Method for producing polymerizable composition for optical material, method for producing optical material, production device for polymerizable composition for optical material, and production system for optical material
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- MITSUI CHEMICALS INC
- Filing Date
- 2026-01-09
- Publication Date
- 2026-08-06
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Figure JP2026000584_06082026_PF_FP_ABST
Abstract
Description
Method for producing polymerizable compositions for optical materials, method for producing optical materials, apparatus for producing polymerizable compositions for optical materials, and system for producing optical materials
[0001] This disclosure relates to a method for producing polymerizable compositions for optical materials, a method for producing optical materials, an apparatus for producing polymerizable compositions for optical materials, and a system for producing optical materials.
[0002] International Publication No. 2022 / 113955 discloses a system for producing optical materials using a polymerizable composition for optical materials containing two or more different monomers for optical materials and a polymerization catalyst. In the system of International Publication No. 2022 / 113955, the polymerizable composition for optical materials is obtained by applying shear force to the first raw material composition and the second raw material composition using a power mixer. Furthermore, in the system of International Publication No. 2022 / 113955, each of the first raw material composition and the second raw material composition is transferred from a tank to the power mixer using a gear pump.
[0003] Here, a gear pump is a pump that uses the meshing of a pair of gears to move fluid inside a case. In a gear pump, as the pair of gears rotate while meshing, fluid is drawn into the gap between the teeth and the case and then sent through the gap between the gears. Because of this, shear stress is easily generated in the fluid.
[0004] Therefore, in a configuration where the first and second raw material compositions are each transferred using a gear pump, the shear stress applied to the first and second raw material compositions tends to be large. As a result, gel may form in the first and second raw material compositions.
[0005] This disclosure aims to suppress gel generation when transferring the first raw material composition and the second raw material composition, respectively.
[0006] The present disclosure provides a method for producing a polymerizable composition for optical materials, comprising: a first transfer step of transferring a first raw material composition to a mixing section in a first transfer section; a second transfer step of transferring a second raw material composition to the mixing section in a second transfer section; and a mixing step of mixing the first raw material composition and the second raw material composition in the mixing section, wherein at least one of the first transfer section and the second transfer section has a value of 500 Pa / (g·s) obtained by dividing the maximum shear stress applied to the object to be transferred by the transfer speed. -1 ) The following:
[0007] The method for manufacturing an optical material according to this disclosure includes a curing step in which a polymerizable composition for optical materials obtained by the method for manufacturing a polymerizable composition for optical materials described above is polymerized and cured to produce an optical material.
[0008] The apparatus for manufacturing polymerizable compositions for optical materials according to the present disclosure is a manufacturing apparatus for manufacturing polymerizable compositions for optical materials by mixing a first raw material composition and a second raw material composition, comprising: a mixing unit for mixing the first raw material composition and the second raw material composition; a first transfer unit for transferring the first raw material composition to the mixing unit; a second transfer unit for transferring the second raw material composition to the mixing unit; and a stirring unit for stirring the mixture of the first raw material composition and the second raw material composition mixed in the mixing unit, wherein at least one of the first transfer unit and the second transfer unit has a value of 500 Pa / (g·s) obtained by dividing the maximum shear stress applied to the object to be transferred by the transfer speed. -1 ) The following:
[0009] The optical material manufacturing system of the present disclosure comprises: a mixing unit for mixing a first raw material composition and a second raw material composition; a first transfer unit for transferring the first raw material composition to the mixing unit; a second transfer unit for transferring the second raw material composition to the mixing unit; a stirring unit for stirring the mixture of the first raw material composition and the second raw material composition mixed in the mixing unit; and a curing unit for polymerizing and curing the polymerizable composition for optical materials obtained by stirring in the stirring unit to manufacture an optical material, wherein at least one of the first transfer unit and the second transfer unit has a maximum shear stress applied to the object to be transferred divided by the transfer speed of 500 Pa / (g·s). -1 ) The following:
[0010] According to this disclosure, gel generation can be suppressed when transferring each of the first raw material composition and the second raw material composition.
[0011] This is a schematic diagram showing the manufacturing system according to this embodiment. This is a side cross-sectional view showing the first pump according to this embodiment. This is a cross-sectional view showing the stator and screw in the first pump according to this embodiment. This is a table showing the compositions of the first and second raw material compositions in the examples and comparative examples. This is a table showing the configurations of the first and second pumps in the examples and comparative examples. This is a table showing the evaluation results of the examples and comparative examples.
[0012] The embodiments of this disclosure are described below. However, this disclosure is not limited to the embodiments described below. In the embodiments described below, the components (including elemental steps, etc.) are not essential unless otherwise explicitly stated. The same applies to numerical values and their ranges, and they do not limit this disclosure.
[0013] In this disclosure, a numerical range indicated by "~" means a range that includes the numbers indicated before and after "~" as the lower and upper limits. In numerical ranges indicated in stages in this disclosure, the upper or lower limit indicated in one numerical range may be replaced with the upper or lower limit of another numerical range indicated in stages. In addition, in numerical ranges indicated in this disclosure, the upper or lower limit of that numerical range may be replaced with the values shown in the examples.
[0014] In this disclosure, each component may contain multiple types of the corresponding substance. If multiple types of the substance corresponding to each component are present in the composition, the content or amount of each component means the total content or amount of the multiple types of substances present in the composition, unless otherwise specified.
[0015] In this disclosure, the term "process" includes not only independent processes but also processes that cannot be clearly distinguished from other processes, as long as their intended purpose is achieved.
[0016] When describing embodiments with reference to the drawings in the present disclosure, the configuration of the embodiment is not limited to the configuration shown in the drawings. Also, the sizes of the components in each drawing are conceptual. Therefore, the front-back, left-right, and up-down dimensional ratios of each component, and the front-back, left-right, and up-down dimensional ratios between components are not limited to the illustrated dimensional ratios. Also, the front-back, left-right, and up-down dimensional ratios of each component may differ from the actual ones.
[0017] Also, unless otherwise specified in the present disclosure, the number of each component of the present disclosure is not limited to one, and there may be a plurality. In the description of the following drawings, the same parts are denoted by the same reference numerals.
[0018] <Optical Material Manufacturing System 10> FIG. 1 is a schematic diagram showing an optical material manufacturing system 10 (hereinafter simply referred to as the manufacturing system 10).
[0019] The manufacturing system 10 is a system for manufacturing an optical material using a first raw material composition 91 and a second raw material composition 92. As shown in FIG. 1, this manufacturing system 10 includes a first supply device 11, a second supply device 12, a mixing device 14, a stirring device 17, a casting device 18, and a curing device 19. Hereinafter, the first raw material composition 91, the second raw material composition 92, and each part of the manufacturing system 10 will be described.
[0020] <First Raw Material Composition 91 and Second Raw Material Composition 92> In the manufacturing system 10, the first raw material composition 91 and the second raw material composition 92 are mixed to produce a polymerizable composition 93 for an optical material containing two or more different monomers for an optical material and a polymerization catalyst.
[0021] Therefore, the first raw material composition 91 and the second raw material composition 92, as a whole of the first raw material composition 91 and the second raw material composition 92 combined, include two or more different monomers for an optical material and a polymerization catalyst.
[0022] For example, the first raw material composition 91 and the second raw material composition 92 may each contain different types of monomers for an optical material, and at least one of the first raw material composition 91 and the second raw material composition 92 may contain a polymerization catalyst.
[0023] The first raw material composition 91 and the second raw material composition 92 are not particularly limited as long as they contain two or more different monomers for optical materials and a polymerization catalyst as a whole.
[0024] <Monomers for optical materials> Examples of the monomers for optical materials include polyisocyanate compounds having two or more isocyanato groups, polythiol compounds having two or more mercapto groups, hydroxy thiol compounds having one or more mercapto groups and one or more hydroxyl groups, polyol compounds having two or more hydroxyl groups, amine compounds, and the like.
[0025] The two or more different monomers for optical materials preferably include a polyisocyanate compound (A) having two or more isocyanato groups and at least one active hydrogen compound (B) selected from the group consisting of a polythiol compound having two or more mercapto groups, a hydroxy thiol compound having one or more mercapto groups and one or more hydroxyl groups, a polyol compound having two or more hydroxyl groups, and an amine compound.
[0026] <Polyisocyanate compound (A)> Examples of the polyisocyanate compound (A) include aliphatic polyisocyanate compounds, alicyclic polyisocyanate compounds, aromatic polyisocyanate compounds, heterocyclic polyisocyanate compounds, etc., and one kind or two or more kinds are mixed and used. These polyisocyanate compounds may include dimers, trimers, and prepolymers. Examples of these polyisocyanate compounds include the compounds exemplified in International Publication No. 2011 / 055540.
[0027] In the present disclosure, the alicyclic polyisocyanate compound refers to a polyisocyanate compound that contains an alicyclic structure and may contain a heterocyclic structure. The aromatic polyisocyanate compound refers to a polyisocyanate compound that contains an aromatic structure and may contain an alicyclic structure and a heterocyclic structure. The heterocyclic polyisocyanate compound refers to a polyisocyanate compound that contains a heterocyclic structure and does not contain an alicyclic structure and an aromatic structure.
[0028] The polyisocyanate compound (A) preferably includes at least one selected from aliphatic polyisocyanate compounds, alicyclic polyisocyanate compounds, aromatic polyisocyanate compounds, and heterocyclic polyisocyanate compounds, and more preferably includes at least one of alicyclic polyisocyanate compounds and aromatic polyisocyanate compounds.
[0029] In this disclosure, from the viewpoint of suppressing striations in optical materials and shortening the manufacturing time of optical materials, the polyisocyanate compound (A) is 2,5-bis(isocyanatomethyl)bicyclo-[2.2.1]-heptane, 2,6-bis(isocyanatomethyl)bicyclo-[2.2.1]-heptane, m-xylylene diisocyanate, 2,4-tole diisocyanate, 2,6-tole diisocyanate, dicyclohexylmethane diisocyanate, 1,3-bis(isocyanatomethyl)cyclohexane, 1,4-bis(isocyanatomethyl)cyclohexane, isophorone diisocyanate, 1,6-hexamethylene diisocyanate, and 1,5-pentamethylene diisocyanate. Preferably, it contains at least one selected from anneates, more preferably at least one selected from 2,5-bis(isocyanatomethyl)bicyclo-[2.2.1]-heptane, 2,6-bis(isocyanatomethyl)bicyclo-[2.2.1]-heptane, m-xylylene diisocyanate, dicyclohexylmethane diisocyanate, and 1,3-bis(isocyanatomethyl)cyclohexane, and even more preferably at least one selected from m-xylylene diisocyanate, 2,5-bis(isocyanatomethyl)bicyclo-[2.2.1]-heptane, and 2,6-bis(isocyanatomethyl)bicyclo-[2.2.1]-heptane.
[0030] <Active hydrogen compounds (B)> Examples of active hydrogen compounds (B) include polythiol compounds having two or more mercapto groups, hydroxythiol compounds having one or more mercapto groups and one or more hydroxyl groups, polyol compounds having two or more hydroxyl groups, amine compounds, and the like.
[0031] As the active hydrogen compound (B), oligomers of the above-mentioned active hydrogen compound or halogen-substituted derivatives of the above-mentioned active hydrogen compound (e.g., chlorine-substituted derivatives, bromine-substituted derivatives, etc.) may be used. Furthermore, the active hydrogen compound may be used alone or as a mixture of two or more types.
[0032] <Polythiol compounds having two or more mercapto groups> Polythiol compounds are compounds having two or more mercapto groups, and examples include the compounds exemplified in International Publication No. 2016 / 125736.
[0033] In this disclosure, from the viewpoint of suppressing striations in optical materials and shortening the manufacturing time of optical materials, the polythiol compounds are 4-mercaptomethyl-1,8-dimercapto-3,6-dithiaoctane, 5,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,8-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, and pentaeri. Preferably, it contains at least one selected from thritol tetrakis(3-mercaptopropionate), bis(mercaptoethyl) sulfide, pentaerythritol tetrakis(2-mercaptoacetate), 2,5-bis(mercaptomethyl)-1,4-dithiane, 1,1,3,3-tetrakis(mercaptomethylthio)propane, 4,6-bis(mercaptomethylthio)-1,3-dithiane, and 2-(2,2-bis(mercaptomethylthio)ethyl)-1,3-dithiane. It is more preferable to include at least one selected from 4-mercaptomethyl-1,8-dimercapto-3,6-dithiaoctane, 5,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,8-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, pentaerythritol tetrakis(3-mercaptopropionate), pentaerythritol tetrakis(2-mercaptoacetate), and 2,5-bis(mercaptomethyl)-1,4-dithiane. It is even more preferable to include at least one selected from 4-mercaptomethyl-1,8-dimercapto-3,6-dithiaoctane, 5,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,8-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, and pentaerythritol tetrakis (3-mercaptopropionate).
[0034] <Hydroxythiol compounds having one or more mercapto groups and one or more hydroxyl groups> Examples of thiol compounds having hydroxyl groups include 2-mercaptoethanol, 3-mercapto-1,2-propanediol, glycerin bis(mercaptoacetate), 4-mercaptophenol, 2,3-dimercapto-1-propanol, pentaerythritol tris(3-mercaptopropionate), pentaerythritol tris(thioglycolate), etc., but are not limited to these example compounds.
[0035] <Polyol Compounds Having Two or More Hydroxyl Groups> Examples of polyol compounds include one or more aliphatic or alicyclic alcohols. Specifically, these include linear or branched aliphatic alcohols, alicyclic alcohols, and alcohols obtained by adding at least one selected from the group consisting of ethylene oxide, propylene oxide, and ε-caprolactone to these alcohols. More specifically, examples include the compounds exemplified in International Publication No. 2016 / 125736.
[0036] The polyol compound is preferably at least one selected from ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, 1,3-propanediol, 1,2-cyclopentanediol, 1,3-cyclopentanediol, 1,2-cyclohexanediol, 1,3-cyclohexanediol, and 1,4-cyclohexanediol.
[0037] <Amine Compounds> Examples of amine compounds include ethylenediamine, 1,2- or 1,3-diaminopropane, 1,2-, 1,3- or 1,4-diaminobutane, 1,5-diaminopentane, 1,6-diaminohexane, 1,7-diaminoheptane, 1,8-diaminooctane, 1,10-diaminodecane, 1,2-, 1,3- or 1,4-diaminocyclohexane, o-, m- or p-diaminobenzene, 3,4- or 4,4'-diaminobenzophenone, 3,4- or 4,4'-diaminodiphenyl ether, 4,4'-diaminodiphenylmethane, 4,4'-diaminodiphenyl sulfide, 3,3'- or primary polyamine compounds such as 4,4'-diaminodiphenylsulfone, 2,7-diaminofluorene, 1,5-, 1,8- or 2,3-diaminonaphthalene, 2,3-, 2,6- or 3,4-diaminopyridine, 2,4- or 2,6-diaminotoluene, m- or p-xylylenediamine, isophoronediamine, diaminomethylbicycloheptane, 1,3- or 1,4-diaminomethylcyclohexane, 2- or 4-aminopiperidine, 2- or 4-aminomethylpiperidine, 2- or 4-aminoethylpiperidine, N-aminoethylmorpholine, N-aminopropylmorpholine, etc. Monofunctional secondary amine compounds such as diethylamine, dipropylamine, di-n-butylamine, di-sec-butylamine, diisobutylamine, di-n-pentylamine, di-3-pentylamine, dihexylamine, dioctylamine, di(2-ethylhexyl)amine, methylhexylamine, diallylamine, N-methylallylamine, piperidine, pyrrolidine, diphenylamine, N-methylamine, N-ethylamine, dibenzylamine, N-methylbenzylamine, N-ethylbenzylamine, dicyclohexylamine, N-methylaniline, N-ethylaniline, dinaphthylamine, 1-methylpiperazine, and morpholine;N,N'-dimethylethylenediamine, N,N'-dimethyl-1,2-diaminopropane, N,N'-dimethyl-1,3-diaminopropane, N,N'-dimethyl-1,2-diaminobutane, N,N'-dimethyl-1,3-diaminobutane, N,N'-dimethyl-1,4-diaminobutane, N,N'-dimethyl-1,5-diaminopentane, N,N'-dimethyl-1,6-diaminohexane, N,N'-dimethyl-1,7-diaminoheptane, N,N'-diethylethylenediamine, N,N'-diethyl-1,2-diaminopropane, N,N'-diethyl-1,3-diaminopropane, N,N'-diethyl-1,2-diamino Examples include secondary polyamine compounds such as nobutane, N,N'-diethyl-1,3-diaminobutane, N,N'-diethyl-1,4-diaminobutane, N,N'-diethyl-1,5-diaminopentane, N,N'-diethyl-1,6-diaminohexane, N,N'-diethyl-1,7-diaminoheptane, piperazine, 2-methylpiperazine, 2,5-dimethylpiperazine, 2,6-dimethylpiperazine, homopiperazine, 1,1-di-(4-piperidyl)methane, 1,2-di-(4-piperidyl)ethane, 1,3-di-(4-piperidyl)propane, 1,4-di-(4-piperidyl)butane, and tetramethylguanidine.
[0038] Among the above, the active hydrogen compound (B) preferably contains a polythiol compound having two or more mercapto groups.
[0039] The content of the polythiol compound having two or more mercapto groups is preferably 60% by mass or more, more preferably 70% by mass or more, and even more preferably 80% by mass or more, based on the total mass of the active hydrogen compound (B).
[0040] Furthermore, in this disclosure, the active hydrogen compound (B) preferably contains 4-mercaptomethyl-1,8-dimercapto-3,6-dithiaoctan in an amount of 60% by mass or more, more preferably 70% by mass or more, and even more preferably 80% by mass or more, based on the total mass of the active hydrogen compound (B).
[0041] In the composition, the molar ratio of the total sum of hydroxyl groups (OH groups) and mercapto groups (SH groups) in the active hydrogen compound (B) to the isocyanate groups (NCO groups) in the polyisocyanate compound (A) (NCO groups / (OH groups + SH groups)) is preferably 0.8 to 1.2, more preferably 0.85 to 1.15, and even more preferably 0.9 to 1.1.
[0042] From the viewpoint of suppressing U-shaped striations in the resulting optical material, the absolute value V (also called viscosity difference V) of the difference between the viscosity Va of the first raw material composition 91, measured with a B-type viscometer under the conditions of 25°C and 30 rpm (revolutions per minute), and the viscosity Vb of the second raw material composition 92, measured with a B-type viscometer under the conditions of 25°C and 30 rpm, is preferably 1500 mPa·s or less, more preferably 1000 mPa·s or less, even more preferably 500 mPa·s or less, and particularly preferably 300 mPa·s or less.
[0043] While viscosity is sometimes increased to shorten polymerization time, this disclosure demonstrates that, for example, good optical quality of optical materials can be maintained even when the viscosity difference V is 10 mPa·s or more.
[0044] From the above viewpoint, the viscosity difference V may be 20 mPa·s or more, or 100 mPa·s or more. Va is the viscosity of the first raw material composition 91 before the shear force is applied, and Vb is the viscosity of the second raw material composition 92 before the shear force is applied.
[0045] The viscosity Va of the first raw material composition 91 described above, measured with a B-type viscometer at 25°C and 30 rpm, is preferably in the range of 10 mPa·s to 2000 mPa·s, more preferably in the range of 50 mPa·s to 1500 mPa·s, and even more preferably in the range of 100 mPa·s to 1000 mPa·s.
[0046] It is preferable that the first raw material composition 91 contains at least one compound selected from the group consisting of polyisocyanate compounds, epoxy compounds, and epithio compounds.
[0047] Furthermore, it is preferable that the second raw material composition 92 contains at least one active hydrogen compound selected from the group consisting of a polythiol compound having two or more mercapto groups, a hydroxythiol compound containing one or more mercapto groups and one or more hydroxyl groups, a polyol compound containing two or more hydroxyl groups, and an amine compound.
[0048] <Polymerization Catalyst> There are no particular restrictions on the polymerization catalyst, but for example, basic catalysts, organometallic catalysts, salt catalysts, zinc carbamate salts, ammonium salts, sulfonic acid, etc., can be used. One of the above polymerization catalysts may be used, or two or more may be used in appropriate combinations.
[0049] <Basic Catalysts> Examples of basic catalysts include amine-based catalysts and imidazole-based catalysts.
[0050] Specifically, examples include tertiary amine catalysts such as triethylenediamine, N,N-dimethylethanolamine, triethylamine, and N-ethylmorpholine, as well as 2-methylpyrazine, pyridine, α-picoline, β-picoline, γ-picoline, 2,6-lutidine, 3,5-lutidine, 2,4,6-collidine, 3-chlorpyridine, N,N-diethylaniline, N,N-dimethylaniline, hexamethylenetetramine, quinoline, isoquinoline, N,N-dimethyl-p-toluidine, N,N-dimethylpiperazine, quinaldine, 4-methylmorpholine, triallylamine, trioctylamine, 1,2-dimethylimidazole, and 1-benzyl-2-methylimidazole.
[0051] Among the basic catalysts mentioned above, amine-based catalysts are preferred. Examples of amine-based catalysts include tertiary amine catalysts such as 3,5-lutidine, 2,6-lutidine, 2,4,6-collidine, triethylenediamine, N,N-dimethylethanolamine, triethylamine, and N-ethylmorpholine.
[0052] The amine catalyst preferably contains at least one selected from 3,5-lutidine, 2,6-lutidine, 2,4,6-collidine, triethylenediamine, N,N-dimethylethanolamine, triethylamine, and N-ethylmorpholine.
[0053] The basic catalyst may also preferably contain a compound represented by the following general formula (2) and / or a compound represented by the following general formula (3).
[0054]
[0055] In general formula (2), R 1 R represents a linear alkyl group having 1 to 20 carbon atoms, a branched alkyl group having 3 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, or a halogen atom, and there are multiple Rs. 1 They may be the same or different. Q represents a carbon atom or a nitrogen atom. m represents an integer from 0 to 5.
[0056]
[0057] In general formula (3), R 2 , R 3 and R 4 Each of these independently represents a linear alkyl group having 1 to 20 carbon atoms, a branched alkyl group having 3 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, or an allyl group.
[0058] The basic catalyst is preferably one with a pKa value of 1 to 9, more preferably 3 to 8, and even more preferably 4 to 8.
[0059] The pKa value (acid dissociation index) can be measured, for example, by (a) the method described in The Journal of Physical Chemistry vol. 68, number 6, page 1560 (1964), (b) a method using a potentiometric automatic titrator manufactured by Kyoto Electronics Manufacturing Co., Ltd. (such as AT-610 (product name)), or (c) the acid dissociation index described in the Chemical Handbook edited by the Chemical Society of Japan (3rd revised edition, June 25, 1984, published by Maruzen Co., Ltd.).
[0060] <Organometallic Catalysts> As organometallic catalysts, there are organotin catalysts; organic acid salts such as iron, nickel, and zinc; acetylacetonate complexes; catalyst compositions composed of carboxylic acid metal compounds and quaternary ammonium salt compounds; catalyst compositions composed of bicyclic tertiary amine compounds and quaternary ammonium salt compounds; metal catalysts in which alkoxy groups, carboxy groups, etc. are coordinated to titanium or aluminum; etc.
[0061] Among the above, organotin catalysts are preferred as organometallic catalysts. Examples of organotin catalysts include dibutyltin dichloride (DBC), dimethyltin dichloride (DMC), dibutyltin dilaurate (DBTDL), dibutyltin diacetate, etc.
[0062] It is preferable that the organotin catalyst contains at least one selected from dibutyltin dichloride, dimethyltin dichloride, dibutyltin dilaurate, and dibutyltin diacetate.
[0063] <Salt Catalysts> As salt catalysts, there are salt compounds of the formula M p+ m Y q- n M is a cation selected from the group consisting of alkali metal cations, alkaline earth metal cations, transition metal cations, and ammonium ions, and Y p+ is an anion that satisfies the condition of 0.5 ≤ pKa ≤ 14 for the corresponding acid YH q- where m, n, p, and q in the formula satisfy n×q = m×p. As M (q-1)- for example, there are Li p+ + , Na + , K + , Cs + , Mg 2+ , Ca 2+ , Mn 2+ , Ag + , Ba 2+ , and Al 3+ , etc. As Y q- for example, there is thiocyanate ion (SCN - -Examples include acetylacetonate, acetate ions, thioacetate ions, formate ions, and benzoate ions.
[0064] The polymerization catalyst preferably includes at least one selected from the group consisting of basic catalysts with a pKa value of 4 to 8 and organometallic catalysts. The polymerization catalyst may also preferably include at least one selected from amine catalysts and organotin catalysts.
[0065] The polymerization catalyst may also preferably include at least one selected from the group consisting of 3,5-lutidine, 2,6-lutidine, 2,4,6-collidine, triethylenediamine, N,N-dimethylethanolamine, triethylamine, N-ethylmorpholine, dibutyltin dichloride, dimethyltin dichloride, dibutyltin dilaurate, and dibutyltin diacetate.
[0066] The first raw material composition 91 and the second raw material composition 92 together comprise, for example, 100 parts by mass of two or more different monomers for optical materials and 0.01 to 2.0 parts by mass of a polymerization catalyst.
[0067] In other words, in this embodiment, 0.01 to 2.0 parts by mass of polymerization catalyst are used for a total of 100 parts by mass of two or more different monomers for optical materials. As described above, the amount of polymerization catalyst used in this disclosure is large compared to conventional methods for producing optical materials.
[0068] This allows the reaction heat of the polymerizable composition 93 to be generated in a short time when polymerizing the monomers for optical materials in the polymerizable composition 93. By further utilizing this reaction heat for polymerization, the polymerization reaction can be effectively promoted, and high-quality optical materials with suppressed striations can be obtained in a shorter time than conventional methods.
[0069] By using 0.01 parts by mass or more of polymerization catalyst with 100 parts by mass of two or more different monomers for optical materials, the polymerization reaction can be effectively promoted, allowing for the production of high-quality optical materials with suppressed striations in a short time. Furthermore, by effectively promoting the polymerization reaction, the release properties when removing the cured product from the mold can be improved.
[0070] From the above viewpoint, it is preferable to use 0.015 parts by mass or more of polymerization catalyst per 100 parts by mass of two or more different monomers for optical materials, more preferably 0.038 parts by mass or more, even more preferably 0.10 parts by mass or more, and particularly preferably 0.17 parts by mass or more.
[0071] <Other Ingredients> The composition of this embodiment may further contain ultraviolet absorbers, antioxidants, light stabilizers, sensitizers, mold release agents, solvents, bluing agents, IR cutters, blue light cutters, organic acids, reactive diluents, oil-soluble dyes, pigments, dyes, fragrances, fillers, adhesion enhancers such as coupling agents, chain extenders, crosslinking agents, defoamers, anti-settling agents, dispersants, plasticizers, anti-sagging agents, antifouling agents, preservatives, bactericides, antifungal agents, antifungal agents, matting agents, thickeners, pigment dispersants, anti-repellent agents, scratch-resistant enhancers, slip agents, surface modifiers, color separation preventatives, emulsifiers, anti-skinning agents, drying agents, antistatic agents, conductive agents (electrostatic additives), flame retardants, thermal conductivity improvers, ion exchange resins, etc.
[0072] Examples of release agents include acidic phosphate ester compounds, polyether-modified silicones, alkyl-modified silicones, polyester-modified silicones, dimethylpolysiloxane, polyoxyalkylene glycol monoalkyl ether compounds, polyoxyalkylene glycol monoester compounds, fluorine atom-containing compounds, surfactants, nonionic surfactants, acrylic surfactants, and the like.
[0073] Examples of UV absorbers include: benzophenone-based UV absorbers such as 2,2'-dihydroxy-4-methoxybenzophenone; triazine-based UV absorbers such as 2-[4-[(2-hydroxy-3-dodecyloxypropyl)oxy]-2-hydroxyphenyl]4,6-bis(2,4-dimethylphenyl)-1,3,5-triazine; and benzotriazole-based UV absorbers such as 2-(2H-benzotriazole-2-yl)-4-methylphenol and 2-(2H-benzotriazole-2-yl)-4-tert-octylphenol. There may be one UV absorber or two or more.
[0074] Examples of organic acids include methanesulfonic acid, trifluoromethanesulfonic acid, benzenesulfonic acid, p-toluenesulfonic acid, 10-camphorsulfonic acid, and trifluoroacetic acid.
[0075] <First Supply Device 11> The first supply device 11 is a device that supplies the first raw material composition 91 to the mixing device 14. As shown in Figure 1, the first supply device 11 includes, as an example, a first tank 30, a first pipe 31, a first valve 34, a first connecting pipe 35, a connecting pipe 27, and a first flow rate adjustment unit 39.
[0076] The first tank 30 is a tank that contains the first raw material composition 91. The first pipe 31 is a pipe for supplying the first raw material composition 91 from the first tank 30 to the mixing device 14. One end of the first pipe 31 is connected to the first tank 30, and the other end is connected to the first connecting pipe 35.
[0077] The first connecting pipe 35 has one end connected to the other end of the first pipe 31. The other end of the first connecting pipe 35 is connected to one end of the connecting pipe 27. The first connecting pipe 35 and the connecting pipe 27 are, for example, T-shaped pipes.
[0078] The first flow rate adjustment unit 39 is a component that adjusts the flow rate of the first raw material composition 91 supplied from the first tank 30 to the mixing device 14. Specifically, the first flow rate adjustment unit 39 includes, for example, a first pump 32 and a first flow meter 33.
[0079] The first pump 32 is a pump that transfers the first raw material composition 91 to the mixing device 14. This first pump 32 is installed in the first pipe 31. The specific configuration of the first pump 32 will be described later.
[0080] The first flow meter 33 is a measuring unit that measures the flow rate of the first raw material composition 91 being transported through the first pipe 31. This first flow meter 33 is located in the first pipe 31 on the downstream side of the first pump 32.
[0081] The first valve 34 is a valve that opens and closes the flow path of the first pipe 31. This first valve 34 is located in the first pipe 31 on the downstream side of the first flow meter 33.
[0082] In the first supply device 11, with the first valve 34 open, the first pump 32 supplies the first raw material composition 91 from the first tank 30 to the mixing device 14 through the first pipe 31, the first connecting pipe 35, and the connecting pipe 27 (see Figure 1). The first flow rate adjustment unit 39 adjusts the flow rate of the first raw material composition 91 supplied to the mixing device 14 by controlling the first pump 32 based on the measurement results of the first flow meter 33.
[0083] <Second Supply Device 12> The second supply device 12 is a device that supplies the second raw material composition 92 to the mixing device 14. As shown in Figure 1, the second supply device 12 includes, for example, a second tank 20, a second pipe 21, a second valve 24, a second connecting pipe 25, a connecting pipe 27, and a second flow rate adjustment unit 29. It can be understood that the connecting pipe 27 is a component common to both the first supply device 11 and the second supply device 12.
[0084] The second tank 20 is a tank that contains the second raw material composition 92. The second pipe 21 is a pipe for supplying the second raw material composition 92 from the second tank 20 to the mixing device 14. One end of the second pipe 21 is connected to the second tank 20, and the other end is connected to the second connecting pipe 25.
[0085] The second connecting pipe 25 has one end connected to the other end of the second pipe 21. The other end of the second connecting pipe 25 is connected to one end of the connecting pipe 27. The second connecting pipe 25 is, for example, made up of a T-shaped pipe.
[0086] The second flow rate adjustment unit 29 is a component that adjusts the flow rate of the second raw material composition 92 supplied from the second tank 20 to the mixing device 14. Specifically, the second flow rate adjustment unit 29 includes, for example, a second pump 22 and a second flow meter 23.
[0087] The second pump 22 is a pump that transfers the second raw material composition 92 to the mixing device 14. This second pump 22 is installed in the second pipe 21. The specific configuration of the second pump 22 will be described later.
[0088] The second flow meter 23 is a measuring unit that measures the flow rate of the second raw material composition 92 being transported through the second pipe 21. This second flow meter 23 is located in the second pipe 21 on the downstream side of the second pump 22.
[0089] The second valve 24 is a valve that opens and closes the flow path of the second pipe 21. This second valve 24 is located in the second pipe 21 on the downstream side of the second flow meter 23.
[0090] In the second supply device 12, with the second valve 24 open, the second pump 22 supplies the second raw material composition 92 from the second tank 20 to the mixing device 14 through the second pipe 21, the second connecting pipe 25, and the connecting pipe 27 (see Figure 1). The second flow rate adjustment unit 29 adjusts the amount of the second raw material composition 92 supplied to the mixing device 14 by controlling the second pump 22 based on the measurement results of the second flow meter 23.
[0091] <Specific Configuration of the First Pump 32 and the Second Pump 22> The first pump 32 is an example of the first transfer unit. The second pump 22 is an example of the second transfer unit. Since the first pump 32 and the second pump 22 are configured similarly, the specific configuration of the first pump 32 will be described here. Figure 2 is a side cross-sectional view showing the first pump 32.
[0092] For example, the first pump 32 is a positive displacement screw pump, such as a positive displacement rotary pump. Specifically, for example, the first pump 32 is a positive displacement single-screw pump, such as a positive displacement screw pump.
[0093] The first pump 32, which is a positive displacement single-screw eccentric pump, has a cylinder 50, a screw 53, and a rotary drive mechanism 54, as shown in Figure 2.
[0094] The cylinder 50 constitutes the main body of the first pump 32. Specifically, the cylinder 50 includes, for example, a case 51 and a stator 52. The case 51 is formed in a cylindrical shape (specifically, a cylindrical shape). A first opening 51A is provided at one axial end of the case 51. A second opening 51B is provided on the outer circumference of the other axial end of the case 51. One of the first opening 51A and the second opening 51B is connected to the first tank 30, and the other of the first opening 51A and the second opening 51B is connected to the mixing device 14. One of the first opening 51A and the second opening 51B functions as an inlet through which the first raw material composition 91 flows into the case 51, and the other of the first opening 51A and the second opening 51B functions as an outlet through which the first raw material composition 91 flows out of the case 51.
[0095] The stator 52 is positioned in contact with the case 51. The stator 52 is formed in a cylindrical shape (specifically, a cylindrical shape) with an internal bore 52A that acts as an internal thread. The internal bore 52A is formed in a spiral shape that rotates around the axial direction of the stator 52.
[0096] The screw 53 is a helical male thread housed in the inner bore 52A. The screw 53 is made of a metal material such as stainless steel. The screw 53 is, for example, a single-start thread with a perfectly circular cross-section (see Figure 3).
[0097] The stator 52 is formed of an elastic material such as rubber. The stator 52 is, for example, a double-start screw with an oval spatial cross-section (see Figure 3). That is, the inner bore 52A is formed with an oval cross-sectional shape. Furthermore, the cross-sectional area of the inner bore 52A is constant in any cross section perpendicular to the axial direction of the stator 52.
[0098] As the screw 53 is housed in the inner bore 52A of the stator 52, a series of independent sealed spaces (hereinafter referred to as cavities) are formed between the outer surface of the screw 53 and the inner surface of the inner bore 52A.
[0099] The screw 53 has a shape in which spheres are continuous in the spiral direction. As a result, the screw 53 has no corners (edges), is rounded, and the entire shape is enclosed by a curved surface.
[0100] Similarly, the inner bore 52A of the stator 52 also has a shape in which the spheres are continuous in the spiral direction. As a result, the inner circumferential surface of the inner bore 52A has no corners (edges) and is rounded, making the entire surface curved.
[0101] Therefore, the contact portions of the screw 53 and stator 52 with the first raw material composition 91 are rounded and have no sharp edges, and the entire surface is curved. Note that the spheres in this context do not need to be perfectly round.
[0102] The rotational drive mechanism 54 is a mechanism that rotates the screw 53 and, in conjunction with this rotation, reciprocates it in the radial direction of the cylinder 50 (specifically, the stator 52). In this way, the rotational drive mechanism 54 causes the screw 53 to rotate eccentrically by reciprocating it in the radial direction of the stator 52.
[0103] Specifically, the rotational drive mechanism 54 includes a drive unit 54A, such as a drive motor, and a transmission mechanism 54B that transmits power from the drive unit 54A to the screw 53. For example, a drive motor such as a stepping motor or a servo motor can be used as the drive unit 54A.
[0104] The transmission mechanism 54B includes, for example, a drive shaft and elements such as a universal joint for a flexible rod. The universal joint has the function of following the displacement caused by the eccentric rotation of the screw 53.
[0105] The rotary drive mechanism 54 rotates the screw 53 eccentrically, causing it to reciprocate in the longitudinal direction of the oval spatial cross-section (i.e., the inner bore 52A) of the stator 52, as shown in Figures 3(A), (B), and (C). This generates new cavities one after another in the axial direction of the stator 52. As new cavities are generated, an attractive force is created, and the first raw material composition 91 is transported in the axial direction of the stator 52. Depending on the rotation direction of the screw 53, the transport direction can be appropriately set to either the direction from the first opening 51A to the second opening 51B or the direction from the second opening 51B to the first opening 51A.
[0106] <Various settings for the first pump 32 and the second pump 22> The rotational speed of the screw 53 in the first pump 32 and the second pump 22 is 20 to 300 rpm. For example, by controlling the drive unit 54A of the rotary drive mechanism 54, the rotational speed of the screw 53 is set to the range of 20 to 300 rpm.
[0107] In this embodiment, the maximum shear stress in each of the first pump 32 and the second pump 22 is, for example, 3500 Pa or less. For example, the maximum shear stress is set to 3500 Pa or less by the shape of the screw 53 and the inner bore 52A of the stator 52, and the rotational speed of the screw 53. Preferably, the maximum shear stress is set in the range of 200 to 3500 Pa.
[0108] The "maximum shear stress / fluid delivery rate" in each of the first pump 32 and the second pump 22 is 500 Pa / (g·s). -1 ) or less. The "maximum shear stress / fluid delivery rate" is preferably 50 to 500 Pa / (g·s) -1 It is set within the range of ). Note that "maximum shear stress / fluid delivery rate" is the value obtained by dividing the maximum shear stress by the fluid delivery rate. Also, the fluid delivery rate is an example of a transfer rate.
[0109] In this embodiment, "maximum shear stress applied to the transport object" refers to the maximum value of the shear stress generated in the transport object (i.e., the first raw material composition 91 or the second raw material composition 92) in the transport space in which the transport object is transported.
[0110] Here, the maximum shear stress is calculated, for example, using computational fluid dynamics (CFD) analysis.
[0111] Specifically, the maximum shear stress is calculated, for example, by the following procedure. First, a three-dimensional geometric model of the wetted parts of the transfer section (pump chamber, flow path, etc.) is created and imported into general-purpose fluid analysis software. Next, the actual transfer conditions (viscosity, density, transfer rate, operating conditions of movable members, etc.) are set in the software, and the Navier-Stokes equations, which are the fluid transport equations, are numerically analyzed.
[0112] Then, from the shear stress distribution within the transport section obtained through analysis, the maximum value of the shear stress applied to the transported object, extracted in the region where physical force is concentrated on the transported object (for example, near the gap between movable members such as screws, gears, and valve bodies, and fixed members such as cylinders and cases), is defined as the "maximum shear stress" in this embodiment.
[0113] In the above analysis, the fluid analysis software can be, for example, FLUENT from Ansys, or other commercially available analysis codes using finite volume methods. Furthermore, as analysis conditions, for example, a laminar flow model without a turbulent flow model, or transient calculations can be applied.
[0114] In this embodiment, "liquid delivery rate" refers to the mass of the fluid being transferred per unit time by the transfer unit, i.e., the mass flow rate.
[0115] The "liquid delivery rate" is calculated, for example, by the following procedure. First, the transfer material being delivered from the transfer unit is made available for collection at the discharge side of the transfer unit (for example, at any position in the flow path connecting the transfer unit and the mixing unit). Next, the transfer unit is operated under predetermined operating conditions, and the transfer material is collected into a container or the like for a predetermined time (collection time). Then, the mass (g) of the collected transfer material is measured, and the value obtained by dividing this mass by the collection time (s) is taken as the "liquid delivery rate" in this embodiment.
[0116] Furthermore, if a measuring instrument such as a mass flow meter is installed in the flow path, the value measured by that instrument may be used as the fluid delivery rate.
[0117] The transfer performance of the first pump 32 and the second pump 22 is 0.8 to 15 ml / rev. For example, the transfer performance is set to the range of 0.8 to 15 ml / rev by the shape of the inner bore 52A of the screw 53 and stator 52, and the rotational speed of the screw 53. Note that "ml / rev" is a unit that indicates the flow rate that can be transferred per rotation of the screw 53.
[0118] In the arrangement range of the screw 53 in the cylinder 50 (inner bore 52A of the stator 52), the inner diameter D1 is 10 to 270 mm, the length L1 is 18 to 5000 mm, and L1 / D1 is 1.8 to 18.6.
[0119] In the area where the screw 53 is positioned in the cylinder 50 (the inner bore 52A of the stator 52), the volume A1 of the transfer space is 30-80% of the volume A2 inside the cylinder 50. Volume A2 is the volume of the inner bore 52A when the screw 53 is not positioned. Volume A1 is the volume of the inner bore 52A when the screw 53 is positioned.
[0120] The temperature of the first raw material composition 91 and the second raw material composition 92 flowing inside the cylinder 50 is 10 to 50°C. For example, the temperatures of the first raw material composition 91 and the second raw material composition 92 are set to a temperature range of 10 to 50°C by a temperature adjustment unit capable of cooling and heating each of them. The temperature adjustment unit adjusts the temperature of the first raw material composition 91 to the aforementioned temperature range in at least one of the first tank 30, the first pipe 31, and the first pump 32. The temperature adjustment unit also adjusts the temperature of the second raw material composition 92 to the aforementioned temperature range in at least one of the second tank 20, the second pipe 21, and the second pump 22.
[0121] The viscosity of the first raw material composition 91 and the second raw material composition 92 flowing inside the cylinder 50 is 30 to 1000 mPa·s. For example, the viscosity of the first raw material composition 91 and the second raw material composition 92 is set to the range of 30 to 1000 mPa·s depending on the composition of the first raw material composition 91 and the second raw material composition 92 and the temperature.
[0122] <Modified Examples of the First Pump 32 and the Second Pump 22> In this embodiment, the first pump 32, which is a positive displacement single-screw eccentric pump, is used as an example of the first transfer unit, and the second pump 22, which is a positive displacement single-screw eccentric pump, is used as an example of the second transfer unit, but the embodiment is not limited to these.
[0123] Examples of the first and second transfer sections of this disclosure may include other positive displacement screw pumps (e.g., twin-screw pumps and triple-screw pumps). Alternatively, examples of the first and second transfer sections of this disclosure may include other positive displacement rotary pumps (e.g., roller pumps). Furthermore, examples of the first and second transfer sections of this disclosure may include other positive displacement pumps (e.g., diaphragm pumps).
[0124] Furthermore, as an example of the first and second transfer sections of this disclosure, a transfer mechanism may be used in which the object to be transferred (specifically, the first raw material composition 91 or the second raw material composition 92) is filled into a container such as a cylinder, and the object to be transferred is pumped using a gas such as an inert gas. Examples of such gases include nitrogen, argon, helium, or dry air. In addition to a method of directly pressurizing the object to be transferred with the pressure of the gas, a method may also be used in which a partition wall such as a slidable piston is provided inside the cylinder, and back pressure of the gas is applied to the back surface of the partition wall (the surface that does not come into contact with the object to be transferred), thereby pushing the object to be transferred through the partition wall.
[0125] In this embodiment, both the first and second transfer units were pumps having the aforementioned cylinder 50, screw 53, and rotary drive mechanism 54 (for example, positive displacement single-screw pumps), but the invention is not limited to these. The first and second transfer units in this disclosure do not need to be transfer mechanisms of the same type; at least one of them may be a pump having the aforementioned cylinder 50, screw 53, and rotary drive mechanism 54 (for example, a positive displacement single-screw pump). In this case, the other of the first and second transfer units may be a pump that does not have the aforementioned configuration (for example, a gear pump, a diaphragm pump, or other type of pump).
[0126] In this embodiment, in both the first and second transfer sections, the "maximum shear stress / liquid transfer rate" is 500 Pa / (g·s). -1 ) or less, but not limited to this. In at least one of the first and second transfer sections of this disclosure, the "maximum shear stress / liquid transfer rate" is 500 Pa / (g·s -1 It is sufficient if it is as follows:
[0127] <Mixing device 14> The mixing device 14 is an example of a mixing unit and is a device for mixing the first raw material composition 91 and the second raw material composition 92. As shown in Figure 1, this mixing device 14 has a container 40 and a mixing member 42.
[0128] <Container 40> Container 40 contains the first raw material composition 91 and the second raw material composition 92 supplied inside. In container 40, for example, the first raw material composition 91 and the second raw material composition 92 are flowed in a predetermined flow direction (specifically downwards). This flow direction can also be described as the direction along the longitudinal direction (i.e., the axial direction) of container 40.
[0129] The container 40 is formed, for example, in a cylindrical shape (specifically, a cylindrical shape). The container 40 has, for example, an inner diameter that is constant along the axial direction. Inside the container 40, a mixing member 42 is provided, as shown in Figure 1.
[0130] In this embodiment, the container 40 has a peripheral wall 40A, a bottom wall 40B, and an upper wall 40C. The peripheral wall 40A is formed in a cylindrical shape with the vertical direction as the axial direction (hereinafter referred to as the container axial direction).
[0131] The upper wall 40C is provided at one end (specifically the upper end) of the peripheral wall 40A in the container axial direction. This upper wall 40C is formed in a circular shape when viewed in the container axial direction. The upper wall 40C is provided with a supply port 41 through which the first raw material composition 91 and the second raw material composition 92 are supplied into the inside of the container 40.
[0132] The other end of a T-shaped connecting pipe 27 is connected to the supply port 41. As a result, the first connecting pipe 35 and the second connecting pipe 25 are connected to the supply port 41 via the connecting pipe 27. The first raw material composition 91 from the first tank 30 is supplied from the supply port 41 into the container 40 through the first pipe 31, the first connecting pipe 35, and the connecting pipe 27. Therefore, in this embodiment, the first pipe 31, the first connecting pipe 35, and the connecting pipe 27 function as the first supply route for the supply of the first raw material composition 91. The second raw material composition 92 from the second tank 20 is supplied from the supply port 41 into the container 40 through the second pipe 21, the second connecting pipe 25, and the connecting pipe 27. Therefore, in this embodiment, the second pipe 21, the second connecting pipe 25, and the connecting pipe 27 function as the second supply route for the supply of the second raw material composition 92.
[0133] The supply port 41 is located above the upper end of the mixing member 42. Therefore, the first raw material composition 91 and the second raw material composition 92 are supplied into the container 40 from above the upper end of the mixing member 42.
[0134] The bottom wall 40B is provided at the other end (specifically, the lower end) of the peripheral wall 40A in the direction of the container axis. This bottom wall 40B is formed in a circular shape when viewed in the direction of the container axis. The bottom wall 40B is provided with an outlet 46 for discharging the mixture of the first raw material composition 91 and the second raw material composition 92 (hereinafter simply referred to as "mixture") from inside the container 40. Therefore, the outlet 46 is located below the supply port 41.
[0135] Furthermore, the outlet 46 is located below the lower end of the mixing member 42. Therefore, the mixture is discharged from inside the container 40 below the lower end of the mixing member 42. A discharge pipe 47 through which the mixture flows is connected to the outlet 46.
[0136] In container 40, the first raw material composition 91 and the second raw material composition 92, supplied to the interior through the supply port 41, are made to flow downward toward the discharge port 46. That is, each of the first raw material composition 91 and the second raw material composition 92 is supplied to the interior of container 40 from the supply port 41 located at the top of container 40, flows downward while being mixed inside container 40, and is discharged from the discharge port 46 located at the bottom of container 40.
[0137] In this embodiment, the inner diameter of the container 40 was constant along the axial direction, but this is not limited to this. For example, the inner diameter of the container 40 may be tapered so that it becomes narrower downstream, and the tube of this disclosure can be any tube through which the first raw material composition 91 and the second raw material composition 92 can flow.
[0138] <Mixing Member 42> As shown in Figure 1, the mixing member 42 is provided inside the container 40 along the longitudinal direction (i.e., the axial direction) of the container 40. The mixing member 42 is composed of, for example, blades formed in a spiral shape that are twisted around the axial direction of the container 40.
[0139] In the mixing device 14, the first raw material composition 91 and the second raw material composition 92 supplied to one end of the container 40 flow toward the other end of the container 40 along the blades of the mixing member 42, repeatedly separating and merging while swirling in one and the other circumferential direction. This generates turbulence in the first raw material composition 91 and the second raw material composition 92 flowing inside the container 40, and the first raw material composition 91 and the second raw material composition 92 are mixed. Turbulence is a flow in which the various parts of a fluid mix irregularly as they flow.
[0140] In this embodiment, the mixing member 42 mixes the first raw material composition 91 and the second raw material composition 92 while stationary, without being driven to rotate. The mixing device 14 does not have a drive unit to rotate the mixing member 42, and the mixing member 42 statically mixes the first raw material composition 91 and the second raw material composition 92.
[0141] The mixing device 14 was a so-called static mixer that statically mixed the first raw material composition 91 and the second raw material composition 92 without the mixing member 42 being driven to rotate, but it is not limited to this. The mixing device 14 may also be a so-called power mixer that dynamically mixes the first raw material composition 91 and the second raw material composition 92 by driving the mixing member 42 to rotate.
[0142] <Agitator 17> The agitator 17 is an example of an agitator, and is a device that agitates the mixture mixed in the mixing device 14 using a driving force. Specifically, as shown in Figure 1, the agitator 17 has an agitator tank 70, an agitator member 72, and a drive unit 73.
[0143] The stirring tank 70 is a container that holds a mixture of the first raw material composition 91 and the second raw material composition 92. The stirring tank 70 is connected to the discharge pipe 47 of the mixing device 14 by a connecting pipe 78. As a result, the mixture discharged from the container 40 of the mixing device 14 is supplied to the stirring tank 70 through the connecting pipe 78. In this embodiment, a filter for filtering the mixture is not provided in the connecting pipe 78. That is, the container 40 of the mixing device 14 and the stirring tank 70 are arranged in series without a filter in between.
[0144] The stirring member 72 is a component that stirs the mixture contained in the stirring tank 70. The stirring member 72 has a shaft 72A and a stirring blade 72B. The shaft 72A extends in the vertical direction. The stirring blade 72B is provided at the lower end of the shaft 72A.
[0145] The drive unit 73 is positioned above the stirring tank 70. This drive unit 73 is, for example, a motor that rotates the shaft 72A of the stirring member 72.
[0146] In the stirring device 17, the drive unit 73 rotates the shaft 72A of the stirring member 72, thereby rotating the stirring blade 72B and stirring the mixture contained in the stirring tank 70. In this way, the mixture of the first raw material composition 91 and the second raw material composition 92 is stirred to produce the polymerizable composition 93 for optical materials. The polymerizable composition 93 for optical materials, as described above, contains, for example, two or more different monomers for optical materials and the polymerization catalyst described above.
[0147] Therefore, in this embodiment, the manufacturing apparatus for producing the polymerizable composition 93 for optical materials is comprised of a first supply device 11, a second supply device 12, a mixing device 14, and a stirring device 17.
[0148] <Filter device 60> The filter device 60 is an example of a filter and is a device for filtering the mixture (i.e., the polymerizable composition 93 for optical materials) stirred by the stirring device 17. The filter device 60 is located downstream of the stirring device 17 and is supplied with the polymerizable composition 93 for optical materials from the stirring device 17.
[0149] Specifically, the filter device 60 includes a filter container 62 and a filter 64. The filter container 62 is a container for holding the polymerizable composition 93 for optical materials. This filter container 62 is connected to the stirring tank 70 in the stirring device 17 by a connecting pipe 68. As a result, the polymerizable composition 93 for optical materials, which has been stirred in the stirring tank 70 of the stirring device 17, is supplied from the stirring tank 70 to the filter container 62 through the connecting pipe 68.
[0150] In the filter container 62, the polymerizable composition 93 for optical materials supplied to the interior through the connecting pipe 68 is allowed to flow downward. The filter 64 is located inside the filter container 62 and filters the polymerizable composition 93 for optical materials that is flowing downward inside the filter container 62.
[0151] <Casting device 18> The casting device 18 is a device for casting the polymerizable composition 93 for optical materials, which has been filtered by the filter device 60, into a mold 84. A static mixer is used as an example in the casting device 18.
[0152] As shown in Figure 1, the casting device 18 is connected to the filter container 62 of the filter device 60 by a connecting pipe 88. As a result, the polymerizable composition 93 for optical materials filtered in the filter container 62 of the filter device 60 is supplied from the filter container 62 to the casting device 18 through the connecting pipe 88. The casting device 18 then pours the polymerizable composition 93 for optical materials into the mold 84 while stirring it.
[0153] In this embodiment, the connecting pipe 88 has branching pipes 88A that branch into multiple pipes. Each of the multiple branching pipes 88A is connected to each of the multiple casting devices 18. Each of the multiple branching pipes 88A is provided with a valve 89 that opens and closes the flow path of the branching pipe 88A. In this embodiment, with one valve 89 open and the other valves 89 closed, the material is supplied from the filter container 62 to the casting device 18. This allows the polymerizable composition 93 for optical materials to be selectively cast into the mold 84.
[0154] <Curing device 19> The curing device 19 is an example of a curing unit and is a device for producing optical materials by curing a polymerizable composition 93 for optical materials, which is cast in the casting device 18, by polymerizing two or more different monomers for optical materials in the polymerizable composition 93 for optical materials. As shown in Figure 1, the curing device 19 is, for example, a heater having a heating chamber 19A.
[0155] In the curing apparatus 19, a mold 84 into which the polymerizable composition 93 for optical materials has been poured is placed in the heating chamber 19A, and the polymerizable composition 93 for optical materials is heated to polymerize the two or more different monomers for optical materials in the polymerizable composition 93. This cures the polymerizable composition 93 for optical materials and produces an optical material.
[0156] <Applications of Optical Materials> The optical materials manufactured by the manufacturing system 10 can be used in plastic lenses, prisms, optical fibers, information recording substrates, filters, light-emitting diodes, etc. Among these, the optical materials can be suitably used in plastic lenses, and are particularly suitably used in plastic lenses for eyeglasses.
[0157] <Method for Manufacturing Optical Materials> The method for manufacturing optical materials is a method for manufacturing optical materials and is performed using the manufacturing system 10 described above. This manufacturing method includes a method for manufacturing polymerizable compositions for optical materials (hereinafter referred to as the composition manufacturing method), and comprises a preparation step, a first transfer step, a second transfer step, a mixing step, a stirring step, a filtration step, a casting step, and a curing step. The composition manufacturing method is a method for manufacturing polymerizable compositions for optical materials, which involves mixing a first raw material composition 91 and a second raw material composition 92 to produce a polymerizable composition 93 for optical materials containing two or more different monomers for optical materials and a polymerization catalyst. The composition manufacturing method comprises a preparation step, a first transfer step, a second transfer step, a mixing step, and a stirring step. The steps of this manufacturing method, including the composition manufacturing method, will be described below.
[0158] <Preparation Process> In the preparation process, the aforementioned manufacturing system 10 including the mixing device 14, the aforementioned first raw material composition 91, and the aforementioned second raw material composition 92 are prepared.
[0159] <First Transfer Process> In the first transfer process, the first raw material composition 91 is transferred to the mixing device 14 by the first pump 32. Specifically, in the first transfer process, with the first valve 34 open, the drive unit 54A of the first pump 32 is driven to transfer the first raw material composition 91 from the first tank 30 into the container 40 of the mixing device 14 through the first pipe 31, the first connecting pipe 35, and the connecting pipe 27. The first transfer process can also be described as a supply process in which the first supply device 11 supplies the first raw material composition 91 to the mixing device 14.
[0160] <Second Transfer Process> In the second transfer process, the second pump 22 transfers the second raw material composition 92 to the mixing device 14. Specifically, in the second transfer process, with the second valve 24 open, the drive unit 54A of the second pump 22 is driven to transfer the second raw material composition 92 from the second tank 20 into the container 40 of the mixing device 14 through the second pipe 21, the second connecting pipe 25, and the connecting pipe 27. The second transfer process can also be described as a supply process in which the second supply device 12 supplies the second raw material composition 92 to the mixing device 14.
[0161] <Mixing Process> In the mixing process, the first raw material composition 91 supplied into the container 40 in the first transfer process and the second raw material composition 92 supplied into the container 40 in the second transfer process are mixed in the mixing device 14. Specifically, in the mixing process, the first raw material composition 91 and the second raw material composition 92 are allowed to flow downwards inside the container 40, and the mixing member 42 of the mixing device 14 generates turbulence in the first raw material composition 91 and the second raw material composition 92, thereby statically mixing the first raw material composition 91 and the second raw material composition 92. In other words, in the mixing process, the first raw material composition 91 and the second raw material composition 92 flowing through the container 40 are mixed by the mixing member 42 without using any driving force.
[0162] <Agitation Process> In the agitation process, the mixture of the first raw material composition 91 and the second raw material composition 92, which were mixed in the mixing process, is agitated using a stirring device 17. Specifically, in the agitation process, the drive unit 73 of the stirring device 17 rotates the shaft 72A of the stirring member 72, thereby rotating the stirring blade 72B and agitating the mixture contained in the stirring tank 70. This produces the polymerizable composition 93 for optical materials.
[0163] When transferring the mixture from the mixing process to the stirring process, methods such as using an inert gas to pressurize the mixture or using a pump can be used.
[0164] <Filtration Process> In the filtration process, the polymerizable composition 93 for optical materials is filtered using a filter device 60. Specifically, in the filtration process, the polymerizable composition 93 for optical materials supplied into the filter container 62 is flowed downwards, and the polymerizable composition 93 for optical materials is filtered by a filter 64 provided inside the filter container 62.
[0165] <Casting Process> In the casting process, the polymerizable composition 93 for optical materials, which has been filtered in the filtration process, is cast into a mold using a casting device 18. Specifically, in the casting process, the casting device 18 casts the polymerizable composition 93 for optical materials into the mold 84 while stirring it.
[0166] <Curing Process> In the curing process, the polymerizable composition 93 for optical materials, which was cast into the mold 84 in the casting process, is cured using a curing apparatus 19. Specifically, the mold 84 into which the polymerizable composition 93 for optical materials was cast is placed in the heating chamber 19A, and the polymerizable composition 93 for optical materials is heated to polymerize and cure the two or more different monomers for optical materials in the polymerizable composition 93. In the curing process, the polymerizable composition for optical materials obtained by the method for manufacturing the polymerizable composition for optical materials is polymerized and cured to produce an optical material.
[0167] <Effects of this embodiment> In the composition manufacturing method, in the first transfer step, the first raw material composition 91 is transferred to the mixing device 14 by the first pump 32. In the second transfer step, the second raw material composition 92 is transferred to the mixing device 14 by the second pump 22.
[0168] The first pump 32 and the second pump 22 use a transfer rate that calculates the maximum shear stress applied to the material being transferred (specifically, the first raw material composition 91 or the second raw material composition 92) to 500 Pa / (g·s). -1 The following is the result. This makes it possible to suppress the shear stress applied when transporting the object to be transported so that it does not become excessive relative to the transport speed. As a result, the localized load on the object to be transported during the transport process can be reduced, and gel generation can be effectively suppressed.
[0169] Furthermore, in this embodiment, the first pump 32 and the second pump 22 each have a helical screw 53 positioned inside the cylinder 50 along the axial direction of the cylinder 50, and a rotational drive mechanism 54 that rotates the screw 53 and reciprocates it in the radial direction of the cylinder 50 as a result of the rotation.
[0170] If gear pumps are used as the first pump 32 and the second pump 22, shear stress is likely to occur in the first raw material composition 91 and the second raw material composition 92, as follows. In other words, in a gear pump, when a pair of gears rotate while meshing, fluid is drawn into the gap between the teeth and the case and sent through the gap between the gears, so shear stress is likely to occur in the first raw material composition 91 and the second raw material composition 92.
[0171] In contrast, in the composition manufacturing method, as described above, the first raw material composition 91 and the second raw material composition 92 are transported by the first pump 32 and the second pump 22, each of which has a rotating screw 53 that reciprocates radially in the cylinder 50 in conjunction with the rotation. Therefore, compared to the case in which a gear pump is used, the shear stress applied to the first raw material composition 91 and the second raw material composition 92 is suppressed. As a result, the setting conditions for the first pump 32 and the second pump 22 (specifically, the value of maximum shear stress / transfer speed) can be easily and stably achieved, and the gel generation suppression effect can be enhanced.
[0172] Furthermore, in this embodiment, the maximum shear stress in each of the first pump 32 and the second pump 22 is 3500 Pa or less. Therefore, gel generation is suppressed when transferring the first raw material composition and the second raw material composition, respectively. The maximum shear stress is preferably set in the range of 200 to 3500 Pa. When the maximum shear stress is 200 Pa or more, the efficiency of transferring the first raw material composition 91 and the second raw material composition 92 is increased.
[0173] Furthermore, in this embodiment, the rotational speed of the screw 53 in each of the first pump 32 and the second pump 22 is 20 to 300 rpm. Thus, in this embodiment, since the rotational speed is 20 rpm or more, the efficiency of transferring the first raw material composition 91 and the second raw material composition 92 is increased. Also, in this embodiment, since the rotational speed is 300 rpm or less, the shear stress applied to each of the first raw material composition 91 and the second raw material composition 92 is suppressed. As a result, gel generation is suppressed when transferring each of the first and second raw material compositions.
[0174] Furthermore, in this embodiment, the first pump 32 and the second pump 22 are each positive displacement single-screw pumps. Therefore, the first pump 32 and the second pump 22 can suppress the shear stress applied to the first raw material composition 91 and the second raw material composition 92, respectively, compared to other positive displacement rotary pumps, including gear pumps. As a result, gel generation is suppressed when transferring the first raw material composition and the second raw material composition, respectively.
[0175] Furthermore, in this embodiment, in both the first pump 32 and the second pump 22, the screw 53 has a shape in which the spheres are continuous in the helical direction. Therefore, compared to the case where the screw 53 has a shape with corners (edges), the shear stress applied to each of the first raw material composition 91 and the second raw material composition 92 is suppressed. As a result, the generation of gel is suppressed when each of the first raw material composition and the second raw material composition is transported.
[0176] Furthermore, in this embodiment, the volume A1 of the transfer space within the arrangement range of the screw 53 in the cylinder 50 (the inner bore 52A of the stator 52) is 30 to 80% of the volume A2 inside the cylinder 50. In this way, since the volume A1 of the transfer space is secured to be 30% or more, the occurrence of localized shear stress in each of the first raw material composition 91 and the second raw material composition 92 being transferred inside the cylinder 50 is suppressed.
[0177] Furthermore, since the volume A1 of the transfer space is 80% or less, space for the screw 53 is secured. Therefore, transfer force can be secured to transfer each of the first raw material composition 91 and the second raw material composition 92.
[0178] As described above, according to this embodiment, gel generation is suppressed when transferring the first raw material composition and the second raw material composition, thus stabilizing the quality of the polymerizable composition for optical materials and the optical materials produced.
[0179] <Evaluation> For Examples 1-5 and Comparative Examples 1-5, the gel mixing rate and the operating time until the gel was confirmed were evaluated as follows. Note that this disclosure is not limited to these examples.
[0180] <Gel Contamination Rate> For each example and comparative example, the optical materials obtained were visually inspected to confirm whether or not gel had formed. The gel contamination rate was calculated as the percentage of the number of optical materials that had formed gel relative to the total number of optical materials obtained (100%).
[0181] <Operating time until gel is confirmed> When manufacturing optical materials using the manufacturing system 10, the time from the start of operation of the manufacturing system 10 until gel was continuously confirmed in the manufactured optical material was measured. In this case as well, the presence or absence of gel was visually confirmed in the manufactured optical material. In Examples 1 to 4, the maximum operating time was set to 8 hours, and in Example 5, the maximum operating time was set to 49 hours to manufacture the optical material. In the comparative example, the maximum operating time was set to 2 hours to manufacture the optical material.
[0182] <Preparation of First Raw Material Composition 91 and Second Raw Material Composition 92> The optical material monomers, catalysts, and additives of the examples and comparative examples were calculated to total approximately 100 parts by mass. [Example 1] As shown in Figure 4, a mixture was prepared by charging 1.5 parts by mass of BASF Tinuvin 329 [ultraviolet absorber] and 46.0 parts by mass of m-xylene diisocyanate [polyisocyanate compound (A)]. This mixture was stirred at 25°C for 15 minutes to completely dissolve the material. Then, 10.4 parts by mass of 4-mercaptomethyl-1,8-dimercapto-3,6-dithiaoctane [active hydrogen compound (B)] was charged into the mixture and stirred at 25°C for 5 minutes to obtain a homogeneous solution. Furthermore, 0.06 parts by mass of 2,6-lutidine [polymerization catalyst a] was charged into the obtained homogeneous solution and stirred at 40°C for 1 hour to polymerize the optical material monomer while adjusting the viscosity, thereby obtaining a mixture containing a prepolymer. Subsequently, 0.13 parts by mass of JP-506H [release agent] manufactured by Johoku Chemical Industry Co., Ltd. and 0.09 parts by mass of 10-camphor sulfonic acid [organic acid] were added to the mixture containing the prepolymer. This mixture was stirred at 25°C for 10 minutes, and degassed at 400 Pa and 25°C for 1 hour to obtain the first raw material composition 91, which is prepolymer A. The viscosity Va of prepolymer A at 25°C was 415 mPa·s.
[0183] 36.8 parts by mass of 4-mercaptomethyl-1,8-dimercapto-3,6-dithiaoctane [active hydrogen compound (B)] and 5.2 parts by mass of m-xylene diisocyanate [polyisocyanate compound (A)] were charged and stirred at 25°C for 5 minutes to prepare a homogeneous solution. Then, 0.01 parts by mass of 2,6-lutidine [polymerization catalyst a] and 0.01 parts by mass of 3,5-lutidine [polymerization catalyst b] were charged and stirred at 40°C for 1 hour, thereby polymerizing the monomer for optical materials while adjusting the viscosity to obtain a mixture containing a prepolymer. Subsequently, this prepolymer liquid was degassed at 400 Pa and 25°C for 1 hour to obtain prepolymer B as the second raw material composition 92. The viscosity Vb of prepolymer B at 25°C was 455 mPa·s.
[0184] [Examples 2-5 and Comparative Examples 1-5] In Examples 2-5 and Comparative Examples 1-5, prepolymer A as the first raw material composition 91 and prepolymer B as the second raw material composition 92 were obtained in the same manner as in Example 1, as shown in Figure 4. In Examples 2-5 and Comparative Examples 1-5, the parts by mass of each material contained in prepolymer A and prepolymer B are as shown in Figure 4.
[0185] <Manufacturing of Optical Materials> Using the first raw material composition 91 and the second raw material composition 92 prepared as described above, and using the manufacturing system 10 described above, optical materials (lenses with a center thickness of 10 mm) were manufactured according to the manufacturing method described above. As shown below, in Examples 1 to 5, the first pump 32 and the second pump 22 were 3NB10F positive displacement single-axis eccentric screw pumps manufactured by Hyoshin Equipment Co., Ltd. On the other hand, in Comparative Examples 1 to 3, gear pumps were used as the first pump 32 and the second pump 22. In Comparative Examples 4 to 5, the first pump 32 and the second pump 22 were XPL-1-STST-MVX diaphragm pumps manufactured by Takumina Co., Ltd. In Examples 1 to 5, manufacturing was carried out by changing the rotation speed of the screw of the positive displacement single-axis eccentric screw pump. In Comparative Examples 1 to 3, manufacturing was carried out by changing the rotation speed of the gear of the gear pump, and in Comparative Examples 4 to 5, manufacturing was carried out by changing the frequency of the pump head of the diaphragm pump.
[0186] <Calculation of Maximum Wall Shear Stress> In this example, computational fluid dynamics (CFD) was used to calculate the maximum wall shear stress inside the pump. SOLIDWORKS CAD was used for pump modeling, and Ansys Meshing from Ansys was used for model mesh refinement. The mesh-refined pump geometry model was imported into Ansys FLUENT 2021 R1, and the shear stress applied to the transported material (in this case, the first raw material composition 91) inside the pump was determined by numerically analyzing the Navier-Stokes equations, which are the fluid transport equations. Subsequently, the maximum value of the maximum wall shear stress inside the pump was determined within the shear stress range applied to the transported material (in this case, the first raw material composition 91) extracted near the screw in the positive displacement screw pump, near the gear in the gear pump, and near the check valve in the diaphragm pump. The CFD for the positive displacement single-screw eccentric pump was performed under the following conditions. Software used: FLUENT 2021 R1 3D 12para Solver: Pressure-based coupled solver Time calculation: Unsteady calculation Turbulence model: None (laminar flow) Spatial discretization scheme: Default Unsteady method: Default CFD of gear pumps and diaphragm pumps was performed under the following conditions: Software used: FLUENT 2021 R1 2D 8para Solver: Pressure-based coupled solver Time calculation: Unsteady calculation Turbulence model: None (laminar flow) Spatial discretization scheme: Default Unsteady method: Default In addition, in the CFD of positive displacement uniaxial eccentric screw pumps, gear pumps, and diaphragm pumps, in Examples 1 to 4 and Comparative Examples 1 to 5, the viscosity of the first raw material composition 91 was 415 mPa·s and the density was 1210 kg / m³ 3 In Example 5, the viscosity of the first raw material composition 91 was 519 mPa·s and the density was 1210 kg / m³. 3 That's what I decided.
[0187] <Calculation of liquid transfer speed> For each example and comparative example, the first raw material composition 91 or the second raw material composition 92 is collected from the first connecting pipe 35 or the second connecting pipe 25 for a predetermined sampling time [s] in the transfer section, and the weight (g) of the obtained first raw material composition 91 or second raw material composition 92 is divided by the sampling time [s] in the transfer section to obtain the value [g·s]. -1This was calculated as the liquid delivery rate.
[0188] [Example 1] As shown in Figure 5, positive displacement single-screw pumps were used as the first pump 32 and the second pump 22. The inner diameter D1 of the inner bore 52A of the stator 52 is 17.8 mm. The length L1 of the inner bore 52A of the stator 52 is 156 mm. L1 / D1 is 8.76.
[0189] The diameter D2 of screw 53 is 14.3 mm. The effective length L2 of screw 53 is 156 mm. L2 / D2 is 10.9. The root diameter is 4.8 mm. The root diameter / diameter is 0.336.
[0190] The volume of the transfer space is 53% of the volume of the inner bore 52A. The volume of the transfer space is the volume of the inner bore 52A with the screw 53 in place. The transfer performance of this screw pump is 3.9 ml / rev.
[0191] In Example 1, the rotational speed of the screw 53 was set to 125 rpm. The maximum wall shear stress / fluid delivery rate in Example 1 was 133 Pa / (g·s). -1 )
[0192] In Examples 1 to 4, the viscosity of the mixture of the first raw material composition 91 and the second raw material composition 92 was 510 mPa·s. This viscosity is the viscosity when the mixture was poured into the mold 84.
[0193] [Example 2] The same positive displacement single-screw eccentric pumps as in Example 1 were used as the first pump 32 and the second pump 22. In Example 2, as in Example 1, the rotation speed of the screw 53 was set to 125 rpm. The maximum wall shear stress / fluid delivery rate in Example 2 was 133 Pa / (g·s). -1 )
[0194] [Example 3] The same positive displacement single-screw eccentric pumps as in Example 1 were used as the first pump 32 and the second pump 22. In Example 3, the rotation speed of the screw 53 was set to 80 rpm. The maximum wall shear stress / fluid delivery rate in Example 3 was 144 Pa / (g·s). -1 )
[0195] [Example 4] The same positive displacement single-screw eccentric pumps as in Example 1 were used as the first pump 32 and the second pump 22. In Example 4, the rotation speed of the screw 53 was set to 250 rpm. The maximum wall shear stress / fluid delivery rate in Example 4 was 123 Pa / (g·s). -1 )
[0196] [Example 5] The same positive displacement single-screw eccentric pumps as in Example 1 were used as the first pump 32 and the second pump 22. In Example 5, the rotation speed of the screw 53 was set to 107 rpm. The maximum wall shear stress / fluid delivery rate in Example 5 was 125 Pa / (g·s). -1 )
[0197] In Example 5, the viscosity of the mixture of the first raw material composition 91 and the second raw material composition 92 was 752 mPa·s. This viscosity is the viscosity when the mixture was poured into the mold 84.
[0198] [Comparative Example 1] Gear pumps were used as the first pump 32 and the second pump 22. The volume of the transfer space is 17% of the volume inside the case. The volume of the transfer space is the volume inside the case with the gears arranged. The transfer performance of the gear pump is 7.6 ml / rev.
[0199] In Comparative Example 1, the gear rotation speed was set to 70 rpm. The maximum wall shear stress / fluid delivery rate in Comparative Example 1 was 832 Pa / (g·s). -1 )
[0200] In Comparative Example 1, the viscosity of the mixture of the first raw material composition 91 and the second raw material composition 92 was 390 mPa·s. This viscosity is the viscosity when the mixture was poured into mold 84.
[0201] [Comparative Example 2] The same gear pumps as in Comparative Example 1 were used as the first pump 32 and the second pump 22. In Comparative Example 2, the gear rotation speed was set to 72 rpm. The maximum wall shear stress / fluid delivery rate in Comparative Example 2 was 818 Pa / (g·s). -1 )
[0202] In Comparative Examples 2 to 5, the viscosity of the mixture of the first raw material composition 91 and the second raw material composition 92 was 370 mPa·s. This viscosity is the viscosity when the mixture was cast into mold 84.
[0203] [Comparative Example 3] The same gear pumps as in Comparative Example 1 were used as the first pump 32 and the second pump 22. In Comparative Example 3, the gear rotation speed was set to 72 rpm. The maximum wall shear stress / fluid delivery rate in Comparative Example 3 was 818 Pa / (g·s). -1 )
[0204] [Comparative Example 4] Diaphragm pumps were used as the first pump 32 and the second pump 22. In Comparative Example 4, the frequency of the pump head was set to 14 Hz. The maximum wall shear stress / fluid delivery rate in Comparative Example 4 was 2208 Pa / (g·s). -1 )
[0205] [Comparative Example 5] The same diaphragm pumps as in Comparative Example 4 were used as the first pump 32 and the second pump 22. In Comparative Example 5, the frequency of the pump head was set to 24 Hz. The maximum wall shear stress / fluid delivery rate in Comparative Example 5 was 1877 Pa / (g·s). -1 )
[0206] <Evaluation Results> As shown in Figure 6, the gel contamination rate was lower in Examples 1 to 5 compared to Comparative Examples 1 to 5. Furthermore, in Comparative Examples 1 to 5, the operating time until gel was continuously detected was within 2 hours, whereas in Examples 1 to 4, gel was not continuously detected for 8 hours or more of operation. In Example 5, gel was not continuously detected for 49 hours or more of operation. Therefore, it was confirmed that gel generation was suppressed in Examples 1 to 5 compared to Comparative Examples 1 to 5.
[0207] The present invention is not limited to the embodiments described above, and various modifications, changes, and improvements are possible without departing from the spirit of the invention. For example, the modified forms shown above may be combined in any way.
[0208] <Note> [Aspect 1] The apparatus comprises: a first transfer step in which a first raw material composition is transferred to a mixing section in a first transfer section; a second transfer step in which a second raw material composition is transferred to the mixing section in a second transfer section; and a mixing step in which the first raw material composition and the second raw material composition are mixed in the mixing section, wherein at least one of the first transfer section and the second transfer section has a value of 500 Pa / (g·s) obtained by dividing the maximum shear stress applied to the object to be transferred by the transfer speed. -1A method for producing a polymerizable composition for optical materials, wherein the first transfer unit and the second transfer unit each have: a cylinder for accommodating an object to be transferred; a helical screw disposed inside the cylinder along the axial direction of the cylinder; and a rotational drive mechanism that rotates the screw and causes it to reciprocate in the radial direction of the cylinder as a result of the rotation. The method for producing a polymerizable composition for optical materials according to Aspect 1. Aspect 3 A method for producing a polymerizable composition for optical materials according to Aspect 2, wherein the rotational speed of the screw is 20 to 300 rpm. Aspect 4 A method for producing a polymerizable composition for optical materials according to Aspect 2 or 3, wherein the first transfer unit and the second transfer unit each have a positive displacement single-screw eccentric pump. Aspect 5 A method for producing a polymerizable composition for optical materials according to any one of Aspects 2 to 4, wherein the screw has a shape in which spheres are continuous in the helical direction. [Aspect 6] A method for producing a polymerizable composition for optical materials according to any one of aspects 2 to 5, wherein the volume of the transfer space inside the cylinder is 30 to 80% of the volume inside the cylinder. [Aspect 7] A method for producing a polymerizable composition for optical materials according to any one of aspects 2 to 6, wherein the viscosity of the first raw material composition or the second raw material composition flowing inside the cylinder is 30 to 1000 mPa·s. [Aspect 8] A method for producing a polymerizable composition for optical materials according to any one of aspects 1 to 7, wherein the polymerizable composition for optical materials contains two or more different monomers for optical materials and a polymerization catalyst. [Aspect 9] A method for producing a polymerizable composition for optical materials according to aspect 8, wherein the two or more different monomers for optical materials include a polyisocyanate compound having two or more isocyanate groups, and an active hydrogen compound which is at least one selected from the group consisting of a polythiol compound having two or more mercapto groups, a hydroxythiol compound having one or more mercapto groups and one or more hydroxyl groups, a polyol compound having two or more hydroxyl groups, and an amine compound.[Aspect 10] The method for producing a polymerizable composition for optical materials according to Aspect 9, wherein the first raw material composition comprises a polyisocyanate compound having two or more isocyanate groups, and the second raw material composition comprises a polythiol compound having two or more mercapto groups. [Aspect 11] The method for producing a polymerizable composition for optical materials according to any one of Aspects 1 to 10, wherein each of the first raw material composition and the second raw material composition has a viscosity of 30 mPa·s or more and 1000 mPa·s or less, as measured with a B-type viscometer at 25°C and 30 rpm. [Aspect 12] The method for producing an optical material, comprising a curing step of polymerizing and curing a polymerizable composition for optical materials obtained by the method for producing a polymerizable composition for optical materials according to any one of Aspects 1 to 11 to produce an optical material. [Aspect 13] A manufacturing apparatus for producing a polymerizable composition for optical materials by mixing a first raw material composition and a second raw material composition, comprising: a mixing section for mixing the first raw material composition and the second raw material composition; a first transfer section for transferring the first raw material composition to the mixing section; a second transfer section for transferring the second raw material composition to the mixing section; and a stirring section for stirring the mixture of the first raw material composition and the second raw material composition mixed in the mixing section, wherein at least one of the first transfer section and the second transfer section has a value of 500 Pa / (g·s) obtained by dividing the maximum shear stress applied to the object to be transferred by the transfer speed. -1 Apparatus for manufacturing polymerizable compositions for optical materials, wherein the maximum shear stress applied to the object to be transported divided by the transport speed is 500 Pa / (g·s) -1 The following is a manufacturing system for optical materials.
[0209] The disclosure of Japanese Patent Application No. 2025-015617, filed on 31 January 2025, is incorporated herein by reference in its entirety. All documents, patent applications, and technical standards described herein are incorporated herein by reference to the same extent as if each individual document, patent application, and technical standard were specifically and individually noted to be incorporated by reference.
Claims
1. The apparatus comprises: a first transfer step in which a first raw material composition is transferred to a mixing section in a first transfer section; a second transfer step in which a second raw material composition is transferred to the mixing section in a second transfer section; and a mixing step in the mixing section in which the first raw material composition and the second raw material composition are mixed. At least one of the first transfer section and the second transfer section has a maximum shear stress applied to the object to be transferred divided by the transfer speed of 500 Pa / (g·s). -1 The following is a method for producing polymerizable compositions for optical materials.
2. The method for producing a polymerizable composition for optical materials according to claim 1, wherein at least one of the first transfer unit and the second transfer unit comprises: a cylinder for accommodating an object to be transferred; a helical screw disposed inside the cylinder along the axial direction of the cylinder; and a rotational drive mechanism that rotates the screw and causes it to reciprocate in the radial direction of the cylinder as a result of the rotation.
3. The method for producing a polymerizable composition for optical materials according to claim 2, wherein the rotational speed of the screw is 20 to 300 rpm.
4. The method for producing a polymerizable composition for optical materials according to claim 2, wherein at least one of the first transfer unit and the second transfer unit is a positive displacement uniaxial eccentric screw pump.
5. The method for producing a polymerizable composition for optical materials according to claim 2, wherein the screw has a shape in which the spheres are continuous in the helical direction.
6. The method for producing a polymerizable composition for optical materials according to claim 2, wherein the volume of the transfer space inside the cylinder is 30 to 80% of the volume inside the cylinder.
7. The method for producing a polymerizable composition for optical materials according to claim 2, wherein the viscosity of the first raw material composition or the second raw material composition flowing inside the cylinder is 30 to 1000 mPa·s.
8. The method for producing the polymerizable composition for optical materials according to claim 1, wherein the polymerizable composition for optical materials contains two or more different monomers for optical materials and a polymerization catalyst.
9. The method for producing a polymerizable composition for optical materials according to claim 8, wherein the two or more different monomers for optical materials include a polyisocyanate compound having two or more isocyanate groups, and an active hydrogen compound which is at least one selected from the group consisting of a polythiol compound having two or more mercapto groups, a hydroxythiol compound having one or more mercapto groups and one or more hydroxyl groups, a polyol compound having two or more hydroxyl groups, and an amine compound.
10. The method for producing a polymerizable composition for optical materials according to claim 9, wherein the first raw material composition comprises a polyisocyanate compound having two or more isocyanate groups, and the second raw material composition comprises a polythiol compound having two or more mercapto groups.
11. The method for producing a polymerizable composition for optical materials according to claim 1, wherein each of the first raw material composition and the second raw material composition has a viscosity measured with a B-type viscometer at 25°C and 30 rpm of 30 mPa·s or more and 1000 mPa·s or less.
12. A method for producing an optical material, comprising a curing step of polymerizing and curing a polymerizable composition for optical materials obtained by the method for producing a polymerizable composition for optical materials described in claim 1, to produce an optical material.
13. A manufacturing apparatus for producing a polymerizable composition for optical materials by mixing a first raw material composition and a second raw material composition, comprising: a mixing section for mixing the first raw material composition and the second raw material composition; a first transfer section for transferring the first raw material composition to the mixing section; a second transfer section for transferring the second raw material composition to the mixing section; and a stirring section for stirring the mixture of the first raw material composition and the second raw material composition mixed in the mixing section, wherein at least one of the first transfer section and the second transfer section has a value of 500 Pa / (g·s) obtained by dividing the maximum shear stress applied to the object to be transferred by the transfer speed. -1 The following is an apparatus for manufacturing polymerizable compositions for optical materials.
14. The apparatus comprises: a mixing section for mixing a first raw material composition and a second raw material composition; a first transfer section for transferring the first raw material composition to the mixing section; a second transfer section for transferring the second raw material composition to the mixing section; a stirring section for stirring the mixture of the first raw material composition and the second raw material composition mixed in the mixing section; and a curing section for polymerizing and curing the polymerizable composition for optical materials obtained by stirring in the stirring section to produce an optical material, wherein at least one of the first transfer section and the second transfer section has a maximum shear stress applied to the object to be transferred divided by the transfer speed of 500 Pa / (g·s). -1 The following is a manufacturing system for optical materials.