JPS62171920A - Production of readily dispersible colloidal calcium carbonate - Google Patents

Production of readily dispersible colloidal calcium carbonate

Info

Publication number
JPS62171920A
JPS62171920A JP1110786A JP1110786A JPS62171920A JP S62171920 A JPS62171920 A JP S62171920A JP 1110786 A JP1110786 A JP 1110786A JP 1110786 A JP1110786 A JP 1110786A JP S62171920 A JPS62171920 A JP S62171920A
Authority
JP
Japan
Prior art keywords
lime
milk
calcium carbonate
substance
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.)
Pending
Application number
JP1110786A
Other languages
Japanese (ja)
Inventor
Takao Morisawa
森沢 孝雄
Setsuji Edakawa
枝川 節治
Isao Matsushita
功 松下
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toyo Denka Kogyo Co Ltd
Original Assignee
Toyo Denka Kogyo Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Toyo Denka Kogyo Co Ltd filed Critical Toyo Denka Kogyo Co Ltd
Priority to JP1110786A priority Critical patent/JPS62171920A/en
Publication of JPS62171920A publication Critical patent/JPS62171920A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/18Carbonates
    • C01F11/182Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
    • C01F11/183Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

PURPOSE:To produce the titled CaCO3 having improved dispersibility and 0.1-1.0mum particle diameter, by adding the first substance to milk of lime, partially carbonating the milk of lime and continuously adding the resultant chainlike particles having high basicity to a solution, containing the second substance and saturated with gaseous carbon dioxide. CONSTITUTION:0.1-5pts. one or two or more of the first substances selected from sodium glutamate, EDTA sulfate and sucrose is added to 100pts. milk of lime in 10-15wt% concentration and CO2 gas is introduced while keeping the milk of lime at 45-50 deg.C to partially carbonate the milk of lime and give a suspension containing chainlike particles having high basicity. The resultant suspension is then continuously added to a solution, containing 0.1-10pts. one or two or more of the second substances selected from malic acid, citric acid, tartaric acid, sodium polyacrylate and bicarbonates added thereto and saturated with gaseous carbon dioxide while keeping the pH at 9-11. When the final concentration attains 5-6wt%, the pH is adjusted to <=7 and the resultant suspension is dehydrated, dried and disintegrated to afford the aimed readily dispersible colloidal CaCO3 having 0.1-1.0mum particle diameter.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は石灰乳を炭酸化して分散性のよい粒径0.1〜
1.0μmの膠質炭酸カルシウムを、1!!造する方法
に関するものである。
[Detailed description of the invention] [Industrial field of application] The present invention carbonates milk of lime to produce particles with a particle size of 0.1 to 0.1 with good dispersibility.
1.0μm colloid calcium carbonate, 1! ! It is about the method of building.

〔従来の技術〕[Conventional technology]

従来沈降製炭酸カルシウムの製法にはcacz2および
N a 2 COaを原料とする溶液法と、石灰乳に炭
酸ガスを反応させる炭酸ガス化合法とがあシ、さらに後
者の場合、石灰乳に炭酸ガスを導入する方法と、炭酸ガ
ス飽和液中九石灰乳を添加反応させる方法とが行なわれ
ている(特開昭50−3098号参照)。
Conventional methods for producing precipitated calcium carbonate include a solution method using cacz2 and N a 2 COa as raw materials, and a carbonation method in which milk of lime is reacted with carbon dioxide gas, and in the latter case, milk of lime is reacted with carbon dioxide gas. Two methods have been used: one is to introduce milk of nine lime into a carbon dioxide saturated solution, and the other is to react by adding milk of nine lime to a carbon dioxide gas-saturated solution (see JP-A-50-3098).

〔発明の解決しようとする問題点3 本法はこの炭酸ガス飽和液中に石灰乳の一部炭酸化した
連鎖状粒子を添加反ろさせる方法に係シ、易分散性の均
一な0.1〜10μmの炭酸カルシウムを得るため、そ
の反応条件を一定範囲に規定し、第1及び第2物質を添
加する事によってはじめて安定均−に所期の目的を達成
し得るものである。
[Problem to be Solved by the Invention 3] This method relates to a method of adding partially carbonated chain-like particles of milk of lime to this carbon dioxide gas-saturated liquid and causing it to curl. In order to obtain calcium carbonate of ~10 .mu.m, the desired purpose can only be achieved stably and uniformly by defining the reaction conditions within a certain range and adding the first and second substances.

〔問題点を解決するための手段・作用〕本発明の詳細な
説明すると、先ず第1物質であるグルタミンばソーダ、
EDTA硫酸塩または庶楯筐たはそれらの混合Wを0.
1〜0,5部/石灰乳100部添加した45〜50tl
:、10〜15係の範囲に規定した石灰乳に炭酸ガスを
導入して、15〜20係まで一部炭酸化する事により塩
基性度の高い連鎖状粒子を作る。
[Means and effects for solving the problems] To explain the present invention in detail, first, glutamine soda, which is the first substance,
0.0% EDTA sulfate or a mixture thereof.
1-0.5 parts/45-50 tl with 100 parts of milk of lime added
: By introducing carbon dioxide gas into the milk of lime specified in the range of 10 to 15 parts and partially carbonating it to 15 to 20 parts, chain particles with high basicity are made.

この懸濁液を第2!w質であるリンゴ酸、クエン酸、酒
石酸、ポリアクリル酸ソーダまたは重炭酸塩またはこれ
らの混合物の0.1〜1.0部/石灰乳100部を添加
した炭酸ガス飽和液中に、pHを9〜11に保ち乍ら連
続添加し、最終濃度が5〜6重t%になった時点でpH
を7以下にし、脱水。
This suspension is the second one! 0.1 to 1.0 parts of malic acid, citric acid, tartaric acid, sodium polyacrylate, bicarbonate, or a mixture thereof/100 parts of milk of lime were added to a carbon dioxide saturated solution, and the pH was adjusted. Continuously add while maintaining the pH at 9 to 11, and when the final concentration reaches 5 to 6 wt%,
Reduce it to 7 or less and dehydrate.

乾燥、解砕する事によシ粒径0.1〜1.0μmの炭酸
カルシウムを製造する方法である。
This method produces calcium carbonate with a particle size of 0.1 to 1.0 μm by drying and crushing.

本発明には5つの要素があシ、この3要素が満足されな
ければ所期の易分散性膠質炭酸カルシウムを製造する事
は困難である。
There are five elements in the present invention, and unless these three elements are satisfied, it is difficult to produce the desired easily dispersible colloidal calcium carbonate.

即ち一部炭酸化した石灰乳を炭酸ガス飽和液中に連続添
加する方法において、 1)温度、濃度を規定した石灰乳に、 2)第1物質を添加し、 3)炭酸ガス飽和液には第2物質を添加する、の3要素
を同時に満足させる事が必要充分条件である。
That is, in a method in which partially carbonated milk of lime is continuously added to a carbon dioxide saturated liquid, 1) a first substance is added to the milk of lime at a specified temperature and concentration, and 3) a liquid is added to the carbon dioxide saturated liquid. It is a necessary and sufficient condition to simultaneously satisfy the three elements of adding the second substance.

これらの条件を満たさない場合、即ち、第1、第2物質
を使用して石灰乳温度が45℃、濃度が10%未満の場
合、生成する炭酸カルシウム0.1μm未満の粒径にな
シ、通常の手段では乾燥時の凝集が激しく、易分散性の
粉体を得る事が困難である。
If these conditions are not met, that is, when the first and second substances are used, the lime milk temperature is 45 ° C., and the concentration is less than 10%, the produced calcium carbonate has a particle size of less than 0.1 μm, With conventional methods, agglomeration during drying is severe and it is difficult to obtain easily dispersible powder.

また、第1、第2物質の一方または両者を使用しない場
合は勿論両者を使用しても温度が45℃、濃度が15%
を超える場合は生成炭酸カルシウムの粒径が1μmを超
える大粒子とな夛膠質炭酸カルシウムを得る事は出来な
い。
In addition, if one or both of the first and second substances are not used, and even if both are used, the temperature is 45°C and the concentration is 15%.
If it exceeds 1 μm, it will not be possible to obtain large particles of colloidal calcium carbonate with a particle size of more than 1 μm.

易分散性の粒径が0.1〜1.0μmの炭酸カルシウム
については種々の有効利用法が考えられ、特に製紙用塗
工剤、シーリング材、プラスチック用充填剤、塗料用等
使用に際し大きな剪断力のかからない分野では、特にそ
の易分散性による優れた機能を発揮し得るものである。
Calcium carbonate, which is easily dispersible and has a particle size of 0.1 to 1.0 μm, can be used in various effective ways, especially when used as a coating agent for paper manufacturing, a sealant, a filler for plastics, a filler for plastics, a paint, etc. In fields where no force is applied, it can exhibit excellent functionality due to its easy dispersibility.

次にその実施例及び応用の一例を示す。Next, an example of its implementation and application will be shown.

実施例1 グルタミン酸ソーダを0.3部/石灰乳100部添加し
た47℃、12%濃度の石灰乳1771jに、30容量
係濃度の炭酸ガスを導入して、17優まで炭酸化した後
、1rI?の炭酸ガス飽和水にポリアクリル酸ソーダを
0.5部/石灰乳100部添加した別の6ぜ攪拌器反応
器に、炭酸ガスの導入を続は乍らpHを10に保ちっつ
簡々と添加する。最終濃度が59!になった時点で添加
を終了し、さらに炭酸ガスを導入してI)H7まで中和
する。
Example 1 Carbon dioxide gas with a concentration of 30% by volume was introduced into milk of lime 1771j with a concentration of 12% at 47°C to which 0.3 parts of sodium glutamate/100 parts of milk of lime was added, and after carbonation to 17%, 1rI ? 0.5 part of sodium polyacrylate/100 parts of milk of lime was added to carbon dioxide gas-saturated water, and then carbon dioxide gas was introduced into another 6-gear stirrer reactor while keeping the pH at 10. and add. Final concentration is 59! The addition is terminated when the temperature reaches 100%, and carbon dioxide gas is further introduced to neutralize to I) H7.

かくして得た炭酸カルシウム懸濁液をフィルタープレス
で脱水後、”乾燥、解砕する事によ)粒径0.3μmの
分散性膠質炭酸カルシウムを得た。
The thus obtained calcium carbonate suspension was dehydrated using a filter press, and then "dried and crushed" to obtain dispersible colloidal calcium carbonate having a particle size of 0.3 μm.

実施例2   ゛ 実施例1と同様の手段で、グルタミン酸ソーダ0.3m
+7)代、!1llKF、DTAを0.5部使用し、4
5℃。
Example 2 ゛By the same means as in Example 1, 0.3 m of sodium glutamate was added.
+7) generation! 1llKF, using 0.5 parts of DTA, 4
5℃.

10%の石灰乳に、炭酸ガスを導入して15チまで炭酸
化した後、重炭酸ソーダを1.0部添加した別の反厄液
にpHを10に保ち乍ら添加し、最終濃度が5優になる
迄反応を続ける方法により、粒径0.1μmの易分散性
膠質炭酸カルシウムを得た。
10% milk of lime was carbonated to 15% by introducing carbon dioxide gas, and then added to another anti-poison liquid containing 1.0 part of bicarbonate of soda while maintaining the pH at 10 until the final concentration was 5%. Easily dispersible colloidal calcium carbonate with a particle size of 0.1 μm was obtained by continuing the reaction until the particle size was 0.1 μm.

比較例1 実施例1でグルタミン酸ソーダを添加しない場合に粒径
1.7μmの炭酸カルシウムを得た。
Comparative Example 1 Calcium carbonate having a particle size of 1.7 μm was obtained in the same manner as in Example 1 without adding sodium glutamate.

比較例2 実施例1でポリアクリル酸ソーダを添加しない場合に粒
径1.2μmの炭酸カルシウムを得た。
Comparative Example 2 Calcium carbonate having a particle size of 1.2 μm was obtained in the same manner as in Example 1 without adding sodium polyacrylate.

比較例3 実施例1で石灰乳の温度が60℃の場合に粒径1.5μ
mの炭酸カルシウムを得た。
Comparative Example 3 In Example 1, when the temperature of milk of lime was 60°C, the particle size was 1.5μ.
m of calcium carbonate was obtained.

応用例 実施例1,2及び比較例1〜3で得た炭酸カルシウムの
水系分散体を紙塗工に応用した結果を示す。
Application Examples The results of applying the calcium carbonate aqueous dispersions obtained in Examples 1 and 2 and Comparative Examples 1 to 3 to paper coating are shown below.

配合 酸化殿粉(日本食品に、に、:MS$4600)   
 7  ttラテックス(JSRO696)     
   j 3 tr上記配合の塗被カラーを市販上質紙
上にコーティングパーを用いて手塗りし、105±1℃
で3分間乾燥した後、20℃、60%RHの恒温恒湿室
で24時間調湿した。
Combined oxidized starch (Japanese Foods, Ni,: MS$4600)
7 tt latex (JSRO696)
j 3 tr The above-mentioned coating color was hand-coated onto commercially available high-quality paper using a coating parlor, and heated to 105±1°C.
After drying for 3 minutes, the humidity was controlled in a constant temperature and humidity room at 20° C. and 60% RH for 24 hours.

塗被量は何れも20±1 ji /rnゝである。The coating amount was 20±1 ji/rn in each case.

得られた塗被紙の性質を次に示す。The properties of the coated paper obtained are shown below.

〔発明の効果〕〔Effect of the invention〕

本発明の製造法によって得られた易分散性膠質炭酸カル
シウムは塗工紙用填剤として白紙光沢および印刷光沢に
おいて非常に顕著な効果を発揮するものである。
The easily dispersible colloidal calcium carbonate obtained by the production method of the present invention exhibits a very remarkable effect as a filler for coated paper in terms of white paper gloss and print gloss.

1、 事件の表示 昭和61年特許願第11107号 2、 発明の名称 易分散性膠質炭酸カルシウムの製造法 3、 補正をする者 4、 代理人1. Display of incident 1986 Patent Application No. 11107 2. Name of the invention Production method of easily dispersible colloid calcium carbonate 3. Person making the amendment 4. Agent

Claims (1)

【特許請求の範囲】 1)石灰乳に第1物質を添加した後、一部炭酸化して塩
基性度の高い連鎖状粒子を作り、この懸濁液を第2物質
含有炭酸ガス飽和溶液中に連続添加することを特徴とす
る易分散性膠質炭酸カルシウムの製造法。 2)第1物質が、グルタミン酸ソーダ、EDTA硫酸塩
または庶糖の何れかまたはそれらの混合物である特許請
求の範囲第1項記載の易分散性膠質炭酸カルシウムの製
造法。 3)第2物質がリンゴ酸、クエン酸、酒石酸、ポリアク
リル酸ソーダまたは重炭酸塩の何れかまたはそれらの混
合物である特許請求の範囲第1項記載の易分散性膠質炭
酸カルシウムの製造法。 4)石灰乳に第1物質を添加した後、一部炭酸化する反
応を温度45〜50℃、濃度10〜15重量%で行う特
許請求の範囲第1項記載の易分散性膠質炭酸カルシウム
の製造法。
[Claims] 1) After adding a first substance to milk of lime, it is partially carbonated to form chain particles with a high degree of basicity, and this suspension is added to a carbon dioxide saturated solution containing a second substance. A method for producing easily dispersible colloidal calcium carbonate, which is characterized by continuous addition. 2) The method for producing easily dispersible colloidal calcium carbonate according to claim 1, wherein the first substance is sodium glutamate, EDTA sulfate, or sucrose, or a mixture thereof. 3) The method for producing easily dispersible colloidal calcium carbonate according to claim 1, wherein the second substance is malic acid, citric acid, tartaric acid, sodium polyacrylate, or bicarbonate, or a mixture thereof. 4) After adding the first substance to the milk of lime, a partial carbonation reaction is carried out at a temperature of 45 to 50°C and a concentration of 10 to 15% by weight. Manufacturing method.
JP1110786A 1986-01-23 1986-01-23 Production of readily dispersible colloidal calcium carbonate Pending JPS62171920A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1110786A JPS62171920A (en) 1986-01-23 1986-01-23 Production of readily dispersible colloidal calcium carbonate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1110786A JPS62171920A (en) 1986-01-23 1986-01-23 Production of readily dispersible colloidal calcium carbonate

Publications (1)

Publication Number Publication Date
JPS62171920A true JPS62171920A (en) 1987-07-28

Family

ID=11768785

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1110786A Pending JPS62171920A (en) 1986-01-23 1986-01-23 Production of readily dispersible colloidal calcium carbonate

Country Status (1)

Country Link
JP (1) JPS62171920A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0556311A1 (en) * 1990-11-07 1993-08-25 Ecc International Inc. Aggregated composite mineral pigments
GB2312670A (en) * 1996-05-03 1997-11-05 Kyu Jae You Producing calcium carbonate particles having a size 0.1 to 1 micron
EP0844213A1 (en) * 1996-11-20 1998-05-27 Ecc International Limited Precipitates and their production
US6172162B1 (en) 1995-08-30 2001-01-09 Morisei Kako Co., Ltd. Fluorine containing elastomeric sealing composition and sealant
KR100342469B1 (en) * 1999-06-10 2002-06-28 규 재 유 Method for preparation of calcium particles for milk

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0556311A1 (en) * 1990-11-07 1993-08-25 Ecc International Inc. Aggregated composite mineral pigments
EP0556311A4 (en) * 1990-11-07 1994-11-23 Ecc Int Inc Aggregated composite mineral pigments
US6172162B1 (en) 1995-08-30 2001-01-09 Morisei Kako Co., Ltd. Fluorine containing elastomeric sealing composition and sealant
GB2312670A (en) * 1996-05-03 1997-11-05 Kyu Jae You Producing calcium carbonate particles having a size 0.1 to 1 micron
GB2312670B (en) * 1996-05-03 1998-05-20 Kyu Jae You Process for producing calcium carbonate particles having size of 0.1 to 1.0mm
EP0844213A1 (en) * 1996-11-20 1998-05-27 Ecc International Limited Precipitates and their production
KR100342469B1 (en) * 1999-06-10 2002-06-28 규 재 유 Method for preparation of calcium particles for milk

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