JPH01167216A - Production of acicular barium carbonate - Google Patents
Production of acicular barium carbonateInfo
- Publication number
- JPH01167216A JPH01167216A JP32614787A JP32614787A JPH01167216A JP H01167216 A JPH01167216 A JP H01167216A JP 32614787 A JP32614787 A JP 32614787A JP 32614787 A JP32614787 A JP 32614787A JP H01167216 A JPH01167216 A JP H01167216A
- Authority
- JP
- Japan
- Prior art keywords
- alcohol
- barium carbonate
- water
- barium
- barium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 9
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 11
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 5
- 229910001626 barium chloride Inorganic materials 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 235000017550 sodium carbonate Nutrition 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000012776 electronic material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 description 1
- 239000004386 Erythritol Substances 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 description 1
- 235000019414 erythritol Nutrition 0.000 description 1
- 229940009714 erythritol Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01F11/188—Barium carbonate
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Landscapes
- 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
【発明の詳細な説明】 産業上の利用分野 従来炭酸バリウムは下記の方法で製造されている。[Detailed description of the invention] Industrial applications Conventionally, barium carbonate has been produced by the following method.
（１）ソーダ灰法
ＢａＳ＋Ｎａ２ＣＯ３→ＢａＣＯ３＋Ｎａ２Ｓ（２）ガ
ス法
２ＢａＳ＋ＣＯ２＋Ｈ２Ｏ→ＢａＣＯ３＋Ｂａ（ＳＨ）
２
Ｂａ（ＳＨ）２＋ＣＯ２＋Ｈ２Ｏ→ＢａＣＯ３＋２Ｈ２
Ｓ
（３）塩化バリウム法
ＢａＣｌ２＋（ＮＨ４）２ＣＯ３→ＢａＣＯ３＋２ＮＨ
４Ｃｌ
ＢａＣｌ２＋Ｎａ２ＣＯ３→ＢａＣＯ３＋２ＮａＣｌ
（４）水酸化バリウム法
Ｂａ（ＯＨ）２＋ＣＯ２→ＢａＣＯ３＋Ｈ２Ｏ（１）、
（２）のソーダ灰法、ガス法は原料に硫化バリウムを使
用するため、水洗等の精製工程を繰り返しても、不純物
として硫黄、硫黄を含む化合物がＳとして０．００４％
〜０．１２％程度残留し、又その形状もソーダ灰法では
ほぼ球状となり、ガス法では棒状となって、ある種の用
途、例えば電子材料用としては好ましくない。(1) Soda ash method BaS+Na2CO3→BaCO3+Na2S (2) Gas method 2BaS+CO2+H2O→BaCO3+Ba(SH)
2 Ba(SH)2+CO2+H2O→BaCO3+2H2
S (3) Barium chloride method BaCl2+(NH4)2CO3→BaCO3+2NH
4Cl BaCl2+Na2CO3→BaCO3+2NaCl (4) Barium hydroxide method Ba(OH)2+CO2→BaCO3+H2O (1),
(2) Since the soda ash method and gas method use barium sulfide as a raw material, even if the purification process such as water washing is repeated, sulfur and sulfur-containing compounds will remain as impurities at 0.004% as S.
Approximately 0.12% remains, and its shape becomes almost spherical in the soda ash method, and rod-shaped in the gas method, which is not preferable for certain uses, such as electronic materials.
一方不純物を殆んど含まない高純度の炭酸バリウムの製
造方法としては（３）、（４）の塩化バリウム、水酸化
バリウムを使用する方法が挙げられる。（３）、（４）
の方法では原料段階での精製、炭酸バリウム段階での精
製がやり易く、高純度品が得られる。On the other hand, methods for producing high-purity barium carbonate containing almost no impurities include methods (3) and (4) using barium chloride and barium hydroxide. (3), (4)
In this method, purification at the raw material stage and at the barium carbonate stage is easy, and a high-purity product can be obtained.
しかし塩化バリウム法、水酸化バリウム法共に得られる
製品の形状は球状あるいは棒状であり、ある種の用途、
例えば電子材料用には好ましくない。However, the shape of the products obtained by both the barium chloride method and the barium hydroxide method is spherical or rod-shaped, and for certain purposes,
For example, it is not preferred for electronic materials.
発明が解決しようとする問題点
本発明は従来見られない高純度であって且つ針状の炭酸
バリウムを製造することを目的とした、高純度で針状の
炭酸バリウムが得られれば、ある種の用途、例えば電子
材料用に好適であると考えたからである。Problems to be Solved by the Invention The present invention aims to produce barium carbonate of high purity and acicular shape that has never been seen before.If high purity and acicular barium carbonate can be obtained, certain This is because it is considered suitable for applications such as electronic materials.
即ち針状にすれば、他の形状に比して、粒子の表面積が
大きくなり、固相反応の原料として使用する場合、表面
積が大きいほど、通常は反応性に富むからである。特に
コンデンサ用として酸化チタンと反応させるような場合
、その傾向が顕著である。ＢａＣＯ３＋ＴｉＯ２→Ｂａ
ＴｉＯ３＋ＣＯ問題点を解決するための手段
本発明者等は、水酸化バリウム水溶液中に水可溶性アル
コールを存在させ、該液中に炭酸ガスを吹き込むことに
より針状高純度の炭酸バリウムが得られることを見出し
本発明を完成したのである。That is, if the particle is shaped like a needle, the surface area of the particle becomes larger than that of other shapes, and when the particle is used as a raw material for a solid phase reaction, the larger the surface area, the richer the reactivity is usually. This tendency is particularly noticeable when reacting with titanium oxide for capacitors. BaCO3+TiO2→Ba
Means for Solving the TiO3+CO Problem The present inventors have discovered that acicular highly pure barium carbonate can be obtained by making water-soluble alcohol exist in an aqueous barium hydroxide solution and blowing carbon dioxide into the solution. Heading: The present invention has been completed.
以下に本発明方法の構成を詳述する。The configuration of the method of the present invention will be explained in detail below.
水酸化バリウム水溶液の濃度はＢａ（ＯＨ）２、８Ｈ２
Ｏとして５ｇ／ｌ〜５００ｇ／ｌ、好ましくは２０ｇ／
ｌ〜１００ｇ／ｌである。The concentration of barium hydroxide aqueous solution is Ba(OH)2,8H2
5g/l to 500g/l as O, preferably 20g/l
1 to 100 g/l.
存在させるアルコールの種類は、水可溶性であれば何で
も良い。例えばメタノール、エタノールブロパノール、
ブタノール、エチレングリコール、グリセリン、エリス
リトール、２−アミノエタノール等が挙げられる。Any type of alcohol may be present as long as it is water-soluble. For example, methanol, ethanolpropanol,
Examples include butanol, ethylene glycol, glycerin, erythritol, 2-aminoethanol, and the like.
アルコールの存在量は水に対して容積で２０％〜１００
％、好ましくは２０〜５０％である。アルコールを多く
使用する程、針状比は大となる。炭酸ガスの吹き込み速
度は特に制限はなく、通常のガス反応と同じである。The amount of alcohol present is 20% to 100% by volume relative to water.
%, preferably 20-50%. The more alcohol used, the higher the acicular ratio becomes. The blowing speed of carbon dioxide gas is not particularly limited and is the same as in a normal gas reaction.
反応温度は１０℃〜３０℃が好ましい範囲である。The reaction temperature is preferably in the range of 10°C to 30°C.
反応終了後の精製操作は公知の方法に従い、濾過、水洗
、乾燥、必要に応じて粉砕すれば良い。Purification operations after the completion of the reaction may be carried out in accordance with known methods such as filtration, washing with water, drying, and pulverization if necessary.
得られる針状炭酸バリウムは短径と長径の比率が２０〜
３０、長径の長さが０．５Ｍ〜５Ｍである。The obtained acicular barium carbonate has a ratio of short axis to long axis of 20~
30, the length of the major axis is 0.5M to 5M.
又表面積は２０ｍ２／ｇ前後である。Moreover, the surface area is around 20 m2/g.
純度は９９．８以上である。Purity is 99.8 or higher.
発明の効果
本発明によれば、上記の如く従来見られなかった高純度
の針状炭酸バリウムが得られ、従来の炭酸バリウムでは
不適とされた分野にも好適に用いられる。Effects of the Invention According to the present invention, as described above, acicular barium carbonate of high purity, which has never been seen before, can be obtained, and it can be suitably used in fields where conventional barium carbonate is unsuitable.
以下実施例により具体的に説明する。This will be explained in detail below using examples.
実施例１
水１０ｌとメタノール１０ｌを混合し、それに水酸化バ
リウム（Ｂａ（ＯＨ）２・８Ｈ２Ｏ）を５０ｇ／ｌにな
るように溶解させ、濾過する。Example 1 10 liters of water and 10 liters of methanol are mixed, barium hydroxide (Ba(OH)2.8H2O) is dissolved therein at a concentration of 50 g/l, and the mixture is filtered.
その溶液を温度３０℃に調節し、攪拌しながら散気管に
て炭酸ガスを６００ｍｌ／ｍｉｎの速度で導通した。反
応終了は電導計、ＰＨ計にて測定し、電導度０．２６ｍ
ｓ／ｃｍ、ＰＨ６．２５にて反応を終了し、炭酸バリウ
ムを得た。The temperature of the solution was adjusted to 30° C., and carbon dioxide gas was passed through the solution at a rate of 600 ml/min through a diffuser tube while stirring. The completion of the reaction was measured using a conductivity meter and a PH meter, and the conductivity was 0.26m.
The reaction was completed at pH 6.25 and barium carbonate was obtained.
得られた炭酸バリウムは下記の平均値を有していた。針
状
長径２μ、長径／短径３０
表面積２０ｍ２／ｇ、純度９９．９％
実施例２
メタノールの代わりにエチレングリコールを用い、実施
例１を同様の反応を行ない炭酸バリウムを得た。The obtained barium carbonate had the following average value. Acicular major axis 2μ, major axis/minor axis 30, surface area 20 m2/g, purity 99.9% Example 2 Barium carbonate was obtained by carrying out the same reaction as in Example 1, using ethylene glycol instead of methanol.
得られた炭酸バリウムは下記の平均値を有していた。針
状
長径１μ、長径／短径２０
表面積２０ｍ２／ｇ、純度９９．９％
比較例１
アルコールを使用せず、他は実施例１と同様にして炭酸
バリウムを得た。The obtained barium carbonate had the following average value. Acicular major axis 1μ, major axis/minor axis 20, surface area 20 m2/g, purity 99.9% Comparative Example 1 Barium carbonate was obtained in the same manner as in Example 1, except that no alcohol was used.
得られた炭酸バリウムは棒状であり、下記の平均値を有
していた。The obtained barium carbonate was rod-shaped and had the following average value.
表面積１５ｍ２／ｇ、純度９９．９％Surface area 15m2/g, purity 99.9%
第１図は実施例１により得られた炭酸バリウム、第２図
は実施例２により得られた炭酸バリウム、第３図は比較
例１により得られた炭酸バリウムそれぞれの電子顕微鏡
写眞（×６０００）を示す。Figure 1 shows the barium carbonate obtained in Example 1, Figure 2 shows the barium carbonate obtained in Example 2, and Figure 3 shows the barium carbonate obtained in Comparative Example 1 using an electron microscope. ) is shown.
Claims (1)
バリウムを製造する方法において、水酸化バリウム水溶
液中に水可溶性アルコールを存在させることを特徴とす
る針状高純度炭酸バリウムの製造方法。1. A method for producing barium carbonate by reacting an aqueous barium hydroxide solution with carbon dioxide gas, which is characterized in that a water-soluble alcohol is present in the aqueous barium hydroxide solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32614787A JPH01167216A (en) | 1987-12-23 | 1987-12-23 | Production of acicular barium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32614787A JPH01167216A (en) | 1987-12-23 | 1987-12-23 | Production of acicular barium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01167216A true JPH01167216A (en) | 1989-06-30 |
Family
ID=18184575
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32614787A Pending JPH01167216A (en) | 1987-12-23 | 1987-12-23 | Production of acicular barium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01167216A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005306640A (en) * | 2004-04-20 | 2005-11-04 | Fuji Photo Film Co Ltd | Method for manufacturing crystal of alkaline earth metal carbonate and crystal of alkaline earth metal carbonate |
| JP2006021987A (en) * | 2004-06-08 | 2006-01-26 | Fuji Photo Film Co Ltd | Method for production of carbonate |
| JP2007176789A (en) * | 2005-12-01 | 2007-07-12 | Ube Material Industries Ltd | Barium carbonate powder and method of manufacturing the same |
| JP2009114015A (en) * | 2007-11-05 | 2009-05-28 | Nippon Chem Ind Co Ltd | Barium carbonate particle powder, method for producing the same, and method for producing perovskite-type barium titanate |
| US8153093B2 (en) | 2004-06-08 | 2012-04-10 | Fujifilm Corporation | Process for producing carbonate particles |
| US10449522B2 (en) * | 2015-07-30 | 2019-10-22 | Basf Corporation | Process for manufacture of NOx storage materials |
-
1987
- 1987-12-23 JP JP32614787A patent/JPH01167216A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005306640A (en) * | 2004-04-20 | 2005-11-04 | Fuji Photo Film Co Ltd | Method for manufacturing crystal of alkaline earth metal carbonate and crystal of alkaline earth metal carbonate |
| JP2006021987A (en) * | 2004-06-08 | 2006-01-26 | Fuji Photo Film Co Ltd | Method for production of carbonate |
| US8153093B2 (en) | 2004-06-08 | 2012-04-10 | Fujifilm Corporation | Process for producing carbonate particles |
| JP2007176789A (en) * | 2005-12-01 | 2007-07-12 | Ube Material Industries Ltd | Barium carbonate powder and method of manufacturing the same |
| JP2009114015A (en) * | 2007-11-05 | 2009-05-28 | Nippon Chem Ind Co Ltd | Barium carbonate particle powder, method for producing the same, and method for producing perovskite-type barium titanate |
| US10449522B2 (en) * | 2015-07-30 | 2019-10-22 | Basf Corporation | Process for manufacture of NOx storage materials |
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