JP2010150067A - Method for producing readily-soluble calcium carbonate powder and calcium carbonate powder obtained thereby - Google Patents
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本発明は、水に容易に溶解し得る炭酸カルシウム粉末の製造方法及びその方法により得られる新規炭酸カルシウム粉末に関する。 The present invention relates to a method for producing a calcium carbonate powder that can be easily dissolved in water, and a novel calcium carbonate powder obtained by the method.
石灰乳化法により得られる軽質炭酸カルシウム粉末は、水系塗料、水性インキなどの体質顔料や、ゴム、プラスチック、紙などの充填剤や、制酸剤、食品添加剤、化粧品添加剤として広く用いられている。 Light calcium carbonate powder obtained by the lime emulsification method is widely used as extender pigments such as water-based paints and water-based inks, fillers such as rubber, plastic and paper, antacids, food additives and cosmetic additives. Yes.
ところで、この軽質炭酸カルシウムの乾燥粉末を調製する方法としては、水酸化カルシウムの水懸濁液と二酸化炭素とを５〜３０℃で反応させてカルサイト型炭酸カルシウムの一次粒子を形成させ、次いでこれを噴霧乾燥して比表面積２０ｍ2／ｇ以上の球状カルサイト型炭酸カルシウム二次粒子を調製する方法（特許文献１参照）、平均粒径０．１〜１００μｍの範囲の炭酸カルシウム粉体粒子５〜２０重量％と、その粉体粒子の１〜４０重量％の分散剤を含む炭酸カルシウムエマルションをスプレードライヤー乾燥又は凍結乾燥して、見掛け比重０．４ｇ／ｍｌ以上の粉体とする方法（特許文献２参照）などが知られている。 By the way, as a method of preparing this dry powder of light calcium carbonate, an aqueous suspension of calcium hydroxide and carbon dioxide are reacted at 5 to 30 ° C. to form primary particles of calcite type calcium carbonate, A method for preparing spherical calcite-type calcium carbonate secondary particles having a specific surface area of 20 m 2 / g or more by spray drying (see Patent Document 1), calcium carbonate powder particles having an average particle size of 0.1 to 100 μm A method of producing a powder having an apparent specific gravity of 0.4 g / ml or more by spray drying or freeze-drying a calcium carbonate emulsion containing 5 to 20% by weight and a dispersant of 1 to 40% by weight of the powder particles ( Patent Document 2) is known.
しかしながら、これらの方法で調製された軽質炭酸カルシウムは、乾燥時に凝集するため、粉体を再溶解分散させる場合、粒子が十分に分散せず、粒径も乾燥前のものよりも大きくなる傾向があり、また嵩密度も小さく、輸送や貯蔵が不利になるという欠点がある。 However, since the light calcium carbonate prepared by these methods aggregates during drying, when the powder is re-dissolved and dispersed, the particles are not sufficiently dispersed and the particle size tends to be larger than that before drying. In addition, the bulk density is small, and there is a disadvantage that transportation and storage are disadvantageous.
他方、炭酸カルシウム粉末の分散性を改善する方法として、スラリー状の炭酸カルシウムを親水性乳化剤の水溶液と混合し、この混合物を脱水処理したのち、真空下に乾燥することにより、分散性の良好な炭酸カルシウム複合体を製造する方法（特許文献３参照）が提案されているが、この方法は、炭酸カルシウム以外の成分を含むため、利用分野が制限される上、ショ糖脂肪酸エステルのような特殊な親水性乳化剤を用いるためにコスト的にも不利になるのを免れない。 On the other hand, as a method for improving the dispersibility of the calcium carbonate powder, slurry-like calcium carbonate is mixed with an aqueous solution of a hydrophilic emulsifier, this mixture is dehydrated, and then dried under vacuum to achieve good dispersibility. A method for producing a calcium carbonate complex (see Patent Document 3) has been proposed. However, since this method includes components other than calcium carbonate, the field of use is limited and special methods such as sucrose fatty acid esters are used. Since a hydrophilic emulsifier is used, it is inevitable that the cost is disadvantageous.
本発明は、このような事情のもとで、従来の軽質炭酸カルシウムの製造方法における欠点を克服し、簡単な手段により効率よく水への溶解性が良好な軽質炭酸カルシウム粉末を製造する方法を提供することを目的としてなされたものである。 Under such circumstances, the present invention overcomes the disadvantages of conventional light calcium carbonate production methods, and provides a method for producing light calcium carbonate powder having good water solubility by simple means. It was made for the purpose of providing.
本発明者らは、易溶性軽質炭酸カルシウムの製造方法について種々研究を重ねた結果、従来方法において製造された軽質炭酸カルシウム粉末の水への溶解性が良好でないのは、乾燥を気流中で行うため、乾燥時に１０μｍ以下の小さな凝集体が発生し、乾燥物として得られる二次凝集粒子中の空隙に空気が取り込まれ、それが水への溶解を妨げていること、したがって、乾燥の際、二次凝集粒子中に空気が取り込まれるのを抑制すれば、溶解しやすい軽質炭酸カルシウム粒子が得られること、それには気流乾燥を用いずに、加熱した固体面に粒子を直接接触させる乾燥方法をとればよいことを見出し、この知見に基づいて本発明をなすに至った。 The inventors of the present invention have conducted various studies on a method for producing easily soluble light calcium carbonate. As a result, the light solubility of light calcium carbonate powder produced by the conventional method is not good. Therefore, a small aggregate of 10 μm or less is generated at the time of drying, and air is taken into the voids in the secondary aggregated particles obtained as a dried product, which prevents the dissolution in water. If air is prevented from being taken into the secondary agglomerated particles, light calcium carbonate particles that are easy to dissolve can be obtained. Based on this finding, the present inventors have made the present invention.
すなわち、本発明は、軽質炭酸カルシウム粉体から、その高濃度分散スラリーを調製し、加熱した固体面に直接接触させることにより、乾燥させることを特徴とする易溶性軽質炭酸カルシウム粉末の製造方法、及びその方法により得られる平均粒径１μｍ未満の一次粒子が凝集して平均粒径１０〜５０μｍで見掛け密度０．５ｇ／ｃｍ3以上、及び細孔容積１．０ｃｍ3／ｇ以下の二次凝集粒子を形成してなる軽質炭酸カルシウム乾燥粉末を提供するものである。ここで平均粒径とはメジアン径を意味する。 That is, the present invention is a method for producing a readily soluble light calcium carbonate powder, characterized in that a high-concentration dispersed slurry is prepared from light calcium carbonate powder and dried by direct contact with a heated solid surface, And primary particles obtained by the method having an average particle size of less than 1 μm aggregate to have an average particle size of 10 to 50 μm, an apparent density of 0.5 g / cm 3 or more, and a pore volume of 1.0 cm 3 / g or less. The present invention provides a light calcium carbonate dry powder formed with particles. Here, the average particle diameter means the median diameter.
軽質炭酸カルシウムは、水酸化カルシウムの水性懸濁液に二酸化炭素を導入して炭酸化反応を行わせて、炭酸カルシウムを生成させ、沈降させることによって製造される。このようにして得られる軽質炭酸カルシウムには、その製造条件によってカルサイト型、アラゴナイト型及びパテライト型の３種の結晶構造を有するものを生じるが、本発明方法においては、そのいずれも用いることができる。この軽質炭酸カルシウムは平均粒径１μｍ未満、好ましくは０．１〜０．５μｍの一次粒子からなる粉末として用いる。 Light calcium carbonate is produced by introducing carbon dioxide into an aqueous suspension of calcium hydroxide to cause a carbonation reaction to produce and precipitate calcium carbonate. The light calcium carbonate thus obtained has three types of crystal structures of calcite type, aragonite type and patelite type depending on the production conditions, and any of them can be used in the method of the present invention. it can. This light calcium carbonate is used as a powder composed of primary particles having an average particle size of less than 1 μm, preferably 0.1 to 0.5 μm.
本発明方法においては、先ず原料の軽質炭酸カルシウムを水に加え、再分散処理して、高濃度水性スラリーを調製する。この水性スラリーの濃度としては、５０質量％以上、好ましくは６０質量％以上が選ばれる。この水性スラリーの調製は、分散剤なしで行ってもよいし、分散剤を用いて行ってもよい。 In the method of the present invention, first, light calcium carbonate as a raw material is added to water and redispersed to prepare a highly concentrated aqueous slurry. The concentration of this aqueous slurry is 50% by mass or more, preferably 60% by mass or more. This aqueous slurry may be prepared without a dispersant or with a dispersant.
この分散剤としては、軽質炭酸カルシウムの水性スラリーを調製する際に慣用されているものの中から任意に選んで用いることができる。このような分散剤としては、例えばポリアクリル酸ナトリウム、ショ糖脂肪酸エステル、グリセリン脂肪酸エステル、アクリル酸−マレイン酸共重合体アンモニウム塩、メタクリル酸−ナフトキシポリエチレングリコールアクリレート共重合体、メタクリル酸−ポリエチレングリコールモノメタクリレート共重合体アンモニウム塩、ポリエチレングリコールモノアクリレートなどがある。これらは、単独で用いてもよいし、また２種以上を組み合わせて用いてもよい。
これらの分散剤を用いる場合には、軽質炭酸カルシウム粉末１００質量部当り、０．１〜５質量部、好ましくは０．５〜２質量部の割合で添加される。
The dispersant can be arbitrarily selected from those commonly used when preparing an aqueous slurry of light calcium carbonate. Examples of such a dispersant include sodium polyacrylate, sucrose fatty acid ester, glycerin fatty acid ester, acrylic acid-maleic acid copolymer ammonium salt, methacrylic acid-naphthoxypolyethylene glycol acrylate copolymer, methacrylic acid-polyethylene. Examples include glycol monomethacrylate copolymer ammonium salts and polyethylene glycol monoacrylate. These may be used alone or in combination of two or more.
When these dispersants are used, they are added at a ratio of 0.1 to 5 parts by weight, preferably 0.5 to 2 parts by weight, per 100 parts by weight of light calcium carbonate powder.
本発明方法においては、上記の軽質炭酸カルシウムの高濃度水性スラリーを乾燥して粉体を形成させるが、この乾燥は、水性スラリーを加熱した固体面に直接接触させ、急速に水分を除去することにより行うことが必要である。この加熱面に直接接触させて行う乾燥は、例えばドラムドライヤー、ディスクドライヤーのような円筒型乾燥機を用いる方法、ホットプレート上で転動させる方法などによって行うことができるが、特にスラリーの撹拌、混合を効率的にするディスク状の熱交換面を備えた乾燥機（特開平９−３２４９８６号公報参照）を用いて行うのが好ましい。
この際の加熱した固体面の温度としては１００〜２００℃、好ましくは１１０〜１５０℃の範囲が選ばれる。
In the method of the present invention, the light calcium carbonate high-concentration aqueous slurry is dried to form a powder. This drying is performed by bringing the aqueous slurry into direct contact with a heated solid surface and rapidly removing moisture. It is necessary to do this. The drying performed by direct contact with the heating surface can be performed by a method using a cylindrical dryer such as a drum dryer or a disk dryer, a method of rolling on a hot plate, etc. It is preferable to use a drier (see JP-A-9-324986) having a disk-shaped heat exchange surface for efficient mixing.
The temperature of the heated solid surface at this time is selected in the range of 100 to 200 ° C, preferably 110 to 150 ° C.
このようにして、見掛け密度０．５ｇ／ｃｍ3以上、かつ細孔容積１．０ｃｍ3／ｇ以下をもつ、平均粒径１μｍ未満の一次粒子の凝集した平均粒径１０〜５０μｍの二次凝集粒子からなる易溶性軽質炭酸カルシウム乾燥粉末が得られる。 In this way, secondary agglomeration with an average particle diameter of 10 to 50 μm in which primary particles having an apparent density of 0.5 g / cm 3 or more and a pore volume of 1.0 cm 3 / g or less and an average particle diameter of less than 1 μm are aggregated. An easily soluble light calcium carbonate dry powder consisting of particles is obtained.
これまでの方法で得られる軽質炭酸カルシウム粉末の見掛け密度は、０．５ｇ／ｃｍ3未満、通常は０．１７〜０．３８ｇ／ｃｍ3程度であり、見掛け密度０．５ｇ／ｃｍ3以上のものを得ることは困難であった。それは従来の軽質炭酸カルシウム粉末の製造に際しては、炭酸カルシウム水性スラリーの乾燥方法として用いられている噴霧乾燥、凍結乾燥はいずれも空気のようなガス気流中で行われており、乾燥時に一次粒子が凝集して、平均粒径１０〜５０μｍの二次凝集粒子が形成する際、一次粒子間の空隙に雰囲気中のガス、例えば空気が取り込まれ、軽質炭酸カルシウムを水に投入した場合、その空隙中のガスが水の浸入を妨げる結果、水への溶解性が低下するためであった。 The apparent density of the light calcium carbonate powder obtained in previous methods, less than 0.5 g / cm 3, typically is about 0.17~0.38g / cm 3, an apparent density of 0.5 g / cm 3 or more It was difficult to get things. In the production of conventional light calcium carbonate powder, spray drying and freeze drying, both of which are used as drying methods for calcium carbonate aqueous slurry, are performed in a gas stream such as air. When secondary agglomerated particles having an average particle diameter of 10 to 50 μm are formed by aggregation, gas in the atmosphere, for example, air is taken into the gaps between the primary particles, and light calcium carbonate is poured into water. This was because the gas in the water hindered the intrusion of water, resulting in a decrease in water solubility.
本発明方法においては、気流ガス粒子中に取り込まれるのを極力避けるために、軽質炭酸カルシウムの高濃度水性スラリーを直接加熱した固体面に接触させ、雰囲気中のガスが一次粒子間空隙に取り込まれない条件下で脱水し、乾燥する。この乾燥に際しては、雰囲気中のガスに取り込まれるのをできるだけ避けるために真空条件下で行うのも有利である。 In the method of the present invention, in order to avoid being taken into the airflow gas particles as much as possible, a high-concentration aqueous slurry of light calcium carbonate is brought into contact with the directly heated solid surface, and the gas in the atmosphere is taken into the primary interparticle voids. Dehydrate and dry under no conditions. It is also advantageous to perform this drying under vacuum conditions in order to avoid as much as possible being taken in by the gas in the atmosphere.
このようにして、含水率１．０質量％以下、好ましくは０．５質量％以下、細孔容積１．０ｃｍ3／ｇ以下、好ましくは０．８ｃｍ3／ｇ以下の二次凝集粒子からなる、水に易溶性の軽質炭酸カルシウム粉末が得られる。そして、このようにして得られた軽質炭酸カルシウム粉末は、従来のガス気流中乾燥により得られたものが、見掛け密度０．５ｇ／ｃｍ3未満という低密度であるのに対し、見掛け密度０．５ｇ／ｃｍ3以上、多くの場合０．６５ｇ／ｃｍ3又はそれ以上という高密度のものとなる。 In this way, it consists of secondary aggregated particles having a water content of 1.0% by mass or less, preferably 0.5% by mass or less, and a pore volume of 1.0 cm 3 / g or less, preferably 0.8 cm 3 / g or less. A light calcium carbonate powder that is readily soluble in water is obtained. The light calcium carbonate powder thus obtained is obtained by conventional drying in a gas stream, while the apparent density is less than 0.5 g / cm 3 , whereas the apparent density is 0.00. The density is 5 g / cm 3 or more, and in many cases 0.65 g / cm 3 or more.
本発明によれば、水中に投入した時、従来のものに比べ、約１／４という短時間で溶解する易溶解性軽質炭酸カルシウム粉末を簡単に得ることができる。 According to the present invention, it is possible to easily obtain an easily soluble light calcium carbonate powder that dissolves in a short time of about 1/4 when compared with conventional ones when put into water.
次に、実施例により、本発明を実施するための最良の形態を説明するが、本発明は、これによりなんら限定されるものではない。 Next, the best mode for carrying out the present invention will be described by way of examples, but the present invention is not limited thereto.
なお、各例中の物性値は以下の方法により測定したものである。
（１）平均粒径（メジアン径）
堀場製作所製レーザー回折散乱式粒度分布測定装置「ＬＡ−９２０」を用いて測定した。
（２）見掛け密度
ＪＩＳ Ｋ ５１０１に規定された方法に従って測定した。
（３）Ｂ型粘度
トキメック社製Ｂ型粘度計を用い、ローター回転数６０ｒｐｍ、スラリー温度２５℃において測定した。
（４）細孔容積
マイクロメリティックス社製、細孔容積測定装置「ポアサイザ９３２０」を用いて測定した。
In addition, the physical-property value in each example is measured with the following method.
(1) Average particle diameter (median diameter)
The measurement was performed using a laser diffraction scattering type particle size distribution analyzer “LA-920” manufactured by HORIBA, Ltd.
(2) Apparent density It measured according to the method prescribed | regulated to JISK5101.
(3) B-type viscosity Using a B-type viscometer manufactured by Tokimec, the viscosity was measured at a rotor rotational speed of 60 rpm and a slurry temperature of 25 ° C.
(4) Pore volume It measured using the pore volume measuring apparatus "pore sizer 9320" by Micromeritics.
参考例１
水酸化カルシウムを２０℃の水に混合して４００ｇ／リットルの濃度に調整したのち、コーレスミキサーで処理して２５℃における粘度２５００ｍＰａ・ｓの水酸化カルシウム水性懸濁液を得た。この水酸化カルシウム水性懸濁液を水で希釈して２００ｇ／リットルに調整し、そのうちの１５リットルを回分式反応槽に供給した。この反応槽中の懸濁液の液温を４０℃に調整したのち、工業用二酸化炭素ガス（純度９９．９ｖｏｌ％）を０．２ｍ3／ｈの割合で導入し、炭酸化反応を行い、平均粒径０．４７μｍのアラゴナイト柱状炭酸カルシウムスラリーを得た。このスラリーをフィルタープレスを用いて脱水処理し、ケーキ状の炭酸カルシウムを得た。
Reference example 1
Calcium hydroxide was mixed with 20 ° C. water to adjust the concentration to 400 g / liter, and then treated with a Coreless mixer to obtain a calcium hydroxide aqueous suspension having a viscosity of 2500 mPa · s at 25 ° C. This calcium hydroxide aqueous suspension was diluted with water to adjust to 200 g / liter, and 15 liters thereof was supplied to the batch reactor. After adjusting the liquid temperature of the suspension in this reaction tank to 40 ° C., carbon dioxide gas for industrial use (purity 99.9 vol%) was introduced at a rate of 0.2 m 3 / h to conduct a carbonation reaction, An aragonite columnar calcium carbonate slurry having an average particle size of 0.47 μm was obtained. This slurry was dehydrated using a filter press to obtain cake-like calcium carbonate.
参考例２
酸化カルシウムを６０℃の水を用いて消化し、１時間撹拌したのち、目開き４４μｍの篩で残渣を除去した。さらにこのスラリーを３液分離型の液体サイクロン（ＴＲ−１０、大石機械社製）で処理を行い、トップ及びミドルより吐出された固形分濃度１０質量％の水酸化カルシウムスラリーを回収した。このスラリーの一部を採取し、水で希釈して１５℃、３質量％に調整したのち、そのうちの３０リットルを回分式反応槽に供給した。この反応槽に工業用二酸化炭素ガス（純度９９．９ｖｏｌ％）を０．０６ｍ3／ｈの割合で導入し、炭酸化率が２０％になるまで炭酸化反応を行い、一次炭酸化スラリーを得た。
一方、液体サイクロンより回収したスラリー２０リットルを別の回分式反応槽に供給し、さらに一次炭酸化スラリー５リットルと水５リットルを加え、３０リットルとしたのち、温度を５０℃に調整し、工業用二酸化炭素ガス（純度９９．９ｖｏｌ％）を０．６ｍ3／ｈの割合で導入し、炭酸化反応を行い、平均粒径０．４９μｍのカルサイト紡錘状炭酸カルシウムスラリーを得た。このスラリーをフィルタープレスを用いて脱水処理し、ケーキ状の炭酸カルシウムを得た。
Reference example 2
Calcium oxide was digested with water at 60 ° C. and stirred for 1 hour, and then the residue was removed with a sieve having an opening of 44 μm. Further, this slurry was treated with a three-liquid separation type liquid cyclone (TR-10, manufactured by Oishi Machine Co., Ltd.), and a calcium hydroxide slurry having a solid content concentration of 10% by mass discharged from the top and middle was recovered. A part of this slurry was sampled, diluted with water and adjusted to 15 ° C. and 3% by mass, and 30 liters of the slurry was supplied to a batch reactor. Industrial carbon dioxide gas (purity 99.9 vol%) was introduced into this reaction tank at a rate of 0.06 m 3 / h, and the carbonation reaction was carried out until the carbonation rate reached 20% to obtain a primary carbonation slurry. It was.
On the other hand, 20 liters of slurry recovered from the hydrocyclone is supplied to another batch reactor, and 5 liters of primary carbonation slurry and 5 liters of water are added to make 30 liters. Carbon dioxide gas (purity 99.9 vol%) was introduced at a rate of 0.6 m 3 / h, and a carbonation reaction was carried out to obtain a calcite spindle-like calcium carbonate slurry having an average particle size of 0.49 μm. This slurry was dehydrated using a filter press to obtain cake-like calcium carbonate.
参考例１で得た炭酸カルシウムケーキ１００質量部（固形分）にポリアクリル酸ナトリウム分散剤を１．２質量％添加し、羽分散機を用いて一次分散を行い、続いてサンドミルを用いて二次分散処理を施し、固形分濃度６３質量％の分散スラリーとした。
この分散スラリーを、間接加熱式伝動加熱型乾燥機（西村鐵工所社製ＣＤドライヤー）を用いて乾燥し、乾燥粉体を得た。得られた粉体は、水分０．３４質量％、見掛け密度０．６７ｇ／ｃｍ3であり、走査型電子顕微鏡で観察したところ、アラゴナイト一次粒子からなる平均粒径１０〜５０μｍの二次凝集粒子であることが分かった。このものの細孔容積は０．６１ｃｍ3／ｇであった。
1.2% by mass of a sodium polyacrylate dispersant is added to 100 parts by mass (solid content) of the calcium carbonate cake obtained in Reference Example 1, followed by primary dispersion using a wing disperser, and then by using a sand mill. Next, a dispersion treatment was performed to obtain a dispersion slurry having a solid concentration of 63% by mass.
The dispersed slurry was dried using an indirect heating type transmission heating type dryer (CD dryer manufactured by Nishimura Seiko Co., Ltd.) to obtain a dry powder. The obtained powder had a moisture content of 0.34% by mass and an apparent density of 0.67 g / cm 3. When observed with a scanning electron microscope, secondary agglomerated particles having an average particle size of 10 to 50 μm composed of primary aragonite particles. It turns out that. The pore volume of this product was 0.61 cm 3 / g.
参考例２で得た炭酸カルシウムケーキにポリアクリル酸ナトリウム分散剤を１．２質量％添加し、羽分散機を用いて一次分散を行い、続いてサンドミルを用いて二次分散処理を施し、固形分濃度６３質量％の分散スラリーとした。
この分散スラリーを、間接加熱式伝導加熱型乾燥機（西村鐵工所社製ＣＤドライヤー）を用いて乾燥し、乾燥粉体を得た。得られた粉体は、水分０．３８質量％、見掛け密度０．７１ｇ／ｃｍ3であり、走査型電子顕微鏡で観察したところ、カルサイト一次粒子からなる１０〜５０μｍの二次凝集粒子であることが分かった。このものの細孔容積は０．７３ｃｍ3／ｇであった。
1.2% by mass of a sodium polyacrylate dispersant is added to the calcium carbonate cake obtained in Reference Example 2, and primary dispersion is performed using a wing disperser, followed by secondary dispersion treatment using a sand mill. A dispersion slurry having a partial concentration of 63% by mass was obtained.
This dispersion slurry was dried using an indirect heating type conductive heating type dryer (CD dryer manufactured by Nishimura Steel Co., Ltd.) to obtain a dry powder. The obtained powder has a water content of 0.38% by mass and an apparent density of 0.71 g / cm 3 , and is 10 to 50 μm secondary aggregated particles composed of calcite primary particles as observed with a scanning electron microscope. I understood that. The pore volume of this product was 0.73 cm 3 / g.
比較例１
参考例１で得た炭酸カルシウムケーキを、ケージミルを備えた気流乾燥機を用いて乾燥、粉砕を行い、乾燥粉体を得た。得られた粉体は、水分０．２９質量％、見掛け密度０．１６ｇ／ｃｍ3であり、走査型電子顕微鏡で観察したところ、主として１０μｍ未満の粒子で構成されていることが分かった。また、このものの細孔容積は１．８３ｃｍ3／ｇであった。
Comparative Example 1
The calcium carbonate cake obtained in Reference Example 1 was dried and ground using an air dryer equipped with a cage mill to obtain a dry powder. The obtained powder had a moisture content of 0.29% by mass and an apparent density of 0.16 g / cm 3. When observed with a scanning electron microscope, it was found that the powder was mainly composed of particles of less than 10 μm. The pore volume of this product was 1.83 cm 3 / g.
比較例２
参考例２で得た炭酸カルシウムケーキを、ケージミルを備えた気流乾燥機を用いて乾燥、粉砕を行い、乾燥粉体を得た。得られた粉体は、水分０．３１質量％、見掛け密度０．１９ｇ／ｃｍ3であり、走査型電子顕微鏡で観察したところ、主として１０μｍ未満のカルサイト粒子で構成されていることが分かった。また、このものの細孔容積は１．６１ｃｍ3／ｇであった。
Comparative Example 2
The calcium carbonate cake obtained in Reference Example 2 was dried and ground using an air dryer equipped with a cage mill to obtain a dry powder. The obtained powder had a water content of 0.31% by mass and an apparent density of 0.19 g / cm 3. When observed with a scanning electron microscope, it was found that the powder was mainly composed of calcite particles of less than 10 μm. . The pore volume of this product was 1.61 cm 3 / g.
参考例３
実施例１及び比較例１で得た炭酸カルシウム乾燥粉体をそれぞれコーレスミキサー（分散羽根：エッジタービン型、３インチ）を用い、回転数６４００ｒｐｍ、分散時間２０分で水中に再分散処理し、固形分濃度７２．５質量％の分散スラリーを得た。
この際、比較例１の粉体に対しては、分散剤としてポリアクリル酸ナトリウム１．２質量％を添加した。
この粉体を水中に投入する場合、１度に多量の投入を行うとスラリーの流動性が著しく低下し、分散処理が不十分になるため、粉体のスラリーの流動性が低下しないように注意しながら徐々に投入した。
この際の各粉体の投入時間と得られたスラリーの物性を表１に示す。また、再分散処理時間と平均粒径の変化を表２に示す。
Reference example 3
The calcium carbonate dry powders obtained in Example 1 and Comparative Example 1 were each redispersed in water at a rotational speed of 6400 rpm and a dispersion time of 20 minutes using a Coreless mixer (dispersion blade: edge turbine type, 3 inches) to obtain a solid. A dispersion slurry having a partial concentration of 72.5% by mass was obtained.
At this time, 1.2% by mass of sodium polyacrylate was added as a dispersant to the powder of Comparative Example 1.
When charging this powder into water, if a large amount is added at once, the fluidity of the slurry will be significantly reduced and the dispersion process will be insufficient, so be careful not to decrease the fluidity of the powder slurry. It was thrown in gradually.
Table 1 shows the charging time of each powder and the physical properties of the obtained slurry. Table 2 shows the changes in the redispersion treatment time and the average particle size.
これらの表から、本発明方法により得られた粉体（実施例１）は、従来方法で得られた粉体（比較例１）に比べ、５分の１の時間で投入が完了しており、また再分散の処理時間も短かくなっているので、易溶性であることが分かる。 From these tables, the powder obtained by the method of the present invention (Example 1) was completely charged in one-fifth as compared with the powder obtained by the conventional method (Comparative Example 1). Also, since the redispersion processing time is shortened, it can be seen that it is easily soluble.
参考例４
実施例２及び比較例２で得た炭酸カルシウム乾燥粉体を参考例３と同様にして再分散処理し、固形分濃度７１．０質量％の分散スラリーを得た。
この際、比較例２の粉体に対しては、分散剤としてポリアクリル酸ナトリウム１．２質量％を添加した。
このようにして得たスラリーの物性を表３に、また再分散処理時間と平均粒径の変化を表４に示す。
Reference example 4
The calcium carbonate dry powder obtained in Example 2 and Comparative Example 2 was redispersed in the same manner as in Reference Example 3 to obtain a dispersion slurry having a solid content concentration of 71.0% by mass.
At this time, 1.2% by mass of sodium polyacrylate was added as a dispersant to the powder of Comparative Example 2.
The physical properties of the slurry thus obtained are shown in Table 3, and the changes in redispersion treatment time and average particle diameter are shown in Table 4.
これらの表から、本発明方法により得られた粉体（実施例２）は、従来方法で得られた粉体（比較例２）に比べ、４分の１の時間で投入が完了しており、また、再分散の処理時間も短かくなっているので、易溶性であることが分かる。 From these tables, the powder obtained by the method of the present invention (Example 2) was completely charged in a quarter of the time compared to the powder obtained by the conventional method (Comparative Example 2). Moreover, since the processing time of redispersion is shortened, it turns out that it is easily soluble.
本発明は、体質顔料、食品添加剤、紙、ゴム、プラスチックの充填料、化粧品成分として有用な軽質炭酸カルシウムの製造方法であり、産業上の利用可能性を有する。 The present invention is a method for producing light calcium carbonate useful as extender pigments, food additives, paper, rubber, plastic fillers, and cosmetic ingredients, and has industrial applicability.
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| JP2021514415A (en) * | 2018-02-21 | 2021-06-10 | イメルテック ソシエテ パル アクシオン サンプリフィエ | Bimodal precipitated calcium carbonate slurry suitable for paper and paperboard applications, methods for making it, and its use |
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