in Table 1. The results are shown in Table 2.

[0129] The evaluation criteria are as follows:

[0130] (Evaluation criteria for filter adhesion) A: 0.1kg or less B: More than 0.1kg, less than 0.3kg C: More than 0.3kg, less than 0.5kg D: More than 0.5kg

[0131] (Cyclone passage evaluation criteria) A: 0.1kg or less B: More than 0.1kg, less than 0.2kg C: More than 0.2kg, less than 0.3kg D: More than 0.3kg

[0132] [Table 2]

[0133] The above results show that the cyclone device having the features of the present invention increases the rotational force and improves separation performance, resulting in less adhesion and enabling improved yield and long-term operation. [Explanation of symbols]

[0134] 1: cyclone device container, 2: cyclone device top plate, 3: cyclone device bottom plate, 4: inlet pipe, 5: outlet pipe, 6: coarse particle discharge pipe, 7: coarse particle discharge pipe valve, 8: cylindrical filter, 9: cyclone device, 10: outer pipe of double pipe, 11: swirling space, 12: second space, 13: inlet pipe primary side flange, 14: rectangular parallelepiped part of container, 15: cylindrical part of container, 16: baffle, a: container inner diameter, b: filter outer diameter, c: container height, d: length of inlet pipe and outer pipe of double pipe, f: length from top plate to upper end of outer pipe of double pipe, θ: downward inclination of inlet pipe relative to horizontal

Claims

1. A method for treating an object to be treated using a cyclone device, comprising: The cyclone device comprises: a vessel that is installed in a substantially vertical direction; and an inlet pipe connected to the vessel in a substantially horizontal direction and in a substantially tangential direction, for supplying the material to be treated into the vessel; and the vessel is generally circular in horizontal cross section including the inlet pipe; The cyclone device comprises: (i) a swirling space in which the material to be treated supplied from the inlet pipe swirls; (ii) a second space located outside the swirl space and adjacent to the inlet pipe; and At least a portion of the material to be treated swirling in the swirling space passes through the second space and then merges with material to be treated newly supplied from the inlet pipe. A method for treating an object to be treated, comprising:

2. 2. The method for treating a workpiece according to claim 1, wherein in a horizontal cross section of the cyclone device where the area of ​​the second space is maximum, the area of ​​the second space is 5.6% or more and 15.2% or less of the area of ​​the swirling space.

3. 3. The method for treating a material to be treated according to claim 1, wherein the inlet pipe is an inner pipe of a double pipe structure.

4. 4. The method for treating an object to be treated according to claim 1, wherein the inlet pipe is inclined downward at an angle of 0° to 15° with respect to the horizontal direction.

5. 5. The method for treating an object to be treated according to claim 1, wherein the container has a substantially cylindrical shape extending in a substantially vertical direction.

6. the object to be treated includes particles, the treatment method is a treatment method for separating and removing coarse particles contained in the particles; The method for treating an object to be treated according to any one of claims 1 to 5.

7. the inlet pipe is connected to an upper portion of the container; an outlet pipe for the treated product obtained by the treatment method is connected to a lower part of the container; A discharge pipe for the coarse particles is connected to the vicinity of the lower part of the side surface of the container. The method for treating an object to be treated according to claim 6.

8. 8. The method for treating a material to be treated according to claim 1, wherein the cyclone device has a cylindrical filter inside the container.

9. 9. The method for treating a material to be treated according to claim 8, wherein the cylindrical filter is one of a punched mesh and a wedge wire screen.

10. A method for producing powder, comprising a step of using the treatment method according to any one of claims 1 to 9.

11. A method for producing a toner, comprising: The manufacturing method comprises: a granulation step of forming toner particle precursors in an aqueous medium to obtain a dispersion containing the toner particle precursors; a coarse particle removal step of removing coarse particles from the dispersion using a cyclone device; a drying step of filtering the toner particle precursor from the dispersion and drying the filtered toner particle precursor; and The cyclone device comprises: a vessel that is installed in a substantially vertical direction; and an inlet pipe connected to the container in a substantially horizontal direction and in a substantially tangential direction, for supplying the dispersion liquid into the container; the vessel is generally circular in horizontal cross section including the inlet pipe; The cyclone device comprises: (i) a swirling space in which the dispersion liquid supplied from the inlet pipe swirls; (ii) a second space located outside the swirl space and adjacent to the inlet pipe; and At least a part of the dispersion swirling in the swirling space passes through the second space and then merges with the dispersion newly supplied from the inlet pipe. A method for producing a toner comprising the steps of:

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