JPS62202817A - Production of fine particle of calcium carbonate - Google Patents
Production of fine particle of calcium carbonateInfo
- Publication number
- JPS62202817A JPS62202817A JP4036086A JP4036086A JPS62202817A JP S62202817 A JPS62202817 A JP S62202817A JP 4036086 A JP4036086 A JP 4036086A JP 4036086 A JP4036086 A JP 4036086A JP S62202817 A JPS62202817 A JP S62202817A
- Authority
- JP
- Japan
- Prior art keywords
- calcium carbonate
- suspension
- particles
- carbon dioxide
- dioxide gas
- 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
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 67
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000010419 fine particle Substances 0.000 title abstract 3
- 239000002245 particle Substances 0.000 claims abstract description 51
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 18
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 14
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 13
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 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 claims abstract description 4
- 229930006000 Sucrose Natural products 0.000 claims abstract description 4
- 239000005720 sucrose Substances 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910002651 NO3 Inorganic materials 0.000 claims abstract 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract 2
- 239000004033 plastic Substances 0.000 abstract description 5
- 229920003023 plastic Polymers 0.000 abstract description 5
- 239000000976 ink Substances 0.000 abstract description 4
- 239000003973 paint Substances 0.000 abstract description 4
- 239000000945 filler Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 14
- 239000000123 paper Substances 0.000 description 12
- 235000011116 calcium hydroxide Nutrition 0.000 description 11
- 239000002002 slurry Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000001238 wet grinding Methods 0.000 description 4
- 239000011575 calcium Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009837 dry grinding Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001935 peptisation Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RGJOEKWQDUBAIZ-IBOSZNHHSA-N CoASH Chemical compound O[C@@H]1[C@H](OP(O)(O)=O)[C@@H](COP(O)(=O)OP(O)(=O)OCC(C)(C)[C@@H](O)C(=O)NCCC(=O)NCCS)O[C@H]1N1C2=NC=NC(N)=C2N=C1 RGJOEKWQDUBAIZ-IBOSZNHHSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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〕
本発明は塗工紙、ゴム、プラスチック、塗料、インク等
の基剤として易分散性を有し、かつ不透明性、光沢等の
光学特性上置も有効とされる０、 １〜０．５μｍの粒
度含有する微細炭酸カルシウム粒子の製造方法に係るも
のである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention has easy dispersibility as a base for coated paper, rubber, plastics, paints, inks, etc., and has excellent optical properties such as opacity and gloss. The present invention relates to a method for producing fine calcium carbonate particles having a particle size of 0.1 to 0.5 μm, which is said to be effective even when the temperature is low.
さらに詳しく云えば、本発明は、特定条件の下１水酸化
カルシウム懸濁液と炭酸ガスとを反応させることにより
得た、解膠し易い紡錘形粒子あるいは紡錘形粒子を１７
２〜１／δに折損させた不定形状の炭酸カルシウム粒子
を、湿式あるいは乾式の摩砕あるいは解砕による解膠を
行なうことにより、原料炭酸カルシウムを構成する基本
結晶１ある粒径０．５μｍ以下の微細な炭酸カルシウム
粒子を製造する方法に関するもの！ある。More specifically, the present invention uses easily peptized spindle-shaped particles or spindle-shaped particles obtained by reacting a calcium hydroxide suspension with carbon dioxide gas under specific conditions.
By peptizing irregularly shaped calcium carbonate particles broken to 2 to 1/δ by wet or dry grinding or disintegration, basic crystals 1 constituting the raw material calcium carbonate have a particle size of 0.5 μm or less. Concerning the method of manufacturing fine calcium carbonate particles! be.
石灰石を単に粉砕分級して得られるＴｏ：質炭峻カルシ
ウムを除き、水酸化カルシウム懸濁液と炭酸ガスとの反
応による沈降炭酸カルシウムとしては、通常長径がｆ、
Ｏａｍを上回る紡錘形又は針状の軽質炭酸カルシウムと
０．５μｍ未満の里方形炭酸カルシウムとがあり、単な
る増量目的１は軽質炭酸カルシウムが使用され、ゴム、
プラスチック等の補強性向上のためにはＱ、１μｍ未満
の超微細炭酸カルシウムが妥当とされている。Except for To:charcoal calcium obtained by simply crushing and classifying limestone, precipitated calcium carbonate produced by a reaction between a calcium hydroxide suspension and carbon dioxide gas usually has a major axis of f,
There are spindle-shaped or needle-shaped light calcium carbonate that is larger than Oam, and square-shaped calcium carbonate that is less than 0.5 μm.For simple weight increase purpose 1, light calcium carbonate is used, and rubber,
For improving the reinforcing properties of plastics, etc., ultrafine calcium carbonate of less than Q, 1 μm is considered appropriate.
一方易分散性、不透明性等を最重点項目とする場合、特
に塗工紙用基剤等については、これらの中間−１％０．
１〜０．５μｍの粒径が最も望ましい粒度とされている
。この粒径範囲の炭酸カルシウム粒子を得る方法として
は
１）０．０１〜０．１μｍの結晶核成長による（特公昭
５８−４ＳＡ５１）、
２） 炭酸ガス飽和水中に予め５〜２０％炭酸化した石
灰乳を滴下し、酸性又は中性域１炭酸化反応を行なわせ
る←特公昭４２−１４７０４）、３）２）と同様にして
ｐＨ７，５〜１１０弱塩基性域１炭酸化反応を行わせる
（特公昭５Ｏ−４０９８）、４） 水酸化カルシウムを
添加した０、１μｍ未満の里方形炭酸カルシウムを含炭
酸ガス気流中に噴霧する工程を繰り返す事による（特公
昭５９−等の方法が提案されている。しかしこれらの倒
れの方法においても０．１μｍ以下の里方形膠質粒子を
母体にし、それを成長あるいは集合させる手段・方法が
発想の根幹をなしている。On the other hand, when dispersibility, opacity, etc. are the top priority, especially for coated paper bases, etc., the intermediate between these - 1% 0.
A particle size of 1 to 0.5 μm is considered the most desirable particle size. Methods for obtaining calcium carbonate particles in this particle size range are 1) by crystal nucleus growth of 0.01 to 0.1 μm (Japanese Patent Publication No. 58-4 SA51), 2) carbonation in advance of 5 to 20% in carbon dioxide saturated water. Drop milk of lime and carry out acidic or neutral range 1 carbonation reaction ←Special Publication No. 42-14704), 3) Similarly to 2), pH 7.5-110 weakly basic range 1 carbonation reaction is carried out. (Japanese Patent Publication No. 50-4098), 4) By repeating the process of spraying rectangular calcium carbonate of less than 0.1 μm to which calcium hydroxide has been added (methods such as Japanese Patent Publication No. 59-1982 have been proposed). However, even in these methods of collapsing, the basis of the idea is the means and method of growing or aggregating the matrix of colloidal colloid particles of 0.1 μm or less.
また粒径１５μｍ以下の普通軽質炭酸カルシウムを振動
ミル等で処理し、粒子表面を改良する方法（特開昭６０
−２１０５２１号）もあるが、これは凝集粒子を単一粒
子に分解させる方法であって、本発明の解膠によるもの
とは根本的に異なるもの１ある。There is also a method of improving the particle surface by treating ordinary light calcium carbonate with a particle size of 15 μm or less with a vibration mill etc.
There is also a method (No. 210521), which is a method of decomposing aggregated particles into single particles, and is fundamentally different from the peptization method of the present invention.
本発明は上記のような従来の方法とは異なり、特定条件
下１の水酸化カルシウム懸濁液の炭酸化反応によって得
られる粒径０．８〜１．０μｍの、解膠し易い炭酸カル
シウム粒子を機械的に摩砕および／または解砕すること
により粒径Ｑ、１〜０．５μｍの微細な炭酸カルシウム
粒子を得ようとするもの１ある。水酸化カルシウム懸濁
液の炭酸化によって得られる従来の紡錘形炭酸カルシウ
ム粒子を電子顕微鏡的に詳細に観察すると、０．１μｍ
以下の結晶粒子の規則的な集合体１あることに着目し、
膠質と軽質との中間的粒子ｆある０、１〜０．５μｍの
比較的立方形に近い粒子を安定的に得る方法を見出して
本発明を完成したのｆある。膠質と軽質の中間的粒子を
得ることを本発明においては解膠と呼ぶ。Unlike the conventional method described above, the present invention uses easily peptized calcium carbonate particles with a particle size of 0.8 to 1.0 μm obtained by carbonation reaction of a calcium hydroxide suspension under specific conditions. There is one method in which fine calcium carbonate particles with a particle size Q of 1 to 0.5 μm are obtained by mechanically grinding and/or crushing. When conventional spindle-shaped calcium carbonate particles obtained by carbonation of calcium hydroxide suspension were observed in detail using an electron microscope, they were found to be 0.1 μm in size.
Focusing on the following regular aggregation of crystal grains,
The present invention was completed by discovering a method for stably obtaining relatively cubic particles of 0.1 to 0.5 μm, which are intermediate particles between colloid and light particles. Obtaining particles intermediate between colloid and light particles is called peptization in the present invention.
〔問題点を解決するための手段・作用〕水酸化カルシウ
ムの特定炭酸化条件としては次の５つの要素があり、こ
れと機械的摩砕および／または解砕とを組合せることに
より、はじめて所期の微細炭酸カルシウム粒子を製造し
得るもの１ある。[Means and actions for solving the problem] There are the following five elements as specific carbonation conditions for calcium hydroxide, and by combining these with mechanical grinding and/or crushing, There is one method that can produce fine calcium carbonate particles.
特定条件：
１）濃度１０〜２０重量％、温度６０〜５０℃の水酸化
カルシウム懸濁液を使用する。Specific conditions: 1) Use a calcium hydroxide suspension with a concentration of 10-20% by weight and a temperature of 60-50°C.
２） その懸濁液に可溶性塩類としてＺｎ、Ｍｇ、ｕ等
の塩酸塩、硫酸塩、硝酸塩、酢酸塩または蔗糖を添加す
る。2) Hydrochlorides, sulfates, nitrates, acetates, or sucrose of Zn, Mg, u, etc. are added to the suspension as soluble salts.
６）可溶液塩類を添加した水酸化カルシウム懸濁液に炭
酸ガスｔ−１５０１／分−ｋｇ Ｃａ （ＯＨ）２以上
の可及的早い供給速度で導入する。6) Carbon dioxide gas is introduced into the calcium hydroxide suspension to which soluble salts have been added at a feed rate of t-1501/min-kg Ca (OH)2 or more as fast as possible.
４） この反応により６０〜８０％炭酸化した懸濁液を
第１反応槽において得る。4) A 60-80% carbonated suspension is obtained in the first reaction tank by this reaction.
５）この懸濁液を炭酸ガス導入中の第２反応槽に連続添
加し、ｐＨを９〜１１に保ち乍ら炭酸化反応を完了する
。5) This suspension is continuously added to the second reaction tank where carbon dioxide gas is being introduced, and the carbonation reaction is completed while maintaining the pH at 9 to 11.
かくして得た解膠し易い粒径０．８〜１．０μｍの炭酸
カルシウム粒子につき、ガラス又はセラミックビーズを
充填したサンドグラインダー、ゼールミル等による湿式
法あるいはローラーミル、ハンマーミル等による乾式摩
砕あるいは解砕を行なうことにより、所期の粒径０．１
〜０．５μｍの立方形に近い炭酸カルシウム粒子が得ら
れる。こうし１得た微細な炭酸カルシウムは製紙用塗工
剤として有効！あるのみならず、その粒子表面を有機物
質ｆ処理し乾燥して得た粉体はゴム、プラスチック、塗
料、インク用の易分散性基剤として有効に利用すること
がｆきる。The thus obtained easily peptized calcium carbonate particles with a particle size of 0.8 to 1.0 μm are subjected to wet grinding using a sand grinder, Zeel mill, etc. filled with glass or ceramic beads, or dry grinding or dissolving using a roller mill, hammer mill, etc. By crushing, the desired particle size of 0.1
Sub-cubic calcium carbonate particles of ~0.5 μm are obtained. The fine calcium carbonate obtained in this way is effective as a coating agent for paper manufacturing! Not only that, but the powder obtained by treating the particle surface with an organic substance and drying it can be effectively used as a readily dispersible base for rubber, plastics, paints, and inks.
しかし特定条件のうち１項目でも満足していない場合は
、所期の粒子を安定的に製造することは困難ｆある。However, if even one of the specific conditions is not satisfied, it may be difficult to stably produce the desired particles.
即ち、
１）特に水酸化カルシウム懸濁液の濃度が１０〜２０重
量％、温度が、５０〜５０℃の範囲を外れる場合、
２）規定した可溶性塩類を添加しない場合、５） 炭
酸カニｘｃＤ供給速度が１５０１１５＋ ・ｋｇ Ｃａ
（ＯＨ）２未満の場合、
４） ｆｉｉ＋動イし−Ｖカニ６ｏ〜３０％の範囲を
外れる場合、
５） 第２反応槽〒の反応ｐＨが９〜１１の範囲を外れ
る場合、
以上の１項あるいは２項以上が反応条件として採用され
た場合いかに摩砕・解砕処理を行なっても、また前記特
定条件で製造しても摩砕・解砕処理を行なわない場合は
、いずれも所期の均一な微細炭酸カルシウムを製造する
ことが困難となる。That is, 1) In particular, when the concentration of the calcium hydroxide suspension is 10 to 20% by weight and the temperature is outside the range of 50 to 50°C, 2) When the specified soluble salts are not added, 5) When carbonate crab xcD is supplied Speed is 150115+ ・kg Ca
If (OH) is less than 2, 4) If it is out of the range of fii + moving - V crab 6o to 30%, 5) If the reaction pH of the second reaction tank is out of the range of 9 to 11, 1) If one or more of the above conditions are adopted as the reaction conditions, no matter how much grinding/crushing treatment is performed, or if grinding/crushing is not performed even if the production is performed under the above specified conditions, the expected results will not be met. It becomes difficult to produce uniform fine calcium carbonate.
以下の実施例によって本発明を更に具体的に説明する。The present invention will be explained in more detail with reference to the following examples.
実施例１
第１反応槽において濃度１５重量％、温度４０℃の水酸
化カルシウム懸濁液１０００に９に対し、１０％濃度の
Ｚｎ（Ｊ２を１５に９添加後、６０％濃度の炭酸ガスを
１７０１／／ｆ＋・ｋｇ ０ａ （ＯＨ）２ テ導入し
て炭酸化反応を８０％行なった後、得られた懸濁液を第
２反応槽においてｐＨ＝１０？炭酸ガスを導入し、炭酸
化を完了する。こうして得られた反応生成物を遠心分離
機で脱水し、固形分７０重量％のケーキ状物を得る。こ
れに分散剤としてＫＴ−１Ｑ。Example 1 In a first reaction tank, a 10% concentration of Zn (J2) was added to 9 to 1000 of a calcium hydroxide suspension at a concentration of 15% by weight and a temperature of 40°C, and then carbon dioxide gas of 60% concentration was added. 1701//f+・kg 0a (OH)2 was introduced to perform 80% carbonation reaction, and the resulting suspension was placed in a second reaction tank at pH=10? Carbon dioxide gas was introduced and carbonation was carried out. Completed. The reaction product thus obtained is dehydrated using a centrifuge to obtain a cake-like product with a solid content of 70% by weight. KT-1Q is added to this as a dispersant.
（花王石鹸■製）を純分換算ｆ０．５部／炭カル固形分
１００部添加して強力に攪拌する。(manufactured by Kao Soap ■) was added in terms of pure f0.5 part/charcoal solid content 100 parts and stirred vigorously.
Ｂ型粘度計によるスラリー粘度が５００ｃｐｓ／６０
ｒｐｍになった時点ｆ、スラリーを浅田鉄工製サンドグ
ラインダー（ベッセル容：１２００ ｌｔ、ガラスピー
ズ添加後容量１０（１）に移し、粘度が１５０ ＣｐＳ
／６０ ｒｐｍになる迄湿式摩砕を続けることにより、
光透過式粒度分布測定器（セイシン企業製）による平均
粒子径が０．４μｍ１粒度分布２μｍ以下が９８％の６
５％スラリーを得た。Slurry viscosity measured by B-type viscometer is 500 cps/60
When the rpm reached f, the slurry was transferred to a sand grinder made by Asada Iron Works (vessel capacity: 1200 lt, capacity after adding glass beads: 10(1), and the viscosity was 150 CpS.
By continuing wet milling until the speed reaches /60 rpm,
The average particle diameter measured by a light transmission particle size distribution analyzer (manufactured by Seishin Enterprises) is 0.4 μm.1 The particle size distribution is 2 μm or less in 98%6.
A 5% slurry was obtained.
実施例２
実施例１−ｒ！ＺｎＣｌ２の代りに１０％濃度の蔗糖を
８ゆ添加するほかは同様の方法↑炭酸カルシウムを製造
し、平均粒子径が０．５μｍ、２μｍ以下が９５％の６
５％スラリーを得た。Example 2 Example 1-r! The same method was used except that 10% sucrose was added instead of ZnCl2 ↑ Calcium carbonate was produced, and the average particle size was 0.5 μm, and 95% of the particles were 2 μm or less.
A 5% slurry was obtained.
実施例６
実施例１の湿式摩砕の代りに、細用ミクロン■製スーパ
ーミクロンミル！解砕した平均粒子径が０．５μｍ１粒
度分布２μｍ以下が９６％の６５％スラリーを得た。Example 6 Instead of wet grinding in Example 1, a super micron mill manufactured by Fine Micron■ is used! A 65% slurry was obtained in which the average particle size of the crushed particles was 0.5 μm and 96% of particles in the particle size distribution were 2 μm or less.
比較例１
実施例１″′Ｉ％ＺｎｅＪｚを添加しないで、そのほか
は同様の方法！炭酸カルシウムを製造し、平均粒子径が
１６０μｍ、２μｍ以下が７５％の６０％スラリーを得
た。Comparative Example 1 Example 1''I% ZneJz was not added, but otherwise the same method was used! Calcium carbonate was produced to obtain a 60% slurry with an average particle diameter of 160 μm and 75% of which was 2 μm or less.
参考例
実施例１．２． ！１及び比較例１の炭酸カルシウム粒
子を塗工紙に応用したときのデーターは次の通りマある
。Reference Examples Example 1.2. ! The data when the calcium carbonate particles of Example 1 and Comparative Example 1 were applied to coated paper are as follows.
塗工紙配合：
炭酸カルシウムスラリー １００部（固形分とし
て）酸化誠粉（日食ＭＳ１６００） ５部（〃）
上記配合の５０％濃度塗被カラーを市販の上質紙にコー
ティングパーを用いて手塗りし、室温乾燥後シーズニン
グし、２０９／−の塗被量で試験した。Coated paper composition: Calcium carbonate slurry 100 parts (as solid content) Oxidized Seishin powder (Eclipse MS1600) 5 parts (〃)
The above-mentioned 50% strength coating color was hand-coated onto commercially available high-quality paper using a coating parlor, dried at room temperature, seasoned, and tested at a coating weight of 209/-.
白紙及び印刷光沢度の試験はＪＩＳＰ８１２！に準拠し
て行った。試験結果は次表の通り１ある。Blank paper and print gloss tests are JISP812! This was done in accordance with the. The test results are as shown in the table below.
表の結果から、本発明による微細炭酸カルシウムは紙に
塗工したときに優れた白紙光沢および印刷光沢を示すこ
とが明らかマある。From the results in the table, it is clear that the finely divided calcium carbonate according to the invention exhibits excellent white paper gloss and print gloss when applied to paper.
本発明の微細炭酸カルシウムの製造方法によれば、粒径
０．１〜０．５μ気の比較的里方体に近い形状の炭酸カ
ルシウム粒子が安定して得られ、こうして得られた炭酸
カルシウム粒子は♂ム、プラスチツク、塗料インクの填
料として有用であるばかりマなく、特に製紙用塗工剤に
使用したときに優れた白紙光沢および印刷光沢を有する
塗工紙が得られる。According to the method for producing fine calcium carbonate of the present invention, calcium carbonate particles having a particle size of 0.1 to 0.5 μm and having a shape relatively close to a culopoid can be stably obtained. Not only is it useful as a filler for boys, plastics, and paint inks, but it also provides coated paper with excellent white paper gloss and printing gloss, especially when used as a coating agent for paper manufacturing.
Claims (1)
カルシウム懸濁液に可溶性塩類を添加した後、炭酸ガス
を１５０ｌ／分・Ｋｇ Ｃａ（ＯＨ）＿２以上の速度で
供給することにより第１反応槽内で６０〜８０％炭酸化
した懸濁液を炭酸ガス導入中の第２反応槽に添加し、ｐ
Ｈを９〜１１に保ち乍ら炭酸化反応を完了した後、磨砕
および／または解砕処理を行なうことを特徴とする粒径
０．１〜０．５μｍの微細炭酸カルシウムの製造方法。 ２）可溶性塩類としてＺｎ、Ｍｇ、Ａｌ等の塩酸塩、硫
酸塩、硝酸塩、酢酸塩または庶糖を使用する特許請求の
範囲第１項記載の微細炭酸カルシウム粒子の製造方法。[Claims] 1) After adding soluble salts to a calcium hydroxide suspension with a concentration of 10 to 20% by weight and a temperature of 30 to 50°C, carbon dioxide gas is added at a rate of 150 l/min·Kg Ca(OH)_2 or more. The suspension, which has been carbonated by 60 to 80% in the first reaction tank by feeding at a high speed, is added to the second reaction tank where carbon dioxide gas is being introduced.
A method for producing fine calcium carbonate having a particle size of 0.1 to 0.5 μm, which comprises completing a carbonation reaction while maintaining H at 9 to 11, and then carrying out a grinding and/or crushing treatment. 2) The method for producing fine calcium carbonate particles according to claim 1, wherein hydrochloride, sulfate, nitrate, acetate, or sucrose of Zn, Mg, Al, etc. is used as the soluble salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4036086A JPS62202817A (en) | 1986-02-27 | 1986-02-27 | Production of fine particle of calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4036086A JPS62202817A (en) | 1986-02-27 | 1986-02-27 | Production of fine particle of calcium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62202817A true JPS62202817A (en) | 1987-09-07 |
Family
ID=12578471
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4036086A Pending JPS62202817A (en) | 1986-02-27 | 1986-02-27 | Production of fine particle of calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62202817A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0226996A (en) * | 1988-06-03 | 1990-01-29 | Pfizer Inc | Production of precipitated calcium carbonate and binder system |
| WO1997020771A1 (en) * | 1995-12-05 | 1997-06-12 | Minerals Technologies Inc. | Process for the preparation of discrete particles of calcium carbonate |
| US5750086A (en) * | 1996-02-02 | 1998-05-12 | Kyu Jae Y | Process for producing ultrafine particles of colloidal calcium carbonate |
| JP2001354415A (en) * | 2000-06-09 | 2001-12-25 | Hokkaido Kyodo Sekkai Kk | Method for manufacturing lightweight calcium carbonate |
| JP2001354416A (en) * | 2000-06-09 | 2001-12-25 | Hokkaido Kyodo Sekkai Kk | Method for manufacturing aragonite type calcium carbonate |
| JP2002128521A (en) * | 2000-10-20 | 2002-05-09 | Hokkaido Kyodo Sekkai Kk | Method of manufacturing calcium carbonate |
| JP2004345932A (en) * | 2003-05-26 | 2004-12-09 | Shiraishi Kogyo Kaisha Ltd | Surface treated colloidal calcium carbonate |
| JP2007176789A (en) * | 2005-12-01 | 2007-07-12 | Ube Material Industries Ltd | Barium carbonate powder and method of manufacturing the same |
| EP2412376A1 (en) * | 2005-09-29 | 2012-02-01 | Raymond Lee Nip | Zink oxide coated particles, compostions containing the same, and methods for making the same |
| US8470282B2 (en) | 2009-10-02 | 2013-06-25 | Calcitech Synthetic Minerals Ltd. | Production of calcium carbonate |
| US8658119B2 (en) | 2009-12-14 | 2014-02-25 | Calcitech Synthetic Minerals Ltd. | Production and/or recovery of products from waste sludge |
| CN103818941A (en) * | 2013-05-27 | 2014-05-28 | 芜湖卓越纳米新材料有限公司 | Preparation method of special low-viscosity activated calcium carbonate for silicone adhesive |
| CN106542557A (en) * | 2016-10-18 | 2017-03-29 | 博广热能股份有限公司 | A kind of preparation technology of nano-calcium carbonate |
| CN112266005A (en) * | 2020-11-10 | 2021-01-26 | 吴亚良 | Preparation method of nano calcium carbonate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57123822A (en) * | 1981-01-23 | 1982-08-02 | Okutama Kogyo Kk | Preparation of calcite-type calcium carbonate crystal |
| JPS59199731A (en) * | 1983-04-27 | 1984-11-12 | Maruo Calcium Kk | Preparation of linearly connected calcium carbonate having high dispersibility |
| JPS59223225A (en) * | 1983-05-27 | 1984-12-15 | Shiraishi Chuo Kenkyusho:Kk | Manufacture of calcium carbonate |
-
1986
- 1986-02-27 JP JP4036086A patent/JPS62202817A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57123822A (en) * | 1981-01-23 | 1982-08-02 | Okutama Kogyo Kk | Preparation of calcite-type calcium carbonate crystal |
| JPS59199731A (en) * | 1983-04-27 | 1984-11-12 | Maruo Calcium Kk | Preparation of linearly connected calcium carbonate having high dispersibility |
| JPS59223225A (en) * | 1983-05-27 | 1984-12-15 | Shiraishi Chuo Kenkyusho:Kk | Manufacture of calcium carbonate |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0226996A (en) * | 1988-06-03 | 1990-01-29 | Pfizer Inc | Production of precipitated calcium carbonate and binder system |
| WO1997020771A1 (en) * | 1995-12-05 | 1997-06-12 | Minerals Technologies Inc. | Process for the preparation of discrete particles of calcium carbonate |
| US5750086A (en) * | 1996-02-02 | 1998-05-12 | Kyu Jae Y | Process for producing ultrafine particles of colloidal calcium carbonate |
| JP2001354415A (en) * | 2000-06-09 | 2001-12-25 | Hokkaido Kyodo Sekkai Kk | Method for manufacturing lightweight calcium carbonate |
| JP2001354416A (en) * | 2000-06-09 | 2001-12-25 | Hokkaido Kyodo Sekkai Kk | Method for manufacturing aragonite type calcium carbonate |
| JP2002128521A (en) * | 2000-10-20 | 2002-05-09 | Hokkaido Kyodo Sekkai Kk | Method of manufacturing calcium carbonate |
| JP2004345932A (en) * | 2003-05-26 | 2004-12-09 | Shiraishi Kogyo Kaisha Ltd | Surface treated colloidal calcium carbonate |
| EP2412376A1 (en) * | 2005-09-29 | 2012-02-01 | Raymond Lee Nip | Zink oxide coated particles, compostions containing the same, and methods for making the same |
| JP2007176789A (en) * | 2005-12-01 | 2007-07-12 | Ube Material Industries Ltd | Barium carbonate powder and method of manufacturing the same |
| US8470282B2 (en) | 2009-10-02 | 2013-06-25 | Calcitech Synthetic Minerals Ltd. | Production of calcium carbonate |
| US8658119B2 (en) | 2009-12-14 | 2014-02-25 | Calcitech Synthetic Minerals Ltd. | Production and/or recovery of products from waste sludge |
| CN103818941A (en) * | 2013-05-27 | 2014-05-28 | 芜湖卓越纳米新材料有限公司 | Preparation method of special low-viscosity activated calcium carbonate for silicone adhesive |
| CN106542557A (en) * | 2016-10-18 | 2017-03-29 | 博广热能股份有限公司 | A kind of preparation technology of nano-calcium carbonate |
| CN112266005A (en) * | 2020-11-10 | 2021-01-26 | 吴亚良 | Preparation method of nano calcium carbonate |
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