JPS62278123A - Production of acicular calcium carbonate particle - Google Patents
Production of acicular calcium carbonate particleInfo
- Publication number
- JPS62278123A JPS62278123A JP12041286A JP12041286A JPS62278123A JP S62278123 A JPS62278123 A JP S62278123A JP 12041286 A JP12041286 A JP 12041286A JP 12041286 A JP12041286 A JP 12041286A JP S62278123 A JPS62278123 A JP S62278123A
- Authority
- JP
- Japan
- Prior art keywords
- calcium carbonate
- acicular
- calcium
- particle
- carbon dioxide
- 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
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 189
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 84
- 239000002245 particle Substances 0.000 title claims abstract description 72
- 238000004519 manufacturing process Methods 0.000 title description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 50
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 25
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 24
- 239000000920 calcium hydroxide Substances 0.000 abstract description 33
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract description 33
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 239000007864 aqueous solution Substances 0.000 abstract description 11
- 235000010216 calcium carbonate Nutrition 0.000 description 82
- 239000007789 gas Substances 0.000 description 27
- 238000000034 method Methods 0.000 description 24
- 239000012153 distilled water Substances 0.000 description 21
- 239000013078 crystal Substances 0.000 description 18
- 239000007788 liquid Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 13
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 12
- 229930006000 Sucrose Natural products 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 229960004793 sucrose Drugs 0.000 description 12
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- 235000013681 dietary sucrose Nutrition 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000005720 sucrose Substances 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 3
- 229910021532 Calcite Inorganic materials 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000001099 ammonium carbonate Substances 0.000 description 3
- 235000012501 ammonium carbonate Nutrition 0.000 description 3
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 3
- 239000001639 calcium acetate Substances 0.000 description 3
- 229960005147 calcium acetate Drugs 0.000 description 3
- 235000011092 calcium acetate Nutrition 0.000 description 3
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 3
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 229940043430 calcium compound Drugs 0.000 description 3
- 150000001674 calcium compounds Chemical class 0.000 description 3
- 238000009388 chemical precipitation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- 238000010299 mechanically pulverizing process Methods 0.000 description 3
- 239000012744 reinforcing agent Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- -1 acicular particles Chemical compound 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 230000009469 supplementation Effects 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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- 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
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】
３、発明の詳細な説明
（産業上の利用分野）
本発明は種々の産業分野に３いて充填剤、補強剤等とし
て多く使用されている炭酸カルシウム、とくに針状粒子
炭酸カルシウムの生成方法に関するものである。Detailed Description of the Invention 3. Detailed Description of the Invention (Field of Industrial Application) The present invention is directed to calcium carbonate, particularly acicular particles, which is widely used as a filler, reinforcing agent, etc. in various industrial fields. This invention relates to a method for producing calcium carbonate.
（従来技術）
実際の工業界での炭酸カルシウムは石灰石を機械的に微
粉砕した重質炭酸カルシウムと化学的沈降法により生成
される沈降炭酸カルシウムに大別される。ｍＷ炭酸カル
シウムの粒子は不定形で、粒子径は数μｍへ１５０μｍ
位までの範囲にある。又、沈降炭酸カルシウムを分類す
ると粒子径１〜３μｍ位の軽微性炭酸カルシウムと称さ
れるものと粒子径０，０２〜０．１μｍ位のコロイド性
炭酸カルシウムと称されるものとになる。さらに、その
形状も立方形、紡錘形、柱状形等で特殊なものとして突
起を有する炭酸カルシウム粒子が特公昭５７−３０８１
５号公報に掲載されており、更に炭酸カルシウム針絡合
体が特公昭５７−３１５３０号公報に掲載されている。(Prior Art) Calcium carbonate in actual industry is roughly divided into heavy calcium carbonate, which is produced by mechanically pulverizing limestone, and precipitated calcium carbonate, which is produced by chemical precipitation. The particles of mW calcium carbonate are amorphous, and the particle size ranges from several μm to 150 μm.
It is in the range of up to Further, precipitated calcium carbonate can be classified into two types: minor calcium carbonate, which has a particle size of about 1 to 3 μm, and colloidal calcium carbonate, which has a particle size of about 0.02 to 0.1 μm. In addition, calcium carbonate particles with special shapes such as cubic, spindle, and columnar shapes with protrusions were published in Japanese Patent Publication No. 57-3081.
It is published in Japanese Patent Publication No. 57-31530, and a calcium carbonate needle-entangled body is also published in Japanese Patent Publication No. 57-31530.
沈降炭酸カルシウムの製法は、炭酸イオンを含む溶Ｍ（
炭酸ナトリウム、炭酸アンモニウム等）とカルシウム化
合物の溶液（塩化カルシウム、酢酸カルシウム等）を触
媒反応させて作る“液：液”法と、水酸化カルシウムと
炭酸ガスの反応によって作る“液＝ガス”法とがある。The method for producing precipitated calcium carbonate is to prepare a solution M containing carbonate ions (
The "liquid:liquid" method involves a catalytic reaction between calcium compound solutions (calcium chloride, calcium acetate, etc.) with sodium carbonate, ammonium carbonate, etc., and the "liquid=gas" method involves the reaction of calcium hydroxide with carbon dioxide gas. There is.
中でも日本で工業的に主に行なわれているのは“液＝ガ
ス”法であり１反応条件（水酸化カルシウムスラリーの
濃度、反応温度、反応方法、添加剤の種類と有無等）に
より種々の粒径、形状の炭酸カルシウムが開発されてい
る。又、“液＝液”法では、特開昭５９−２０３７２８
に、針状（直径２〜３μｍ、長さ３０〜６０μｍ）の炭
酸カルシウム結晶の製法が掲載されている。Among them, the one that is mainly used industrially in Japan is the "liquid=gas" method, which can be used in various ways depending on the reaction conditions (calcium hydroxide slurry concentration, reaction temperature, reaction method, type and presence of additives, etc.). Calcium carbonate with various particle sizes and shapes has been developed. In addition, in the "liquid=liquid" method, Japanese Patent Application Laid-Open No. 59-203728
describes a method for producing acicular calcium carbonate crystals (2 to 3 μm in diameter, 30 to 60 μm in length).
（発明が解決しようとする問題点）
以上の如く種々の粒径、形状の炭酸カルシウムが開発さ
れているが、“液＝ガス”法で、長径５〜１００μｍ、
短径０．２〜５μｍのような粒子で、しかも単結晶の様
を呈した針状粒子炭酸カルシウムは従来の工業生産には
ない。(Problems to be Solved by the Invention) As mentioned above, calcium carbonate with various particle sizes and shapes has been developed.
Acicular calcium carbonate particles having a short diameter of 0.2 to 5 μm and having the appearance of a single crystal are not available in conventional industrial production.
（問題点を解決するための手段）
したがって本発明の技術的課題は長径５〜１１００Ａ１
、短径０．２〜５μｍのような粒子で、しかも単結晶の
様を呈した画期的な針状粒子炭酸カルシウムを提供する
ことを目的とするもので、その技術的課題を解決する本
発明の技術的手段は、炭酸ガス又は炭酸ガスを含むガス
体が吹き込まれている水に（水は攪拌されてもよい）、
水酸化カルシウム水溶液（各種薬品、たとえばサッカロ
ース等で水酸化カルシウムの溶解度を上げた溶液含む）
を適切な流量調整のうえ、滴下あるいは注入して、炭酸
カルシウムを生成させることである。(Means for solving the problem) Therefore, the technical problem of the present invention is to
The purpose of this book is to provide innovative acicular calcium carbonate particles with a minor axis of 0.2 to 5 μm that look like single crystals, and to solve this technical problem. The technical means of the invention is that water into which carbon dioxide gas or a gaseous body containing carbon dioxide gas is blown (the water may be stirred),
Calcium hydroxide aqueous solution (including solutions in which the solubility of calcium hydroxide is increased with various chemicals, such as saccharose)
Calcium carbonate is produced by dripping or injecting it with appropriate flow rate adjustment.
（発明の効果）
この方法によれば、さきに出願人が出願した特願昭６０
−１６５４３号“針状′粒子炭酸カル゛ シウムの生成
方法”すなわち炭酸水素カルシウム水溶液に適切な加熱
制御を施すことにより針状粒子炭酸カルシウムを生成さ
せる方法よりも、少なくとも数倍の生産性をあげること
が出来、しかもそれにより相当のコストダウンが可能に
なる。なかでも、各種薬品、たとえばサッカロース等で
、水酸化カルシウムの溶解度を上げた方が、生産性やコ
ストダウンに大きく寄与する。(Effect of the invention) According to this method, the patent application filed in 1983 by the applicant
No. 16543 "Method for producing acicular 'particles of calcium carbonate'" In other words, the productivity is at least several times higher than that of the method of producing acicular particles of calcium carbonate by applying appropriate heating control to an aqueous solution of calcium hydrogen carbonate. This allows for considerable cost reduction. Among these, increasing the solubility of calcium hydroxide with various chemicals such as sucrose will greatly contribute to productivity and cost reduction.
又、針状粒子の大きさの調節については、適切な操作条
件を選択することにより、たとえば、水酸化カルシウム
の滴下や注入速度、あるぃは反応中の温度等を適切に選
ぶことにより、比較的簡却に出来る。In addition, the size of the acicular particles can be adjusted by selecting appropriate operating conditions, such as the dropping and injection rate of calcium hydroxide, or the temperature during the reaction. It can be simplified.
（実施例） 以下、実施例にもとづき、その内容を説明する。(Example) The contents will be explained below based on examples.
実施例１
酸化カルシウムを温度約８０℃の攪拌されている蒸留水
中に投入し、水酸化カルシウムスラリーを生成させ、室
温まで放冷後、フィルターにより濾過し、水成化カルシ
ウム水溶液を得、これを５０ｍ１１分の流量で、攪拌さ
れている８０℃異常の蒸留水１２中に滴下して、針状粒
子炭酸カルシウムを生成させた。この時、その蒸留水中
に吹き込んでいる炭酸ガスはｉｎ／分、１．５ｋｇ／ｃ
ｒｎ’であった。Example 1 Calcium oxide was poured into distilled water with stirring at a temperature of about 80°C to produce a calcium hydroxide slurry. After cooling to room temperature, it was filtered through a filter to obtain an aqueous calcium aqueous solution, which was It was dropped into distilled water 12 at an abnormal temperature of 80° C. which was being stirred at a flow rate of 50 ml for 11 minutes to generate acicular particle calcium carbonate. At this time, the carbon dioxide gas being blown into the distilled water is in/min, 1.5 kg/c.
It was rn'.
生成した針状粒子炭酸カルシウムをフィルターにて濾過
脱水し、電気乾燥機にて、約１００℃で乾燥してサンプ
ルＡを得る。第４図にこのサンプルＡのＳＥＭによる観
察写真を示す。また第１図はサンプルＡのＸ線回折パタ
ーンで、はとんどアラゴナイト結晶であることを示して
いる。The produced acicular calcium carbonate particles are filtered and dehydrated using a filter, and dried at about 100° C. using an electric dryer to obtain sample A. FIG. 4 shows an SEM observation photograph of this sample A. FIG. 1 shows the X-ray diffraction pattern of sample A, which shows that it is mostly aragonite crystal.
実施例２
実施例１と同様な方法で得た水酸化カルシウム水溶液を
１５０ｍｌ１分（実施例１と比較して３倍）の流量で、
攪拌されている８０℃以上の蒸留水１１に滴下して、針
状粒子炭酸カルシウムを生成させた。この時の蒸留水中
に吹き込んでいる炭酸ガスは１２／分、１．５ｋｇ／ａ
ｒｒＩ’であった。実施例１と同様に、脱水、乾燥して
サンプルＢを得る。第５図にこのサンプルＢのＳＥＭに
よる観察写真を示す。第４図のものくサンプルＡ）と比
較して、小さい形状の針状粒子炭酸カルシウムが生成さ
れている。第２図はサンプルＢのＸ線回折パターンを示
し、アラゴナイトに混ってカルサイトのピークが認めら
れる。Example 2 A calcium hydroxide aqueous solution obtained in the same manner as in Example 1 was added at a flow rate of 150 ml for 1 minute (3 times as much as in Example 1).
It was added dropwise to distilled water 11 at 80° C. or higher that was being stirred to produce acicular particle calcium carbonate. The carbon dioxide gas being blown into the distilled water at this time is 12/min, 1.5 kg/a.
It was rrI'. Sample B is obtained by dehydration and drying in the same manner as in Example 1. FIG. 5 shows an SEM observation photograph of this sample B. Compared to sample A) in FIG. 4, acicular calcium carbonate particles with smaller shapes are produced. FIG. 2 shows the X-ray diffraction pattern of Sample B, in which a peak of calcite is observed mixed with aragonite.
実施例３
水酸化カルシウムスラリー（濃度：ｃａ（ＯＨ） ２０
、７５ ｇ ／ Ｈ２０−１００ｍ ｆｌ ）約１２
にサッカロース５０ｇを添加し、フイ、レターにより濾
過する。この濾液を５０ ｍ Ｉｔ ／ 分ノ１重量で
攪拌されている８０℃以上の蒸留水１１に通下して針状
粒子炭酸カルシウムを生成させた。この時の蒸留水中に
吹き込んでいる炭酸ガスは１２／分、１．５ｋｇ／ａｍ
″であった。実施例１と同様に、脱水、乾燥してサンプ
ルＣとする。サッカロース添加により、水酸化カルシウ
ムの溶解度が増し、針状粒子炭酸カルシウムの収量は実
施例１のそれよりも約４倍に達した。第６図に、このサ
ンプルＣのＳＥＭにより観察写真を示す。また、第３図
はサンプルＣのＸ線回折パターンでほとんどアラゴナイ
ト結晶であることを示している。Example 3 Calcium hydroxide slurry (concentration: ca (OH) 20
, 75 g/H20-100m fl) approx. 12
Add 50 g of saccharose to the solution and filter through a filter. This filtrate was passed through distilled water 11 at 80° C. or higher that was being stirred at a rate of 50 mIt/min to produce acicular particle calcium carbonate. The carbon dioxide gas being blown into the distilled water at this time is 12/min, 1.5kg/am.
Sample C was obtained by dehydration and drying in the same manner as in Example 1. By adding sucrose, the solubility of calcium hydroxide was increased, and the yield of acicular particle calcium carbonate was approximately Figure 6 shows an SEM photograph of sample C. Figure 3 shows the X-ray diffraction pattern of sample C, which shows that it is mostly aragonite crystal.
第１．２．３図はＸ線回折パターン図
第４．５．６図は各人なる針状粒子炭酸カルシウムの図
面代用の結晶写真である。
手 続 補 正 書 （方式）昭和６１年８月
１４日
特許庁長官 黒 １）明 雄 殿
１、事件の表示
昭和６１年特許願第１２０４１２号
２、発明の名称
針状粒子炭酸カルシウムの生成方法
３、補正をする者
事件との関係 出願人
住 所 岐阜県大垣市赤坂町１８８ の１名称矢橋工
業株式会社
代表者 矢 橋 宗 −
４、代理人
住 所 東京都千代田区六番町７番地下条ピル３階
氏 名 （７１５６）弁理士 網 野 誠（外 ２
名）
５、補正命令の日付
昭和６１年７月 ２日
（発送日 昭和６１年７月２９日）
６、補正の対象
委任状及び明細書と図面
７、補正の内容
（１）委任状を補充する。
（２）明細書全文を別紙のとおり補正する。
（３）図面第３図〜第６図を別紙のように補正する。
明細書
１、発明の名称
針状粒子炭酸カルシウムの生成方法
２、特許請求の範囲
炭酸ガス又は炭酸ガスを含むガス体が吹き込まれている
水に、水酸化カルシウム水溶液を適切な流量調整のうえ
、滴下あるいは注入して、炭酸カルシウムを生成させる
ことを特徴とする針状粒子炭酸カルシウムの生成方法。
３、発明の詳細な説明
（産業上の利用分野）
本発明は種々の産業分野において充填剤、補強剤等とし
て多く使用されている炭酸カルシウム、とくに針状粒子
炭酸カルシウムの生成方法に関するものである。
（従来技術）
実際の工業界での炭酸カルシウムは石灰石を機械的に微
粉砕した重質炭酸カルシウムと化学的沈降法により生成
される沈降炭酸カルシウムに大別される。重質炭酸カル
シウムの粒子は不定形で、粒子径は数μｍ〜１５０μｍ
位までの範囲にある。又、沈降炭酸カルシウムを分類す
ると粒子径１〜３μｍ位の軽微性炭酸カルシウムと称さ
れるものと粒子径０．０２〜０．１μｍ位のコロイド性
炭酸カルシウムと称されるものとになる。さらに、その
形状も立方形、紡錘形、柱状形等で特殊なものとして突
起を有する炭酸カルシウム粒子が特公昭５７−３０８１
５号公報に掲載されており、更に炭酸カルシラ
・ム針絡合体が特公昭５７−３１５３０号公報に掲載
されている。
沈降炭酸カルシウムの製法は、炭酸イオンを含む溶液（
炭酸ナトリウム、炭酸アンモニウム等）とカルシウム化
合物の溶Ｗ（塩化カルシウム、酢酸カルシウム等）を接
触反応させて作る“液＝液”法と、水酸化カルシウムと
炭酸ガスの反応によって作る“液＝ガス”法とがある。
中でも日本で工業的に主に杵なわれているのは“液＝ガ
ス”法であり、反応条件（水酸化カルシウムスラリーの
濃度、反応温度、反応方法、添加剤の種類と存無等）に
より種々の粒径、形状の炭酸カルシウムが開発されてい
る。又。
“液＝液“法では、特開昭５９−２０３７２８に、針状
（直径２〜３μｍ、長さ３０〜６０μＩｎ）の炭酸カル
シウム結晶の製法が掲載されている。
（発明が解決しようとする問題点）
以上の如く種々の粒径、形状の炭酸カルシウムが開発さ
れているが、“液＝ガス”法で、長径５〜１００μｍ、
短径０．２〜５μｍのような粒子で、しかも単結晶の様
を呈した針状粒子炭酸カルシウムは従来の工業生産には
ない。
（問題点を解決するための手段）
したがって本発明の技術的課題は長径５〜′１００μｍ
、短径０，２〜５μｍのような粒子で、しかも単結晶の
様を呈した画期的な針状粒子炭酸カルシウムを提供する
ことを目的とするもので、その技術的課題を解決する本
発明の技術的手段は、炭酸ガス又は炭酸ガスを含むガス
体が吹き込まれている水に（水は攪拌されてもよい）、
水酸化カルシウム水溶液（各種薬品、たとえばサッカロ
ース等で水酸化カルシウムの溶解度を上げた溶液含む）
を適切な流量調整のうえ、滴下あるいは注入して、炭酸
カルシウムを生成させることである。
（発明の効果）
この方法によれば、さきに出願人が出願した特願昭６０
−１６５４３号“針状粒子炭酸カルシウムの生成方法”
すなわち炭酸水素カルシウム水溶液に適切な加熱制御を
施すことにより針状粒子炭酸カルシウムを生成させる方
法よりも、少なくとも数倍の生産性をあげることが出来
、しかもそれにより相当のコストダウンが可能になる。
なかでも、各種薬品、たとえばサッカロース等で、水酸
化カルシウムの溶解度を上げた方が、生産性やコストダ
ウンに大きく寄与する。
又、針状粒子の大きさの調節については、通切な操作条
件を選択することにより、たとえば、水酸化カルシウム
の滴下や注入速度、あるいは反応中の温度等を適切に選
ぶことにより、比較的簡単に出来る。
（実施例）
以下、実施例にもとづき、その内容を説明する。
実施例１
酸化カルシウムを温度約８０℃の攪拌されている蒸留水
中に投入し、水酸化カルシウムスラリーを生成させ、室
温まで放冷後、フィルターにより濾過し、水酸化カルシ
ウム水溶液を得、これを５０ｍｌ１Ｚ分の流量で、攪拌
されている８０℃以上の蒸留水１２中に滴下して、針状
粒子炭酸カルシウムを生成させた。この時、その蒸留水
中に吹き込んでいる炭酸ガスは１ｆｆｉ／分、１．５ｋ
ｇ／ｃばであった。
生成した針状粒子炭酸カルシウムをフィルターにて濾過
脱水し、電気乾燥機にて、約１００℃で乾燥してサンプ
ルＡを得る。第４図にこのサンプルＡのＳＥＭによる観
察写真を示す。また第１図はサンプルＡのＸ線回折パタ
ーンで、はとんどアラゴナイト結晶であることを示して
いる。
実施例２
実施例１と同様な方法で得た水酸化カルシウム水溶液を
１５０ｍ１！／分（実施例１と比較して３倍）の−ＪＡ
Ｎで、攪拌されている８０℃以上の蒸留水１２に滴下し
て、針状粒子炭酸カルシウムを生成させた。この時の蒸
留水中に吹き込んでいる炭酸ガスは１１７分、１．５ｋ
ｇ／ｃゴであった。実施例１と同様に、脱水、乾燥して
サンプルＢを得る。第５図にこのサンプルＢのＳＥＭに
よる観察写真を示す。第４図のもの（サンプルＡ）と比
較して、小さい形状の針状粒子炭酸カルシウムが生成さ
れている。第２図はサンプルＢのＸ線回折パターンを示
し、アラゴナイトに混ってカルサイトのピークが認めら
れる。
実施例３
水酸化カルシウムスラリー（濃度：Ｃａ（ＯＨ）２０．
７５ｇ／Ｈ２０１００ｍｕ）約１ｆＬにサッカロース５
０ｇを添加し、フィルターにより濾過する。この１！液
を５０ｍｆｆ１／分の流量で攪拌されている８０℃以上
の蒸留水ｉＩｔに通下して針状粒子炭酸カルシウムを生
成させた。この時の蒸留水中に吹き込んでいる炭酸ガス
はＩＩＬ／分、１．５ｋｇ／ｃばであった。実施例１と
同様に、脱水、乾燥してサンプルＣとする。サッカロー
ス添加により、水酸化カルシウムの溶解度が増し、針状
粒子炭酸カルシウムの収量は実施例１のそれよりも約４
倍に達した。第６図に、このサンプルＣのＳＥＭにより
観察写真を示す。また、第３図はサンプルＣのＸ線回折
パターンでほとんどアラゴナイト結晶であることを示し
ている。
４、図面の簡単な説明
第１．２．３図はＸ線回折パターン図
第４．５．６図は容具なる針状粒子炭酸カルシウムの図
面代用の結晶写真である。
第６図
サンプル Ｃ
Ｘ１００Ｏｂａｒ ： １０μｍ
３図
手 続 補 正 書 （自発）昭和６１年８月
２７日
特許庁長官 黒 １）明 雄 殿
１、事件の表示
昭和６１年特許願第１２０４１２号
２、発明の名称
針状粒子炭酸カルシウムの生成方法
３、補正をする者
事件との関係 出願人
住 所 岐阜県大垣市赤坂町１８８ の１名称矢橋工
業株式会社
代表者 矢 橋 宗 −
４、代理人
住 所 東京都千代田区六番町７番地゛下条ビル３階
氏 名 （７１５６）弁理士 網 野 誠（外 ２
名）
５、補正命令の日付
自 発
６、補正の対象
明細書
７、補正の内容
明細書全文を別紙のとおり補正する。
明 細 書
１、発明の名称
針状粒子炭酸カルシウムの生成方法
２、特許請求の範囲
炭酸ガス又は炭酸ガスを含むガス体が吹き込まれていて
、しか ゛ な口 Ｃ′がなされてｇｚ玉水に、水酸
化カルシウム水溶液を適切な流ｍ：ＡＶのうえ、滴下あ
るいは注入して、炭酸カルシウムを生成させることを特
徴とする針状粒子炭酸カルシウムの生成方法。
３、発明の詳細な説明
（産業上の利用分野）
本発明は種々の産業分野において充填剤、補強剤等とし
て多く使用されている炭酸カルシウム、とくに針状粒子
炭酸カルシウムの生成方法に関するものである。
（従来技術）
実際の工業界での炭酸カルシウムは石灰石を機械的に微
粉砕した重質炭酸カルシウムと化学的沈降法により生成
される沈降炭酸カルシウムに大別される。重質炭酸カル
シウムの粒子は不定形で、粒子径は数μｍへ１５０μｍ
位までの範囲にある。又、沈降炭酸カルシウムを分類す
ると粒子径１〜３μｍ位の軽微性炭酸カルシウムと称さ
れるものと粒子径０．０２〜０．１μｍ位のコロイド性
炭酸カルシウムと称されるものとになる。さらに、その
形状も立方形、紡錘形、柱状形等で特殊なものとして突
起を有する炭酸カルシウム粒子が特公昭５７−３０８１
５号公報に掲載されており、更に炭酸カルシウム針絡合
体が特公昭５７−３１５３０号公報に掲載されている。
沈降炭酸カルシウムの製法は、炭酸イオンを含む溶ｉ（
炭酸ナトリウム、炭酸アンモニウム等）とカルシウム化
合物の溶液（塩化カルシウム、酢酸カルシウム等〉を接
触反応させて作る“液＝液”法と、水酸化カルシウムと
炭酸ガスの反応によって作る“液：ガス”法とがある。
中でも日本で工業的に主に行なわれているのは“液＝ガ
ス”法であり、反応条件（水酸化カルシウムスラリーの
濃度、反応温度、反応方法、添加剤の種類と有無等）に
より種々の粒径、形状の炭酸カルシウムが開発されてい
る。又、“液＝液”法では、特開昭５９−２０３７２８
に、針状（直径２〜３μｍ、長さ３０〜６０μｍ）の炭
酸カルシウム結晶の製法が掲載されている。
（発明が解決しようとする問題点）
以上の如く種々の粒径、形状の炭酸カルシウムが開発さ
れているが、“液＝ガス”法で、長径５〜１００μｍ、
短径０．２〜５μｍのような粒子で、しかも単結晶の様
を呈した針状粒子炭酸カルシウムは従来の工業生産には
ない。
（問題点を解決するための手段）
したがって本発明の技術的課題は長径５〜１００μｍ、
短径０．２〜５μｍのような粒子で、しかも単結晶の様
を呈した画期的な針状粒子炭酸カルシウムを提供するこ
とを目的とするもので、その技術的課題を解決する本発
明の技術的手段は、炭酸ガス又は炭酸ガスを含むガス体
が吹き込まれている７０℃以上の水１２に（水は攪拌さ
れてもよい）、水酸化カルシウム水溶液（各種薬品、た
とえばサッカロース等で水酸化カルシウムの溶解度を上
げた溶液を含む）を適切な流量調整（，１５０ｍｊ！／
分以下）のうえ、滴下あるいは注入して、炭酸カルシウ
ムを生成させることである。
（発明の効果）
この方法によれば、さきに出願人が出願した特願昭６０
−１６５４３号“針状粒子炭酸カルシウムの生成方法”
すなわち炭酸水素カルシウム水溶液に適切な加熱制御を
施すことにより針状粒子炭酸カルシウムを生成させる方
法よりも、少なくとも数倍の生産性をあげることが出来
、しかもそれにより相当のコストダウンが可能になる。
なかでも、各種薬品、たとえばサッカロース等で、水酸
化カルシウムの溶解度を上げた方が、生産性やコストダ
ウンに大きく寄与する。
又、針状粒子の大きさの調節については、適切な操作条
件を選択することにより、たとえば、水酸化カルシウム
の滴下や注入速度、あるいは反応中の温度等を適切に選
ぶことにより、比較的簡単に出来る。
（実施例）
以下、実施例にもとづき、その内容を説明する。
実施例１
酸化カルシウムを温度約８０℃の攪拌されている蒸留水
中に投入し、水酸化カルシウムスラリーを生成させ、室
温まで放冷後、フィルターにより濾過し、水酸化カルシ
ウム水溶液を得。
これを５０ｍｌ１Ｚ分の流量で、攪拌されている８０℃
以上の蒸留水１２中に滴下して、針状粒子炭酸カルシウ
ムを生成させた。この時、その蒸留水中に吹き込んでい
る炭酸ガスは１ＩｌＺ分、１．５ｋｇ／ｃゴであった。
生成した針状粒子炭酸カルシウムをフィルターにて濾過
脱水し、電気乾燥機にて、約１００℃で乾燥してサンプ
ルＡを得る。第４図にこのサンプルＡのＳＥＭによる観
察写真を示す。また第１図はサンプルＡのＸ線回折パタ
ーンで、はとんどアラゴナイト結晶であることを示して
いる。
実施例２
実施例１と同様な方法で得た水酸化カルシウム水溶液を
１５０ｍＩＬ／分（実施例１と比較して３倍）の流量で
、攪拌されている７０℃以上の蒸留水１１に滴下して、
針状粒子炭酸カルシウムを生成させた。この時の蒸留水
中に吹き込んでいる炭酸ガスは１１．７分、１．ｓｓｃ
ｇ／Ｃゴであった。実施例１と同様に、脱水、乾燥して
サンプルＢを得る。第５図にこのサンプルＢのＳＥＭに
よる！ｌｌ寮写真を示す。第４図のもの（サンプルＡ）
と比較して、小さい形状の針状粒子炭酸カルシウムが生
成されている。
第２図はサンプルＢのＸ線回折パターンを示し、アラゴ
ナイトに混ってカルサイトのピークが認められる。
実施例３
水酸化カルシウムスラリー（濃度：Ｃａ（ＯＨ）２０．
７５ｇ／Ｈ２０−Ｈ２Ｏ−１Ｏ０約１１にサッカロース
５０ｇを添加し、フィルターにより濾過する。この濾液
を５０ｍ１７分の流量で攪拌されている８０℃以上の蒸
留水ＩＪ２に通下して針状粒子炭酸カルシウムを生成さ
せた。この時の蒸留水中に吹き込んでいる炭酸ガスはＩ
ＩＬ／分、１．５ｋｇ／ｃｒｎ’であった。実施例１と
同様に、脱水、乾燥してサンプルＣとする。サッカロー
ス添加により、水酸化カルシウムの溶解度が増し、針状
粒子炭酸カルシウムの収量は実施例１のそれよりも約４
倍に達した。第６図に、このサンプルＣのＳＥＭにより
観察写真を示す。また、第３図はサンプルＣのＸ線回折
パターンでほとんどアラゴナイト結晶であることを示し
ている。
４、図面の簡単な説明
第１．２．３図はＸ線回折パターン図
第４．５．６図は各人なる針状粒子炭酸カルシウムの図
面代用の結晶写真である。Figures 1.2.3 are X-ray diffraction patterns, and Figures 4.5.6 are crystal photographs of each individual's acicular particle calcium carbonate as a drawing. Procedural Amendment (Method) August 14, 1986 Director-General of the Patent Office Kuro 1) Mr. Yu Akira 1, Indication of the case 1985 Patent Application No. 120412 2, Name of the invention Method for producing acicular particle calcium carbonate 3. Relationship with the case of the person making the amendment Applicant address: 188 Akasaka-cho, Ogaki City, Gifu Prefecture Name: Yabashi Kogyo Co., Ltd. Representative: So Yahashi - 4. Agent address: 7-basement, Rokuban-cho, Chiyoda-ku, Tokyo Article Pill 3rd Floor Name (7156) Patent Attorney Makoto Amino (Outside 2
5. Date of amendment order: July 2, 1986 (Shipping date: July 29, 1986) 6. Power of attorney subject to amendment, specification and drawings 7. Contents of amendment (1) Supplementation of power of attorney do. (2) The entire specification shall be amended as shown in the attached sheet. (3) Correct the drawings in Figures 3 to 6 as shown in the attached sheet. Description 1, Name of the invention Method for producing acicular particle calcium carbonate 2, Claims A calcium hydroxide aqueous solution is added to water into which carbon dioxide gas or a gaseous body containing carbon dioxide gas is blown, after adjusting the flow rate appropriately. A method for producing acicular particle calcium carbonate, which comprises producing calcium carbonate by dropping or injecting it. 3. Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for producing calcium carbonate, particularly acicular particle calcium carbonate, which is widely used as a filler, reinforcing agent, etc. in various industrial fields. . (Prior Art) Calcium carbonate in actual industry is roughly divided into heavy calcium carbonate, which is produced by mechanically pulverizing limestone, and precipitated calcium carbonate, which is produced by chemical precipitation. The particles of heavy calcium carbonate are amorphous and have a particle size of several μm to 150 μm.
It is in the range of up to Further, precipitated calcium carbonate can be classified into two types: minor calcium carbonate, which has a particle size of about 1 to 3 μm, and colloidal calcium carbonate, which has a particle size of about 0.02 to 0.1 μm. In addition, calcium carbonate particles with special shapes such as cubic, spindle, and columnar shapes with protrusions were published in Japanese Patent Publication No. 57-3081.
It is published in Publication No. 5, and furthermore, Calcilla carbonate
・Mu-needle entangled body is published in Japanese Patent Publication No. 57-31530. Precipitated calcium carbonate is produced using a solution containing carbonate ions (
The "liquid=liquid" method is created by contacting a solution of calcium (sodium carbonate, ammonium carbonate, etc.) with a dissolved calcium compound (calcium chloride, calcium acetate, etc.), and the "liquid=gas" method is created by reacting calcium hydroxide with carbon dioxide gas. There is a law. Among them, the "liquid=gas" method is mainly used industrially in Japan, and the process depends on the reaction conditions (concentration of calcium hydroxide slurry, reaction temperature, reaction method, type and presence of additives, etc.). Calcium carbonate with various particle sizes and shapes has been developed. or. In the "liquid-liquid" method, Japanese Patent Laid-Open No. 59-203728 describes a method for producing acicular calcium carbonate crystals (diameter 2 to 3 .mu.m, length 30 to 60 .mu.In). (Problems to be Solved by the Invention) As mentioned above, calcium carbonate with various particle sizes and shapes has been developed.
Acicular calcium carbonate particles having a short diameter of 0.2 to 5 μm and having the appearance of a single crystal are not available in conventional industrial production. (Means for solving the problem) Therefore, the technical problem of the present invention is to
The purpose of this book is to provide innovative acicular calcium carbonate particles with a minor axis of 0.2 to 5 μm that look like single crystals, and to solve this technical problem. The technical means of the invention is that water into which carbon dioxide gas or a gaseous body containing carbon dioxide gas is blown (the water may be stirred),
Calcium hydroxide aqueous solution (including solutions in which the solubility of calcium hydroxide is increased with various chemicals, such as saccharose)
Calcium carbonate is produced by dripping or injecting it with appropriate flow rate adjustment. (Effect of the invention) According to this method, the patent application filed in 1983 by the applicant
-No. 16543 “Method for producing acicular particle calcium carbonate”
In other words, productivity can be increased at least several times as much as in the method of producing acicular particle calcium carbonate by subjecting an aqueous calcium hydrogen carbonate solution to appropriate heating control, and it also enables considerable cost reduction. Among these, increasing the solubility of calcium hydroxide with various chemicals such as sucrose will greatly contribute to productivity and cost reduction. In addition, the size of the acicular particles can be adjusted relatively easily by selecting appropriate operating conditions, such as the dropping and injection rate of calcium hydroxide, or the temperature during the reaction. I can do it. (Example) Hereinafter, the content will be explained based on an example. Example 1 Calcium oxide was poured into distilled water with stirring at a temperature of about 80°C to produce a calcium hydroxide slurry. After cooling to room temperature, it was filtered through a filter to obtain a calcium hydroxide aqueous solution, which was added to 50 ml of 1Z The mixture was dropped into distilled water 12 at a temperature of 80° C. or higher while being stirred at a flow rate of 12 min to generate acicular particle calcium carbonate. At this time, the carbon dioxide gas being blown into the distilled water is 1ffi/min, 1.5k
It was g/c. The produced acicular calcium carbonate particles are filtered and dehydrated using a filter, and dried at about 100° C. using an electric dryer to obtain sample A. FIG. 4 shows an SEM observation photograph of this sample A. FIG. 1 shows the X-ray diffraction pattern of sample A, which shows that it is mostly aragonite crystal. Example 2 150ml of calcium hydroxide aqueous solution obtained in the same manner as in Example 1! /min (3 times compared to Example 1) -JA
The solution was added dropwise to distilled water 12 at 80° C. or higher that was being stirred with N to generate acicular particle calcium carbonate. The carbon dioxide gas being blown into the distilled water at this time was 117 minutes and 1.5k.
It was g/c. Sample B is obtained by dehydration and drying in the same manner as in Example 1. FIG. 5 shows an SEM observation photograph of this sample B. Compared to the sample in FIG. 4 (sample A), smaller acicular particle calcium carbonate particles are produced. FIG. 2 shows the X-ray diffraction pattern of Sample B, in which a peak of calcite is observed mixed with aragonite. Example 3 Calcium hydroxide slurry (concentration: Ca(OH) 20.
75g/H20100mu) saccharose 5 to about 1fL
Add 0 g and filter through a filter. This one! The liquid was passed through distilled water iIt at 80° C. or higher that was stirred at a flow rate of 50 mff1/min to generate acicular particle calcium carbonate. The carbon dioxide gas blown into the distilled water at this time was IIL/min, 1.5 kg/c. Sample C was obtained by dehydration and drying in the same manner as in Example 1. The addition of saccharose increases the solubility of calcium hydroxide, and the yield of acicular particle calcium carbonate is approximately 4% higher than that of Example 1.
It has doubled. FIG. 6 shows an SEM photograph of this sample C. Furthermore, FIG. 3 shows the X-ray diffraction pattern of sample C, which shows that it is mostly aragonite crystal. 4. Brief description of the drawings Figures 1.2.3 are X-ray diffraction patterns, and Figures 4.5.6 are crystal photographs of acicular particle calcium carbonate, which is a container, as a substitute for drawings. Figure 6 Sample C Name: Method of producing acicular particle calcium carbonate 3, Relationship with the case of the person making the amendment Applicant address: 1, 188 Akasaka-cho, Ogaki City, Gifu Prefecture Name: Yabashi Kogyo Co., Ltd. Representative: Sou Yahashi - 4, Agent address: 3rd Floor, Shimojo Building, 7 Rokuban-cho, Chiyoda-ku, Tokyo Name (7156) Patent Attorney Makoto Amino (Outside 2)
5. The date of the amendment order. 6. The specification to be amended. 7. The full text of the specification of the contents of the amendment shall be amended as attached. Description 1, Title of the invention: Method for producing acicular particle calcium carbonate 2, Claims Carbon dioxide gas or a gas body containing carbon dioxide gas is blown into the gz tama water, and an opening C' is made. A method for producing acicular particle calcium carbonate, which comprises producing calcium carbonate by dropping or injecting an aqueous calcium hydroxide solution over an appropriate flow m:AV. 3. Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for producing calcium carbonate, particularly acicular particle calcium carbonate, which is widely used as a filler, reinforcing agent, etc. in various industrial fields. . (Prior Art) Calcium carbonate in actual industry is roughly divided into heavy calcium carbonate, which is produced by mechanically pulverizing limestone, and precipitated calcium carbonate, which is produced by chemical precipitation. The particles of heavy calcium carbonate are amorphous, and the particle size ranges from several μm to 150 μm.
It is in the range of up to Further, precipitated calcium carbonate can be classified into two types: minor calcium carbonate, which has a particle size of about 1 to 3 μm, and colloidal calcium carbonate, which has a particle size of about 0.02 to 0.1 μm. In addition, calcium carbonate particles with special shapes such as cubic, spindle, and columnar shapes with protrusions were published in Japanese Patent Publication No. 57-3081.
It is published in Japanese Patent Publication No. 57-31530, and a calcium carbonate needle-entangled body is also published in Japanese Patent Publication No. 57-31530. The method for producing precipitated calcium carbonate involves using a solution containing carbonate ions (
The "liquid=liquid" method is created by contacting a solution of calcium compounds (calcium chloride, calcium acetate, etc.) with sodium carbonate, ammonium carbonate, etc., and the "liquid: gas" method is created by reacting calcium hydroxide with carbon dioxide gas. Among them, the "liquid=gas" method is mainly used industrially in Japan, and the reaction conditions (concentration of calcium hydroxide slurry, reaction temperature, reaction method, type and presence of additives, etc.) ) has developed calcium carbonate with various particle sizes and shapes.Also, in the "liquid=liquid" method, Japanese Patent Application Laid-Open No. 59-203728
describes a method for producing acicular calcium carbonate crystals (2 to 3 μm in diameter, 30 to 60 μm in length). (Problems to be Solved by the Invention) As mentioned above, calcium carbonate with various particle sizes and shapes has been developed.
Acicular calcium carbonate particles having a short diameter of 0.2 to 5 μm and having the appearance of a single crystal are not available in conventional industrial production. (Means for solving the problem) Therefore, the technical problem of the present invention is to
The present invention aims to provide innovative acicular calcium carbonate particles with a minor diameter of 0.2 to 5 μm and a single-crystal appearance, and to solve the technical problems. The technical means is to add a calcium hydroxide aqueous solution (various chemicals, such as sucrose, etc. (including a solution with increased solubility of calcium oxide) by adjusting the flow rate appropriately (150mj!/
(minutes or less) and then dripping or injecting it to produce calcium carbonate. (Effect of the invention) According to this method, the patent application filed in 1983 by the applicant
-No. 16543 “Method for producing acicular particle calcium carbonate”
In other words, productivity can be increased at least several times as much as in the method of producing acicular particle calcium carbonate by subjecting an aqueous calcium hydrogen carbonate solution to appropriate heating control, and it also enables considerable cost reduction. Among these, increasing the solubility of calcium hydroxide with various chemicals such as sucrose will greatly contribute to productivity and cost reduction. In addition, the size of the acicular particles can be adjusted relatively easily by selecting appropriate operating conditions, such as the dropping and injection rate of calcium hydroxide, or the temperature during the reaction. I can do it. (Example) Hereinafter, the content will be explained based on an example. Example 1 Calcium oxide was poured into distilled water being stirred at a temperature of about 80° C. to produce a calcium hydroxide slurry, which was allowed to cool to room temperature and then filtered through a filter to obtain an aqueous calcium hydroxide solution. This was heated to 80°C while being stirred at a flow rate of 50ml 1Z.
It was dropped into the above distilled water 12 to generate acicular particle calcium carbonate. At this time, the amount of carbon dioxide gas blown into the distilled water was 1 IlZ, or 1.5 kg/c. The produced acicular calcium carbonate particles are filtered and dehydrated using a filter, and dried at about 100° C. using an electric dryer to obtain sample A. FIG. 4 shows an SEM observation photograph of this sample A. FIG. 1 shows the X-ray diffraction pattern of sample A, which shows that it is mostly aragonite crystal. Example 2 An aqueous calcium hydroxide solution obtained in the same manner as in Example 1 was dropped into distilled water 11 at a temperature of 70° C. or higher that was being stirred at a flow rate of 150 mL/min (3 times as much as in Example 1). hand,
Acicular particle calcium carbonate was produced. The carbon dioxide gas being blown into the distilled water at this time was 11.7 minutes, 1. ssc
It was g/C. Sample B is obtained by dehydration and drying in the same manner as in Example 1. Figure 5 shows the SEM of this sample B! Show photos of the dormitory. The one in Figure 4 (Sample A)
Compared to this, acicular particle calcium carbonate with a smaller shape is produced. FIG. 2 shows the X-ray diffraction pattern of Sample B, in which a peak of calcite is observed mixed with aragonite. Example 3 Calcium hydroxide slurry (concentration: Ca(OH) 20.
Add 50 g of sucrose to 75 g/H20-H2O-100 and filter through a filter. This filtrate was passed through distilled water IJ2 at a temperature of 80° C. or higher that was being stirred at a flow rate of 50 ml and 17 minutes to generate acicular particle calcium carbonate. The carbon dioxide gas blown into the distilled water at this time is I
IL/min was 1.5 kg/crn'. Sample C was obtained by dehydration and drying in the same manner as in Example 1. The addition of saccharose increases the solubility of calcium hydroxide, and the yield of acicular particle calcium carbonate is approximately 4% higher than that of Example 1.
It has doubled. FIG. 6 shows an SEM photograph of this sample C. Furthermore, FIG. 3 shows the X-ray diffraction pattern of sample C, which shows that it is mostly aragonite crystal. 4. Brief description of the drawings Figures 1.2.3 are X-ray diffraction patterns, and Figures 4.5.6 are crystal photographs of acicular particle calcium carbonate used in place of drawings.
Claims (1)
水に、水酸化カルシウム水溶液を適切な流量調整のうえ
、滴下あるいは注入して、炭酸カルシウムを生成させる
ことを特徴とする針状粒子炭酸カルシウムの生成方法。Acicular particle calcium carbonate characterized by producing calcium carbonate by dripping or injecting an aqueous calcium hydroxide solution into water into which carbon dioxide or a gas containing carbon dioxide is blown, after adjusting the flow rate appropriately. How to generate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12041286A JPS62278123A (en) | 1986-05-26 | 1986-05-26 | Production of acicular calcium carbonate particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12041286A JPS62278123A (en) | 1986-05-26 | 1986-05-26 | Production of acicular calcium carbonate particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62278123A true JPS62278123A (en) | 1987-12-03 |
| JPH0319166B2 JPH0319166B2 (en) | 1991-03-14 |
Family
ID=14785581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12041286A Granted JPS62278123A (en) | 1986-05-26 | 1986-05-26 | Production of acicular calcium carbonate particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62278123A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01234437A (en) * | 1988-03-12 | 1989-09-19 | Okutama Kogyo Kk | Filler for plastic |
| JP2014524876A (en) * | 2011-06-21 | 2014-09-25 | オムヤ インターナショナル アーゲー | Method for producing precipitated calcium carbonate, precipitated calcium carbonate and use thereof |
-
1986
- 1986-05-26 JP JP12041286A patent/JPS62278123A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01234437A (en) * | 1988-03-12 | 1989-09-19 | Okutama Kogyo Kk | Filler for plastic |
| JP2014524876A (en) * | 2011-06-21 | 2014-09-25 | オムヤ インターナショナル アーゲー | Method for producing precipitated calcium carbonate, precipitated calcium carbonate and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0319166B2 (en) | 1991-03-14 |
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