JPH0360729A - Production of fine particles - Google Patents
Production of fine particlesInfo
- Publication number
- JPH0360729A JPH0360729A JP1197272A JP19727289A JPH0360729A JP H0360729 A JPH0360729 A JP H0360729A JP 1197272 A JP1197272 A JP 1197272A JP 19727289 A JP19727289 A JP 19727289A JP H0360729 A JPH0360729 A JP H0360729A
- Authority
- JP
- Japan
- Prior art keywords
- solution
- water
- particles
- solns
- salts
- 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.)
- Granted
Links
- 239000010419 fine particle Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000002245 particle Substances 0.000 claims abstract description 26
- 150000003839 salts Chemical class 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000011882 ultra-fine particle Substances 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 239000012047 saturated solution Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 abstract description 6
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 abstract description 5
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 abstract description 5
- 229910001626 barium chloride Inorganic materials 0.000 abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 abstract description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 abstract description 4
- 235000011130 ammonium sulphate Nutrition 0.000 abstract description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 abstract description 3
- 239000001099 ammonium carbonate Substances 0.000 abstract description 3
- 239000001110 calcium chloride Substances 0.000 abstract description 3
- 229910001628 calcium chloride Inorganic materials 0.000 abstract description 3
- 239000011736 potassium bicarbonate Substances 0.000 abstract description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 abstract description 3
- 235000015497 potassium bicarbonate Nutrition 0.000 abstract description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 abstract description 3
- 235000011181 potassium carbonates Nutrition 0.000 abstract description 3
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 abstract description 3
- 229940086066 potassium hydrogencarbonate Drugs 0.000 abstract description 3
- 235000017550 sodium carbonate Nutrition 0.000 abstract description 3
- 235000011148 calcium chloride Nutrition 0.000 abstract description 2
- 238000000635 electron micrograph Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 6
- 238000000502 dialysis Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 239000012266 salt solution Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 2
- 239000001639 calcium acetate Substances 0.000 description 2
- 235000011092 calcium acetate Nutrition 0.000 description 2
- 229960005147 calcium acetate Drugs 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000010414 supernatant solution Substances 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000019700 dicalcium phosphate Nutrition 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- AYOOGWWGECJQPI-NSHDSACASA-N n-[(1s)-1-(5-fluoropyrimidin-2-yl)ethyl]-3-(3-propan-2-yloxy-1h-pyrazol-5-yl)imidazo[4,5-b]pyridin-5-amine Chemical compound N1C(OC(C)C)=CC(N2C3=NC(N[C@@H](C)C=4N=CC(F)=CN=4)=CC=C3N=C2)=N1 AYOOGWWGECJQPI-NSHDSACASA-N 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Colloid Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用範囲）
本発明は、微粒子の製造方法に関する。詳しくは、水に
難溶性の塩で単分散性の優れた微粒子または超微粒子の
製造方法である。DETAILED DESCRIPTION OF THE INVENTION (Scope of Industrial Application) The present invention relates to a method for producing fine particles. Specifically, it is a method for producing fine particles or ultrafine particles of a salt that is poorly soluble in water and has excellent monodispersity.
（従来の技術）
微粒子あるいは超微粒子の製造においては、乾式法と湿
式法とが公知である。しかし、塩の製造においては蒸着
、スバタリング等の乾式法は塩が分解してしまうため適
さない。(Prior Art) In the production of fine particles or ultrafine particles, dry methods and wet methods are known. However, dry methods such as vapor deposition and sputtering are not suitable for the production of salt because the salt decomposes.
（解決しようとする問題点）
湿式法においては、従来濃厚溶液では行われていないが
、そのため希薄溶液の反応では、製造効率が悪く、又粒
子の単分散性が良くないという欠点があった。(Problems to be Solved) Conventionally, the wet method has not been carried out using a concentrated solution, and therefore, a reaction using a dilute solution has the drawbacks of poor production efficiency and poor monodispersity of particles.
（問題点を解決する為の手段）
本発明者らは、鋭意研究を重ねた結果、水に難溶性の塩
を製造する際、二種の塩の含水飽和溶液または濃厚溶液
を混合するとき、単分散性の優れた微粒子または超微粒
子を効率よく製造することが出来ることを見いだした。(Means for solving the problem) As a result of extensive research, the present inventors have found that when mixing a water-containing saturated solution or a concentrated solution of two types of salts when producing a salt that is poorly soluble in water, It has been found that fine particles or ultrafine particles with excellent monodispersity can be efficiently produced.
すなわち、反応方法としては二種の飽和溶液または濃厚
溶液を調製し、一方の溶液を反応槽に入れ撹拌しつつ他
方の溶液を加える方法があるがこの方法に限定されるわ
けでなく、たとえば撹拌しながら二種の溶液を同時に反
応槽にいれることも可能であるし、二種の溶液を反応槽
に入れ終わってから撹拌してもよい。加え終わったら撹
拌を続け、ゲル化した時点で撹拌をやめしばらく放置す
る。ゲル化しないときはさらにしばらく撹拌を続ける。In other words, the reaction method includes preparing two types of saturated or concentrated solutions, placing one solution in a reaction tank and adding the other solution while stirring, but is not limited to this method. For example, stirring However, it is also possible to put the two types of solutions into the reaction tank at the same time, or it is possible to stir the two types of solutions after they have been put into the reaction tank. When the addition is complete, continue stirring, and when it becomes a gel, stop stirring and leave it for a while. If the mixture does not gel, continue stirring for a while longer.
両者とも放置するとゾル化し流動性を示す。When both are left to stand, they turn into sol and exhibit fluidity.
微粒子、超微粒子をゾル液から分離するには、ゾル液は
上澄み液と粒子系に分離するので、又分離しにくいとき
は水で希釈すると分離するのでその上澄み液を捨てる。To separate fine particles and ultrafine particles from a sol solution, the sol solution is separated into a supernatant solution and a particle system, and if separation is difficult, diluting with water will separate the sol solution, and the supernatant solution is discarded.
粒子の精製には水を加えて上澄みを取る操作を繰り返す
か、透析を行う。To purify the particles, repeat the process of adding water and removing the supernatant, or perform dialysis.
本発明の反応に用いられる塩は、もう一方の塩と反応し
て水に難溶の塩を形成するものならばなんでもよい。例
えば、塩化カルシウム、炭酸ナトリウム、炭酸カリウム
、炭酸水素カリウム、炭酸水素アンモニウム、塩化バリ
ウム、硫酸ナトリウム、酢酸バリウム、酢酸カルシウム
、硫酸アンモニウム、 リン酸水素ナトリウム等がある
。The salt used in the reaction of the present invention may be any salt that reacts with the other salt to form a salt that is sparingly soluble in water. Examples include calcium chloride, sodium carbonate, potassium carbonate, potassium hydrogen carbonate, ammonium hydrogen carbonate, barium chloride, sodium sulfate, barium acetate, calcium acetate, ammonium sulfate, sodium hydrogen phosphate, and the like.
本発明の製造方法で製造される微粒子または超微粒子で
水に難溶性の塩は、例えば硫酸バリウム、炭酸バリウム
、炭酸カルシウム、 リン酸水素カルシウム等がある。Examples of the fine particles or ultrafine particles and sparingly water-soluble salts produced by the production method of the present invention include barium sulfate, barium carbonate, calcium carbonate, calcium hydrogen phosphate, and the like.
本発明における微粒子とは、粒子径が１μｍ以下、超微
粒子とは粒子径１１００ｎ以下のものをいう。In the present invention, fine particles refer to particles with a particle size of 1 μm or less, and ultrafine particles refer to particles with a particle size of 1100 nm or less.
本発明における濃厚溶液は、塩によって溶解度が異なる
ので一概にはいえｔｔいが、塩それぞれの溶解度の６０
％以上、好ましくは８０％以上であれば、本発明の効果
は充分に達成できる。Since the solubility of the concentrated solution in the present invention differs depending on the salt, it cannot be generalized, but the solubility of the concentrated solution is 60%
% or more, preferably 80% or more, the effects of the present invention can be fully achieved.
本発明の反応に用いる塩の溶液は水溶液が好ましいがア
ルコールなどが含有されても塩が溶解すれば問題はない
。The salt solution used in the reaction of the present invention is preferably an aqueous solution, but there is no problem even if alcohol or the like is contained as long as the salt is dissolved.
反応させる二種の塩の溶液及び混合した塩溶液は加温加
圧する必要はないが、加温または加圧しても構わない。The solution of the two salts to be reacted and the mixed salt solution do not need to be heated and pressurized, but may be heated or pressurized.
本発明における塩の水溶液の量は反応の理論量あれば充
分である。In the present invention, it is sufficient that the amount of the aqueous salt solution is the theoretical amount for the reaction.
さらに、反応に用いる塩に酢酸塩を使用すると粒子径が
非常に小さくなることを見いだした。例えば、酢酸バリ
ウムと硫酸アンモニウム、硫酸アルミニウム、または硫
酸カルシウムの組合せ、または、酢酸カルシウムと炭酸
カルシウム、炭酸ナトリウム、炭酸カリウム、炭酸水素
アンモニウム、または炭酸水素カリウムの組合せで本発
明の製造方法で製造するといずれの組合せにおいても粒
子径が約５０ｎｍ以下の超微粒子を生成した。Furthermore, we found that the particle size becomes extremely small when acetate is used as the salt used in the reaction. For example, when produced by the production method of the present invention using a combination of barium acetate and ammonium sulfate, aluminum sulfate, or calcium sulfate, or a combination of calcium acetate and calcium carbonate, sodium carbonate, potassium carbonate, ammonium hydrogen carbonate, or potassium hydrogen carbonate, Ultrafine particles having a particle diameter of about 50 nm or less were also produced in the combination of the above.
（実施例）
以下、本発明の実施例を示すが、本発明はこれに限定さ
れるものではない。(Example) Examples of the present invention will be shown below, but the present invention is not limited thereto.
実施例−１（炭酸カルシウムの製造）
４０％の塩化カルシウム水溶液１５．７ｇを激しく撹拌
しながら１９．０％の炭酸ナトリウム水溶液を３１．２
１加える。加え終わった後ゲル化するが、撹拌を続ける
と数分でゾル状になる。透析後の粒子の電顕写真を図１
に示した。粒径のそろった立方体粒子で一辺約５００ｎ
ｍであった。Ｘ線解析によるとカルサイト構造で結晶化
度は非常に高かった（図２）。Example-1 (Manufacture of calcium carbonate) While vigorously stirring 15.7 g of 40% calcium chloride aqueous solution, 31.2 g of 19.0% sodium carbonate aqueous solution was added.
Add 1. It will turn into a gel after the addition is complete, but if you keep stirring it will turn into a sol in a few minutes. Figure 1 shows an electron micrograph of the particles after dialysis.
It was shown to. Cubic particles with uniform particle size, approximately 500n on a side
It was m. According to X-ray analysis, it had a calcite structure and a very high degree of crystallinity (Figure 2).
炭酸カルシウムの収率は理論量の９８．７％であった。The yield of calcium carbonate was 98.7% of the theoretical amount.
実施例−２（炭酸バリウムの製造）
２６％の塩化バリウム水溶液２４ｇを撹拌しながらこれ
に２３％の炭酸ナトリウム水溶液１４ｇを加える。加え
る過程でゲル状のものが部分的に生成するが、全部加え
終わった時点ではゾル状になっている。Example 2 (Manufacture of barium carbonate) 14 g of a 23% sodium carbonate aqueous solution is added to 24 g of a 26% barium chloride aqueous solution with stirring. During the addition process, a gel-like substance is partially formed, but by the time the addition is complete, it has become a sol-like substance.
粒子の光学顕微鏡写真を図３に示す。An optical micrograph of the particles is shown in FIG.
炭酸バリウムの収率は理論量の９９．３％であった。The yield of barium carbonate was 99.3% of the theoretical amount.
実施例−３（硫酸バリウムの製造）
２５％の塩化バリウム水溶液１７ｇを撹拌しながら、こ
れに１８．０％の硫酸ナトリウム水溶液１６．２ｇを加
える。途中ゲル状物が部分的に生成するが、全体として
ゲル化せず、加え終わった時点でゾル状となっている。Example 3 (Manufacture of barium sulfate) While stirring 17 g of a 25% barium chloride aqueous solution, 16.2 g of an 18.0% sodium sulfate aqueous solution is added thereto. A gel-like substance is partially formed during the process, but it does not gel as a whole and becomes a sol-like substance when the addition is finished.
透析後の粒子の電顕写真を図４に示した。単分散性の良
い立方体粒子で一辺約１１００ｎであった。Ｘ線解析に
よると図５のような重晶石構造で、結晶化度は非常に高
い。An electron micrograph of the particles after dialysis is shown in FIG. The particles were cubic particles with good monodispersity and each side was approximately 1100 nm. According to X-ray analysis, it has a barite structure as shown in Figure 5, with a very high degree of crystallinity.
硫酸バリウムの収率は理論量の９９．６％であった。The yield of barium sulfate was 99.6% of the theoretical amount.
実施例−４（硫酸バリウムの製造）
４１％の酢酸バリウム水溶液９ｍ１（１２，２ｇ）を撹
拌しながらこれに２８％の硫酸アンモニウム水溶液９＋
ｎ１（１０，４ｇ）を加えると全体がゲル化し、後流動
性が少し出るがチキソトロヒックな状態であった。水で
希釈すると上澄み液と粒子群に分離した。透析後電顕写
真をとると、図６のようなほぼ立方体粒子で単分散性の
良い、−選的３０〜４０ｎｍの超微粒子である。Ｘ線解
析の結果は、実施例−３のものと全く同じであった。Example 4 (Manufacture of barium sulfate) 9 ml (12.2 g) of a 41% barium acetate aqueous solution was added with 28% ammonium sulfate aqueous solution 9+ while stirring.
When n1 (10.4 g) was added, the entire mixture turned into a gel, and although there was some after-fluidity, it was in a thixotropic state. When diluted with water, it was separated into a supernatant liquid and a particle group. An electron micrograph taken after dialysis shows that the particles are approximately cubic particles with good monodispersity, as shown in FIG. 6, and ultrafine particles with a diameter of 30 to 40 nm. The results of X-ray analysis were exactly the same as those of Example-3.
硫酸バリウムの収率は理論量の９８．９％であった。The yield of barium sulfate was 98.9% of the theoretical amount.
実施例−５（硫酸バリウムの製造）
２５％の塩化バリウム水溶液１１ｇを撹拌しながらこれ
に２３％の硫酸アルミニウム水溶液１５ｇを加えていく
。途中ゲル状物を生じるが最終的に全体のゲル化はみら
れない。透析後の電顕写真は図７のようで柱状〜楕円形
で長径的４０〜７０Ｔｌｌ１１の超微粒子であった。Example 5 (Manufacture of barium sulfate) 15 g of a 23% aluminum sulfate aqueous solution is added to 11 g of a 25% barium chloride aqueous solution while stirring. A gel-like substance is formed during the process, but no gelation is observed in the end. The electron micrograph after dialysis was as shown in FIG. 7, which showed ultrafine particles having a columnar to elliptical shape and a major diameter of 40 to 70 Tll11.
硫酸バリウムの収率は理論量の９９．８％であった。The yield of barium sulfate was 99.8% of the theoretical amount.
実施例−６（硫酸バリウムの製造）
４１％の酢酸バリウム水溶液１９ｇを撹拌しつつ、これ
に２３％の硫酸アルミニウム水溶液１９τを加えていく
。ゲル化の状況は実施例−５と同捻 透析後の電顕写真
は図８のようで、楕円形に近く長径４０ ｎｈ短径２０
〜３０ｎｍである。Ｘ線解析によると、結晶型、結晶化
度に変化はない。Example-6 (Manufacture of barium sulfate) While stirring 19 g of a 41% aqueous barium acetate solution, 19 τ of a 23% aqueous aluminum sulfate solution was added. The gelation situation is the same as in Example 5. The electron micrograph after dialysis is as shown in Figure 8, and it is nearly elliptical with a major axis of 40 nh and a minor axis of 20 nm.
~30 nm. According to X-ray analysis, there is no change in crystal type or crystallinity.
硫酸バリウムの収率は理論量の９９．４％であった。The yield of barium sulfate was 99.4% of the theoretical amount.
（発明の効果）
本発明によれば、水に難溶性の塩を製造する際、二種の
含水飽和溶液または濃厚溶液を、加温も加圧もすること
なく常温常圧で単に混合することによりゲル状態または
それに近い状態を経て計算量に近い収量で単分散性の優
れた微粒子または超微粒子を得ることができ、しかも操
作が簡単であり、簡易な装置で充分という利点がある。(Effects of the Invention) According to the present invention, when producing a salt that is poorly soluble in water, two types of water-containing saturated solutions or concentrated solutions can be simply mixed at room temperature and normal pressure without heating or pressurizing. By this method, it is possible to obtain fine particles or ultrafine particles with excellent monodispersity through a gel state or a state close to it, with a yield close to the calculated amount, and it has the advantage that the operation is simple and a simple device is sufficient.
図１は炭酸カルシウム粒子の電顕写尤 図２はそのＸ線
解析図である。図３は炭酸バリウムの電顕写真である。
図４．６．７．８、はいずれも硫酸バリウムの電顕写真
図５は硫酸バリウムのＸ線解析図である。Figure 1 is an electron micrograph of calcium carbonate particles, and Figure 2 is an X-ray analysis diagram thereof. FIG. 3 is an electron micrograph of barium carbonate. Figures 4.6, 7.8 are all electron micrographs of barium sulfate. Figure 5 is an X-ray analysis diagram of barium sulfate.
Claims (6)
飽和溶液または濃厚溶液を混合することにより、単分散
性の優れた、粒子径が１０μｍ以下である微粒子または
超微粒子の製造方法(1) When producing salts that are sparingly soluble in water, fine or ultrafine particles with excellent monodispersity and a particle size of 10 μm or less can be obtained by mixing a water-containing saturated solution or a concentrated solution of two types of salts. manufacturing method
飽和溶液または濃厚溶液を調製し、一方の溶液を反応槽
にいれ撹拌しつつ、他方の溶液を加えることを特徴とす
る請求項（１）の製造方法(2) A claim characterized in that, when producing a salt that is sparingly soluble in water, two kinds of water-containing saturated solutions or concentrated solutions are prepared, one solution is put into a reaction tank, and while stirring, the other solution is added. Manufacturing method of item (1)
はリン酸塩である請求項（１）記載の製造方法(3) The production method according to claim (1), wherein the water-insoluble salt produced is a carbonate, sulfate, or phosphate.
は濃厚水溶液である請求項（１）記載の製造方法(4) The manufacturing method according to claim (1), wherein the water-containing saturated solution or concentrated solution is a saturated aqueous solution or a concentrated aqueous solution.
酸カルシウムであることを特徴とする請求項（１）また
は（３）の製造方法(5) The manufacturing method according to claim (1) or (3), wherein the water-insoluble salt produced is barium sulfate or calcium carbonate.
とする請求項（１）の製造方法。(6) The method of claim (1), wherein one of the salts used in the reaction is an acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19727289A JP3321155B2 (en) | 1989-07-29 | 1989-07-29 | Method for producing fine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19727289A JP3321155B2 (en) | 1989-07-29 | 1989-07-29 | Method for producing fine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0360729A true JPH0360729A (en) | 1991-03-15 |
| JP3321155B2 JP3321155B2 (en) | 2002-09-03 |
Family
ID=16371710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19727289A Expired - Fee Related JP3321155B2 (en) | 1989-07-29 | 1989-07-29 | Method for producing fine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3321155B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006309999A (en) * | 2005-04-27 | 2006-11-09 | Mitsubishi Electric Corp | Electric operation device for switch |
| US7858684B2 (en) | 2006-10-06 | 2010-12-28 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Solid composite material and production method thereof |
| CN109641808A (en) * | 2016-07-05 | 2019-04-16 | 苏黎世联邦理工学院 | The high-performance ceramic made of cold sintering nanometer grade powder |
-
1989
- 1989-07-29 JP JP19727289A patent/JP3321155B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006309999A (en) * | 2005-04-27 | 2006-11-09 | Mitsubishi Electric Corp | Electric operation device for switch |
| US7858684B2 (en) | 2006-10-06 | 2010-12-28 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Solid composite material and production method thereof |
| CN109641808A (en) * | 2016-07-05 | 2019-04-16 | 苏黎世联邦理工学院 | The high-performance ceramic made of cold sintering nanometer grade powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3321155B2 (en) | 2002-09-03 |
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