Method for producing a composition and mixing method

Abstract

To provide a novel mixing method for efficiently making a liquid and powder uniform, a composition production method using the mixing method, and a mixing method for making high viscous liquid, low viscous liquid and powder uniform in a single agitation blade and agitation tank, and a composition production method.SOLUTION: A composition production method includes an agitation and dissolution step of agitating liquid and powder excluding coarse powder by a ribbon blade 4 in an agitation tank arranged with the ribbon blade consisting of a ribbon-shaped blade 3, and dissolving the powder in the liquid.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a new mixing method for efficiently homogenizing liquids and powders, and a method for manufacturing a composition using the mixing method.

Background Art

[0002] Dissolution and homogenization of heterogeneous components by stirring are indispensable techniques in all fields. In the manufacturing industry, if components that should originally be in a uniform state are in a non-uniform state, it is impossible to guarantee product quality and the product cannot be established as an industrial product. For example, in pharmaceuticals, a threshold value for impurities that have an adverse effect on the human body is set. However, when the components are non-uniform, the value fluctuates, making it impossible to determine whether the product quality meets the standards. Also, in materials for state-of-the-art displays and semiconductors, if there is undissolved residue of components in the material, it becomes a foreign substance and causes defects during molding, greatly reducing the yield in subsequent processes.

[0003] Particularly in materials for semiconductors, a highly viscous liquid such as a silicone resin is used as the main component (base polymer), making it possible to stabilize the dimensions during product molding after curing. Usually, a reactive monomer such as a different-viscosity liquid or an additive powder such as a polymerization initiator or an antioxidant is added to this base polymer and uniformly dissolved to make a product varnish. Therefore, regarding highly viscous liquids and low-viscosity liquids, or low-viscosity liquids and powders, research and development of technologies that can efficiently dissolve and homogenize them by stirring are still being actively carried out, and a large number of prior arts have been reported.

[0004] For example, to stir and dissolve powder in a low-viscosity liquid, a turbine blade with high shear force is suitable and widely used (see, for example, Patent Document 1). However, the fluid flow pattern in the turbine blade is from the center of the blade to the outside (radial direction), and the discharge force in the vertical direction is limited. Therefore, it exhibits a high stirring effect in a low-viscosity liquid, but in a high-viscosity liquid, it becomes local stirring, and the discharge force is insufficient, making overall homogenization impossible. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Japanese Patent Publication No. 61-263622 Summary of the Invention [Problem to be solved by the invention]

[0006] An object of the present invention is to provide a new mixing method for efficiently homogenizing a liquid and a powder, and a method for producing a composition using the mixing method. Another object of the present invention is to provide a mixing method and a method for producing a composition that enable high viscosity liquids, low viscosity liquids, and powders to be homogenized using a single stirring blade and stirring vessel. [Means for solving the problem]

[0007] As a result of extensive research, the present inventors have found that the above-mentioned problems can be solved, and have completed the present invention having the following gist.

[0008] That is, the present invention includes the following. [1] A method for producing a composition, comprising a stirring and dissolving step of stirring a liquid and a powder from which coarse particles have been removed in a stirring tank equipped with a ribbon impeller, using the ribbon impeller to dissolve the powder in the liquid. [2] The method for producing a composition according to [1], wherein the liquid is a highly viscous liquid. [3] The method for producing the composition according to [1] further comprises, after the stirring and dissolving step, a stirring step of adding a second liquid having a lower viscosity than the first liquid to the stirring tank and stirring the second liquid with the ribbon impeller. [4] The method for producing a composition according to [3], wherein the first liquid is a highly viscous liquid and the second liquid is a low viscous liquid. [5] The method for producing a composition according to [1], wherein the liquid is a low viscosity liquid. [6] Further, after the stirring and dissolving step, a second liquid having a higher viscosity than the first liquid which is the liquid is added to the stirring tank, and the stirring step of stirring with the ribbon blade is included, the method for producing the composition according to [1]. [7] The method for producing the composition according to [6], wherein the first liquid is a low-viscosity liquid and the second liquid is a high-viscosity liquid. [8] The method for producing the composition according to any one of [1] to [7], wherein the powder contains a photoinitiator. [9] The method for producing the composition according to any one of [1] to [8], wherein the powder from which the coarse powder has been removed is a powder from which the coarse powder has been removed by classification.

[10] A mixing method characterized by including a stirring and dissolving step of stirring a liquid and a powder from which coarse powder has been removed with the ribbon blade in a stirring tank and dissolving the powder in the liquid.

[11] The mixing method according to

[10] , wherein the liquid is a high-viscosity liquid.

[12] Further, after the stirring and dissolving step, a second liquid having a lower viscosity than the first liquid which is the liquid is added to the stirring tank, and the stirring step of stirring with the ribbon blade is included, the mixing method according to

[10] .

[13] The mixing method according to

[12] , wherein the first liquid is a high-viscosity liquid and the second liquid is a low-viscosity liquid.

[14] The mixing method according to

[10] , wherein the liquid is a low-viscosity liquid.

[15] Further, after the stirring and dissolving step, a second liquid having a higher viscosity than the first liquid which is the liquid is added to the stirring tank, and the stirring step of stirring with the ribbon blade is included, the mixing method according to

[10] .

[16] The mixing method according to

[15] , wherein the first liquid is a low-viscosity liquid and the second liquid is a high-viscosity liquid.

[17] The mixing method according to any one of

[10] to

[16] , wherein the powder contains a photoinitiator.

[18] The mixing method according to any one of

[10] to

[17] , wherein the powder from which the coarse powder has been removed is a powder from which the coarse powder has been removed by classification.

Advantages of the Invention

[0009] According to the present invention, it is possible to provide a new mixing method for efficiently homogenizing a liquid and a powder, and a method for producing a composition using the mixing method. Furthermore, the present invention can provide a mixing method and a method for producing a composition that enable high viscosity liquids, low viscosity liquids, and powders to be homogenized using a single stirring blade and stirring vessel. According to the present invention, it is possible to efficiently produce existing compositions for semiconductor materials, display materials, basic chemical materials, pharmaceutical and agrochemical preparations, cosmetics, and foods. In addition, it is possible to efficiently produce compositions that have been difficult to homogenize using conventional methods (especially compositions consisting of highly viscous liquids and powders). [Brief explanation of the drawings]

[0010] [Figure 1] FIG. 1 is a perspective view of an example of a ribbon wing. DETAILED DESCRIPTION OF THE INVENTION

[0011] The present inventors have conducted extensive research in order to provide a new mixing method for efficiently homogenizing liquids and powders, and a method for producing a composition using said mixing method, and further to provide a mixing method and method for producing a composition that make it possible to homogenize high-viscosity liquids, low-viscosity liquids, and powders using a single stirring blade and stirring vessel.

[0012] Generally, the action of mixing can be divided into two: the force that shears the material (H) and the discharge force that circulates the liquid (Q). If the stirring power is P, then P ∝ H·Q, and the shear force (H) and the discharge force (Q) have opposing effects. Therefore, for efficient dissolution and homogenization, it is necessary to select multiple stirring blades that are suited to the combination of materials to be dissolved.

[0013] As mentioned above, the fluid flow pattern in the turbine blades is from the center to the outside (radial direction), and the vertical discharge force is limited. Therefore, while it is effective in low-viscosity liquids, in high-viscosity liquids, localized stirring occurs, and the discharge force is insufficient, making it impossible to uniformize the entire liquid.

[0014] On the other hand, it is known that ribbon impellers, which have a large discharge force and can easily move the liquid up and down, are suitable for mixing and uniformly dissolving high-viscosity and low-viscosity liquids (see, for example, Japanese Patent Application Laid-Open No. 6-154573). Double helical ribbon impellers are capable of mixing and uniformly dissolving liquids over a wide viscosity range. However, when dissolving powder in a highly viscous liquid, the powder adheres to the impeller and rotates together, preventing the dissolution from being fully promoted.In addition, the powder accumulates inside the ribbon impeller where the shear force is not sufficient, making it impossible to achieve uniform dissolution between the solid (powder) and the liquid.

[0015] Furthermore, instead of turbine or ribbon impellers, mixing impellers that integrate multiple impellers, such as paddle and gate impellers, have been developed (see, for example, JP 9-108557 A), and devices that use multiple mixing shafts to increase mixing power and combine different mixing impellers (see, for example, JP 4-215829 A). However, the former are applicable to a lower high-viscosity range than ribbon impellers and are not suitable for high-viscosity materials such as silicone polymers, which range from tens to millions of mPa·s. The latter require increased power consumption and more complex mixing impellers and equipment, resulting in increased operating, installation, and maintenance costs. Furthermore, they also impair the cleanability of the vessel interior, requiring large amounts of cleaning solvent for each campaign to prevent cross-contamination, increasing equipment cleaning costs.

[0016] That is, a method for uniformly dissolving a highly viscous liquid, a low-viscosity liquid, and a powder in a single stirring blade and a stirring tank has not been known heretofore. In order not to wastefully consume stirring power, it is necessary to use a stirring tank for low-viscosity liquids and a stirring tank for high-viscosity liquids in the manner shown in Japanese Patent Application Laid-Open No. 11-140179. As a first step, the powder is dissolved in the low-viscosity liquid in a stirring tank equipped with a turbine blade excellent in shearing force to obtain a uniform solution. As a subsequent step, it is necessary to put the previous uniform solution into the high-viscosity liquid in another stirring tank equipped with a ribbon blade excellent in discharge power and stir it to obtain a final uniform solution. However, in this case, it is necessary to use a plurality of stirring blades and stirring tanks, and as a result, the cleaning process and the like increase, and the production efficiency is significantly reduced.

[0017] Based on the above, the present inventor has conducted intensive studies and found that when stirring a liquid and a powder using a ribbon blade, by using a powder excluding coarse powder, it is possible to avoid the powder adhering to the stirring blade and causing a co-rotation phenomenon, and it is possible to prevent poor dissolution of the powder due to retention inside the ribbon blade. That is, it has been found that even when using a ribbon blade, the powder can be efficiently dissolved in the liquid. That is, in a stirring tank equipped with a ribbon blade, by performing a stirring and dissolving step of stirring a liquid and a powder excluding coarse powder with the ribbon blade and dissolving the powder in the liquid, it has been found that the liquid and the powder can be efficiently homogenized. The ribbon blade is suitable for mixing and stirring a highly viscous liquid and a low-viscosity liquid. Therefore, in the above stirring and dissolving step, first, a highly viscous liquid is used as the liquid together with the powder excluding coarse powder, and after efficiently homogenizing the liquid and the powder, a liquid having a lower viscosity than the highly viscous liquid is added to the stirring tank and stirred with the ribbon blade. It has been found that it is possible to homogenize a highly viscous liquid, a low-viscosity liquid, and a powder in a single stirring blade and a stirring tank. In the stirring and dissolving step, first, a low-viscosity liquid is used as the liquid together with the powder from which coarse powder has been removed. After efficiently homogenizing the liquid and the powder, a liquid having a higher viscosity than the low-viscosity liquid is added to the stirring tank, and a stirring step of stirring with a ribbon blade is performed. It has been found that it is possible to homogenize the high-viscosity liquid, the low-viscosity liquid, and the powder in a single stirring blade and stirring tank.

[0018] In one embodiment of Japanese Patent Application Laid-Open No. 2011-42746, polymer solids having a specified particle size are charged into a low-viscosity monomer in a single stirring tank, stirred, and dissolved. However, in this publication, the purpose of specifying the particle size of the polymer solids is to suppress clogging in the tank by reducing the terminal settling velocity of the polymer particles, and no mention is made of the influence of the particle size of the polymer solids on the dissolution phenomenon itself.

[0019] <Mixing method, method for producing a composition> The mixing method of the present invention includes a stirring and dissolving step, preferably including a stirring step. The method for producing a composition of the present invention includes a stirring and dissolving step, preferably including a stirring step.

[0020] <<Stirring and dissolving step>> The stirring and dissolving step is not particularly limited as long as it is a step of stirring a liquid and powder from which coarse powder has been removed with a ribbon blade in a stirring tank provided with a ribbon blade and dissolving the powder in the liquid.

[0021] <<<Ribbon blade and stirring tank>>> The ribbon blade is a stirring blade having a ribbon-shaped blade twisted in a spiral shape, and is also called a helical ribbon blade. In the description of the present invention, the ribbon blade and the stirring blade do not refer only to the blade, but refer to the entire rotating part (excluding the stirring motor) including the stirring shaft during stirring.

[0022] The number of the ribbon-shaped blades spirally twisted in the ribbon blade (hereinafter sometimes referred to as "ribbon-shaped blade") is not particularly limited, and may be one or two or more. However, from the viewpoint of facilitating cleaning after use with an appropriate number while realizing more suitable stirring, it is preferably 1 to 2. The width and thickness of the ribbon-shaped blade are not particularly limited. The material of the ribbon-shaped blade is not particularly limited as long as it is used for this kind of application, and examples thereof include stainless steel. The ribbon-shaped blade may be provided with a protruding portion protruding from the outer end portion, as described in FIG. 1 of JP-A-2000-233122, for example.

[0023] The ribbon blade has a stirring shaft in addition to the ribbon-shaped blade. The stirring shaft may penetrate the rotation center axis of the helical ribbon blade 3 from the upper part to the lower part, like the stirring shaft 1 of the vertical reactor described in FIG. 1(B) of JP-A-11-181086. In this embodiment, the ribbon-shaped blade (the helical ribbon blade 3 of JP-A-11-181086) is fixed to the stirring shaft by, for example, a support rod extending vertically from the stirring shaft. The stirring shaft may be in a mode where it does not exist on the rotation center axis within the cylindrical space formed by the rotation of the helical ribbon blade 3, like the stirring shaft 1 of the vertical reactor described in FIG. 1(A) of JP-A-11-181086. In this embodiment, the ribbon-shaped blade (the helical ribbon blade 3 of JP-A-11-181086) is fixed to, for example, a frame connected to the stirring shaft and in contact with the ribbon-shaped blade.

[0024] Further, the ribbon blade may have other blades or the like in addition to the ribbon-shaped blade. The ribbon blade may, for example, as another blade, have a strip-shaped bottom ribbon blade (7) in which a base end portion (a) is continuously provided on a helical ribbon blade (6) (the ribbon-shaped blade in the present invention) and a tip end portion (c) is disposed substantially perpendicular to the bottom plate (3) and near its center, as described in claim 1 and FIG. 1 of JP-A-06-154573. Further, the ribbon blade may, as another blade, have a shear blade having a rotation center concentric with the rotation center of the flow blade (ribbon-shaped blade), as described in claim 1 and FIG. 1 of PCT Re-2017 / 002905.

[0025] Examples of the ribbon blade include a V-type helical ribbon blade, a single helical ribbon blade, and a double helical ribbon blade. The ribbon blade may be a commercially available product or a non-commercially available product. Examples of commercially available products of the stirring device provided with the ribbon blade include SUPERBLEND (registered trademark) and NANOVisK (registered trademark) manufactured by Sumitomo Heavy Industries, Ltd.

[0026] Here, an example of the ribbon blade is shown in FIG. 1. Note that the ribbon blade used in the present invention can take various forms as described above, and thus is not limited to the ribbon blade in FIG. 1. The ribbon blade in FIG. 1 has one stirring shaft 1, four support rods 2, two ribbon-shaped blades 3, and two bottom ribbon blades 4. The stirring shaft 1 exists on the rotation center axis of the two ribbon-shaped blades 3 and vertically penetrates the cylindrical space formed by the rotation of the two ribbon-shaped blades 3. The two ribbon-shaped blades 3 are fixed to the stirring shaft 1 by four support rods 2 extending vertically from the stirring shaft 1. One end of each of the two bottom ribbon blades 4 is connected to the lower end of the ribbon-shaped blade 3, and the other end is connected near the lower end of the stirring shaft 1.

[0027] The stirring tank is not particularly limited in terms of its material, size, shape, structure, etc. The size of the stirring tank is not particularly limited as long as the ribbon blade can be stored. As the material of the stirring tank, for example, it may be stainless steel or glass. The cross-sectional shape of the inner peripheral wall of the stirring tank is usually circular. The tank volume of the stirring tank is not particularly limited, but it is usually 0.5 L to 1000 L. From the viewpoint of realizing more uniform mixing with good reproducibility and suppressing the space of the stirring tank, etc., the upper limit value is preferably 500 L, more preferably 150 L, even more preferably 100 L, still more preferably 50 L, and even more preferably 30 L. From the viewpoint of efficiently manufacturing the mixture by mixing on a larger scale, etc., the lower limit value is preferably 1 L, more preferably 10 L, and even more preferably 20 L. The stirring tank is usually a vertical stirring tank having an opening at the upper part.

[0028] The distance between the outermost peripheral part of the ribbon blade during rotation of the ribbon blade and the inner peripheral wall of the stirring tank when the ribbon blade is arranged in the stirring tank is not particularly limited, but in one aspect, it is 1% to 20% of the inner diameter of the stirring tank, and in another aspect, it is 1% to 10%.

[0029] The stirring power when rotating the ribbon blade in the stirring and dissolving step is not particularly limited, and it can be appropriately selected according to the amounts of the liquid and the powder, the ratio of the liquid to the powder, the viscosity of the liquid, etc.

[0030] The time of the stirring and dissolving step is not particularly limited, but for example, it may be 0.5 hours to 10 hours or 1 hour to 5 hours. During the stirring and dissolving in the stirring and dissolving step, heating may be appropriately performed as necessary within the range where no deterioration of the components to be mixed occurs. The temperature during the stirring and dissolving in the stirring and dissolving step may be, for example, 20°C to 60°C, or 20°C to 50°C, or 25°C to 45°C.

[0031] The mixing method and the method for manufacturing a composition, the stirring device having a ribbon blade and a stirring tank may have other members such as baffles and deflectors. However, from the viewpoint of enhancing the ease of cleaning the stirring device after use, it is preferable that the stirring device does not have baffles and deflectors.

[0032] <<<Liquid>>> The liquid to be used is not particularly limited. For example, it may be a mixture of one or more liquids used exclusively as organic solvents, a mixture of one or more liquids used exclusively as organic materials, or a mixture thereof.

[0033] Liquids can be classified into high-viscosity liquids and low-viscosity liquids according to the magnitude of their viscosities. There is a stirring Reynolds number Re as an index related to the stirring state and viscosity, and Re = inertial force / viscous force = d 2 ·n·ρ / μ (where d = blade diameter, n = rotational speed, ρ = liquid density, μ = viscosity). Generally, it is said that when Re < 50, it is in the laminar flow region, when 50 ≤ Re ≤ 1000, it is in the transition region, and when 1000 < Re, it is in the turbulent flow region. When a liquid having a viscosity near the boundary between the laminar flow region and the transition region where the viscous force is dominant is defined as a high-viscosity liquid in stirring, the high-viscosity liquid refers to, for example, a viscous liquid having a viscosity of 10,000 mPa·s or more. Also in the present invention, the high-viscosity liquid means a liquid having a viscosity of 10,000 mPa·s or more. In this regard, the viscosity of the high-viscosity liquid used in the present invention is not particularly limited as long as it is 10,000 mPa·s or more. For example, it may be 50,000 mPa·s or more, 100,000 mPa·s or more, or 1,000,000 mPa·s or more. On the other hand, when a liquid having a viscosity near the boundary between the turbulent flow region and the transition region where the inertial force is dominant is defined as a low-viscosity liquid in stirring, the low-viscosity liquid refers to, for example, a viscous liquid having a viscosity of 1,000 mPa·s or less. Also in the present invention, the low-viscosity liquid means a liquid having a viscosity of 1,000 mPa·s or less. In this regard, the viscosity of the low-viscosity liquid used in the present invention is not particularly limited as long as it is 1,000 mPa·s or less. For example, it may be 500 mPa·s or less, 100 mPa·s or less, or 10 mPa·s or less. In the present invention, a medium-viscosity liquid may be set as the viscous liquid between the high-viscosity liquid and the low-viscosity liquid. For example, a liquid having a viscosity greater than 1,000 mPa·s and less than 10,000 mPa·s may be set as the medium-viscosity liquid. The medium-viscosity liquid can be used as needed in manufacturing the composition.

[0034] The viscosity defined in the present invention can be measured under the following conditions. · Apparatus: E-type viscometer TV-35H manufactured by Toki Sangyo Co., Ltd. · Cone rotor type: 1°34×R24 · Temperature: 25°C · Rotation speed: 1 rpm · Standby time: 2 minutes

[0035] The liquid or the high-viscosity liquid contains, for example, a polymer. The liquid or the low-viscosity liquid contains, for example, a reactive monomer, a reactive additive, and an additive. The polymer, the reactive monomer, and the reactive additive have, for example, a polymerizable group. Examples of the polymerizable group include a radical polymerizable group, a cationic polymerizable group, and an anionic polymerizable group. Examples of the radical polymerizable group include a vinyl group, an acryloyl group, and a methacryloyl group.

[0036] <<<Powder>>> The powder used in the stirring and dissolving step has had coarse powder removed in advance. The method for removing coarse powder from the powder is not particularly limited. For example, it may be a method of removing coarse powder by classification, or a method of eliminating coarse powder from the powder by pulverizing the powder containing coarse powder. Examples of the method for removing coarse powder by classification include sieving. For example, in the method for producing and mixing the composition of the present invention, a step of removing coarse powder from the powder containing coarse powder may be included. And, as the step of removing coarse powder, for example, a step of removing coarse powder by classification may be used, or a step of eliminating coarse powder from the powder by pulverizing the powder containing coarse powder may be used.

[0037] The size of the powder is not particularly limited, but from the viewpoint of reproducibly realizing suitable stirring and homogenization, it is preferably a size that passes through a sieve with an opening of 3 mm, more preferably a size that passes through a sieve with an opening of 2 mm, and even more preferably a size that passes through a sieve with an opening of 1 mm.

[0038] The powder is not particularly limited as long as it is soluble in the liquid to be used. For example, it is a powder of a material containing an organic component. Containing an organic component Materials Examples of the powder include various additives, polymerization initiators, and the like. Examples of the polymerization initiator include radical polymerization initiators, cationic polymerization initiators, anionic polymerization initiators, and the like. The polymerization initiator may be a thermal polymerization initiator or a photoinitiator.

[0039] In the present invention, as an example in which the effect is exhibited, stirring and dissolution of a photoinitiator of powder are mentioned. This is because, due to its characteristics, a photoinitiator often contains an aromatic ring or a heterocyclic ring as a site that absorbs light, so it is easy for molecules to stack due to large intermolecular interactions, and at room temperature, it often becomes a powder of large particles and is difficult to dissolve in a liquid. Under such circumstances, photoinitiators with an alkyl structure added to the side chain to improve solubility and photoinitiators previously dissolved in a liquid compound have been developed, but in any case, it may cause problems such as an increase in total cost and curing failure due to a decrease in the concentration of the effective component for generating active species for initiating polymerization (for example, the effective component for radical generation). In this regard, in the present invention, even a photoinitiator that is likely to stack and is likely to become a powder of large particles at room temperature can be suitably dissolved in a liquid and suitable homogenization can be realized.

[0040] The photoinitiator for the powder is not particularly limited. For example, alkylphenones, benzophenones, acylphosphine oxides, Michler's ketones, benzoyl benzoates, oxime esters, tetramethylthiuram monosulfides, thioxanthones, etc. can be mentioned. In particular, the effect of homogenization is exhibited in the case of a photo-cleavage type photo-radical polymerization initiator. Examples of the photo-cleavage type photo-radical polymerization initiator include those described in the Latest UV Curing Technology (page 159, publisher: Kazuhiro Takasuga, publisher: Technical Information Association Co., Ltd., published in 1991). Examples of commercially available photo-radical polymerization initiators include OMNIRAD (registered trademark) 127, 184, 369, 369E, 379EG, 410, 500, 651, 819, 907, 2959, 4MBZ FLAKES, 4PBZ, BMS, BP FLAKES, DETX, EMK, ITX, OMBB, TPO-H, ESACURE (registered trademark) KIP100F, KIP150 (solidifies at low temperature), KIP160, 1001M, A1980, ONE, 3644 [manufactured by iGM Resins B.V.]; IRGACURE (registered trademark) 379, 784, 1800, 1870, OXE01, OXE02, OXE03, OXE04, Darocur (registered trademark) EDB [manufactured by BASF Japan Ltd.], etc.

[0041] Examples of the combination of liquid and powder include a combination of a highly viscous liquid containing a polymer, a low-viscosity liquid containing a reactive monomer, and a powder of a material containing an organic component (e.g., a polymerization initiator).

[0042] The combination of liquid and powder is not particularly limited. For example, the following compositions in the polymerizable composition described in Japanese Patent Publication No. 2014-510159 can be mentioned. Highly viscous liquid: A reactive silicone compound obtained by polycondensation of a diarylsilicic acid compound represented by formula [1] with a silicon compound selected from the compounds represented by formula [2] and formula [2b] in the presence of an acid or a base. Low viscosity liquid: a compound having at least one polymerizable group selected from the group consisting of an alkenyl group and a (meth)acrylic group Powder: Polymerization initiator (e.g., photopolymerization initiator) [ka] (In the formula, Ar 1 and Ar 2 each independently represents a phenyl group optionally substituted by an alkyl group having 1 to 6 carbon atoms; X represents a group capable of undergoing a hydrolytic condensation reaction; where Ar 3 represents a naphthyl or anthracyl group substituted with at least one group having a polymerizable double bond, or Ar 3 represents a phenyl group substituted with at least one group having a polymerizable double bond other than a vinyl group, or a phenyl group substituted with at least two groups having a polymerizable double bond.

[0043] Other examples of the combination of liquid and powder include the following compositions in the composition for forming an optical waveguide described in Japanese Patent No. 6156673. Highly viscous liquid: A reactive silicone compound consisting of a polycondensate of a diarylsilicic acid compound A represented by formula [1] and an alkoxysilicon compound B represented by formula [2], or a polycondensate of the diarylsilicic acid compound A, the alkoxysilicon compound B, and another polycondensable compound. Low viscosity liquid: Di(meth)acrylate compound represented by formula [3] Powder: Polymerization initiator (e.g., photopolymerization initiator) [ka] (In formula [1], Ar 1 and Ar 2Each independently represents a phenyl group which may be substituted with an alkyl group having 1 to 6 carbon atoms, a naphthyl group which may be substituted with an alkyl group having 1 to 6 carbon atoms, or a biphenyl group which may be substituted with an alkyl group having 1 to 6 carbon atoms. In formula [2], Ar 3 represents a phenyl group having at least one group with a polymerizable double bond, a naphthyl group having at least one group with a polymerizable double bond, or a biphenyl group having at least one group with a polymerizable double bond, and R 1 each independently represents a methyl group or an ethyl group, and R 2 represents a methyl group, an ethyl group or a vinylphenyl group, and a represents 2 or 3. In formula [3], R 3 and R 4 each independently represents a hydrogen atom or a methyl group, and R 5 represents a hydrogen atom, a methyl group or an ethyl group, L 1 and L 2 each independently represents an alkylene group having 2 to 6 carbon atoms, and m and n represent 0 or positive integers such that m + n is 0 to 20.)

[0044] In addition, as other combinations of a liquid and a powder, for example, a photocurable resin composition used for a wafer-level lens can be mentioned. Specifically, for example, the following compositions in the photocurable resin composition described in JP-A-2013-043982 can be mentioned. High-viscosity liquid: a resin having an aliphatic cyclic hydrocarbon group and a weight average molecular weight of 40,000 or less Low-viscosity liquid: a compound having an aliphatic cyclic hydrocarbon group and a polymerizable group Powder: a compound that generates radicals or an acid upon irradiation with actinic rays or radiation

[0045] In addition, as other combinations of a liquid and a powder, a combination of a liquid and a powder in an imprint photocurable composition used for a wafer-level lens described in the pamphlet of WO2020 / 003863 may also be used. Among the liquids described in the WO2020 / 003863 pamphlet, examples of the low-viscosity liquid include compounds having at least two (meth)acryloyloxy groups in one molecule of Compound 1 and not containing an aromatic ring. Here, the aromatic ring refers to a carbocyclic or heterocyclic ring that satisfies Hückel's rule, such as benzene, naphthalene, azulene, anthracene, tetracene, pentacene, phenanthrene, pyrene, furan, thiophene, pyrrole, pyrazole, imidazole, oxazole, thiazole, pyridine, pyridazine, pyrimidine, pyrazine, and triazine. Therefore, not containing an aromatic ring means not containing a carbocyclic or heterocyclic ring that satisfies Hückel's rule. Examples of the polyfunctional (meth)acrylate compound not containing the aromatic ring include ethylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, ethoxylated trimethylolpropane tri(meth)acrylate, ethoxylated glycerin tri(meth)acrylate, ethoxylated pentaerythritol tetra(meth)acrylate, ethoxylated dipentaerythritol hexa(meth)acrylate, polyglycerin monoethylene oxide poly(meth)acrylate, dipentaerythritol hexa(meth)acrylate, neopentyl glycol di(meth)acrylate, pentaerythritol tri(meth)acrylate, trimethylolpropane tri(meth)acrylate, tricyclodecane dimethanol di(meth)acrylate, 1,3-adamantanediol di(meth)acrylate, 1,4-cyclohexanedimethanol di(meth)acrylate, 1,4-butanediol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate, 1,9-nonanediol di(meth)acrylate, and tris(2-acryloyloxyethyl) isocyanurate.

[0046] Commercially available products may be used as the polyfunctional (meth)acrylate compound containing no aromatic ring. For example, NK Ester A-200, A-400, A-600, A-1000, A-9300, A-9300-1CL, 1G, 2G, 3G, 4G, 9G, 14G, 23G, A-GLY-3E, A-GLY-9E, A-GLY-20E, A-TMPT-3EO, A-TMPT-9EO, ATM-4E, ATM-35E, A-DPH, A-TMPT, A-DCP, A-HD-N, A-NOD-N, AD-TMP, A-DOG, TMPT, DCP, NPG, HD-N, NOD-N, D-TMP (all manufactured by Shin-Nakamura Chemical Co., Ltd.), KAYARAD (registered trademark) DPHA, NPGDA, PET30, DPEA-12, PEG400DA, RP-1040 (all manufactured by Nippon Kayaku Co., Ltd.), M-210, M-350 (all manufactured by Toagosei Co., Ltd.) may be mentioned.

[0047] <<Stirring Step>> In the mixing method and the method for manufacturing the composition, it is preferable to further include a stirring step. One aspect of the stirring step is a step of adding a second liquid having a lower viscosity than the first liquid, which is a liquid, to the stirring tank and stirring with a ribbon blade after the stirring and dissolving step. Here, for example, the first liquid is a high-viscosity liquid and the second liquid is a low-viscosity liquid. An example of another aspect of the stirring step is, for example, a step of adding a second liquid having a higher viscosity than the first liquid, which is a liquid, to the stirring tank and stirring with a ribbon blade after the stirring and dissolving step. Here, for example, the first liquid is a low-viscosity liquid and the second liquid is a high-viscosity liquid.

[0048] When rotating the ribbon blade in the stirring process, the stirring power is not particularly limited and can be appropriately selected according to the amounts of the first liquid and the second liquid, the viscosities of the first liquid and the second liquid, etc. Preferably, a reducer and an inverter are used to adjust and set the stirring rotation speed preferable for dissolution and homogenization by stirring within a range that does not overload the motor. The examination results regarding the required stirring power in the ribbon blade (Non-Patent Document J.Chem.Eng.Japan, 15, 77-79 (1982)) are for reference.

[0049] The time of the stirring process is not particularly limited, and for example, it may be 0.05 hours to 5 hours, or it may be 0.1 hours to 3 hours. The temperature during stirring in the stirring process is not particularly limited, and for example, it may be 20°C to 60°C, or it may be 20°C to 50°C, or it may be 25°C to 45°C.

[0050] The ratio of the liquid and the powder to be stirred may be adjusted in a timely manner according to the solubility of the powder in the liquid. For example, the amount of the liquid is equal to or more than the amount that becomes the saturation solubility at the stirring temperature, preferably 2 times or more thereof, more preferably 5 times or more thereof.

[0051] In a mixing method using a highly viscous liquid, a low-viscous liquid, and a powder, and a method for producing a composition, consider the case where a polymerization initiator such as a photoinitiator is used as the powder and a reactive monomer is used as the low-viscous liquid. In such a case, when trying to dissolve the powder in the low-viscous liquid, the temperature inside the system rises due to stirring energy, heat of dissolution, etc. (for example, it reaches about 45°C), which may trigger a runaway polymerization reaction by the reactive monomer. On the other hand, such a possibility is less in the highly viscous liquid. Therefore, in such a case, first, it is preferable to dissolve the powder in the highly viscous liquid in the stirring and dissolution process, then cool it to ensure safety, and then add the low-viscous liquid to the stirring tank in the stirring process to perform mixing and production of the composition.

Examples

[0052] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to the following examples.

[0053] The stirring and mixing conditions (1) and (2) using ribbon impeller A used in this example are shown below. (1): Stirring and mixing conditions (1) Equipment: Ribbon blade agitation mixer ·Tank volume: 10L ·Total length inside the tank: 450mm ·Tank inner diameter: 200mm Agitating blade: Ribbon blade A-1 Mixing blade total height: 390mm Stirring blade outer diameter: 190mm Stirring blade width: 20mm Baffles, baffles: None Material: SUS304 (stainless steel) Agitator: Explosion-proof inverter motor with cyclo reducer, reduction ratio 1 / 21, output 0.4kW, number of poles 4P, frequency 60Hz, power supply 200V

[0054] (2): Stirring and mixing conditions (2) ·Equipment: Ribbon blade stirring and mixing device Tank volume: 5L ·Total length inside the tank: 360mm ·Tank inner diameter: 150mm Agitating blade: Ribbon blade A-2 Mixing blade total height: 220mm Stirring blade outer diameter: 140mm Baffles, baffles: None Material: Glass tank, SUS304 agitator blades Mixer: IKA EUROSTAR200 electronically controlled mixer, output 0.135 kW, frequency 60 Hz, power supply 100 V

[0055] (3) Mixing blades and mixing vessel The combinations of stirring blades and stirring vessels used in this example are summarized in Table 1 below.

[0056] [Table 1]

[0057] <<<Explanation of ribbon blade>> The paddle-equipped anchor blade is a blade having the same shape as a blade in which a support rod that extends vertically from the rotation axis and supports the blade at the lower part of the anchor-shaped blade is replaced with a paddle in the anchor blade described in https: / / www.shi-pe.shi.co.jp / technology / mixing-lecture / basic001 / index.html. The cross-panel blade A is a blade having the same shape as the stirring blade (BENDLEAF blade) described in http: / / www.hakko-sangyo.co.jp / ?page_id=542. The cross-panel blade B is a blade having the same shape as FULLZONE (the second from the left) described in Fig. 2 of "Yoshihito Kato et al., Stirring Power Required for Various Large Two-Paddle Blades, Journal of Chemical Engineering of Japan, Vol. 38, No. 3, pp. 139-143 (2012), https: / / nitech.repo.nii.ac.jp / ?action=pages_view_main&active_action=repository_view_main_item_detail&item_id=5651&item_no=1&page_id=13&block_id=21". The large panel blade is a blade having the same shape as Supermix MR203 described in Fig. 2 of "Yoshihito Kato et al., Stirring Power Required for Various Large Two-Paddle Blades, Journal of Chemical Engineering of Japan, Vol. 38, No. 3, pp. 139-143 (2012), https: / / nitech.repo.nii.ac.jp / ?action=pages_view_main&active_action=repository_view_main_item_detail&item_id=5651&item_no=1&page_id=13&block_id=21". The paddle-equipped gate impeller is an impeller with a shape similar to that of the MAXBLEND shown in Fig. 2 of "Kato Yoshito et al., Mixing Power Requirements of Various Large Two-Paddle Impellers, Journal of Chemical Engineering, Vol. 38, No. 3, pp. 139-143 (2012), https: / / nitech.repo.nii.ac.jp / ?action=pages_view_main&active_action=repository_view_main_item_detail&item_id=5651&item_no=1&page_id=13&block_id=21." Ribbon wings A-1, A-2, B, and C are herringbone wings with two ribbon-shaped blades. The stirring shafts of ribbon impellers A-1, A-2, and C do not lie on the central axis of rotation within the cylindrical space formed by the rotation of helical ribbon impeller 3, unlike the stirring shaft 1 of the vertical reaction apparatus described in Figure 1(A) of JP-A-11-181086. The ribbon-shaped blade (helical ribbon impeller 3 in JP-A-11-181086) is connected to the stirring shaft and is fixed to a frame that is in contact with the ribbon-shaped blade. The stirring shaft of ribbon impeller B penetrates the central axis of rotation of helical ribbon impeller 3 from top to bottom, like stirring shaft 1 of the vertical reactor shown in FIG. 1(B) of JP-A-11-181086. The ribbon blades B and C have bottom ribbon blades as described in claim 1 and FIG. 1 of JP-A-06-154573.

[0058] (4) Viscosity measurement Viscosity measurements were carried out under the following conditions. However, when the measurement temperature is also listed for the viscosity described below, the viscosity refers to the viscosity at the measurement temperature also listed. Equipment: Toki Sangyo E-type viscometer TV-35H Cone rotor type: 1°34×R24 ·Temperature: 25℃ Rotation speed: 1 rpm Waiting time: 2 minutes

[0059] The abbreviations of the compounds have the following meanings. ·STMS: Trimethoxy(4-vinylphenyl)silane [manufactured by Shin-Etsu Chemical Co., Ltd.] Viscosity 2 mPa·s (25 °C) ·DDT: N-Dodecyl mercaptan [manufactured by NOF Corporation] Viscosity 2 mPa·s (25 °C) ·DOG: Dioxane glycol diacrylate [manufactured by Shinnakamura Chemical Co., Ltd. NK Ester A-DOG] Viscosity 300 mPa·s (25 °C) ·DVB: Divinylbenzene [manufactured by Nippon Steel & Sumikin Chemical Co., Ltd. DVB-810, purity 81%] Viscosity 1 mPa·s (25 °C) ·TPO: Diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide [manufactured by iGM Resin Co., Ltd. Omnirad® TPO-H] (equivalent to [manufactured by BASF Japan Ltd. IRGACURE® TPO]) ·184: Hydroxycyclohexyl phenyl ketone [manufactured by iGM Resin Co., Ltd. Omnirad® 184](equivalent to [manufactured by BASF Japan Ltd. IRGACURE® 184])

[0060] [Uniform dissolution of high-viscosity liquid and low-viscosity liquid] As a confirmation that the ribbon blade is excellent in the uniform solubility of the high-viscosity liquid and the low-viscosity liquid, the following Reference Examples 1 to 16 were carried out. When the liquid temperature during stirring is not described below, stirring was carried out at room temperature (25 °C).

[0061] [Reference Example 1] Confirmation of the efficiency of uniform dissolution of high-viscosity liquid and low-viscosity liquid (ribbon blade A-2) A ribbon blade A-2 made of SUS304 with a blade diameter of 140 mm and a total blade height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm), and stirring was carried out under the above-mentioned stirring and mixing conditions (2). Specifically, it is as follows. 4299 g of starch syrup (colorless and transparent) whose viscosity was adjusted to 292000 mPa·s by adding ion-exchanged water in advance was gently placed in this container. Subsequently, 96 g of an iodine aqueous solution (brown) (viscosity: 1 mPa·s) was gently added as a coloring liquid for visually confirming the mixing state. The total height of the liquid separated into two layers was 215 mm. The agitator used was an electronically controlled agitator, EUROSTAR200, manufactured by IKA, which drives the agitating blades from the top of the vessel, and the agitation power per unit volume was 4.2 kW / m. 3 The rotation speed was adjusted so that the temperature became 0.05°C, and stirring was started. The time it took for the two liquids to dissolve was measured visually and determine whether the entire mixture was uniformly colored brown, which was 10 minutes. The viscosity of the brown liquid after uniform dissolution was 81,370 mPa s. The results are shown in Table 2.

[0062] [Reference Example 2] Confirmation of the efficiency of uniform dissolution of high viscosity liquid and low viscosity liquid (ribbon blade B) A ribbon impeller B made of SUS304 and having an impeller diameter of 125 mm and an impeller total height of 140 mm was set in a 3 L round-bottom separable glass reaction vessel (inner diameter 130 mm, height 310 mm). 3005 g of starch syrup (colorless and transparent), which had been adjusted to a viscosity of 239,400 mPa·s with the addition of ion-exchanged water, was gently poured into the container. 69 g of an iodine solution (brown, viscosity: 1 mPa·s) was then gently added as a coloring agent to visually confirm the mixture. The total height of the two separated liquid layers was 210 mm. The agitator used was an electronically controlled agitator, EUROSTAR200, manufactured by IKA, which drives the agitating blades from the top of the vessel, and the agitation power per unit volume was 4.2 kW / m. 3 The rotation speed was adjusted so that the temperature became 0.05°C, and stirring was started. The time it took for the two liquids to dissolve was measured visually and determine whether the entire mixture was uniformly colored brown, which was 10 minutes. The viscosity of the brown liquid after uniform dissolution was 80100 mPa s. The results are shown in Table 2.

[0063] [Reference Example 3] Confirmation of the efficiency of uniform dissolution of high viscosity liquid and low viscosity liquid (Ribbon blade C) A ribbon impeller C made of SUS304 and having an impeller diameter of 120 mm and an impeller total height of 180 mm was set in a 2 L round-bottom separable glass reaction vessel (inner diameter 130 mm, height 220 mm). 2,634 g of maltose (colorless and transparent) with the viscosity adjusted to 292,000 mPa·s by adding deionized water in advance was gently placed into this container. Subsequently, 61 g of an aqueous iodine solution (brown, viscosity: 1 mPa·s) was gently added as a coloring solution for visually confirming the mixing state. The total height of the liquid separated into two layers was 180 mm. As a stirrer for driving the stirring blade from the upper part of the container, an IKA electronic control stirrer EUROSTAR200 was used, and the stirring power per unit volume was adjusted to 4.2 kW / m 3 and stirring was started by adjusting the rotation speed so as to achieve this. The time taken for the two liquids to dissolve until the whole was visually observed to be completely uniformly colored brown was measured, and it was 20 minutes. The viscosity of the brown liquid after uniform dissolution was 60,300 mPa·s. The results are shown in Table 2.

[0064]

Table 2

[0065] [Reference Examples 4 - 8] Confirmation of the efficiency of uniform dissolution of a highly viscous liquid and a low-viscosity liquid (other than ribbon blades) The stirring blade was changed from the ribbon blades in Reference Examples 1 - 3 to those shown in Table 1 other than that. As the mixing tank, it was changed to a 2 L round-bottom separable glass reaction vessel (inner diameter 120 mm, height 170 mm). Otherwise, in the same manner as in Reference Example 1, the stirring power per unit volume was made equivalent, and the efficiency of uniform dissolution of the highly viscous liquid and the low-viscosity liquid was confirmed. As a result, as shown in Table 3, it was confirmed that longer stirring time was required compared to the ribbon blade, and the efficiency of uniform dissolution of the highly viscous liquid and the low-viscosity liquid was poor.

[0066]

Table 3

[0067] [Reference Example 9] Confirmation of the efficiency of uniform dissolution of a highly viscous liquid and a low-viscosity liquid (ribbon blade A-2) After conducting Reference Example 1, the following experiment was conducted using the mixing and stirring device used. To the brown liquid with a viscosity of 81370 mPa·s obtained in Reference Example 1, 266 g of an aqueous sodium thiosulfate solution (viscosity: 1 mPa·s) was gently added as a decolorizing liquid for visually confirming the mixing state. The total height of the liquid separated into two layers was 230 mm. As a stirrer for driving the stirring blade from the upper part of the container, an electronically controlled stirrer EUROSTAR200 manufactured by IKA was used, and stirring was started by adjusting the rotation speed so that the stirring power per unit volume was 3.4 kW / m 3 ³. The time required for the two liquids to dissolve until the whole became completely uniformly colorless by visual observation was measured, and it was 10 minutes. The viscosity of the colorless and transparent liquid after uniform dissolution was 7880 mPa·s. The results are shown in Table 4.

[0068] [Reference Example 10] Confirmation of the efficiency of uniform dissolution of a highly viscous liquid and a low-viscosity liquid (ribbon blade B) After performing Reference Example 2, the following experiment was conducted using the mixed stirring device used. To the brown liquid with a viscosity of 80100 mPa·s obtained in Reference Example 2, 218 g of an aqueous sodium thiosulfate solution (viscosity: 1 mPa·s) was gently added as a decolorizing liquid for visually confirming the mixing state. The total height of the liquid separated into two layers was 225 mm. As a stirrer for driving the stirring blade from the upper part of the container, an electronically controlled stirrer EUROSTAR200 manufactured by IKA was used, and stirring was started by adjusting the rotation speed so that the stirring power per unit volume was 3.4 kW / m 3 ³. The time required for the two liquids to dissolve until the whole became completely uniformly colorless by visual observation was measured, and it was 10 minutes. The viscosity of the colorless and transparent liquid after uniform dissolution was 5677 mPa·s. The results are shown in Table 4.

[0069] [Reference Example 11] Confirmation of the efficiency of uniform dissolution of a highly viscous liquid and a low-viscosity liquid (ribbon blade C) After performing Reference Example 3, the following experiment was conducted using the mixed stirring device used. To the brown liquid with a viscosity of 60300 mPa·s obtained in Reference Example 3, 191 g of an aqueous sodium thiosulfate solution (viscosity: 1 mPa·s) was gently added as a decolorizing liquid for visually confirming the mixing state. The total height of the liquid separated into two layers was 195 mm. As a stirrer for driving the stirring blade from the upper part of the container, an electronically controlled stirrer EUROSTAR200 manufactured by IKA was used, and the stirring was started by adjusting the rotational speed so that the stirring power per unit volume was 3.4 kW / m 3 ³. When measured as the time required for the two liquids to dissolve until the whole became completely uniformly colorless by visual inspection, it was 15 minutes. The viscosity of the colorless transparent liquid after uniform dissolution was 6540 mPa·s. The results are shown in Table 4.

[0070]

Table 4

[0071] [Reference Examples 12 - 16] Confirmation of the efficiency of uniform dissolution of a highly viscous liquid and a low-viscosity liquid (other than ribbon blades) After conducting Reference Examples 4 - 8 respectively, the following experiments were conducted using the mixing and stirring device used. Using the brown liquids (viscosity approximately 80000 mPa·s) obtained in Reference Examples 4 - 8 respectively, an aqueous sodium thiosulfate solution was gently added as a decolorizing liquid for visually confirming the mixing state. In the same manner as in Reference Example 9, with the stirring power per unit volume being made equivalent, the efficiency of uniform dissolution of the highly viscous liquid and the low-viscosity liquid was confirmed. As a result, as shown in Table 5, it was confirmed that longer stirring time was required compared to the ribbon blade, and the efficiency of uniform dissolution of the highly viscous liquid and the low-viscosity liquid was poor.

[0072]

Table 5

[0073] From the results of Reference Examples 1 - 16, it became clear that the ribbon blade is excellent for stirring and dissolving a highly viscous liquid and a low-viscosity liquid. The following examples and comparative examples in which high viscosity liquids and powders, and low viscosity liquids, were stirred and dissolved were carried out by selecting ribbon blade A-1 or A-2.

[0074] [Example 1] Stirring and uniformly dissolving a high-viscosity liquid and powder, and stirring and uniformly dissolving a low-viscosity liquid in the same tank (ribbon impeller A-2) Stirring was carried out under the above-mentioned stirring and mixing conditions (2), specifically as follows. A ribbon impeller A-2 made of SUS304 and having an impeller diameter of 140 mm and an impeller total height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm). 2,260 g of silicone resin with a viscosity of approximately 50,000 mPa·s at 25°C was gently placed in the container. Next, 70 g of TPO powder that had been previously classified using a sieve with 250 μm openings was gently added, taking care not to create powder. An electronically controlled agitator, EUROSTAR200, manufactured by IKA, was used as an agitator that drives an agitating blade from the top of the vessel, and agitation was started at 10 rpm. A 5 L round-bottom separable glass reaction vessel was heated in an oil bath to adjust the temperature to 40 to 45°C, and the stirring speed was increased to 65 rpm, followed by stirring for a total of 3 hours. To prevent polymerization of the DVB and STMS that were subsequently added, heating was stopped, the mixture was cooled, and stirring was stopped. After the air bubbles that had become trapped in the liquid during stirring were released, visual inspection revealed that the TPO had completely dissolved, with no residual TPO remaining. To this was gently added 70 g of DVB, a low-viscosity liquid with a viscosity of 1 mPa·s at 25°C, and the mixture was stirred at 50 rpm for 2 hours at 20-25°C. Next, 12 g of DDT, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, and 23 g of STMS, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, were gently added and the mixture was stirred at 60 rpm for 2 hours at 20-25°C. After stirring was stopped, the mixed liquid was sampled from two locations in the tank and the viscosity was measured. The results showed that the viscosity at 25°C was 5001 mPa·s and 4848 mPa·s, and there was no variation in viscosity, confirming that the high-viscosity liquid and the low-viscosity liquid were dissolved uniformly. Subsequently, the liquid after stirring was filtered through a flat filter medium with a pore size of 3 μm (metal fiber sheet manufactured by ADVANTEC). When observing the surface of the filter medium after filtration, TPO was completely dissolved, and no residue was confirmed. As a conclusion, it was confirmed that the highly viscous liquid, powder, and low viscous liquid were completely and uniformly dissolved. The results are shown in Table 6.

[0075] [Example 2] Stirring and uniform dissolution of a highly viscous liquid and a powder, and stirring and uniform dissolution of a low viscous liquid in the same tank (ribbon blade A-2) Stirring was carried out under the above-mentioned stirring and mixing conditions (2). Specifically, it is as follows. A ribbon blade A-2 made of SUS304 with a blade diameter of 140 mm and a total blade height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm). 2170 g of a silicone resin with a viscosity of about 300000 mPa·s at 25 °C was gently placed in this vessel. Subsequently, 100 g of the undersize powder of TPO that had been previously classified using a sieve with an opening size of 250 μm, and 67 g of the undersize powder of 184 obtained in the same manner were gently added without powdering. Using an IKA electronic control stirrer EUROSTAR200 as a stirrer to drive the stirring blade from the upper part of the vessel, stirring was started at 6 rpm. The 5 L round-bottom separable glass reaction vessel was heated in an oil bath to adjust the temperature to 40 - 45 °C, and the stirring speed was increased to 60 rpm and stirred for a total of 3 hours. Subsequently, heating was stopped and cooling was carried out for the purpose of preventing the polymerization of DOG and STMS to be added later, and stirring was stopped. After visually confirming that the bubbles bitten into the liquid during stirring had escaped, TPO and 184 were completely dissolved and there was no residue. Here, 1170 g of DOG, a low viscous liquid with a viscosity of 300 mPa·s at 25 °C, was gently added and stirred at a stirring speed of 50 rpm at 20 - 25 °C for 2 hours. Subsequently, 17 g of DDT, a low viscous liquid with a viscosity of 2 mPa·s at 25 °C, and 33 g of STMS, a low viscous liquid with a viscosity of 2 mPa·s at 25 °C, were gently added and stirred at a stirring speed of 60 rpm at 20 - 25 °C for 2 hours. After stirring was stopped, the mixed liquid was sampled from two locations in the tank and the viscosity was measured. The results showed that the viscosity at 25°C was 2357 mPa·s and 2313 mPa·s, and since there was no variation in viscosity, it was confirmed that the high-viscosity liquid and the low-viscosity liquid were dissolved uniformly. The stirred solution was then filtered through a flat filter medium with a pore size of 3 μm (metal fiber sheet manufactured by ADVANTEC Co., Ltd.). Observation of the surface of the filter medium after filtration revealed that TPO and 184 had completely dissolved, with no residue remaining. In conclusion, it was confirmed that the high viscosity liquid, powder, and low viscosity liquid were completely and uniformly dissolved. The results are shown in Table 6.

[0076] [Example 3] Stirring and uniformly dissolving a high-viscosity liquid and powder, and stirring and uniformly dissolving a low-viscosity liquid in the same tank (ribbon impeller A-1) Stirring was carried out under the above-mentioned stirring and mixing conditions (1), specifically as follows. 6,790 g of silicone resin with a viscosity of approximately 50,000 mPa·s at 25°C was gently added to a 10 L manufacturing agitator mixer (ribbon impeller A-1). Next, 211 g of undersized TPO powder, which had been previously classified using a 1 mm sieve, was gently added, taking care not to create powder. Stirring was started using an explosion-proof inverter motor-equipped cyclo reducer with a reduction ratio of 1 / 21, output of 0.4 kW, number of poles 4, frequency of 60 Hz, and power supply of 200 V as the agitator that drives the agitator blades from the top of the device. The internal temperature was adjusted to 40-45°C by heating from the jacket, and the agitation speed was increased to 110 rpm, and stirring was continued for a total of 3 hours. To prevent polymerization of the DVB and STMS that were subsequently added, heating was stopped, the mixture was cooled, and stirring was stopped. After the air bubbles that had become trapped in the liquid during stirring were released, visual inspection revealed that the TPO had completely dissolved, with no residual TPO remaining. To this was gently added 205 g of DVB, a low-viscosity liquid with a viscosity of 1 mPa·s at 25°C, and the mixture was stirred at 130 rpm for 2 hours at 20-25°C. Next, 33 g of DDT, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, and 67 g of STMS, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, were gently added, and the mixture was stirred at 130 rpm for 3 hours at 20-25°C. After stirring was stopped, the mixed liquid was sampled from three locations in the tank and the viscosity was measured. The results showed that the viscosities at 25°C were 5310 mPa·s, 5330 mPa·s, and 5313 mPa·s, and since there was no variation in viscosity, it was confirmed that the high-viscosity liquid and the low-viscosity liquid were dissolved uniformly. The stirred solution was then filtered through a flat filter medium with a pore size of 3 μm (Microscreen E, manufactured by 3M Co.). When the surface of the filter medium was observed after filtration, it was found that the TPO had completely dissolved, with no undissolved residue remaining. In conclusion, it was confirmed that the high viscosity liquid, powder, and low viscosity liquid were completely and uniformly dissolved. The results are shown in Table 6.

[0077] [Example 4] Stirring and uniformly dissolving a high-viscosity liquid and powder, and stirring and uniformly dissolving a low-viscosity liquid in the same tank (ribbon impeller A-1) Stirring was carried out under the above-mentioned stirring and mixing conditions (1), specifically as follows. 6067 g of silicone resin with a viscosity of approximately 300,000 mPa·s at 25°C was gently added to a 10 L manufacturing agitator mixer (ribbon impeller A-1). Next, 280 g of TPO powder that had previously been classified using a 1 mm mesh sieve and that had fallen below the sieve size, and 187 g of 184 powder that had been obtained in the same way and that had fallen below the sieve size, were gently added, taking care not to create powder. Stirring was started using an explosion-proof inverter motor-equipped cyclo reducer with a reduction ratio of 1 / 21, output of 0.4 kW, number of poles 4, frequency of 60 Hz, and power supply of 200 V as the agitator that drives the agitator blades from the top of the device. The internal temperature was adjusted to 40-45°C by heating from the jacket, and the agitation speed was increased to 110 rpm, and stirring was continued for a total of 2 hours. Subsequently, heating was stopped and cooling was performed to prevent the polymerization of DOG and STMS to be added, and stirring was stopped. When visually checking after the bubbles that had bitten into the liquid during stirring had escaped, TPO and 184 were completely dissolved and there was no residue. Here, 1170 g of DOG, which is a low-viscosity liquid with a viscosity of 300 mPa·s at 25°C, was gently added and stirred at 130 rpm for 3 hours at 20 - 25°C. Subsequently, 45 g of DDT, which is a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, and 89 g of STMS, which is a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, were gently added and stirred at 130 rpm for 2 hours at 20 - 25°C. After stopping stirring, samples of the mixed liquid were taken from three locations in the tank to measure the viscosity. As a result, the viscosities at 25°C were 2152 mPa·s, 2150 mPa·s, and 2151 mPa·s. Since there was no variation in viscosity, it was confirmed that the high-viscosity liquid and the low-viscosity liquid were uniformly dissolved. Subsequently, the liquid after stirring was filtered through a flat filter medium (Micro Screen E manufactured by 3M) with a pore size of 3 μm. When observing the surface of the filter medium after filtration, TPO and 184 were completely dissolved and no residue was confirmed. As a conclusion, it was confirmed that the high-viscosity liquid, the powder, and the low-viscosity liquid were completely uniformly dissolved. The results are shown in Table 6.

[0078] [Example 5] Stirring and uniform dissolution of high-viscosity liquid and powder, and stirring and uniform dissolution of low-viscosity liquid in the same tank (ribbon blade A-1) Stirring was performed under the aforementioned stirring and mixing conditions (1). Specifically, it was as follows. 8120 g of a silicone resin with a viscosity of about 50000 mPa·s at 25°C was gently charged into a 10 L stirring and mixing machine (ribbon blade A-1). Subsequently, 250 g of the sieved powder of TPO, which had been classified in advance using a sieve with a mesh size of 1 mm, was gently added so as not to cause powdering. As a stirrer for driving the stirring blade from the upper part of the device, a cycloidal speed reducer with an explosion-proof inverter motor was used to start stirring, with a reduction ratio of 1 / 21, an output of 0.4 kW, 4 poles, a frequency of 60 Hz, and a power supply of 200 V. Heating was carried out from the jacket to adjust the internal temperature to 35 - 40 °C, and the stirring speed was increased to 110 rpm and stirred for a total of 1 hour. Subsequently, heating was stopped and cooling was carried out for the purpose of preventing the polymerization of DVB and STMS to be added, and stirring was stopped. After visually confirming that the bubbles bitten into the liquid during stirring had escaped, it was found that TPO was completely dissolved and there was no residue. Here, 251 g of DVB, a low-viscosity liquid with a viscosity of 1 mPa·s at 25 °C, was gently added and stirred at 130 rpm for 1 hour at 20 - 25 °C. Subsequently, 41 g of DDT, a low-viscosity liquid with a viscosity of 2 mPa·s at 25 °C, and 83 g of STMS, a low-viscosity liquid with a viscosity of 2 mPa·s at 25 °C, were gently added and stirred at 130 rpm for 1 hour at 20 - 25 °C. After stopping stirring, the viscosity was measured by sampling the mixed liquid from three locations in the tank. As a result, the viscosities at 25 °C were 5052 mPa·s, 5055 mPa·s, and 5044 mPa·s. Since there was no variation in viscosity, it was confirmed that the high-viscosity liquid and the low-viscosity liquid were uniformly dissolved. Subsequently, the liquid after stirring was filtered through a flat filter medium (Micro Screen E manufactured by 3M) with a pore size of 3 μm. When observing the surface of the filter medium after filtration, it was found that TPO was completely dissolved and no residue was confirmed. As a conclusion, it was confirmed that the high-viscosity liquid, the powder, and the low-viscosity liquid were completely uniformly dissolved. The results are shown in Table 6.

[0079] [Example 6] Stirring and uniform dissolution of high-viscosity liquid and powder, and stirring and uniform dissolution of low-viscosity liquid in the same tank (Ribbon blade A-1) Stirring was carried out under the above-mentioned stirring and mixing conditions (1). Specifically, it was as follows. 6,499 g of a silicone resin having a viscosity of about 300,000 mPa·s at 25°C was gently charged into a stirring and mixing machine for 10 L production (ribbon blade A-1). Subsequently, 300 g of the sieved powder of TPO that had been previously classified using a sieve with an aperture of 1 mm and 200 g of the sieved powder of 184 obtained in the same manner were gently added so as not to cause powder scattering. Stirring was started using an explosion-proof inverter motor with a cycloidal speed reducer, reduction ratio 1 / 21, output 0.4 kW, number of poles 4P, frequency 60 Hz, and power supply 200 V as a stirrer for driving the stirring blade from the upper part of the apparatus. Heating was carried out from the jacket to adjust the internal temperature to 40 - 45°C, and the stirring speed was increased to 110 rpm and stirred for a total of 1 hour. Subsequently, heating was stopped and cooling was carried out for the purpose of preventing the polymerization of DOG and STMS to be added subsequently, and stirring was stopped. After visually confirming that the bubbles bitten into the liquid during stirring had escaped, it was found that TPO and 184 were completely dissolved and there was no residue. Here, 3,466 g of DOG, which is a low-viscosity liquid having a viscosity of 300 mPa·s at 25°C, was gently added and stirred at a stirring speed of 130 rpm at 20 - 25°C for 1 hour. Subsequently, 49 g of DDT, which is a low-viscosity liquid having a viscosity of 2 mPa·s at 25°C, and 99 g of STMS, which is a low-viscosity liquid having a viscosity of 2 mPa·s at 25°C, were gently added and stirred at a stirring speed of 130 rpm at 20 - 25°C for 1 hour. After stopping stirring, sampling of the mixed liquid was carried out at three locations in the tank to measure the viscosity. As a result, the viscosities at 25°C were 2,231 mPa·s, 2,241 mPa·s, and 2,240 mPa·s, and since there was no variation in viscosity, it was confirmed that the high-viscosity liquid and the low-viscosity liquid were uniformly dissolved. Subsequently, the liquid after stirring was filtered through a flat filter medium (Micro Screen E manufactured by 3M) with a pore diameter of 3 μm. When observing the surface of the filter medium after filtration, TPO and 184 were completely dissolved and no residue was confirmed. As a conclusion, it was confirmed that the high-viscosity liquid, the powder, and the low-viscosity liquid were completely and uniformly dissolved. The results are shown in Table 6.

[0080] [Example 7] Stirring and uniform dissolution of a high-viscosity liquid and a powder, and stirring and uniform dissolution of a low-viscosity liquid in the same tank (ribbon blade A-1) Stirring was carried out under the above-mentioned stirring and mixing conditions (1). Specifically, it is as follows. 5948 g of silicone resin with a viscosity of about 50000 mPa·s at 25°C was gently charged into a 10 L stirring and mixing machine for production (ribbon blade A). Subsequently, 184 g of the sieved powder of TPO that had been classified in advance using a sieve with a mesh size of 1 mm was gently added so as not to form powder lumps. Stirring was started using an explosion-proof inverter motor with a cycloidal speed reducer, reduction ratio 1 / 21, output 0.4 kW, number of poles 4P, frequency 60 Hz, and power supply 200V as a stirrer for driving the stirring blade from the upper part of the apparatus. Heating was carried out from the jacket to adjust the internal temperature to 40 - 45°C, and the stirring speed was increased to 110 rpm and stirred for a total of 1 hour. Subsequently, heating was stopped and cooling was carried out for the purpose of preventing the polymerization of DVB and STMS to be added later, and stirring was stopped. When visually confirmed after the bubbles that had bitten into the liquid during stirring had escaped, TPO had completely dissolved and there was no residue. Here, 182 g of DVB, a low-viscosity liquid with a viscosity of 1 mPa·s at 25°C, was gently added and stirred at a stirring speed of 130 rpm at 20 - 25°C for 1 hour. Subsequently, 30 g of DDT, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, and 60 g of STMS, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, were gently added and stirred at a stirring speed of 130 rpm at 20 - 25°C for 1 hour. After stopping stirring, sampling of the mixed liquid was carried out at three locations in the tank to measure the viscosity. As a result, the viscosities at 25°C were 5531 mPa·s, 5519 mPa·s, and 5503 mPa·s. Since there was no variation in viscosity, it was confirmed that the high-viscosity liquid and the low-viscosity liquid were uniformly dissolved. Subsequently, the liquid after stirring was filtered through a flat filter medium (Micro Screen E manufactured by 3M) with a pore size of 3 μm. When observing the surface of the filter medium after filtration, TPO had completely dissolved and no residue was confirmed. As a conclusion, it was confirmed that the high-viscosity liquid, the powder, and the low-viscosity liquid were completely uniformly dissolved. The results are shown in Table 6.

[0081] [Example 8] Stirring and uniform dissolution of a highly viscous liquid and powder, and stirring and uniform dissolution of a low-viscosity liquid in the same tank (ribbon blade A-1) Stirring was carried out under the above-mentioned stirring and mixing conditions (1). Specifically, it is as follows. 6933 g of a silicone resin having a viscosity of about 300000 mPa·s at 25°C was gently charged into a 10 L stirring and mixing machine (ribbon blade A-1). Subsequently, 320 g of the undersize powder of TPO that had been previously classified using a sieve with an aperture of 2 mm, and 213 g of the undersize powder of 184 obtained in the same manner were gently added so as not to cause powder to fly up. As a stirrer for driving the stirring blade from the upper part of the apparatus, a cyclo with an explosion-proof inverter motor The reduction gear, reduction ratio 1 / 21, output 0.4 kW, number of poles 4P, frequency 60 Hz, and power supply 200V were used to start stirring. Heating was carried out from the jacket to adjust the internal temperature to 40 - 45°C, and the stirring speed was increased to 110 rpm and stirred for a total of 1 hour. Subsequently, heating was stopped and cooling was carried out for the purpose of preventing the polymerization of the subsequently added DOG and STMS, and stirring was stopped. After visually confirming that the bubbles bitten into the liquid during stirring had escaped, most of the TPO and 184 were dissolved and only a small amount of undissolved residue was confirmed. Here, 3709 g of DOG, a low-viscosity liquid having a viscosity of 300 mPa·s at 25°C, was gently added and stirred at a stirring speed of 130 rpm at 20 - 25°C for 1 hour. Subsequently, 53 g of DDT, a low-viscosity liquid having a viscosity of 2 mPa·s at 25°C, and 106 g of STMS, a low-viscosity liquid having a viscosity of 2 mPa·s at 25°C, were gently added and stirred at a stirring speed of 130 rpm at 20 - 25°C for 1 hour. After stopping stirring, the mixed liquid was sampled from three locations in the tank to measure the viscosity. As a result, the viscosities at 25°C were 2303 mPa·s, 2295 mPa·s, and 2288 mPa·s. Since there was no variation in viscosity, it was confirmed that the highly viscous liquid and the low-viscosity liquid were uniformly dissolved. Subsequently, the liquid after stirring was filtered through a flat filter medium (Micro Screen E manufactured by 3M) with a pore size of 3 μm. When observing the surface of the filter medium after filtration, the TPO and 184 were almost completely dissolved and only a small amount of undissolved residue was confirmed. As a conclusion, it was confirmed that the highly viscous liquid, powder, and low-viscosity liquid were almost completely and uniformly dissolved. The results are shown in Table 6.

[0082]

Table 6

[0083] [Comparative Example 1] Confirmation of the particle size at which stirring and dissolution in a highly viscous liquid become difficult (ribbon blade A-2) Stirring was carried out under the above-mentioned stirring and mixing conditions (2). Specifically, it is as follows. A ribbon blade A-2 made of SUS304 with a blade diameter of 140 mm and a total blade height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm). 1114 g of a silicone resin with a viscosity of about 50000 mPa·s at 25°C was gently placed in this container. Subsequently, 35 g of DVB, a low-viscosity liquid with a viscosity of 1 mPa·s at 25°C, and 38 g of untreated TPO powder were gently added. The untreated TPO powder contained lumps with a maximum total length of about 15 to 60 mm. Using an IKA electronic control stirrer EUROSTAR20 as a stirrer to drive the stirring blade from the upper part of the container, stirring was started at 6 rpm. The 5 L round-bottom separable glass reaction vessel was heated in an oil bath to adjust the temperature to 50 - 60°C. Since the powder was difficult to dissolve, while observing the situation, the stirring speed was finally increased to 140 rpm and stirred for a total of 3 hours. Heating was stopped and cooling was carried out to 20 - 25°C, and stirring was stopped. After the bubbles trapped in the liquid escaped during stirring and visual confirmation was made, it was found that TPO was not completely dissolved and a clear residue was confirmed. At this point, the viscosity of the mixed liquid had decreased to about 7400 mPa·s. 6 g of DDT, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, and 13 g of STMS, a low-viscosity liquid with a viscosity of 2 mPa·s at 25°C, were gently added and stirred at 50 rpm for 4 hours at 20 - 25°C. After stirring, the liquid was filtered through a flat filter medium, and upon observing the surface of the filter medium, it was confirmed that TPO was not completely dissolved and undissolved residues remained. As a conclusion, it was confirmed that it is difficult for untreated TPO to be completely dissolved into high-viscosity and low-viscosity liquids even when the stirring speed is increased and stirred for a long time at high temperatures. The results are shown in Table 7.

[0084] In addition, instead of Comparative Example 1, in Example 1, mixing was carried out in the same manner as in Example 1 except that the TPO that had been classified in advance using a sieve with an opening size of 250 μm was changed to unclassified TPO (TPO containing lumps with a maximum overall length of about 15 - 60 mm). Undissolved residues of TPO were confirmed, and the same results as in Comparative Example 1 were obtained.

[0085] [Comparative Example 2] Confirmation of particle size at which stirring and dissolution into a high-viscosity liquid become difficult (Ribbon impeller A-2) Stirring was carried out under the aforementioned stirring and mixing conditions (2). Specifically, it was as follows. A ribbon impeller A-2 made of SUS304 with a blade diameter of 140 mm and an overall blade height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm). 732 g of a silicone resin with a viscosity of about 300000 mPa·s at 25°C was gently placed in this vessel. Subsequently, a suspension in which 34 g of untreated TPO powder and 23 g of untreated 184 powder were dispersed in 394 g of DOG, a low-viscosity liquid with a viscosity of 300 mPa·s at 25°C, was gently added. The untreated TPO powder contained lumps with a maximum overall length of about 15 - 60 mm. The untreated 184 powder contained lumps with a maximum overall length of about 5 - 30 mm. Stirring was started at 6 rpm using an IKA electronic control stirrer EUROSTAR20 as a stirrer for driving the stirring impeller from the upper part of the vessel. A 5 L round-bottom separable glass reaction vessel was heated in an oil bath to adjust the temperature to 50 - 55 °C. Since the powder was difficult to dissolve, the stirring speed was finally increased to 130 rpm while observing the situation, and stirring was carried out for a total of 7 hours. Heating was stopped and cooling was carried out to 20 - 25 °C, and stirring was stopped. After visually confirming after the bubbles that had bitten into the liquid during stirring had escaped, it was found that TPO and 184 were not completely dissolved, and a clear residue was confirmed. At this point, the viscosity of the mixed liquid had decreased to about 2800 mPa·s. Here, 6 g of DDT, a low-viscosity liquid with a viscosity of 2 mPa·s at 25 °C, and 11 g of STMS, a low-viscosity liquid with a viscosity of 2 mPa·s at 25 °C, were gently added, and stirring was carried out at 60 rpm at 20 - 25 °C for 3 hours. After filtering the liquid after stirring through a flat filter medium and observing the surface of the filter medium, it was again found that TPO and 184 were not completely dissolved, and a residue was confirmed. As a conclusion, it was confirmed that it is difficult for untreated TPO and 184 to completely dissolve into high-viscosity and low-viscosity liquids even when the stirring speed is increased and stirring is carried out for a long time at high temperatures. The results are shown in Table 7.

[0086] In addition, when, instead of Comparative Example 2, in Example 2, mixing was carried out in the same manner as in Example 2 except that the TPO that had been classified in advance using a sieve with an aperture of 250 μm was changed to unclassified TPO (TPO containing lumps with a maximum overall length of about 15 - 60 mm), a residue of TPO was confirmed, and the same results as in Comparative Example 2 were obtained.

[0087] [Table 7] * The upper limit temperature during stirring of the high-viscosity liquid and the powder is 60 °C

[0088] [Example 9] Stirring and uniform dissolution of the low-viscosity liquid and the powder (ribbon blade A-2) Stirring was carried out under the above-mentioned stirring and mixing conditions (2). Specifically, it is as follows. A ribbon blade A-2 made of SUS304 with a blade diameter of 140 mm and an overall blade height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm). DOG1170 g, a low-viscosity liquid with a viscosity of 300 mPa·s at 25°C, was gently placed into this container. Subsequently, 100 g of the undersize powder of TPO that had been previously classified using a sieve with an aperture of 1 mm and 67 g of the undersize powder of 184 obtained in the same manner were gently added without causing powder to fly up. As a stirrer for driving the stirring blade from the upper part of the container, an electronically controlled stirrer EUROSTAR200 manufactured by IKA was used, and stirring was started at 6 rpm. The temperature of a 5 L round-bottom separable glass reaction vessel was adjusted to 20 - 25°C for the purpose of preventing the polymerization of DOG, and the stirring speed was increased to 60 rpm and stirred for a total of 4 hours. After stopping the stirring and visually confirming after the bubbles that had bitten into the liquid during stirring had escaped, TPO and 184 were almost completely dissolved and there was almost no residue.

[0089] [Comparative Example 3] Stirring and uniform dissolution of low-viscosity liquid and powder (Ribbon blade A-2) Stirring was carried out under the aforementioned stirring and mixing conditions (2). Specifically, it is as follows. A ribbon blade A-2 made of SUS304 with a blade diameter of 140 mm and a total blade height of 220 mm was set in a 5 L round-bottom separable glass reaction vessel (inner diameter 150 mm, height 360 mm). DOG1170 g, a low-viscosity liquid with a viscosity of 300 mPa·s at 25°C, was gently placed into this container. Subsequently, 100 g of the powder of untreated TPO and 67 g of the powder of untreated 184 were gently added without causing powder to fly up. The powder of untreated TPO contained lumps with a maximum total length of about 15 - 60 mm. The powder of untreated 184 contained lumps with a maximum total length of about 5 - 30 mm. As a stirrer for driving the stirring blade from the upper part of the container, an electronically controlled stirrer EUROSTAR200 manufactured by IKA was used, and stirring was started at 6 rpm. The temperature of a 5 L round-bottom separable glass reaction vessel was adjusted to 20 - 25°C for the purpose of preventing the polymerization of DOG, and the stirring speed was increased to 60 rpm and stirred for a total of 4 hours. When stirring was stopped and visually confirmed after the bubbles bitten into the liquid during stirring escaped, it was found that TPO and 184 were not completely dissolved, and a clear residue was confirmed.

Industrial Applicability

[0090] According to the present invention, liquids and powders can be efficiently homogenized. Furthermore, highly viscous liquids, low-viscosity liquids, and powders can be homogenized in a single stirring blade and stirring tank. Therefore, the present invention is useful for various uniform mixing of liquids and powders, and for the production of compositions obtained by dissolving powders in liquids.

Explanation of Symbols

[0091] 1 Stirring shaft 2 Support rod 3 Ribbon-shaped blade 4 Bottom ribbon blade

Claims

1. In a stirring tank equipped with ribbon blades, a highly viscous liquid having a viscosity of 10,000 mPa·s or more determined by the following viscosity measurement method and a powder from which coarse powder has been removed are stirred by the ribbon blades, and a stirring and dissolving step of dissolving the powder in the highly viscous liquid; a step of cooling the first composition obtained through the stirring and dissolving step; a stirring step of adding a low-viscosity liquid having a viscosity of 1,000 mPa·s or less determined by the following viscosity measurement method to the stirring tank containing the first composition and stirring with the ribbon blades; a step of filtering the composition obtained through the stirring step with a filter medium; A method for producing a composition, comprising: (Viscosity measurement method) - Apparatus: E-type viscometer - Cone rotor type: 1°34 × R24 - Temperature: 25 °C - Rotation speed: 1 rpm - Waiting time: 2 minutes

2. Furthermore, the method for producing a composition according to claim 1, further comprising a step of visually observing the filter medium after the filtering step to confirm that the powder is dissolved.

3. The method for producing a composition according to claim 1 or 2, wherein the powder contains a photoinitiator.

4. The method for producing a composition according to any one of claims 1 to 3, wherein the powder from which coarse powder has been removed is a powder from which coarse powder has been removed by classification.

5. The method for producing a composition according to any one of claims 1 to 4, wherein the low-viscosity liquid contains a reactive monomer.

6. In a stirring tank equipped with ribbon blades, a highly viscous liquid having a viscosity of 10,000 mPa·s or more determined by the following viscosity measurement method and a powder from which coarse powder has been removed are stirred by the ribbon blades, and a stirring and dissolving step of dissolving the powder in the highly viscous liquid; a step of cooling the first composition obtained through the stirring and dissolving step; a stirring step of adding a low-viscosity liquid having a viscosity of 1,000 mPa·s or less determined by the following viscosity measurement method to the stirring tank containing the first composition and stirring with the ribbon blades, comprising: The powder contains a photoinitiator, characterized by a mixing method. (Viscosity measurement method) - Apparatus: E-type viscometer - Cone rotor type: 1°34 × R24 - Temperature: 25 °C - Rotation speed: 1 rpm - Waiting time: 2 minutes

7. The mixing method according to claim 6, wherein the powder from which coarse powder has been removed is a powder from which coarse powder has been removed by classification.

8. The mixing method according to claim 6 or 7, wherein the low-viscosity liquid contains a reactive monomer.

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