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WO2001030700A1 - Carbonate de calcium et son procede de production - Google Patents

Carbonate de calcium et son procede de production Download PDF

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Publication number
WO2001030700A1
WO2001030700A1 PCT/JP2000/007195 JP0007195W WO0130700A1 WO 2001030700 A1 WO2001030700 A1 WO 2001030700A1 JP 0007195 W JP0007195 W JP 0007195W WO 0130700 A1 WO0130700 A1 WO 0130700A1
Authority
WO
WIPO (PCT)
Prior art keywords
calcium carbonate
calcium
particles
weight
average
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.)
Ceased
Application number
PCT/JP2000/007195
Other languages
English (en)
Japanese (ja)
Inventor
Yoshihito Sasahara
Yoshimi Goto
Tetsushi Iwashita
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.)
Yabashi Industries Co Ltd
YABASHI IND CO Ltd
Original Assignee
Yabashi Industries Co Ltd
YABASHI IND 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 Yabashi Industries Co Ltd, YABASHI IND CO Ltd filed Critical Yabashi Industries Co Ltd
Priority to AU76881/00A priority Critical patent/AU7688100A/en
Priority to KR1020017006248A priority patent/KR20010080481A/ko
Publication of WO2001030700A1 publication Critical patent/WO2001030700A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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
    • C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Definitions

  • the present invention relates to calcium carbonate produced by a reaction between calcium hydroxide and carbon dioxide gas and a method for producing the same.
  • the primary particles having a good dispersibility have an average minor axis of 0.1 to 0.5 m
  • the present invention relates to a carbonated calcium carbonate having a primary particle average major axis of 0.15 to 1.5 m and an aspect ratio of 1.5 to 3.0, and a method for producing the same.
  • a typical method of producing synthetic carbonated calcium carbonate is a "liquid-gas" method in which a gaseous carbonate is blown into a hydroxylated calcium sulfate slurry to cause a reaction.
  • concentration of the calcium hydroxide slurry, the reaction temperature, and the reaction method are used. It is known that calcium carbonate having various particle sizes and shapes can be obtained by controlling the reaction conditions such as the presence or absence and the type of additives.
  • the short diameter of primary particles with good dispersibility is 0.1 to 0.5 m, and the average length of primary particles is 0.1 to 0.5 m.
  • the production technology of calcium carbonate with ⁇ of 0.15 to 1.5 yum and aspect ratio of 1.5 to 3.0 has not been established.
  • Such calcium carbonate has various properties such as coating pigments and internal additives for papermaking, which require highly controlled particle size, shape, and particle size distribution, and anti-blocking fillers for magnetic tape. It is suitable for improvement and an inexpensive manufacturing method is desired.
  • the carbonic acid produced does not have a cubic shape and is rhombohedral, so the particles tend to overlap, and when used as a coating pigment for papermaking, the surface smoothness and gloss of the coated paper are also improved. hard.
  • Spindle-shaped calcium carbonate is susceptible to particle corner damage due to its shape. This may reduce the surface strength of the coated paper when used in coating pigments for papermaking, for example, and may cause dropout due to powder generation when used in anti-blocking fillers for magnetic tape. It is possible that
  • an object of the present invention is to provide a primary particle having a good average dispersibility of 0.1 to 0.5 ⁇ m, a primary particle average major axis of 0.1 to 1.5 Atm, and an aspect ratio of 1.5. It is an object of the present invention to provide a carbonated calcium carbonate of about 3.0 and a method for producing calcium carbonate by which such a carbonated calcium can be obtained easily and inexpensively. Disclosure of the invention
  • the present invention provides a method for producing calcium carbonate having excellent dispersibility by reacting calcium hydroxide and carbon dioxide gas, wherein calcium ions and carbonate ions coexist with an organic compound having a hydroxyl group.
  • the method for producing calcium carbonate was constituted by adding organic compounds.
  • the organic compound having a hydroxyl group is added before or after the start of carbonation, and after the start of the carbonation reaction, a predetermined amount of the total amount is added until the carbonation rate becomes about 20%.
  • the organic compound is kneaded with the powdered lime or slaked lime raw material before the start of the carbonation reaction, or added dropwise to digested water. In addition, it is added by spraying powder material in a mixer or by dripping it into calcium hydroxide slurry.
  • the organic compound is added in an amount of 10 to 200 parts by weight based on 100 parts by weight of calcium oxide (CaO) as a raw material calcium source. If the amount is less than 100 parts by weight, the particle shape becomes close to a cubic shape, and the desired shape of rice granules, bales, or rounded columnar carbonic acid calcium particles cannot be obtained. The effect leveled off and was not cost effective. Preferably 50 to 180 parts by weight are added. In this range, the primary particles have an aspect ratio of 2 or more, so that when used as a papermaking pigment or the like, particles having excellent shapes that can easily improve smoothness and the like can be obtained.
  • CaO calcium oxide
  • the raw lime or slaked lime powder raw material is kneaded in a kneading manner or dropped and dissolved in digested water or water used for preparing a slurry. It may be sprayed by a spray in a mixer, or may be dropped onto the calcium hydroxide slurry before the carbonation reaction is started or after the carbonation reaction is started until the carbonation ratio becomes about 20%.
  • the addition method is not particularly limited as long as a state where calcium ions and carbonate ions and an organic compound having a hydroxyl group coexist during the reaction is obtained.
  • the organic compound having a hydroxyl group preferably has a molecular weight of 600 or less, and glycols such as ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, propylene glycol, polypropylene glycol, and butylene glycol; monoethanolamine And ethanolamines such as diethanolamine and triethanolamine; glycerins such as glycerin and polyglycerin, and mixtures thereof, and are preferably propylene glycol and ethylene glycol.
  • glycols such as ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, propylene glycol, polypropylene glycol, and butylene glycol
  • monoethanolamine And ethanolamines such as diethanolamine and triethanolamine
  • glycerins such as glycerin and polyglycerin, and mixtures thereof, and are preferably propylene glycol and ethylene glycol.
  • the calcium hydroxide slurry is preferably used before the reaction. Adjusted to 10-20 ° C. By blowing carbon dioxide gas or a mixed gas containing carbon dioxide gas into the calcium hydroxide slurry, the reaction is performed until the carbonation ratio becomes substantially 100%. If the concentration of calcium hydroxide is less than 3% by weight, the industrial productivity is poor. If the concentration exceeds 20% by weight, the slurry viscosity increases and the handling properties deteriorate, which is undesirable. Same as the method. On the other hand, if the temperature before the start of the reaction is lower than 10 ° C, on the other hand, aggregates tend to form and form aggregates, whereas if the temperature is higher than 20 ° C, aggregates of spun particles and aggregates of aggregates form. It is also well known that it is difficult to obtain a uniform and well-dispersed product.
  • the primary particles having a good dispersibility have an average minor axis of 0.1 to 0.5 m, The average primary particle diameter is 0.15 to 1.5 m, the aspect ratio is 1.5 to 3.0, and the shape is rice grain, bale, or column with rounded corners.
  • Calcium carbonate can be obtained.
  • the organic compound having a hydroxyl group is preferably added at the latest until the carbonation rate of calcium hydroxide becomes 20%.
  • the generated particles will be agglomerated if the amount of carbon dioxide gas is large, and if the amount is small, the generated particles will be enlarged, resulting in good dispersibility. It is hard to expect to get.
  • the calcium carbonate obtained by the present invention has a very good dispersibility, so it is not necessary to disintegrate it with a media mill or the like. It is desirable to keep the slurry treatment only for a short time.
  • the average primary particle minor axis of uniformity and good dispersibility is 0.1 to 0.5 m, and the average primary particle length is 0.15 to 0.15. 1.5 m and an aspect ratio of 1.5 to 3.0, it is possible to obtain calcium carbonate with high uniformity and rice grain, bale or square column shape.
  • an organic compound having a hydroxyl group is mixed or dissolved in raw material powder, digested water, or a calcium hydroxide slurry having a carbonation ratio of about 20% or less. Only the equipment for addition by existing equipment It can be implemented simply by adding to it, and can be realized simply and inexpensively.
  • the water separated by dewatering is in a state in which the organic compound is dissolved and is circulated as digestion water or water for preparing calcium hydroxide slurry.
  • the uniformity of the particles is good, the glossiness is improved when used as a coating pigment for papermaking, and the anti-blocking property is improved when used as an anti-blocking filler.
  • it has a grain shape, bale shape, or rounded column shape, and coating is difficult because particles do not overlap, improving the smoothness and glossiness of the paper surface, and coating because the corners of the particles are not easily damaged. It is possible to prevent a drop in surface strength of paper and dropout due to generation of powder when used in an anti-blocking filter.
  • the primary particles having an average dispersibility of 0.1 to 0.5 m, the primary particles having an average length of 0.1 to 1.5 and 1.5% It is possible to obtain calcium carbonate having an energy ratio of 1.5 to 3.0 and preferably in the shape of rice grains, bale, or column with rounded corners.
  • FIG. 1 is an electron micrograph ( ⁇ 10,000) of the calcium carbonate obtained in Example 2.
  • FIG. 2 is an electron micrograph ( ⁇ 10,000) of the calcium carbonate obtained in Example 5.
  • In-house manufactured lime mass (JIS industrial lime quick lime special number) was pulverized to a particle size of 1 mm or less and used as a calcium oxide raw material.
  • this calcium oxide powder 30 parts by weight of ethylene glycol is added and mixed, and about 1.5 times (48 parts by weight) the theoretical amount of water required for calcium oxide to be digested into calcium hydroxide.
  • Water at 20 ° C was stirred and mixed, digested and aged to obtain calcium hydroxide powder.
  • the slurry concentration was adjusted to 7%, and the temperature was adjusted to 15 ° C.
  • the carbonation gas was adjusted to 4 L / min. The reaction was completed by introducing the solution until the concentration reached 00%, and calcium carbonate was obtained.
  • the obtained calcium carbonate was observed with an electron microscope.
  • the average primary particle diameter 0 was 0.4; am, the average primary particle diameter was 0.6 ⁇ , and the median diameter determined by laser diffraction method was 1
  • O ⁇ m was uniform and well-dispersed, and was rice-shaped, bale-shaped, or rounded cylindrical particles. That is, as shown in the electron micrograph of FIG. 1, the particles are roughly cylindrical at the center and hemispherical at both ends. Of course, cylinders and hemispheres contain some distortion.
  • the diameter in the axial direction of the columnar shape is the major axis, and the diameter in the radial direction is the minor axis.
  • the average primary particle diameter is the shortest chord of the particle (i.e., the particle circle) of two diagonal particles in a random electron micrograph taken at 30,000 magnifications with an electronic caliper. The diameter of the column in the semi-monstrous direction) was measured and used as the minor axis of the particle. Similarly, in an electron micrograph, the longest chord of two diagonal particles (that is, the length of the particle in the axial direction of the column) is measured, and this is taken as the major axis of the particle. The average primary particle length S was used.
  • the median diameter obtained by the laser diffraction method is a value measured by a laser diffraction particle size distribution analyzer LA-500 manufactured by Horiba Seisakusho Co., Ltd. I have. The median diameter is this value compared to the primary particle diameter. Is a value indicating that the smaller the value, the better the dispersibility.
  • Calcium carbonate was obtained in the same manner as in Example 1 except that ethylene glycol was added and mixed with 100 parts by weight of calcium oxide powder and 80 parts by weight. Observed by electron microscopy, the resulting calcium carbonate was uniform and dispersed with an average primary particle diameter of 0.4 m, an average primary particle diameter of 0.8 ytm, and a median ⁇ ⁇ ⁇ of 1.2 m by laser diffraction method. It was confirmed that the particles were rice grains having good properties. An electron micrograph (10,000 magnification) is shown in FIG.
  • Calcium carbonate was obtained in the same manner as in Example 1, except that ethylene glycol was added and mixed with 150 parts by weight based on 100 parts by weight of the calcium oxide powder. According to electron microscopic observation, the obtained carbonic acid lumps have a uniform primary particle average of 0.4 m, average primary particle length of 1.0 m, and a median suspicion of 1. with laser-diffraction method and good dispersibility. It was confirmed that the rice grains were fine.
  • FIG. 2 shows a diagram similar to FIG. 1 for the fifth embodiment.
  • Example 4 Average particle diameter of primary particles: 0.2 m. Average particle diameter of primary particles: 0.3 Atm, and uniform and good dispersibility rice granular particles having a median diameter of 0.6 m by a laser diffraction method. : Average particle diameter of primary particles: 0.2 m, average particle diameter of primary particles: 0.4 yam, uniform and good dispersibility rice granular particles having a median ⁇ ⁇ ⁇ by laser diffraction method of 0.6 Aim
  • Example 6 1 Uniform and well-dispersed rice granule particles with average secondary minor particle diameter of 0.2 yam, primary primary particle average major diameter of 0.5 m, and laser-diffraction median diameter of 0.8 m (Example 7)
  • the obtained calcium carbonate has a primary particle average minor axis of 0.4 m, a primary particle average length of 0.8 Atm, and a median diameter by laser diffraction method of 1.3. It was confirmed that the particles were rice granules having uniform m and good dispersibility.
  • a carbonation reaction was carried out in the same process as in Examples 7 to 8 except that the flow rate of the carbon dioxide gas was changed to 10 L / min ⁇ kg-Ca (OH), thereby obtaining carbon dioxide.
  • the results observed with an electron microscope are listed below.
  • Example 9 Uniform and well-dispersed rice granular particles having a primary particle average minor axis of 0.2 m, an average primary particle major axis of 0.3 m, and a median diameter of 0.6 ⁇ m as measured by laser diffraction.
  • Example 10 Uniform and well-dispersed rice granular particles having an average primary particle diameter of 0.2 m, an average primary particle diameter of 0.4 ⁇ , and a median diameter of 0.6 m by laser diffraction method. (Comparative Examples 1-4)
  • Carbonation reaction was performed in the same process as in Examples 1, 4, 7, and 9 except that the added amount of ethylene glycol or propylene glycol was 5% by weight, and the obtained calcium carbonate was observed with an electron microscope.
  • the added amount of ethylene glycol or propylene glycol was 5% by weight, and the obtained calcium carbonate was observed with an electron microscope.
  • Comparative Example 1 Uniform and well-dispersed cubic particles having an average primary particle diameter of 0.5 m and a median diameter of 1.1 m as measured by a laser diffraction method.
  • the average primary particle ⁇ refers to the change of the particle with an electronic caliper for two diagonal particles in an electron micrograph taken at a magnification of 30,000 and photographed at random. This was measured and defined as the particle diameter, and the average value was determined as the primary particle average particle diameter. Comparative Example 2: First-order average particle size 0.2 / am, median ⁇ ⁇ by laser-diffraction method was 0.
  • Comparative Example 3 Primary mean particle diameter 0.4 mm, median diameter determined by laser diffraction method was 0.4 mm.
  • Comparative Example 4 Uniform and well-dispersed cubic particles having a primary average particle diameter of 0.2 xm and a median ⁇ ⁇ ⁇ by laser-diffraction method of 0.6 m
  • a carbonation reaction was carried out in the same manner as in Examples 1, 4, 7, and 9 except that ethylene glycol or propylene glycol was not added, and the results obtained by observing the obtained carbonated calcium carbonate with an electron microscope are listed below. I do.
  • Comparative Example 5 Polyhedral particles having a primary average particle size of more than 1 Atm and a median size of 3 by laser-diffraction
  • Comparative Example 6 Aggregate of aggregated particles having a primary particle average particle size of less than 0.1 Atm and a median diameter of 4.3 Atm by laser diffraction method
  • Comparative Example 7 Polyhedral particle with primary particle average particle exceeding 1 Atm and median ⁇ ⁇ ⁇ 3.1 m by laser-diffraction method
  • Comparative Example 8 Aggregate of aggregated particles having an average primary particle size of less than 0.1 Aim and a median of 4.0 m by laser diffraction method
  • Table 1 summarizes the synthesis conditions and results of the above Examples and Comparative Examples.
  • the calcium carbonate obtained in Examples 1 and 4 and Comparative Examples 1 and 5 was dehydrated by a filter press to obtain a cake having a solid content of 65.5% by weight. Next, 0.6% by weight of a dispersant in terms of solid content was added to the dewatered cake to carry out a dispersion treatment to obtain a high-concentration calcium carbonate slurry having a solid content concentration of 65.0% by weight. This slurry was used as a coating pigment, and 100 parts by weight of calcium carbonate was added to 6 parts by weight of starch (Japanese food processing # 4600), 12 parts by weight of latex (Nippon Synthetic Rubber No.
  • a printability improver Toho Chemical Co., Ltd.-Ito Master GT360
  • water-resistant agent Suditomo Chemical Sumireze Resin 61 3
  • water and a pigment with a solid concentration of 50.0% by weight The composition was prepared and coated on a 65 g / m ; base paper with a hand-painted rod so that the coating amount per side was 15 g / m ; and the super calendering was performed twice. After that, the physical properties of the coated paper were evaluated.
  • Table 2 summarizes the physical properties of coated paper in application examples. Table 2

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  • Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

La présente invention concerne des particules de carbonate de calcium comprenant des particules primaires à diamètre moyen plus court compris entre 0,1 et 0,5 micron, des particules primaires à diamètre moyen plus long compris entre 0,15 et 1,5 micron présentant un rapport de forme compris entre 1,5 et 3,0 et ayant de préférence la forme d'un grain de riz, un sac à riz allongé ou un cylindre à coins arrondis; et un procédé de production de carbonate de calcium. Le procédé de production de carbonate de calcium consiste à faire réagir de l'hydroxyde de calcium avec du dioxyde de carbone, le procédé se caractérisant en ce qu'un composé organique comprenant un groupe hydroxyle est ajouté dans le système de réaction de carbonisation suivant une quantité comprise entre 20 et 200 parties en poids pour 100 parties en poids d'oxyde de calcium lequel est une matière brute utilisée en tant que source de calcium. Les particules de carbonate de calcium présentent une bonne dispersabilité et sont produites au moyen du procédé décrit ci-avant.
PCT/JP2000/007195 1999-10-26 2000-10-17 Carbonate de calcium et son procede de production Ceased WO2001030700A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU76881/00A AU7688100A (en) 1999-10-26 2000-10-17 Calcium carbonate, and method for producing the same
KR1020017006248A KR20010080481A (ko) 1999-10-26 2000-10-17 탄산칼슘 및 그 제조방법

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP30344899 1999-10-26
JP11/303448 1999-10-26

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CN (1) CN1167620C (fr)
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WO (1) WO2001030700A1 (fr)

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JP2006076828A (ja) * 2004-09-09 2006-03-23 Kyushu Institute Of Technology バテライト型結晶系炭酸カルシウムと澱粉との複合体、被記録媒体、印字物、インクジェット記録方法及び被記録媒体の製造方法
JP2012224535A (ja) * 2011-04-08 2012-11-15 Oji Holdings Corp 塗工用軽質炭酸カルシウム含有スラリー及びそれを用いた塗被紙
JP2013079192A (ja) * 2005-04-11 2013-05-02 Omya Development Ag 特にインクジェット印刷紙コーティングで使用するための沈殿炭酸カルシウム顔料
CN111874933A (zh) * 2020-08-14 2020-11-03 王权广 米粒状轻质碳酸钙快速制备工艺
WO2021029351A1 (fr) * 2019-08-15 2021-02-18 日本製紙株式会社 Papier chargé de carbonate de calcium léger
JP2021070868A (ja) * 2019-10-30 2021-05-06 株式会社神戸製鋼所 カルシウムの抽出方法、カルシウムの回収方法及び二酸化炭素の固定化方法

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Cited By (8)

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JP2006076828A (ja) * 2004-09-09 2006-03-23 Kyushu Institute Of Technology バテライト型結晶系炭酸カルシウムと澱粉との複合体、被記録媒体、印字物、インクジェット記録方法及び被記録媒体の製造方法
JP2013079192A (ja) * 2005-04-11 2013-05-02 Omya Development Ag 特にインクジェット印刷紙コーティングで使用するための沈殿炭酸カルシウム顔料
JP2012224535A (ja) * 2011-04-08 2012-11-15 Oji Holdings Corp 塗工用軽質炭酸カルシウム含有スラリー及びそれを用いた塗被紙
WO2021029351A1 (fr) * 2019-08-15 2021-02-18 日本製紙株式会社 Papier chargé de carbonate de calcium léger
JPWO2021029351A1 (ja) * 2019-08-15 2021-11-04 日本製紙株式会社 軽質炭酸カルシウムを内添した紙
JP7029028B2 (ja) 2019-08-15 2022-03-02 日本製紙株式会社 軽質炭酸カルシウムを内添した紙
JP2021070868A (ja) * 2019-10-30 2021-05-06 株式会社神戸製鋼所 カルシウムの抽出方法、カルシウムの回収方法及び二酸化炭素の固定化方法
CN111874933A (zh) * 2020-08-14 2020-11-03 王权广 米粒状轻质碳酸钙快速制备工艺

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