CN1623903A - Process for producing calcium carbonate - Google Patents
Process for producing calcium carbonate Download PDFInfo
- Publication number
- CN1623903A CN1623903A CNA2004100713895A CN200410071389A CN1623903A CN 1623903 A CN1623903 A CN 1623903A CN A2004100713895 A CNA2004100713895 A CN A2004100713895A CN 200410071389 A CN200410071389 A CN 200410071389A CN 1623903 A CN1623903 A CN 1623903A
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- China
- Prior art keywords
- slake
- lime
- water
- carbonate
- slurry
- 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.)
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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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2/00—Lime, magnesia or dolomite
- C04B2/02—Lime
- C04B2/04—Slaking
- C04B2/045—After-treatment of slaked lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2/00—Lime, magnesia or dolomite
- C04B2/02—Lime
- C04B2/04—Slaking
- C04B2/06—Slaking with addition of substances, e.g. hydrophobic agents ; Slaking in the presence of other compounds
- C04B2/066—Making use of the hydration reaction, e.g. the reaction heat for dehydrating gypsum; Chemical drying by using unslaked lime
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)
- Paper (AREA)
Abstract
A process for producing calcium carbonate whose average major-axis length can be controlled. Wet slaking in which quick lime is slaked with water to prepare a slaked lime slurry is conducted in two steps. In the first step, water is reacted with quick lime in a changeable water/quick lime ratio in the range of 1.5 to 10 by weight. A slaked lime slurry is prepared through the first step, in which the water/quick lime weight ratio is regulated, and through the second step. Carbon dioxide is bubbled into the slurry to conduct carbonation. Thus, calcium carbonate particles with high evenness of size are produced in which the primary particles have an average major-axis length of 0.5 to 10 mu m.
Description
The present invention relates to a kind of method of producing lime carbonate, comprise that water makes the white lime slurry with the unslaked lime slake,, can control the particle diameter of this lime carbonate like this by the control reaction conditions then with this white lime slurry and carbon dioxide gas precursor reactant.
The exemplary process of producing synthetic calcium carbonate is " liquid-gas " method, and wherein lime carbonate is made by carbon dioxide is blown in the white lime slurry.Know that the lime carbonate of various particle diameters and different shape can be by the control reaction conditions, as concentration, temperature of reaction, the reaction method of white lime slurry, whether have the kind etc. of additive, additive (if existence) and make.
But do not know a kind of simple process of producing granular calcium carbonate as yet, it can utilize " liquid-gas " method that is widely used in industry that the average longer diameter of primary particle is controlled in the scope of 0.5-2 μ m.The granular synthetic calcium carbonate that the average longer diameter of primary particle is 0.5-2 μ m is suitable for makes pigment or additive to be used for the paper grade (stock) coating composition, therefore needs a kind of production method that can produce granular calcium carbonate cheaply.In order to overcome this problem, Japanese patent laid-open publication gazette (Kokoku) 7-5303 and 3-19165 have described and have a kind ofly added in white lime slurry or method in part carbonating white lime slurry as nucleus crystal seed.But the problem of this method is, the overall craft complexity is because crystal seed must prepare in independent step and gas flow rate must be controlled.
Japanese patent laid-open publication gazette (Kokoku) 3-3605 has described a kind of like this method, wherein carries out the part carbonating under the pH value is not less than 0.2 condition, generates plate shape calcium carbonate, proceeds carbonating then and finishes up to reaction.The flow velocity of carbonic acid gas must limit and change according to the pH value, so this method is time-consuming and complicated but in the method.
Japanese patent application (Kokai) 5-221634 has described a kind of like this method, and wherein the white lime slurry with the part carbonating grinds under wet condition, adds secondary white lime slurry then to finish carbonating.But owing to after the part carbonating, use the sand shredder condition that wets to grind, so overall craft complexity.
On the other hand, " liquid-gas " method is a kind of like this technology, wherein mainly will comprise the solution (aqueous sodium carbonate, ammonium carbonate solution or analogue) of carbanion and solution (calcium chloride water, the lime acetate aqueous solution or the analogue) reaction of calcium cpd and obtain calcium carbonate granule.Japanese patent application (Kokai) 7-196316 has described a kind of method that obtains the granular calcium carbonate of particle diameter 0.1-20 μ m, the carbonate solution that wherein comprises reaction buffer mixes by one of these two kinds of solution are added drop-wise in another solution with calcium salt soln, carry out carbonation reaction like this, can form water-insoluble salt then by reaction or be added drop-wise in this mixture than the moisture salt or the aqueous acids of water-insoluble salt with calcium.But in order to realize this technology, every kind of material all needs a material tank and drop rate to control, and therefore is used to realize that the overall device of this technology is complicated.
Therefore, an object of the present invention is to provide a kind of method of producing lime carbonate, thus can be simply and obtain the granular calcium carbonate that its particle diameter is controlled to desired size cheaply.
To achieve these goals, the invention provides a kind of method of producing lime carbonate, comprise the slake step, wherein by continuous processing or batch technology, via wet slake process of two steps, water with the unslaked lime slake to prepare the white lime slurry; And carbonation step, wherein, carbonic acid gas is blown in the white lime slurry of making in the slake step by continuous processing or batch technology, the method is characterized in that the water in the slake step the first step/unslaked lime weight ratio (water ratio) is 1.5-10.
Fig. 1 is the electron photomicrograph of the lime carbonate that obtains in embodiment 2.
Fig. 2 is the electron photomicrograph of the lime carbonate that obtains in embodiment 4.
Fig. 3 is the electron photomicrograph of the lime carbonate that obtains in Comparative Examples 1.
Fig. 4 is the electron photomicrograph of the lime carbonate that obtains in Comparative Examples 2.
The present invention is based on the inventor's following discovery: by in the first step of slake step with the water rate of change to the scope of 1.5-10, can change according to the water ratio particle diameter of gained calcium carbonate. More particularly, verified, be the particle of 0.5-2 μ m if the water ratio in the scope of 1.5-10, can obtain the average longer diameter of its primary granule, this particle has basically uniformly particle diameter, and wherein longer diameter is measured by method described below.
In the present invention, the water ratio in the slake process first step is controlled in the scope of 1.5-10, and this depends on the required particle diameter of calcium carbonate. In the scope of 1.5-10, the water ratio is larger, and the particle diameter of gained calcium carbonate is larger. If the water ratio is lower than 1.5, the steam slake just appears during slake so, and the calcium carbonate that obtains in the step especially greatly and afterwards of the particle diameter of gained quick lime solidifies like this. On the other hand, if the water ratio greater than 10, bad dispersibility of gained calcium carbonate so, this is undesirable in product quality.
In a preference pattern, in order to obtain the lime carbonate of high uniformity, in the first step of slake process, basically by slake reaction beginning and basically in the whole zone that the slake reaction takes place, the unslaked lime of specified amount contacted with water make, slake carries out being selected under the specific water ratio of 1.5-10.That is, after beginning this reaction, simultaneously or under specific basically water ratio, carry out this reaction immediately.More particularly, for example, from adding, the unslaked lime of specified amount was added in the water of specified amount in about 1 minute.If the time that unslaked lime is added in the water of specified amount surpasses 1 minute, initial slake temperature heats up slow and therefore the slake reaction is slow, and the white lime particle solidifies easily like this.This problem that causes is, the calcium carbonate granule that is generated by white lime also solidifies easily, and this quality at some purposes calcium carbonate product is unfavorable.In industrial production, may need to control the feed rate of unslaked lime, therefore suitable speed depends on the uniform particles that amount, reaction conditions such as the slake method of batch of material and temperature and commercially available prod are required and can allow degree of solidifying.
Wet slake method of two steps comprises the first step of water and unslaked lime reaction, wherein selects the water ratio; With second step that the white lime slurry is adjusted to normality and slaking gains.In the present invention, can adopt continuous wet slake method of two steps or wet slake method of two steps of batch-type.
In the first step of two step wet slake crafts, slake can be bathed method by the batch-type slake, be used the continuous-mixture method or the similar approach of the continuous-mixture method of oar, the continuous-mixture method that uses screw rod, use kneader to carry out.As long as the condition that satisfied wherein slake carries out under specific water ratio can adopt any slake method.In order to add the unslaked lime of specified amount basically simultaneously, can be by the disposable adding of the hopper with gauger.
Because second step of slake technology is that slurry is adjusted to normality and this slurry of slaking, so method is not limited to.
Before the carbonation reaction of carbonation step, the concentration of white lime preferably is adjusted to 3-15% weight and its temperature preferably is adjusted to 30-90 ℃.Carbon dioxide or the mixed gas that comprises carbon dioxide are blown in this calcium hydroxide slurry, reach basically 100% up to carbonation reaction.Be similar to the conventional production method of calcium hydroxide, if the concentration of calcium hydroxide is lower than 3% weight, the industrial production rate variance, if but this concentration surpasses 15% weight, the viscosity of slurry is too high cause not easy to operate.If the temperature of white lime slurry before reaction is lower than 30 ℃, be easy to generate the colloidal state calcite solidifying these particles, if but temperature is higher than 90 ℃, the cost of energy height, and this is disadvantageous.Carbonation step can be continuous processing or batch technology.
By method, can obtain the controlled average granular calcium carbonate of longer diameter in the 0.5-2 mu m range of its primary particle according to production lime carbonate of the present invention.Can use conventional equipment to carry out basically and need not to improve conventional equipment according to the method for production lime carbonate of the present invention, also need not to wherein adding new device, this method can be simply and is realized cheaply and need not expensive facility investment.
The lime carbonate of being produced by the inventive method has excellent particle size uniformity.Therefore, if this lime carbonate is used as pigment or the interior filler of paper grade (stock) in the coating composition, expection can improve gloss and slickness.
The present invention is existing to be described by embodiment.Undoubtedly, the present invention is not limited to following examples, therefore can carry out various improvement in the scope of purport of the present invention.
Embodiment 1
The caustic lime block (JIS commercial lime, particular stage unslaked lime, particle diameter 3-35 millimeter) that use is produced by applicant company is as the unslaked lime raw material.In the first step of slake technology, unslaked lime is added in 70 ℃ of water so that water/unslaked lime ratio is 1.5, then with the gained mixture reaction.In second step of slake technology, regulate concentration and temperature and also carry out slaking, obtaining a kind of temperature and be 60 ℃ and concentration is the white lime slurry of 5% weight.In this slurry, with 34 liters of/minute kilogram Ca (OH)
2Flow velocity add carbonated gas (CO
2Concentration; 20% volume), reaches 100%, can finish reaction like this to obtain lime carbonate up to the ratio of carbonating.
Observation post gets lime carbonate with electron microscope.The result confirms that this lime carbonate is that the average longer diameter of its primary particle is the single-size form of 0.5 μ m.
Term " the on average longer diameter of primary particle " is meant, on two diagonal lines of the electron photomicrograph of arbitrarily taking under 30000 times of magnifications, and the mean value of the length of the long-chord of particulate, the length of long-chord uses the electronics clamp to measure.
Embodiment 2
Same way as according to embodiment 1 is produced lime carbonate, and just water/unslaked lime the ratio in the first step of slake technology is 3.Electron microscope observation confirms that this lime carbonate is that the average longer diameter of its primary particle is the single-size form of 1 μ m.
Embodiment 3
Same way as according to embodiment 1 is produced lime carbonate, and just water/unslaked lime the ratio in the first step of slake technology is 5.Electron microscope observation confirms that this lime carbonate is that the average longer diameter of its primary particle is the single-size form of 1.3 μ m.
Embodiment 4
Same way as according to embodiment 1 is produced lime carbonate, and just water/unslaked lime the ratio in the first step of slake technology is 7.Electron microscope observation confirms that this lime carbonate is that the average longer diameter of its primary particle is the single-size form of 1.7 μ m.
Embodiment 5
Same way as according to embodiment 1 is produced lime carbonate, and just water/unslaked lime the ratio in the first step of slake technology is 10.Electron microscope observation confirms that this lime carbonate is that the average longer diameter of its primary particle is the single-size form of 2 μ m.
Comparative Examples 1
Same way as according to embodiment 1 is produced lime carbonate, and just water/unslaked lime the ratio in the first step of slake technology is 1.Electron microscope observation confirms that this lime carbonate is the non-homogeneous solidified particle form that the average longer diameter of its primary particle is 0.5 μ m.
Comparative Examples 2
Produce lime carbonate according to the same way as of embodiment 1, just water/unslaked lime the ratio in the first step of slake technology be 26 and slake technology in the single consecutive steps that adopts usually, carry out.Electron microscope observation confirms that this lime carbonate is the non-homogeneous solidified particle form that the average longer diameter of its primary particle is 2.5 μ m.
Table 1 has gathered the water ratio in each embodiment and Comparative Examples and the relation of lime carbonate particle diameter.
Table 1
| Water/unslaked lime weight ratio [-] | The median radius * [μ m] that laser diffractometry is measured | The on average longer diameter [μ m] of primary particle | |
| Comparative Examples 1 | ????1 | ????6.4 | ????0.5 |
| Embodiment 1 | ????1.5 | ????2.5 | ????0.5 |
| Embodiment 2 | ????3 | ????2.9 | ????1.0 |
| Embodiment 3 | ????5 | ????3.1 | ????1.3 |
| Embodiment 4 | ????7 | ????3.4 | ????1.7 |
| Embodiment 5 | ????10 | ????4.1 | ????2.0 |
| Comparative Examples 5 | ????26 | ????7.6 | ????2.5 |
* testing apparatus: HORIBA LA-500
Claims (5)
1. a method of producing lime carbonate comprises the slake step, wherein goes on foot wet slake craft water slake unslaked limes with preparation white lime slurry via two; And carbonation step, wherein carbonic acid gas is blown in the described white lime slurry of in described slake step, making, it is characterized in that,
Water in the first step of described slake step/unslaked lime weight ratio is 1.5-10.
2. according to the process of claim 1 wherein that described two step wet slake crafts are a kind of continuous processings.
3. according to the process of claim 1 wherein that described two step wet slake crafts are a kind of batch technologies.
4. according to any one method among the claim 1-3, wherein the on average longer diameter of the primary particle of gained lime carbonate is 0.5-2 μ m.
5. according to any one method among the claim 1-4, slake in the first step of wherein said slake step carries out under water/unslaked lime weight ratio of 1.5-10 from described slake reaction beginning basically, and described water/unslaked lime weight ratio is met in the whole zone that the slake reaction takes place basically.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP75881/1999 | 1999-03-19 | ||
| JP07588199A JP3626620B2 (en) | 1999-03-19 | 1999-03-19 | Method for producing calcium carbonate |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00800342A Division CN1296463A (en) | 1999-03-19 | 2000-03-06 | Process for producing calcium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1623903A true CN1623903A (en) | 2005-06-08 |
Family
ID=13589081
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00800342A Pending CN1296463A (en) | 1999-03-19 | 2000-03-06 | Process for producing calcium carbonate |
| CNA2004100713895A Pending CN1623903A (en) | 1999-03-19 | 2000-03-06 | Process for producing calcium carbonate |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00800342A Pending CN1296463A (en) | 1999-03-19 | 2000-03-06 | Process for producing calcium carbonate |
Country Status (9)
| Country | Link |
|---|---|
| JP (1) | JP3626620B2 (en) |
| KR (1) | KR20010042713A (en) |
| CN (2) | CN1296463A (en) |
| AU (1) | AU768281B2 (en) |
| ID (1) | ID28095A (en) |
| MY (1) | MY136783A (en) |
| NZ (1) | NZ507531A (en) |
| TW (1) | TW593151B (en) |
| WO (1) | WO2000056661A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104204351A (en) * | 2012-03-23 | 2014-12-10 | 欧米亚国际集团 | Process for preparing scalenohedral precipitated calcium carbonate |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058246B (en) * | 2012-12-24 | 2016-03-30 | 刘立文 | A kind of calcium sulfate produces the method for high-purity calcium oxide |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6086067A (en) * | 1983-10-18 | 1985-05-15 | 奥多摩工業株式会社 | Manufacture of plate-like calcium hydroxide |
| DE3587060T2 (en) * | 1984-10-18 | 1993-05-19 | Pfizer | SPHERICAL FILLED CALCIUM CARBONATE, ITS PRODUCTION AND USE. |
| JP2652032B2 (en) * | 1988-04-12 | 1997-09-10 | 丸尾カルシウム株式会社 | Method for producing aragonite crystalline calcium carbonate |
| JP3874449B2 (en) * | 1996-05-21 | 2007-01-31 | 奥多摩工業株式会社 | Method for producing light calcium carbonate |
-
1999
- 1999-03-19 JP JP07588199A patent/JP3626620B2/en not_active Expired - Lifetime
-
2000
- 2000-03-06 ID IDW20002537A patent/ID28095A/en unknown
- 2000-03-06 CN CN00800342A patent/CN1296463A/en active Pending
- 2000-03-06 KR KR1020007011433A patent/KR20010042713A/en not_active Application Discontinuation
- 2000-03-06 CN CNA2004100713895A patent/CN1623903A/en active Pending
- 2000-03-06 WO PCT/JP2000/001338 patent/WO2000056661A1/en not_active Application Discontinuation
- 2000-03-06 NZ NZ507531A patent/NZ507531A/en unknown
- 2000-03-06 AU AU28298/00A patent/AU768281B2/en not_active Ceased
- 2000-03-17 MY MYPI20001059A patent/MY136783A/en unknown
- 2000-03-17 TW TW089105019A patent/TW593151B/en not_active IP Right Cessation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104204351A (en) * | 2012-03-23 | 2014-12-10 | 欧米亚国际集团 | Process for preparing scalenohedral precipitated calcium carbonate |
| CN104204351B (en) * | 2012-03-23 | 2019-03-12 | 欧米亚国际集团 | The method for being used to prepare scalenohedron winnofil |
Also Published As
| Publication number | Publication date |
|---|---|
| ID28095A (en) | 2001-05-03 |
| AU768281B2 (en) | 2003-12-04 |
| NZ507531A (en) | 2002-04-26 |
| MY136783A (en) | 2008-11-28 |
| JP2000264631A (en) | 2000-09-26 |
| JP3626620B2 (en) | 2005-03-09 |
| KR20010042713A (en) | 2001-05-25 |
| WO2000056661A1 (en) | 2000-09-28 |
| TW593151B (en) | 2004-06-21 |
| CN1296463A (en) | 2001-05-23 |
| AU2829800A (en) | 2000-10-09 |
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