WO2012111691A1 - 針状炭酸ストロンチウム粒子の製造方法 - Google Patents
針状炭酸ストロンチウム粒子の製造方法 Download PDFInfo
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- WO2012111691A1 WO2012111691A1 PCT/JP2012/053479 JP2012053479W WO2012111691A1 WO 2012111691 A1 WO2012111691 A1 WO 2012111691A1 JP 2012053479 W JP2012053479 W JP 2012053479W WO 2012111691 A1 WO2012111691 A1 WO 2012111691A1
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- carbonate particles
- strontium carbonate
- strontium
- hydrocarbon group
- dicarboxylic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/186—Strontium or barium carbonate
- C01F11/187—Strontium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Definitions
- the present invention relates to a method for producing acicular strontium carbonate particles.
- acicular strontium carbonate particles is as a polymer resin filler, which offsets the birefringence of the polymer resin or actively imparts birefringence to the polymer resin.
- the polymer resin whose birefringence is canceled is used as a non-birefringent optical resin material as a lens or a transparent plate.
- the polymer resin imparted with birefringence is used as a retardation plate.
- acicular strontium carbonate particles having an average particle size of 500 nm or less along the major axis in a polymer resin are described as follows: the extending direction (longitudinal direction) of the binding chain of the polymer resin and the acicular strontium carbonate particles.
- the major axis direction (longitudinal direction) is parallel or perpendicular to each other, the birefringence caused by the orientation of the polymer resin bonding chain is canceled by the birefringence caused by the orientation of the strontium particles.
- a birefringent optical resin material is described.
- urea is added to a strontium salt aqueous solution, the temperature of the solution is reduced to below the freezing point, and urea is hydrolyzed in the aqueous solution.
- needle-like strontium carbonate particles having an average length of 200 nm or less are obtained using the above method (Example 3).
- Patent Document 2 as a method for producing fine acicular strontium carbonate particles, an aqueous solution containing a carbonic acid source is added to an alcohol liquid containing a strontium ion source to react alkali with the strontium and the carbonic acid source. A method of adding an agent is described. Also in the examples of this document, acicular strontium carbonate particles having an average major axis length of 200 nm or less are obtained using the above method.
- Patent Document 3 as a method for producing fine rod-shaped strontium carbonate particles, strontium hydroxide and a carbonic acid source selected from carbon dioxide or soluble carbonate, polyhydric alcohol, pyrophosphoric acid, ascorbic acid, carboxylic acid, carboxylic acid, Acicular strontium carbonate particles obtained by reacting in an aqueous solvent in the presence of a particle growth inhibitor selected from the group consisting of acid salts, polycarboxylic acids or polycarboxylic acid salts, and the obtained acicular strontium carbonates It is described that the particles are further heat-treated in water at a temperature of 50 ° C. or higher to form rod-shaped strontium carbonate particles.
- a carbonic acid source selected from carbon dioxide or soluble carbonate, polyhydric alcohol, pyrophosphoric acid, ascorbic acid, carboxylic acid, carboxylic acid, Acicular strontium carbonate particles obtained by reacting in an aqueous solvent in the presence of a particle growth inhibitor selected from the group consisting
- rod-shaped strontium carbonate particles having an average length of 200 nm or less are obtained by using the above method.
- the rod-shaped strontium carbonate particles obtained by using the above method have a fragile portion having a shape similar to a constriction, and by having this fragile portion, airflow It is said that it can be easily made into granular particles by pulverizing with a type pulverizer or the like.
- an object of the present invention is to provide a method capable of producing fine and hard acicular strontium carbonate particles that do not need to have a temperature below the freezing point, and without using alcohol. There is to do.
- the inventor of the present invention provides a divalent chain hydrocarbon group having 1 to 4 carbon atoms which may be substituted with one or two or more alkyl groups having 1 to 6 carbon atoms, and the chain carbonization thereof.
- a dicarboxylic acid containing a carboxylic acid group bonded to each of both ends of a hydrogen group carbon dioxide gas is introduced into an aqueous solution or suspension of strontium hydroxide to carbonate strontium hydroxide,
- strontium hydroxide to carbonate strontium hydroxide
- the present invention provides a divalent chain hydrocarbon group having 1 to 4 carbon atoms while stirring an aqueous solution or suspension of strontium hydroxide having a concentration in the range of 1 to 20% by mass, A dicarboxylic acid containing a carboxylic acid group bonded to each of both ends of the chain hydrocarbon group, provided that the chain hydrocarbon group is substituted with one or two or more alkyl groups having 1 to 6 carbon atoms.
- carbon dioxide gas is introduced into the aqueous solution or suspension at a flow rate of 0.5 to 200 mL / min with respect to 1 g of strontium hydroxide.
- the present invention relates to a method for producing acicular strontium carbonate particles.
- Preferred embodiments of the present invention are as follows. (1) The chain hydrocarbon group of the dicarboxylic acid is not bonded to a hydroxyl group. (2) The dicarboxylic acid includes a divalent chain hydrocarbon group substituted with a methyl group or an ethyl group. (3) The dicarboxylic acid is malonic acid having an alkyl group having 1 to 6 carbon atoms or maleic acid having an alkyl group having 1 to 6 carbon atoms. (4) The dicarboxylic acid is dissolved in an aqueous solution or suspension of strontium hydroxide in an amount of 1 to 20 parts by mass with respect to 100 parts by mass of strontium hydroxide. (5) The obtained acicular strontium carbonate particles have a size in which the average length of the major axis is in the range of 10 to 500 nm and the average aspect ratio is in the range of 2 to 10.
- the production method of the present invention it is not necessary to adjust the aqueous solution or aqueous suspension of the raw material strontium hydroxide to a temperature below the freezing point or to use a large amount of alcohol as the reaction solvent, and the average length of the major axis Can produce fine acicular strontium carbonate particles of 500 nm or less, particularly 200 nm or less.
- the acicular strontium carbonate particles obtained by the production method of the present invention are usually composed of acicular single crystal particles and do not have a brittle portion resembling a constriction, so that the strength is high and the particles are not easily granulated. For this reason, the acicular strontium carbonate particles obtained by the production method of the present invention can be advantageously used as a filler for a non-birefringent optical resin material.
- FIG. 2 is a scanning electron micrograph of strontium carbonate powder produced in Example 1.
- FIG. 2 is a scanning electron micrograph of strontium carbonate powder produced in Example 2.
- FIG. 2 is a scanning electron micrograph of strontium carbonate powder produced in Example 2.
- an aqueous solution or aqueous suspension of strontium hydroxide having a concentration of 1 to 20% by mass is used as a starting material.
- concentration of the aqueous solution or suspension of strontium hydroxide is preferably in the range of 2 to 15% by mass, more preferably in the range of 3 to 8% by mass.
- carbon dioxide gas is supplied to the aqueous solution or aqueous suspension at a flow rate in the range of 0.5 to 200 mL / min with respect to 1 g of strontium hydroxide.
- the flow rate of carbon dioxide gas is preferably in the range of 0.5 to 100 mL / min, more preferably in the range of 1 to 50 mL / min.
- carbonation of strontium hydroxide is carried out by dicarboxylation containing a divalent chain hydrocarbon group having 1 to 4 carbon atoms and carboxylic acid groups bonded to both ends of the chain hydrocarbon group. Performed in the presence of acid.
- the dicarboxylic acid is preferably a carboxylic acid represented by the following formula (I).
- L is a divalent chain hydrocarbon group having 1 to 4 carbon atoms.
- the chain hydrocarbon group may have a double bond.
- the number of carbon atoms in the chain hydrocarbon group is preferably in the range of 1 to 3, and preferably 1 or 2.
- the chain hydrocarbon group is preferably not bonded to a hydroxyl group.
- all or part of the hydrogen atoms are preferably substituted with an alkyl group having 1 to 6 carbon atoms, particularly a methyl group or an ethyl group.
- dicarboxylic acids examples include methylmalonic acid, dimethylmalonic acid, ethylmalonic acid, diethylmalonic acid, methylsuccinic acid, 2,2-dimethylsuccinic acid, 2,3-dimethylsuccinic acid, methylmaleic acid (citraconic acid) and Mention may be made of dimethylmaleic acid.
- the dicarboxylic acid is preferably dissolved in an aqueous solution or suspension of strontium hydroxide in an amount of 1 to 20 parts by mass with respect to 100 parts by mass of strontium hydroxide. More preferably, it is dissolved in
- the temperature of the aqueous solution or suspension of strontium hydroxide when carbonating strontium hydroxide is generally in the range of 1 to 100 ° C., preferably in the range of 5 to 50 ° C.
- the end point of carbonation of strontium hydroxide is generally when the pH of the aqueous solution or aqueous suspension becomes 7 or less.
- the suspension after the acicular strontium carbonate particles are formed can be dried using a normal dryer such as a spray dryer or a drum dryer to obtain strontium carbonate powder.
- the acicular strontium carbonate particles obtained by the production method of the present invention usually have an average length of a major axis determined from an SEM (scanning electron microscope) image in the range of 10 to 500 nm, particularly in the range of 10 to 200 nm. .
- the average aspect ratio (major axis / minor axis) obtained from the SEM image is in the range of 2 to 10, particularly in the range of 2 to 5.
- Example 1 366 g of strontium hydroxide octahydrate was added to 3 L of pure water having a water temperature of 10 ° C. and stirred to prepare an aqueous suspension of strontium hydroxide having a concentration of 5.6% by mass. To this aqueous strontium hydroxide suspension, 17.2 g of dimethylmalonic acid (10.3 parts by mass with respect to 100 parts by mass of strontium hydroxide) was added and stirred to dissolve. Next, while maintaining the liquid temperature of the aqueous strontium hydroxide suspension at 10 ° C., while continuing stirring, carbon dioxide gas was supplied to the aqueous suspension at a flow rate of 3.75 L / min (based on 1 g of strontium hydroxide).
- FIG. 1 An SEM photograph of the obtained strontium carbonate powder is shown in FIG. From the photograph of FIG. 1, it can be seen that the obtained strontium carbonate powder has a needle-like particle shape.
- the obtained strontium carbonate powder had a BET specific surface area of 66.3 m 2 / g.
- the aspect ratio and the length of the major axis of 300 strontium carbonate particles were measured by image analysis, and the average value was obtained.
- the average aspect ratio was 2.99, and the average of the major axis
- the length was 110 nm.
- Example 2 In place of dimethylmalonic acid, 8.5 g of methylmaleic acid (5.1 parts by mass with respect to 100 parts by mass of strontium hydroxide) was added, and the flow rate of carbon dioxide gas was 0.5 L / min (strontium hydroxide). A strontium carbonate powder was produced in the same manner as in Example 1 except that the flow rate was 3.0 mL / min for 1 g.
- FIG. 2 An SEM photograph of the obtained strontium carbonate powder is shown in FIG. From the photograph of FIG. 2, it can be seen that the particle shape of the obtained strontium carbonate powder is needle-like.
- the resulting strontium carbonate powder had a BET specific surface area of 56.0 m 2 / g.
- the average aspect ratio was 2.78, and the average of the major axis The length was 103 nm.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
従って、本発明の目的は、微細でかつ容易に粒状になりにくい針状炭酸ストロンチウム粒子を、特には氷点以下の温度とする必要がなく、またアルコールを用いなくとも製造することができる方法を提供することにある。
(1)上記ジカルボン酸の鎖状炭化水素基が水酸基と結合していない。
(2)上記ジカルボン酸がメチル基もしくはエチル基で置換された二価の鎖状炭化水素基を含む。
(3)上記ジカルボン酸が炭素原子数1~6のアルキル基を有するマロン酸もしくは炭素原子数1~6のアルキル基を有するマレイン酸である。
(4)上記ジカルボン酸が水酸化ストロンチウムの水溶液もしくは水性懸濁液中に、水酸化ストロンチウム100質量部に対して1~20質量部の範囲にて溶解している。
(5)得られる針状炭酸ストロンチウム粒子が、長径の平均長さが10~500nmの範囲にあって、平均アスペクト比が2~10の範囲のサイズを持つ。
水温10℃の純水3Lに水酸化ストロンチウム八水和物366gを投入し、撹拌して濃度5.6質量%の水酸化ストロンチウム水性懸濁液を調製した。この水酸化ストロンチウム水性懸濁液にジメチルマロン酸17.2g(水酸化ストロンチウム100質量部に対して10.3質量部)を加えて撹拌して溶解させた。次いで、水酸化ストロンチウム水性懸濁液の液温を10℃に維持しつつ、撹拌を続けながら、該水性懸濁液に二酸化炭素ガスを3.75L/分の流量(水酸化ストロンチウム1gに対して22.4mL/分の流量)にて、該水性懸濁液のpHが7になるまで吹き込んで、炭酸ストロンチウム粒子を生成させた後、さらに30分間撹拌を続けて、炭酸ストロンチウム粒子水性懸濁液を得た。得られた水性懸濁液を乾燥して炭酸ストロンチウム粉末を得た。
ジメチルマロン酸の代わりにメチルマレイン酸8.5g(水酸化ストロンチウム100質量部に対して5.1質量部)を加えたこと、二酸化炭素ガスの流量を0.5L/分の流量(水酸化ストロンチウム1gに対して3.0mL/分の流量)としたこと以外は、実施例1と同様にして、炭酸ストロンチウム粉末を製造した。
Claims (6)
- 濃度が1~20質量%の範囲にある水酸化ストロンチウムの水溶液もしくは水性懸濁液を撹拌しながら、炭素原子数が1~4の二価の鎖状炭化水素基と、その鎖状炭化水素基の両端のそれぞれに結合したカルボン酸基とを含むジカルボン酸、但し、鎖状炭化水素基は一もしくは二以上の炭素原子数が1~6のアルキル基で置換されていてもよい、の存在下にて、該水溶液もしくは水性懸濁液に二酸化炭素ガスを水酸化ストロンチウム1gに対して0.5~200mL/分の範囲の流量にて導入して、水酸化ストロンチウムを炭酸化させることを特徴とする針状炭酸ストロンチウム粒子の製造方法。
- 上記ジカルボン酸の鎖状炭化水素基が水酸基と結合していない請求項1に記載の針状炭酸ストロンチウム粒子の製造方法。
- 上記ジカルボン酸がメチル基もしくはエチル基で置換された二価の鎖状炭化水素基を含む請求項1に記載の針状炭酸ストロンチウム粒子の製造方法。
- 上記ジカルボン酸が炭素原子数1~6のアルキル基を有するマロン酸もしくは炭素原子数1~6のアルキル基を有するマレイン酸である請求項1に記載の針状炭酸ストロンチウム粒子の製造方法。
- 上記ジカルボン酸が水酸化ストロンチウムの水溶液もしくは水性懸濁液中に、水酸化ストロンチウム100質量部に対して1~20質量部の範囲にて溶解している請求項1に記載の針状炭酸ストロンチウム粒子の製造方法。
- 得られる針状炭酸ストロンチウム粒子が、長径の平均長さが10~500nmの範囲にあって、平均アスペクト比が2~10の範囲のサイズを持つ請求項1に記載の針状炭酸ストロンチウム粒子の製造方法。
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US13/985,322 US9187338B2 (en) | 2011-02-15 | 2012-02-15 | Process for manufacturing needle-shaped strontium carbonate particles |
JP2012557985A JP5798574B2 (ja) | 2011-02-15 | 2012-02-15 | 針状炭酸ストロンチウム粒子の製造方法 |
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Cited By (4)
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WO2015141817A1 (ja) * | 2014-03-20 | 2015-09-24 | 宇部マテリアルズ株式会社 | 針状炭酸ストロンチウム微粒子及びその分散液 |
WO2017014219A1 (ja) * | 2015-07-21 | 2017-01-26 | 宇部興産株式会社 | 位相差調整組成物並びにそれを用いた接着層、位相差フィルム、光学積層体及び画像表示装置 |
WO2017029995A1 (ja) * | 2015-08-20 | 2017-02-23 | 宇部興産株式会社 | 光学フィルム及び画像表示装置 |
EP3061728A4 (en) * | 2013-10-25 | 2017-06-21 | Ube Material Industries, Ltd. | Needle-like strontium carbonate fine powder and method for producing same |
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- 2012-02-15 WO PCT/JP2012/053479 patent/WO2012111691A1/ja active Application Filing
- 2012-02-15 TW TW101105186A patent/TWI516448B/zh not_active IP Right Cessation
- 2012-02-15 JP JP2012557985A patent/JP5798574B2/ja active Active
- 2012-02-15 US US13/985,322 patent/US9187338B2/en not_active Expired - Fee Related
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Cited By (6)
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EP3061728A4 (en) * | 2013-10-25 | 2017-06-21 | Ube Material Industries, Ltd. | Needle-like strontium carbonate fine powder and method for producing same |
WO2015141817A1 (ja) * | 2014-03-20 | 2015-09-24 | 宇部マテリアルズ株式会社 | 針状炭酸ストロンチウム微粒子及びその分散液 |
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WO2017029995A1 (ja) * | 2015-08-20 | 2017-02-23 | 宇部興産株式会社 | 光学フィルム及び画像表示装置 |
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JPWO2012111691A1 (ja) | 2014-07-07 |
TWI516448B (zh) | 2016-01-11 |
TW201238900A (en) | 2012-10-01 |
US9187338B2 (en) | 2015-11-17 |
JP5798574B2 (ja) | 2015-10-21 |
US20140065052A1 (en) | 2014-03-06 |
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