JP2006334533A - Manufacturing method of paste and paste manufacturing apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing a paste which has a sufficient dispersibility and which reduces the intrusion of a foreign matter into a paste product and reduces the breakage failure of a dispersing machine member and to provide a manufacturing apparatus of a paste. <P>SOLUTION: In the manufacturing method of the paste comprising conducting the dispersing treatment to drive a rotor and to knead the paste to be treated which is injected between the rotor and the inner wall of a cylindrical vessel by conducting the rotation and revolution while the rotor is allowed to contact with the inner wall of the cylindrical vessel, using the rotor type dispersing machine having a rotatable rotor arranged coaxially with the cylindrical vessel and having the rotatable and revolvable rotor arranged at the outer peripheral of the rotor in the cylindrical vessel, it retains the pressure of the dispersing machine during the dispersion treatment to 20 kPa or more. The paste manufacturing apparatus is also provided. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a paste manufacturing method and a paste manufacturing apparatus, and more particularly to a paste manufacturing method and a paste manufacturing apparatus suitable for manufacturing a display paste.

  In recent years, circuit materials and displays have been reduced in size and definition, and a paste dispersion technique that can cope with this has been demanded. In particular, in the plasma display, inorganic particles such as glass powder are used at the time of partition formation, and paste containing conductive powder such as silver is used at the time of electrode formation, and these are patterned with high precision to form the partition and electrodes.

  In order to carry out high-precision pattern processing, the inorganic particles and conductive powder contained in the paste component used must be sufficiently dispersed while maintaining the required particle size and surface characteristics. Is required.

  As a method for dispersing these pastes, media type dispersers such as attritors, paint shakers, sand mills, ball mills, and bead mills have been proposed.

  However, a ball mill or bead mill filled with balls or beads as a medium disperses the paste to be dispersed containing inorganic particles by applying a collision or impact force with the medium, and high dispersibility is obtained, It was difficult to obtain a paste having predetermined characteristics due to the surface characteristics and chemical changes such as a decrease in the particle size of the dispersed particles and an increase in specific surface area due to excessive grinding force due to collision and impact of the medium. .

  As a means for solving such a problem, a roller type disperser has been proposed (for example, Patent Document 1). The roller type disperser disperses the object to be dispersed including inorganic particles by sliding the roller and the vessel, and the change in the state of the particles in the object to be dispersed is less than that of other dispersing devices. This can be preferably used when it is not desired to change the particle shape when dispersing the treated particles or soft particles.

  However, if it is attempted to disperse hard particles using this disperser, the above object can be achieved, but the member constituting the disperser is harder than the particles to be dispersed or has a similar hardness. It is necessary to compose from. When the particles to be dispersed are ceramic powder, a ceramic member is used as a member constituting the disperser.

In a roller type disperser made of a ceramic member, breakage such as cracking or chipping often occurs during the dispersing action. As a result, foreign matter such as disperser components are mixed in the paste product and the quality deteriorates.In addition, the disperser breaks down and the operating rate decreases due to repairs, resulting in decreased productivity. There was a problem.
JP-A-11-197479

  The present invention has been made in view of such a background, and when dispersing surface-treated particles and soft particles, sufficient dispersibility is obtained without changing the particle diameter and surface state of the particles in the dispersion-treated product. An object of the present invention is to provide a paste manufacturing method and a manufacturing apparatus capable of reducing contamination of foreign substances in a paste product and reducing breakage of a disperser member.

  In order to solve the above-described problems, the paste manufacturing method according to the present invention includes a roller in which a rotor that can rotate coaxially with the cylindrical container and a roller that can rotate and revolve on the outer periphery of the rotor are disposed in the cylindrical container. Manufacturing method including a dispersion process of kneading the paste to be treated injected between the roller and the inner wall of the cylindrical container by driving the rotor and rotating and revolving while the roller is in contact with the inner wall of the cylindrical container by using a rotary disperser And the pressure of the paste in the disperser during the dispersion treatment is maintained at a pressure of 20 kPa or more.

  In the disperser used in the paste manufacturing method, when the rotor rotates in the cylindrical container, the roller loaded in each groove of the rotor comes into contact with the inner wall surface of the cylindrical container by the centrifugal force and rotates while the roller rotates. Revolve inside. The paste in the gap between the cylindrical container and the rotor is pressed against the inner wall surface of the cylindrical container by this roller, and is subjected to compression and shearing action to promote dispersion. Furthermore, due to the centrifugal force due to the rotation of the rotor, a gap is formed between the inner wall of the groove and the outer peripheral surface of the roller, and the paste also enters this gap. Dispersion is promoted by a shearing action.

  Here, when the paste is repeatedly subjected to compression and shearing action in the cylindrical container, the paste is foamed and fine bubbles are generated. Since the inside of the cylindrical container has a substantially sealed structure, the generated foam stays in the cylindrical container together with the paste for a certain time, and then flows out together with the paste. The fine bubbles accumulate while staying in the cylindrical container to form bubbles of a certain size, and form voids in which the paste is excluded in the cylindrical container. Since this gap is not filled with paste, the cylindrical container, rotor and roller of the gap will rotate and slide while directly contacting without being lubricated by the paste, and the cylindrical container, rotor and roller will be directly Because of rubbing, local heat generation and wear occur, and the cylindrical container, rotor, and roller are easily damaged by thermal expansion and thermal shock.

  At this time, if the paste pressure in the cylindrical container is 20 kPa or more, foaming of the paste can be suppressed, and accumulation of large bubbles can be suppressed. Since the bubbles staying in the cylindrical container can be reduced, the chances of rotating and sliding while the rotor and roller are in direct contact without being lubricated by the paste are reduced, and the dispersing machine members such as the cylindrical container, rotor and roller are reduced. Wear and breakage can be reduced, and a high-quality paste with less contamination of foreign matters such as wear powder can be obtained.

  The cylinder container paste pressure is preferably 20 to 1000 kPa. When the paste pressure in the disperser is less than 20 kPa, as described above, when the paste is compressed and sheared in the dispersion portion, the effect of suppressing the generation of bubbles is not sufficient, which is not preferable. The upper limit of the paste pressure in the disperser is not particularly limited from the viewpoint of foam generation, but is preferably 1000 kPa or less in consideration of practical aspects such as the pressure resistance of the disperser and the pump performance.

  By performing the paste dispersion treatment by the paste production method of the present invention, it is possible to produce a paste that is in a good dispersion state and that contains little foreign matter such as wear powder. As described above, high definition is progressing in the plasma display, and there is a demand for a highly accurate paste dispersion technique that can cope with this. The method for producing a paste with less foreign matter mixing according to the present invention is suitable for plasma display member forming paste (electrode forming paste, dielectric layer forming paste, barrier rib forming paste, phosphor forming paste, etc.).

The present invention also provides:
(A) paste injection means;
(B) A roller-type disperser in which a rotor that can rotate coaxially with the cylindrical container and a roller that can rotate and revolve around the outer periphery of the rotor are disposed in a cylindrical container, connected to the paste injection means. A dispersion part consisting of
(C) a flow control means installed in connection with the dispersing section;
A paste manufacturing apparatus is provided.

(A) Paste injection means, (B) Roller type disperser with a cylindrical container, and (C) Flow rate control means are sequentially provided. The pressure can be controlled to an appropriate pressure, which suppresses the generation of bubbles caused by the compression / shearing action caused by the movement of the rotor / roller in the dispersion section, resulting in wear of the cylindrical container, roller, and rotor. Can be provided, and a paste manufacturing apparatus having a long life can be provided.

  When attempting to maintain the paste pressure in the cylindrical container at 20 kPa or higher, if only the paste injection means is used, the paste flow rate increases with the increase in paste pressure, the residence time of the paste in the cylindrical container decreases, and sufficient dispersion is achieved. Is not made. Further, when only the flow rate control means is used, when the paste pressure in the cylindrical container is held at 20 kPa or more, the paste flow rate decreases with an increase in the paste pressure, and the predetermined production capacity cannot be exhibited. In this paste manufacturing apparatus, it is necessary to have both paste injection means and flow rate control means.

  As the paste injection means, a means using a normal pump or a method of pressurizing and feeding a paste tank can be used as appropriate. Examples of pumps as paste injection means include single stage centrifugal pumps, multistage centrifugal pumps, single stage turbine pumps, centrifugal pumps such as borehole pumps, propeller pumps such as axial flow pumps and diagonal flow pumps, single stage vortex flow pumps, Viscous pumps such as multi-stage vortex pumps, horizontal piston pumps, solid piston pumps, horizontal brander pumps, rigid brander pumps, diaphragm pumps, tube pumps, reciprocating pumps such as tube pumps, wing pumps, external gear pumps, internal gear pumps, Examples include rotary screw pumps, vane pumps, and roller pumps. Furthermore, a metering pump is preferable. By using the metering pump, the pressure fluctuation of the paste in the cylindrical container can be kept small, and the generation of bubbles can be suppressed. As a specific example of a pump with good quantitativeness, an eccentric screw pump, a diaphragm pump, a roller pump, or the like is preferable.

  Moreover, it is preferable that the wetted part of these pumps is made of a ceramic material such as alumina, zirconia, an alumina / zirconia mixture, silicon carbide, or sialon because the wear resistance can be improved.

  Moreover, in the paste manufacturing apparatus of this invention, it is preferable that disperser structural members, such as a cylindrical container, a rotor, and a roller of the said roller type disperser, consist of ceramic materials. The cylindrical container, rotor, and roller are made of ceramic material for the disperser components, so it is possible to dramatically reduce the abrasion powder compared to plastic materials, metal materials, etc. Mixing can be prevented. In addition, when the paste is an insulating paste, the mixing of metal powder is fatal, and as examples of ceramic materials, alumina, zirconia, zirconia reinforced alumina, silicon carbide, or the like can be used.

  Moreover, in the paste manufacturing apparatus of this invention, it is preferable that the said flow control means consists of a filtration member which has many pores. By arranging the filtration member connected to the cylindrical container, it is possible to prevent the abrasive powder generated in the disperser from the members (cylindrical container, roller, rotor, etc.) constituting the disperser from being mixed into the paste as foreign matter. . Further, the degree of pressurization of the paste in the cylindrical container can be adjusted by the opening of the filter member, the porosity, and the like.

  Examples of the member having a large number of pores include metal powder sintered bodies, metal fiber nonwoven fabrics, polymer fiber nonwoven fabrics, glass fiber paper, cellulose fiber paper, and polymer flat membranes having pores. These can be formed into a plate shape, a cylindrical shape, a pleated shape and processed into a cylindrical shape. More preferably, a nonwoven fabric made of polyethylene, polypropylene or the like is folded in a pleat shape to form a cylindrical shape. Further, a member having an inclined hole shape configured such that the pore diameter of the member having pores becomes smaller as the paste flows from the paste inflow side to the paste outflow side can be preferably used.

  The aperture of the member having a large number of pores is preferably in the range of 5 μm to 1000 μm. If the aperture of the pores is smaller than this range, the pressure loss in the flow rate control unit becomes large, which is not preferable because an excessive pressure is generated in the dispersing device. Further, if the pore opening is larger than this range, the required filtration accuracy cannot be obtained. Furthermore, the retained particle diameter of the member having many pores is preferably 10 μm to 100 μm.

  Further, the paste manufacturing apparatus of the present invention comprises a means for detecting the pressure in the dispersion part, a plurality of filters connected to the dispersion part, and a means for switching the plurality of filters, and the pressure in the dispersion part is It is also a preferable aspect to have a mechanism for sequentially switching the filter and maintaining the pressure in the disperser within the upper limit when the upper limit pressure is exceeded. Thereby, when the pressure in a disperser exceeds an upper limit pressure, a filter can be switched without stopping a disperser, and a production operation rate can be improved. Further, the paste pressure in the disperser can be controlled within a certain range, and the paste quality can be maintained.

  As the pressure detecting means, a Bourdon tube pressure gauge, a diaphragm pressure gauge, an electronic pressure gauge, or the like can be used. As the filter switching means, a system in which a ball valve or the like is arranged in the flow path and the valve is operated by a signal from a pressure gauge can be used.

  As described above, according to the present invention, by using a roller type disperser, the generation of foam in the dispersion part can be suppressed by maintaining the paste pressure in the dispersion part at 20 kPa or more, and the cylindrical container, the rotor, and the rotor are Therefore, the wear of the member generated by direct contact can be reduced, and a paste with less foreign matter can be manufactured. In addition, by having a flow rate control means connected to the dispersing section, wear of the cylindrical container, rotor, and rotor can be reduced, and a long-life roller type dispersing machine can be provided. Moreover, since the coarse thing in a paste can be removed collectively, a high quality paste can be provided.

  Hereinafter, the present invention will be described in detail with reference to the drawings together with preferred embodiments. In the following, the present invention will be described by taking a plasma display (PDP) member forming paste as an example. However, the present invention is not limited to this, and is preferably applied to paints, inks, and production.

  FIG. 1 shows a roller type disperser according to one embodiment of the present invention, and FIG. 2 shows one roller portion of FIG. In the figure, reference numeral 1 denotes a cylindrical container. In the cylindrical container 1, a rotor 2 that can rotate coaxially with the cylindrical container 1 (coaxially with respect to the rotation shaft 3), and an outer peripheral portion of the rotor 2. It is configured as a roller type disperser provided with a self-revolving roller 5 arranged in Each roller 5 is arranged in a groove 4 formed on the outer peripheral surface of the rotor 2, and a gap sufficient for each roller 5 to rotate and revolve between the cylindrical container 1 and the outer peripheral surface of the rotor 2. 7 is formed. A slight gap 6 is formed between the roller 5 and the groove 4 to allow the roller 5 to rotate while holding the roller 5 in the groove 4. In this embodiment, the cylindrical container 1 is covered with a jacket 11, and a cooling / heating medium that introduces a coolant or a heating medium controlled to a predetermined temperature between the jacket 11 and the outer peripheral surface of the cylindrical container 1. An introduction path a (12) is formed, and a cooling / heating medium introduction path b (13) is formed in the rotary shaft 3.

  In the roller type disperser as described above used in the paste manufacturing method and the paste manufacturing apparatus according to the present invention, when the rotor 2 rotates in the cylindrical container 1, the centrifugal force is inserted into each groove 4 of the rotor 2. The roller 5 that is in contact with the inner wall surface of the cylindrical container 1 revolves inside the cylindrical container 1 while rotating. The paste in the gap 7 between the cylindrical container 1 and the rotor 2 is pressed against the inner wall surface of the cylindrical container 1 by the roller 5 and is subjected to compression and shearing action to promote dispersion. Further, due to the centrifugal force caused by the rotation of the rotor 2, a gap 6 is formed between the inner wall of the groove 4 and the outer peripheral surface of the roller 5, and paste enters the gap 6, and the roller 5 rotating in the groove 4 However, dispersion is promoted by strong compression and shearing action.

  The roller-type disperser as described above constitutes the dispersion unit in the present invention. The paste manufacturing apparatus according to the present invention is configured as shown in FIGS. 3 and 4, for example, using the roller type disperser as described above as a dispersing unit in the present invention.

  In the paste manufacturing apparatus 100 shown in FIG. 3, the coarsely dispersed paste from the coarsely dispersed paste tank 21 containing the coarsely dispersed paste in advance is composed of a roller-type disperser via a liquid feed pump 22 as paste injection means. The paste supplied and dispersed in the dispersion unit 23 is sent into the dispersion-treated paste tank 25 through a filtration unit 24 having a large number of pores as a flow rate control means.

  In the paste manufacturing apparatus 200 shown in FIG. 4, the coarsely dispersed paste from the coarsely dispersed paste tank 31 containing the coarsely dispersed paste in advance is composed of a roller type disperser via a liquid feed pump 32 as a paste injection means. The paste supplied and dispersed in the dispersion unit 33 is sent to a filtration unit having a large number of pores as a flow rate control means. In this embodiment, the filtering unit is composed of a plurality of filtering units (filtering unit a (35), filtering unit b (36)), and is switched sequentially by switching valve a (34) and switching valve b (37). It has become. The paste that has passed through the filtration part a (35) or the filtration part b (36) is sent into the paste tank 38 that has been subjected to the dispersion treatment.

  The components constituting the paste for PDP use can be broadly classified into inorganic powders and organic components. Examples of the inorganic powder include glass powder, phosphor powder, metal powder, and pigment. It is also preferable to add a refractory filler. The glass powder is preferably used for partition wall formation among PDP applications.

The glass powder is preferably composed mainly of low-melting glass. The glass transition temperature of the low-melting glass is preferably 430 to 500 ° C, and the glass softening point is preferably 470 to 620 ° C. When the glass transition temperature and the glass softening point are in this range, the distortion of the substrate is small during firing, and a dense partition layer is obtained. Further, the glass preferably has a thermal expansion coefficient of 50 × 10 ^{−7 to} 100 × 10 ⁻⁷ ° C. ⁻¹ at 50 to 400 ° C. Moreover, it is required as a partition wall for electrical insulation, strength, coefficient of thermal expansion, denseness of insulating layer, etc. by blending silicon oxide in glass in the range of 3 to 60% by weight and boron oxide in the range of 5 to 50% by weight. Improved electrical, mechanical and thermal properties.

The particle size of the glass powder may be selected in consideration of the line width and height of the desired partition wall, but the center diameter of the volume-based distribution is 1 to 6 μm, the maximum particle size is 30 μm or less, the ratio The surface area is preferably 1.5 to ⁴ cm ² / g.

The phosphor powder is suitably used for phosphor layer formation among PDP applications. As the phosphor powder, for example, in red, Y ₂ O ₃ : Eu, YVO ₄ : Eu, (Y, Gd) BO ₃ : Eu, Y ₂ O ₃ S: Eu, γ-Zn ₃ (PO ₄ ) ₂ : Mn, (ZnCd) S: Ag + In ₂ O _{3 and the} like. In green, Zn ₂ GeO ₂ : M, BaAl ₁₂ O ₁₉ : Mn, Zn ₂ SiO ₄ : Mn, LaPO ₄ : Tb, ZnS: (Cu, Al), ZnS: (Au, Cu, Al), (ZnCd) S: (Cu, Al), Zn ₂ SiO ₄ : (Mn, As), Y ₃ Al ₅ O ₁₂ : Ce, CeMgAl ₁₁ O ₁₉ : Tb, Gd ₂ O ₂ S: Tb, Y ₃ Al ₅ O ₁₂ : Tb, ZnO: Zn, etc. are mentioned. In blue, Sr ₅ (PO ₄ ) ₃ Cl: Eu, BaMgAl ₁₄ O ₂₃ : Eu, BaMgAl ₁₆ O ₂₇ : Eu, BaMg ₂ Al ₁₄ O ₂₄ : Eu, ZnS: Ag + red pigment, Y ₂ SiO ₃ : Ce, etc. Is mentioned.

  Further, the size of the phosphor powder is preferably 1.0 to 2.5 μm, more preferably 1.2 to 2.3 μm as the area average diameter Ds, and 1.8 to as the center diameter Dv of the volume-based distribution. 4.5 μm is preferable, 2.0 to 4.2 μm is more preferable, and Ds / Dv is preferably 1.2 to 2.5, and more preferably 1.3 to 2.3. When Ds, Dv, and Ds / Dv are within these ranges, the filterability of the paste is improved.

  The metal powder is suitably used for electrode formation among PDP applications. As metal powder, what contains at least 1 sort (s) chosen from the group of Ag, Au, Pd, Ni, Cu, Al, and Pt can be used. Each of these may be used alone, as an alloy, or as a mixture of powders.

  The size of the metal powder is preferably 0.7 to 6 μm, more preferably 1.3 to 4 μm, as the center diameter of the volume-based distribution. When the center diameter of the volume reference distribution is within this range, a dense fine pattern can be formed.

  The refractory filler is preferably added to stabilize the shape during firing. As the refractory filler, those that do not soften at a firing temperature of about 500 to 650 ° C. can be widely used, and high melting point glass and ceramic powders such as alumina, magnesia, calcia, cordierite, silica, mullite, zircon, zirconia are exemplified. it can.

  The pigment is preferably employed for adjusting the light reflection characteristics of the partition walls on the back plate of the PDP. For example, Co-Cr-Fe, Co-Mn-Fe, Co-Fe-Mn-Al, Co-Ni-Cr-Fe, Co-Ni-Mn-Cr-Fe, Co-Ni-Al When black pigments such as -Cr-Fe and Co-Mn-AL-Cr-Fe-Si are used, the diplomatic reflection can be reduced and the contrast of the displayed image can be increased. For example, when a white pigment such as titania is used, the light emission of the phosphor can be effectively guided to the front surface of the panel, and a more vivid color can be displayed.

  As content with respect to the paste of an inorganic powder, 35 to 95 weight% is preferable and 40 to 90 weight% is more preferable. By setting it within this range, shrinkage and shape change during firing can be suppressed.

  Examples of the organic component include a binder resin, an organic solvent, a plasticizer, an antioxidant, an antifoaming agent, a dispersant, and a leveling agent. The binder resin is preferably one that is oxidized and / or decomposed and / or vaporized at the time of firing, so that the carbide does not remain in the inorganic substance, such as ethyl cellulose, methyl cellulose, nitrocellulose, cellulose acetate, cellulose propionate, and cellulose butyrate. Cellulosic resin, or methyl (meth) acrylate, ethyl (meth) acrylate, normal butyl (meth) acrylate, isobutyl (meth) acrylate, isopropyl (meth) acrylate, 2-ethylmethyl (meth) acrylate, 2-hydroxylethyl An acrylic resin, poly-α-methylsulfone, polyvinyl alcohol, polybutene and the like made of a polymer such as (meth) acrylate or a copolymer thereof are preferably used. As content with respect to the paste of binder resin, 5-65 weight% is preferable and 10-60 weight% is more preferable.

  The organic solvent is used for adjusting the viscosity of the paste. Examples of the organic solvent include diethylene glycol monobutyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol mono-2-ethylhexyl ether, diethylene glycol mono-2-ethylhexyl ether, 2,2,4-trimethyl-1,3-pentanediol monoiso Butyrate, 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, 2-ethyl-1,3-hexanediol, terpineol, benzyl alcohol, 1-butoxy-2-propane, 1,2-di Acetoxypropane, 1-methoxy-2-propanol, 2-acetoxy-1-ethoxypropane, (1,2-methoxypropoxy) -2-propanol, (1,2-ethoxypropoxy) -2-propanol, 2 Hydroxy-4-methyl-2-pentanone, 3-methoxy-3-methylbutyl acetate, 2-methoxyethanol, 2-ethoxyethanol, 2- (methoxymethoxy) ethanol, 2-isopropoxyethanol, 2-butoxyethanol, 2 -(Isopentyloxy) ethanol, 2- (hexyloxy) ethanol, 2-phenoxyethanol, 2- (benzyloxy) ethanol, benzyl alcohol, furfuryl alcohol, tetrafurfuryl alcohol, 2,2'-dihydroxydiethyl ether, 2 -(2-methoxyethoxy) ethanol, 2- [2- (2-methoxyethoxy) ethoxy] ethanol, 2-methyl-1-butanol, 3-methyl-2-butanol, 2-methyl-1-pentanol, 4 -Methyl-2-pen Nord, 2-ethyl-1-butanol, 2-methoxyethyl acetate, 2-ethoxyethyl acetate, 2-butoxyethyl acetate, 2-phenoxyethyl acetate, 1,2-dimethoxyethane, 1,2-diethoxyethane, 1 , 2-dibutoxyethane, cyclohexanenone, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, 1-methylpentyl acetate, 2-ethylbutyl acetate, 2-ethylhexyl acetate, cyclohexyl acetate, benzyl acetate, hexane, Examples include cyclohexane, methyl ethyl ketone, 2-pentanone, 3-pentanone, 2-hexanone, methyl isobutyl ketone, 2-heptanone, 4-heptanone, and diisobutyl ketone.

  The organic solvent can be selected mainly considering its volatility and the solubility of the binder resin to be used. The organic solvent is preferably a good solvent for the binder resin used. If the solubility in the binder resin is high, the use of an organic solvent makes it easy to adjust the viscosity of the paste, and good coating characteristics can be obtained.

  As a content rate with respect to the paste of an organic solvent, 35 to 65 weight% is preferable, More preferably, it is 40 to 60 weight%. By setting the content to 35% by weight or more, the defoaming treatment can be easily performed. Moreover, by setting it as 65 weight% or less, a stable dispersion state can be obtained and the energy and time required for drying can be saved.

  When the paste is used as a photosensitive paste, as an organic component, a photosensitive component such as a photosensitive polymer, a photosensitive oligomer, and a photosensitive monomer, a photopolymerization initiator, a sensitizer, an ultraviolet absorber, a polymerization inhibitor, etc. The additive component can be mentioned.

  As the photosensitive monomer, a compound having a functional group having an active carbon-carbon unsaturated double bond can be preferably employed. As the functional group, for example, monofunctional and polyfunctional compounds having a vinyl group, an allyl group, an acrylate group, a methacrylate group, or an acrylamide group can be applied. Examples of the compound include 2- (2-ethoxyethoxy) ethyl acrylate, 1,3-butanediol diacrylate, pentaerythritol triacrylate, ditrimethylolpropane tetraacrylate, cyclohexyl methacrylate, ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate. And glycidyl methacrylate.

  The photosensitive polymer and / or the photosensitive oligomer can also be used as a binder resin for the photosensitive paste. The photosensitive polymer and the photosensitive oligomer are obtained by polymerization or copolymerization of the photosensitive monomer as described above.

  For example, an unsaturated acid such as an unsaturated carboxylic acid is preferable as the other copolymerization component copolymerized with the photosensitive monomer as described above, since the developability of the aqueous alkali solution after the exposure can be improved. Specific examples of the unsaturated carboxylic acid include acrylic acid, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, vinyl acetic acid, and acid anhydrides thereof.

  The addition amount of the photopolymerization initiator to the photosensitive paste is preferably 0.005 to 5% by weight in view of the photosensitive properties.

[Measurement and evaluation method]
(1) Paste viscosity It measured at 25 degreeC using the B-type rotational viscometer.

(2) Dispersibility use apparatus: Grind gauge (Eriksen, 0-15 μm and 0-50 μm).
Measuring method: Observed the distribution density of the crush, and read the scale where the dense crush appeared. However, if a dense crushing boundary appears between the scales or the two grooves are different, read the scale with the larger number and paste the median of the three measurements. The degree of dispersion was.
Judgment criteria: Large numbers indicate poor dispersibility.

(3) Observation of surface condition of cylindrical container, rotor and roller The surface condition of the cylindrical container, rotor and roller after 100 hours of use was observed visually and with a microscope (magnification: 80 times), and the derived state of surface cracks was observed. It was evaluated according to the criteria.
A: There is no crack that can be confirmed with a microscope.
B: There is a crack that can be confirmed with a microscope but cannot be confirmed with the naked eye.
C: There is a crack that can be visually confirmed.

(4) Paste pressure The indication value of the diaphragm type pressure gauge installed in the connection part of a cylindrical container and a filtration part was made into paste pressure.

Examples 1-4, Comparative Examples 1-2
[Preparation of coarse dispersion paste]
52% by weight of glass powder having an average particle diameter of 2 μm obtained by grinding glass mainly composed of lead oxide, boron oxide, zinc oxide, silicon oxide, and barium oxide, methyl methacrylate / methacrylic acid copolymer (weight composition ratio) 60/40, weight average molecular weight 32000) 12% by weight, dipentaerythritol hexaacrylate 12% by weight, benzophenone 1.94% by weight, 1,6-hexanediol-bis [(3,5-di-t-butyl-4 -Hydroxyphenyl) propionate] 0.05% by weight, organic dye (basic blue 7) 0.01% by weight, and organic solvent (propylene glycol monomethyl ether acetate) 22% by weight were used as constituents of the photosensitive paste.

  The paste of this composition was weighed 300 kg in each example and comparative example, and stirred at 60 rpm for 60 minutes with a planetary mixer (manufactured by Inoue Seisakusho) to obtain a coarse dispersion paste.

[Kneading process]
Subsequently, the roller in which the coarsely dispersed paste is rotated in a cylindrical container coaxially with the cylindrical container and a roller capable of rotating and revolving in a groove disposed on the outer periphery of the rotor is disposed in the cylindrical container via a screw-type pump. The paste is supplied to a dispersion unit composed of a type disperser and a flow rate control unit provided with members having a large number of pores connected to the dispersion unit, so that the rotational speed of the rotor is 400 rpm and the supply speed is 2.5 kg / hr. A metering pump was set up and dispersed to obtain a dispersed paste. In addition, 15 degreeC cooling water was circulated through the cold / warm medium introduction path.

  Table 1 shows the specifications of the roller-type dispersion section and the specifications of the filtration section composed of the pore member. Table 1 shows the results of measuring the paste pressure during dispersion obtained in Examples 1 to 4 and Comparative Examples 1 and 2, the viscosity and dispersibility of the paste after the dispersion treatment.

It is a schematic cross-sectional view showing an example of a roller type disperser in the present invention. It is an expanded sectional view of the II section of FIG. It is a schematic block diagram of the paste manufacturing apparatus which concerns on an example of this invention. It is a schematic block diagram of the paste manufacturing apparatus which concerns on another example of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Cylindrical container 2 Rotor 3 Rotating shaft 4 Groove 5 Roller 6 Slight gap 7 Gap 11 Jacket 12 Cooling medium introduction path a
13 Cooling medium introduction path b
21 Coarse Dispersion Paste Tank 22 Feed Pump 23 Dispersion Unit 24 Filtration Unit 25 Dispersed Paste Tank 31 Coarse Dispersion Paste Tank 32 Feed Pump 33 Dispersion Unit 34 Switching Valve a
35 Filtration part a
36 Filtration part b
37 Switching valve b
38 Dispersed paste tanks 100, 200 Paste production equipment

Claims (4)

  Using a roller-type disperser in which a rotor that can rotate coaxially with the cylindrical container and a self-revolving roller disposed on the outer periphery of the rotor is driven in the cylindrical container, the rotor is driven, and the roller is A paste manufacturing method including a dispersion process of kneading a paste to be treated injected between a roller and an inner wall of a cylindrical container by rotating and revolving while contacting an inner wall, wherein the pressure of the paste in the disperser during the dispersion process is 20 kPa The paste manufacturing method characterized by holding at the above pressure. (A) paste injection means;
(B) A roller-type disperser in which a rotor that can rotate coaxially with the cylindrical container and a roller that can rotate and revolve around the outer periphery of the rotor are disposed in a cylindrical container, connected to the paste injection means. A dispersion part consisting of
(C) a flow rate control means installed in connection with the dispersion unit;
A paste manufacturing apparatus comprising:   The paste manufacturing apparatus according to claim 2, wherein the flow rate control means includes a filtration part having a large number of pores.   A means for detecting the pressure in the dispersion section; a plurality of filters connected to the dispersion section; and a means for switching the plurality of filters. When the pressure in the dispersion section exceeds the upper limit pressure, the filters are sequentially installed. The paste manufacturing apparatus according to claim 2 or 3, further comprising a mechanism for switching to maintain the pressure in the disperser within an upper limit value.

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