CN110740981A - Hydraulic composition - Google Patents
Hydraulic composition Download PDFInfo
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- CN110740981A CN110740981A CN201880039081.2A CN201880039081A CN110740981A CN 110740981 A CN110740981 A CN 110740981A CN 201880039081 A CN201880039081 A CN 201880039081A CN 110740981 A CN110740981 A CN 110740981A
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- hydraulic composition
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
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- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present invention provides hydraulic compositions which are prepared by using part containing black particles as a binder, and which can sufficiently suppress the occurrence of black spots on the surface of a cured product obtained from the hydraulic composition even in a hydraulic composition having high fluidity, and can obtain a cured product having excellent surface appearance, and which are prepared by using a water-soluble cellulose ether containing at least selected from the group consisting of hydroxyalkyl alkylcelluloses and hydroxyalkyl celluloses.
Description
Technical Field
The present invention relates to hydraulic compositions, and more particularly to hydraulic compositions which can sufficiently suppress the occurrence of black spots (black ずみ) on the surface of a cured product obtained from a hydraulic composition containing a binder, and can provide a cured product having an excellent surface appearance.
Background
In recent years, fly ash, blast furnace slag powder, silica fume, limestone powder, etc. have been used as binding materials for hydraulic compositions from cement in order to reduce the environmental load, for the purpose of utilizing industrial by-products or reducing the amount of carbon dioxide emission, in addition, natural substances have been used in hydraulic compositions, lignite has been used in some cases, etc. these substances used as binding materials from cement contain black particles mainly of carbon particles, in particular, fly ash contains a lot of unburned carbon as black particles, in JIS standard for fly ash (JIS a6201), the burning loss as a reference for the amount of carbon is controlled to 8.0% or less, in addition, the black particles contained in these substances float on the surface of a cured product obtained from a hydraulic composition in part using these substances as binding materials and become black stains, thereby deteriorating the appearance, in particular, when a polycarboxylic acid-based water reducing agent is used as a dispersant for binding materials, the generation of black is very significant, in addition, when the hydraulic composition is increased, the separation of the hydraulic composition is reduced, the energy consumption is reduced, and the generation of a cement-based hardened product having a high weight average carbon number of carbon atoms, which is not enough, but the weight-reducing the generation of a cement-based hardening-based mono-olefin copolymer, which has been obtained from a cement-based hardened product, and a cement-based hardening copolymer, which has been obtained by a conventional method which has been found to a high-inhibiting the weight-reducing the generation of a cement-based hardening process, and which is not resulted from a cement-based cement-reducing agent, and which has been found to-reducing the cement-forming a cement-reducing the cement-based hardening process, and is not a cement-reducing the problem, and is found in addition, but the cement-reducing the problem of a cement-based hardening-based cement-based hardening-reducing the cement-based.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2004-83303
Patent document 2: japanese patent laid-open No. 2004-175651
Disclosure of Invention
Problems to be solved by the invention
The problem to be solved by the present invention is to provide hydraulic compositions which can sufficiently suppress the occurrence of black spots on the surface of a cured product obtained from the hydraulic compositions even when the hydraulic compositions have high fluidity and can give a cured product having excellent surface appearance, among hydraulic compositions prepared by using parts containing black particles as a binder.
Means for solving the problems
Accordingly, the present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have found that a hydraulic composition prepared by using a water-soluble cellulose ether containing at least selected from the group consisting of hydroxyalkyl alkylcelluloses and hydroxyalkyl celluloses is accurate and suitable.
Specifically, the present invention relates to hydraulic compositions comprising a binder, a water-soluble cellulose ether, a polycarboxylic acid water reducing agent, and water, wherein the binder comprises cement and at least selected from fly ash, blast furnace slag powder, silica fume, limestone powder, and lignite, and the water-soluble cellulose ether comprises at least selected from hydroxyalkyl alkylcellulose and hydroxyalkyl cellulose.
The binder used in the hydraulic composition according to the present invention contains cement and at least black-particle-containing substances selected from the group consisting of fly ash, blast furnace slag powder, silica fume, limestone powder and lignite.
The cement may be any of various portland cements such as ordinary portland cement, medium-heat portland cement, low-heat portland cement, high-strength portland cement, super high-early portland cement, and sulfate-resistant portland cement.a material containing black particles such as fly ash, blast furnace slag powder, silica fume, limestone powder, and lignite may be prepared as a mixed cement, or may be prepared in a factory for producing a hydraulic composition, or may be included as part of portland cement prepared as a small amount of a mixed component used in JIS R5210 in a ratio of 0 to 5% in JIS R5210. in a binder used in a hydraulic cement composition, the ratio of cement to the material containing black particles is not particularly limited, but it is preferable that the binder contains cement in a ratio of 10 to 95% by mass and contains a material containing black particles in a ratio of 5 to 90% by mass, and the total of both is 100% by mass.
The water-soluble cellulose ether used in the hydraulic composition according to the present invention is at least selected from the group consisting of 1) hydroxyalkyl alkylcelluloses such as hydroxyethyl methylcellulose, hydroxypropyl methylcellulose, and hydroxyethyl ethylcellulose, and 2) hydroxyalkyl celluloses such as hydroxypropyl cellulose and hydroxyethyl cellulose.
As the hydroxyalkyl alkylcellulose, preferred is an MS (the number of substitution moles of the hydroxyalkyl group, hereinafter also the same) of 0.1 to 3.0 and a DS (the degree of substitution of the alkyl group, hereinafter also the same) of 1.0 to 2.2, more preferred is an MS of 0.1 to 1.0 and a DS of 1.0 to 2.0, and particularly preferred is an MS of 0.1 to 0.3 and a DS of 1.1 to 1.7. Among them, hydroxypropyl methylcellulose and hydroxyethyl methylcellulose are preferable. As the hydroxyalkyl cellulose, preferred is a hydroxyalkyl cellulose having an MS of 2.0 to 3.3, more preferred is a hydroxyalkyl cellulose having an MS of 2.0 to 2.8, and particularly preferred is a hydroxyalkyl cellulose having an MS of 2.0 to 2.4. Among them, hydroxyethyl cellulose is preferable.
The MS represents the number of moles of substitution (molar substitution) of the hydroxyalkyl group, and is the average number of moles of hydroxyalkoxy groups added per glucose ring unit of the cellulose. In addition, DS represents the degree of substitution (degree of substitution) of an alkyl group, and is the number of alkoxy groups present in the glucose ring per cellulose. The MS or DS can be measured by converting a value measured by a substitution degree analysis method of hypromellose (hydroxypropylmethylcellulose) described in revised japanese pharmacopoeia, 17 th edition.
In the hydraulic composition according to the present invention, as for the water-soluble cellulose ether, it is preferable that the viscosity of a2 mass% aqueous solution thereof at 20 ℃ (hereinafter, simply referred to as 2% viscosity) is 5000 mPas or more and the viscosity of a1 mass% aqueous solution thereof at 20 ℃ (hereinafter, simply referred to as 1% viscosity) is 30000 mPas or less, more preferably the 2% viscosity is 5000 mPas or more and the 1% viscosity is 20000 mPas or less, and particularly preferably the 2% viscosity is 10000 mPas or more and the 1% viscosity is 15000 mPas or less. The above viscosities are all values at 20rpm for a B-H type viscometer.
The water-soluble cellulose may be added in any of parts among the water-soluble cellulose ether powder, the aqueous solution of the water-soluble cellulose ether, the water-soluble cellulose ether dispersed or dissolved in the polycarboxylic acid water reducing agent, and the water-soluble cellulose ether dispersed or dissolved in the liquid shrinkage reducing agent, the liquid defoaming agent, etc. from the viewpoint of the fluidity of the hydraulic composition, the water-soluble cellulose ether is preferably added in an amount of 0.01 to 0.20 parts by mass, more preferably 0.01 to 0.15 parts by mass, and particularly preferably 0.02 to 0.10 parts by mass, based on 100 parts by mass of the binder, and when the amount of the water-soluble cellulose ether added is less than 0.01 parts by mass based on 100 parts by mass of the binder, sufficient black stain-inhibiting effect and material separation resistance cannot be obtained, and on the contrary, when the amount exceeds 0.20 parts by mass, the black stain-inhibiting effect is obtained, but the fluidity of the hydraulic material is lowered.
The average particle diameter obtained by a laser diffraction method of the water-soluble cellulose ether according to the present invention is preferably 20 to 500 μm, more preferably 20 to 120 μm, and particularly preferably 40 to 100 μm from the viewpoint of the effect of suppressing black spots. The average particle diameter is a volume-converted particle diameter and is a value obtained by a powder particle diameter measurement method using a laser diffraction method. The average particle diameter can be measured using, for example, HELOS & RODOS (trade name, manufactured by japan レーザー).
The unsaturated carboxylic acid monomer and/or salt thereof which forms the structural unit of the (co) polymer as the polycarboxylic acid water reducing agent includes (meth) acrylic acid, crotonic acid, maleic acid (anhydride), itaconic acid (anhydride), fumaric acid, and/or salt thereof, the unsaturated dicarboxylic acid monomer having 2 or more carboxyl groups in 1 molecule may have ester bonds or amide bonds in addition to kinds of carboxylic acids or salts thereof, and the kind of the salt is not particularly limited, and examples thereof include sodium salts, potassium salts, alkali metal salts such as calcium salts or magnesium salts, alkaline earth metal salts such as ammonium salts, diethanolamine salts, and amine salts such as triethanolamine salts.
Examples of the monomer other than the carboxylic acid and/or a salt thereof which forms the constituent unit of the (co) polymer include unsaturated monomers having a polyoxyalkylene group composed of an oxyalkylene unit having 1 to 300 carbon atoms and 2 to 4 in the molecule, for example, α -vinyl- ω -hydroxy (poly) butylene oxide (poly) ethylene oxide, α -allyl- ω -methoxy (poly) ethylene oxide, α -allyl- ω -methoxy- (poly) ethylene oxide (poly) propylene oxide, α -allyl- ω -hydroxy- (poly) ethylene oxide, α -allyl- ω -hydroxy- (poly) ethylene oxide (poly) propylene oxide, α -methallyl- ω -alkylene oxide- ω -hydroxy- (poly) ethylene oxide, α -methallyl- ω -methoxy- (poly) ethylene oxide, α -methallyl- ω -hydroxy- (poly) ethylene oxide (poly) propylene oxide, α -methallyl-allyl- ω -acetyl- (poly) ethylene oxide, α - (3-methyl-3- ω -hydroxy) -butylene oxide, poly (ethylene oxide) ethylene oxide (poly) ethylene oxide, poly (ethylene oxide) ethylene oxide having an active bond in the molecule, α -methallyl- ω -alkylene-hydroxy- (poly) ethylene oxide, poly (ethylene oxide), poly (ω -butylene) ethylene oxide), poly (ethylene oxide) ethylene oxide having an active bond in the molecule, poly (ω -butylene oxide, poly (ethylene oxide) ethylene oxide, poly (ethylene oxide) amine oxide, poly (ω -butylene oxide, poly (ethylene oxide) amine oxide, poly (ethylene oxide) amine oxide, poly (ethylene oxide) amine (butylene oxide) amine oxide, poly (butylene oxide) amine oxide having an active epoxy amide having an active bond in the addition of the poly (ω -butylene oxide of the poly (ethylene oxide of the poly (ω -butylene oxide of the poly (ω -.
The (co) polymer as the polycarboxylic acid-based water reducing agent is preferably composed of the following structural units: a structural unit composed of an unsaturated carboxylic acid monomer and/or a salt thereof, and a structural unit composed of an unsaturated monomer having a polyoxyalkylene group composed of an oxyalkylene unit having 1 to 300 carbon atoms of 2 to 4 in the molecule. In addition, the mass average molecular weight thereof is preferably 2000 to 500000, more preferably 5000 to 100000.
In the hydraulic composition according to the present invention, the polycarboxylic acid-based water-reducing agent may be used as an aqueous solution or as a powder, and as for the amount thereof used, it is preferable that the polycarboxylic acid-based water-reducing agent, i.e., the (co) polymer, is set to 0.01 to 2% by mass, more preferably 0.05 to 0.5% by mass, relative to the binder.
As the aggregate, fine aggregates such as river sand, mountain sand, ground sand, silica sand, crushed sand, fine blast furnace slag aggregates and the like, and coarse aggregates such as river sand stone, mountain crushed stone, ground gravel, crushed stone, coarse blast furnace slag aggregates and the like are used in the hydraulic composition according to the present invention, and in order to reduce drying shrinkage or self-shrinkage and further to , to suppress heat generation by the binder, the hydraulic composition preferably contains an aggregate such as a fine aggregate or a coarse aggregate.
In the hydraulic-setting composition according to the present invention, the mass ratio of water/binding material is preferably 0.35 to 0.65. When the mass ratio of water/binder is less than 0.35, the fluidity of the hydraulic composition is liable to deteriorate, and when the mass ratio of water/binder is more than 0.65, it is difficult to impart sufficient material separation resistance.
The hydraulic composition of the present invention may be used in combination with: AE modifiers composed of, for example, anionic surfactants, antifoaming agents of, for example, oxyalkylene type, retarders composed of, for example, oxycarboxylate, curing accelerators composed of, for example, alkanolamines, drying shrinkage reducers composed of, for example, polyoxyalkylene alkyl ethers, preservatives composed of, for example, isothiazoline type compounds, water repellents composed of, for example, higher fatty acid derivatives, rust inhibitors composed of, for example, nitrite salts, and the like.
The details of the mechanism for achieving the effect of the present invention are not clear at present, but are presumed as follows. It is presumed that the water-soluble cellulose ether adsorbs black particles produced from fly ash, blast furnace slag powder, silica powder, limestone powder, and lignite, and at the same time, in the hydraulic composition, the material separation resistance is also increased by the thickening effect of the water-soluble cellulose ether, thereby achieving both the inhibition of black spots and the inhibition of material separation at high fluidity. This property varies depending on the chemical structure, and the use of a specific water-soluble cellulose ether makes it possible to obtain a hydraulic composition according to the present invention having both black stain inhibition and material separation resistance.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, the hydraulic composition prepared by using part containing black particles as a binder can sufficiently suppress the occurrence of black spots on the surface of a cured product obtained from the hydraulic composition even if the hydraulic composition has high fluidity, and can give a cured product having excellent surface appearance.
Examples
Hereinafter, examples and the like are given to further embody the configuration and effects of the present invention, but the present invention is not limited to the examples. In the following examples and the like, "part" means "part by mass" and "%" means "% by mass" unless otherwise specified.
Test class 1 (preparation of mortar as Hydraulic composition)
A mortar mixer in accordance with JIS R5201 cement physical test method was used to add an antifoaming agent (trade name "AFK-2" manufactured by bamboo grease Co.) in an amount of 0.005 parts by mass per 100 parts by mass of a binder, and kneading was performed under the compounding conditions shown in Table 1 for 240 seconds as shown in Table 2. the kneading and the following tests were performed under conditions in which the material temperature was 20. + -.3 ℃, the room temperature was 20. + -.3 ℃ and the humidity was 60% or more. the mortar flow was an unhardened mortar flow, and the objective was to fill the mortar into a cylindrical mold (diameter: 5cm, height: 10cm) and age the mortar in the room at 20 ℃ for 24 hours without using an additive other than a polycarboxylic acid-based water reducing agent and an antifoaming agent, determine the degree of black stain, determine the separation resistance after 3 minutes from pulling up the mortar flow cone, and determine the degree of black stain of hardened mortar in and show the results of the hardening mortar in Table 2.
[ Table 1]
In the context of table 1, the following,
and (3) OPC: ordinary portland cement
BB: blast furnace cement B
FA 1: fly ash (burning loss 5.3%)
FA 2: fly ash (burning loss 2.1%)
SF: silicon powder (burning loss 4.3%)
Fine aggregate: ground sand produced by river water in large well
[ Table 2]
In the context of table 2, the following,
the use amount is as follows: amount (%) used relative to the binding material (in the case of using an aqueous solution, the amount (%) used relative to the binding material is the solid content in the aqueous solution)
PC-1: polycarboxylic acid type high-performance AE water reducing agent (trade name: チューポール HP-11) manufactured by bamboo fats & oils Ltd
PC-2: polycarboxylic acid type high-performance AE water reducing agent manufactured by BASF Japan K.K. (trade name "マスターグレニウム SP8 SV")
PC-3: polycarboxylic acid type high-performance AE water-reducing agent (trade name "シーカメント NT")
CB: black spot inhibitor of a specific polycarboxylic acid type surfactant (trade name: スキッシュ 21B) manufactured by Kao corporation
Water-soluble cellulose ether: the substances described in Table 3 were used
[ Table 3]
In the context of table 3, the results are,
viscosity: viscosity (mPas) of a2 mass% aqueous solution at 20 ℃. The viscosity of a1 mass% aqueous solution is noted (1%).
The degree of black staining was determined visually based on the following criteria.
Criterion for judging degree of black stain
◎ the black stain is very inconspicuous
○ slight confirmation of staining
X: the black spots can be clearly confirmed
The separation resistance was determined visually based on the following criteria.
Criterion for determining separation resistance
◎ very good (no separation)
○ good (although not separated, the surface of the hydraulic composition is slightly whitish)
△ slight leakage of Water into Hydraulic composition
X: there is a significant leakage of water from the hydraulically setting composition
Test class 2 (preparation of concrete as Hydraulic composition)
The following concrete was prepared according to the contents shown in table 5 under the compounding conditions shown in table 4. Ordinary portland cement (density 3.16 g/cm) was charged into a 50L disk type intensive kneading mixer3) Fly ash (density 2.29 g/cm)32.3 percent of burning loss), and blast furnace slag powder (density 2.88 g/cm)3) And fine aggregate (ground sand made of Dajing Sichuan water system, density 2.58g/cm3) And coarse aggregate (crushed stone from Okazaki, density 2.68 g/cm)3) After 10 seconds of mixing, a defoaming agent (product name "AFK-2" manufactured by bamboo & fat Co.) was added in an amount of 0.005 parts by mass based on 100 parts by mass of the binder, and a polycarboxylic acid water reducing agent used in test type 1 were mixed togetherWater-soluble cellulose ether was kneaded, and then charged with water , and further kneaded for 120 seconds so that the slump flow became 65. + -.2 cm and the air amount became within the range of 2% or less, it should be noted that the polycarboxylic acid water reducing agent and the antifoaming agent were regarded as parts of water, the slump immediately after kneading was measured in accordance with JIS-A1150, and the air amount was measured in accordance with JIS-A1128 for the prepared concrete composition, the slump flow of unhardened concrete, the degree of black spots and the separation resistance were all determined after pulling up the slump cone for 3 minutes, the unhardened concrete was filled into a cylindrical mold (diameter 10cm and height 20cm) and aged in the room at 20 ℃ for 24 hours, and then demolded to determine the degree of black spots of hardened concrete, and the results are shown in Table 5.
[ Table 4]
[ Table 5]
In the context of table 5, the results are,
the use amount is as follows: amount (%) used relative to the binding material (in the case of using an aqueous solution, the amount (%) used relative to the binding material is the solid content in the aqueous solution)
Polycarboxylic acid water reducing agents and water-soluble cellulose ethers: substances used in test class 1
The degree of black staining was determined visually based on the following criteria.
Criterion for judging degree of black stain
◎ little black stain
○ slight confirmation of staining
X: the black spots can be clearly confirmed
The separation resistance was determined visually based on the following criteria.
Criterion for determining separation resistance
◎ very good (aggregate not separated from mortar/slurry)
○ good (aggregate slightly separated from mortar/slurry)
△ poor (aggregate and mortar/slurry separation)
X: very poor (aggregate separated significantly from mortar/slurry).
Claims (10)
- A hydraulic composition comprising a binder, a water-soluble cellulose ether, a polycarboxylic acid water-reducing agent and water, wherein the binder comprises a cement and at least selected from the group consisting of fly ash, blast furnace slag powder, silica fume, limestone powder and lignite, and the water-soluble cellulose ether comprises at least selected from the group consisting of hydroxyalkyl alkylcellulose and hydroxyalkyl cellulose.
- 2. The hydraulic composition according to claim 1, wherein the hydroxyalkyl alkylcellulose has a molar substitution of the hydroxyalkyl groups of 0.1 to 3.0 and a degree of substitution of the alkyl groups of 1.0 to 2.2.
- 3. The hydraulic composition according to claim 1 or 2, wherein the hydroxyalkyl alkylcellulose is selected from the group consisting of hydroxypropyl methylcellulose and hydroxyethyl methylcellulose.
- 4. The hydraulic composition according to any of of claims 1 to 3, wherein the molar number of substitution of hydroxyalkyl groups in the hydroxyalkyl cellulose is 2.0 to 3.3.
- 5. The hydraulic composition according to any one of claims 1 to 4, wherein the hydroxyalkyl cellulose is hydroxyethyl cellulose .
- 6. The hydraulic composition according to any of claims 1 to 5, wherein a 2% by mass aqueous solution of a water-soluble cellulose ether has a viscosity of 5000 mPas or more at 20 ℃ and a 1% by mass aqueous solution of a water-soluble cellulose ether has a viscosity of 30000 mPas or less at 20 ℃.
- 7. The hydraulic composition according to of any one of claims 1 to 6, wherein the binder contains cement in a proportion of 10 to 95% by mass and a substance selected from the group consisting of fly ash and blast furnace slag powder in a proportion of 5 to 90% by mass, and the total of the cement and the substance selected from the group consisting of fly ash and blast furnace slag powder is 100% by mass.
- 8. The hydraulic composition according to any of claims 1 to 7, wherein the hydraulic composition contains a water-soluble cellulose ether in a proportion of 0.01 to 0.20 parts by mass relative to 100 parts by mass of a binder.
- 9. The hydraulic composition of any of claims 1 to 8, , further comprising steps of aggregate.
- 10. The hydraulic composition of any of claims 1 to 9, , wherein the water/binding material mass ratio is 0.35 to 0.65.
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| JP2017118548A JP7011248B2 (en) | 2017-06-16 | 2017-06-16 | Hydraulic composition |
| JP2017-118548 | 2017-06-16 | ||
| PCT/JP2018/005221 WO2018230037A1 (en) | 2017-06-16 | 2018-02-15 | Hydraulic composition |
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| JP2635884B2 (en) * | 1991-06-25 | 1997-07-30 | 日本国土開発株式会社 | Concrete composition |
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- 2017-06-16 JP JP2017118548A patent/JP7011248B2/en active Active
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2018
- 2018-02-15 WO PCT/JP2018/005221 patent/WO2018230037A1/en active Application Filing
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| JP7011248B2 (en) | 2022-01-26 |
| WO2018230037A1 (en) | 2018-12-20 |
| TWI759436B (en) | 2022-04-01 |
| TW201904909A (en) | 2019-02-01 |
| JP2019001690A (en) | 2019-01-10 |
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