CN112299464A - Preparation method of multipurpose calcium carbonate superfine powder - Google Patents

Preparation method of multipurpose calcium carbonate superfine powder Download PDF

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Publication number
CN112299464A
CN112299464A CN202011076617.3A CN202011076617A CN112299464A CN 112299464 A CN112299464 A CN 112299464A CN 202011076617 A CN202011076617 A CN 202011076617A CN 112299464 A CN112299464 A CN 112299464A
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Prior art keywords
calcium carbonate
calcium hydroxide
superfine powder
slurry
drying
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Chinese (zh)
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颜培刚
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Zhejiang Jiande Zhengfa Pharmaceutical Co ltd
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Zhejiang Jiande Zhengfa Pharmaceutical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/18Carbonates
    • C01F11/181Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/65Chroma (C*)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • C01P2006/82Compositional purity water content

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  • 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

The invention discloses a preparation method of multipurpose calcium carbonate superfine powder, which comprises the steps of 1, preparing calcium hydroxide slurry, 2, carrying out carbonization reaction, 3, filtering and drying, and 4, grinding a finished product; selecting calcined calcium oxide with impurity content less than 4%, mixing water and calcium oxide, carrying out digestion reaction, and adding water to prepare calcium hydroxide slurry with concentration of 8%; adding a crystal form control agent, and ventilating to carry out carbonization reaction; filtering and drying to obtain calcium carbonate particles; carrying out secondary grinding to obtain calcium carbonate superfine powder; the calcium carbonate superfine powder prepared by the method has the characteristics of simple process and high product purity, and effectively solves the defects of the prior art.

Description

Preparation method of multipurpose calcium carbonate superfine powder
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a preparation method of multipurpose calcium carbonate superfine powder.
Background
The calcium carbonate ultrafine powder is widely applied to the fields of plastics, building materials and the like; the preparation of the calcium carbonate ultrafine powder is to introduce carbon dioxide gas into a suspension of calcium hydroxide with a certain concentration for carbonization so as to obtain calcium carbonate after the calcium hydroxide reacts with calcium dioxide, and then to grind the generated calcium carbonate and the like so as to obtain the calcium carbonate ultrafine powder with a specified particle size.
The patent with publication number CN011264055 discloses an industrial preparation method of nano active calcium carbonate, which comprises the steps of introducing carbon dioxide gas into a suspension of Ca (OH)2 with a certain concentration for carbonization; controlling the nucleation rate of calcium carbonate crystal nucleus by controlling the temperature of the Ca (OH)2 suspension and the flow of the carbon dioxide gas; after the carbonization is carried out until a certain number of crystal nuclei are formed, the crystal nucleus formation control is converted into crystal growth control, and at the moment, a crystal form regulator is added to control the growth rate of each crystal face, so that the controllable appearance is achieved; and continuously carbonizing until the end point, adding a dispersing agent to adjust the surface charge of the particles, and obtaining the uniformly dispersed cubic calcium carbonate nano particles.
The nucleation of calcium carbonate needs calcium hydroxide molecules and carbon dioxide molecules to carry out contact reaction, so whether the calcium hydroxide can be in full contact with the carbon dioxide molecules or not is also a big key factor for promoting the nucleation of the calcium carbonate; however, in the above patent, the nucleation rate of calcium carbonate crystal nuclei is controlled by controlling the temperature of the suspension of ca (oh)2 and the flow rate of carbon dioxide gas, but calcium hydroxide molecules cannot be well dispersed, so that the reaction between calcium hydroxide molecules and carbon dioxide molecules is affected, and the nucleation rate of calcium carbonate crystal nuclei is reduced.
Disclosure of Invention
The invention aims to solve the technical problem of poor preparation effect of calcium carbonate superfine powder, and provides a preparation method of multipurpose calcium carbonate superfine powder to solve the defects of the prior art.
In order to achieve the above object, the present invention comprises the following solutions:
a preparation method of multipurpose calcium carbonate superfine powder comprises the steps of 1, preparing calcium hydroxide slurry, 2, carrying out carbonization reaction, 3, filtering and drying, and 4, grinding to obtain a finished product.
Specifically, step 1, calcined quicklime with impurity content less than 4% is selected, and water and the quicklime are mixed according to the mass ratio of 5-6: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 6-8%;
step 2, adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240-300 r/min; introducing carbon dioxide gas to carry out carbonization reaction, reducing the stirring rotation speed to 120-180r/min, reducing the ventilation volume when the PH value is reduced to 7, and continuing stirring and carbonizing for 3-5 hours to obtain calcium carbonate slurry;
3, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid matter, controlling the water content ratio to be below 60% to obtain wet calcium carbonate, cleaning and filtering by using an ethanol solution with the mass fraction of 30%, repeating for 2-3 times, and then drying at the drying temperature of 90-100 ℃ to obtain calcium carbonate particles;
and 4, putting the calcium carbonate particles into a grinding machine for secondary grinding to obtain calcium carbonate superfine powder.
Furthermore, in the step 2, the ventilation of the carbon dioxide gas is not less than 0.2 cubic meter per second based on 1000L of calcium hydroxide slurry, and the ventilation after the ventilation is reduced is 5-10% of the normal value.
Further, in the step 3, the washed calcium carbonate slurry is centrifuged again, the centrifuged solid is sprayed and dried, and then the dried particles are placed in a dryer to be dried continuously until the moisture content is less than 0.3%.
Further, in the step 4, the calcium carbonate superfine powder obtained by grinding has the particle size of less than 0.5 mu m.
The calcium carbonate superfine powder prepared by the method has the characteristics of simple process and high product purity, and effectively solves the defects of the prior art.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it is obvious that the embodiments described below are some, but not all embodiments of the present invention in the description of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1, a method for preparing multi-purpose calcium carbonate ultra-fine powder, comprising the steps of 1, preparing calcium hydroxide slurry, 2, carbonizing, 3, filtering and drying, and 4, grinding the finished product.
Specifically, step 1, calcined quicklime with impurity content less than 4% is selected, and water and the quicklime are mixed according to the mass ratio of 5-6: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 6-8%;
step 2, adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240-300 r/min; introducing carbon dioxide gas to carry out carbonization reaction, reducing the stirring rotation speed to 120-180r/min, reducing the ventilation volume when the PH value is reduced to 7, and continuing stirring and carbonizing for 3-5 hours to obtain calcium carbonate slurry;
3, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid matter, controlling the water content ratio to be below 60% to obtain wet calcium carbonate, cleaning and filtering by using an ethanol solution with the mass fraction of 30%, repeating for 2-3 times, and then drying at the drying temperature of 90-100 ℃ to obtain calcium carbonate particles;
and 4, putting the calcium carbonate particles into a grinding machine for secondary grinding to obtain calcium carbonate superfine powder.
In the step 2, the ventilation volume of the carbon dioxide gas is not less than 0.2 cubic meter per second based on 1000L of calcium hydroxide slurry, and the ventilation volume after the ventilation volume is reduced is 5-10% of the normal value.
And 3, centrifuging the cleaned calcium carbonate slurry again, spraying and drying the solid obtained by centrifuging, and then placing the dried particles in a dryer for continuous drying until the water content is less than 0.3%.
In the step 4, the calcium carbonate superfine powder is obtained by grinding, and the particle size of the calcium carbonate superfine powder is less than 0.5 mu m.
Example 2, a method for preparing multi-purpose calcium carbonate ultra-fine powder, comprising the steps of 1, preparing calcium hydroxide slurry, 2, carbonizing, 3, filtering and drying, and 4, grinding the finished product.
Specifically, step 1, calcined quicklime with impurity content less than 4% is selected, and water and the quicklime are mixed according to the mass ratio of 6: 1, carrying out digestion reaction, then aging for 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 8 percent;
step 2, adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, raising the temperature to 40 ℃, introducing carbon dioxide gas, continuously stirring at the stirring speed of 180r/min, and carrying out carbonization reaction; when the PH value is reduced to 8.5, adding the crystal form control agent, accelerating the stirring, wherein the stirring speed is 240r/min, the ventilation volume is unchanged, and continuing the carbonization reaction; when the PH value is reduced to 7, the stirring speed is reduced to 120r/min, the ventilation volume is reduced, and the stirring and carbonization are continued for 2 hours to obtain calcium carbonate slurry;
3, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing filter pressing on a solid substance, controlling the water content ratio to be below 60% to obtain wet calcium carbonate, cleaning and filtering by using an ethanol solution with the mass fraction of 30%, repeating for 3 times, and then drying until the water content is less than 0.5% to obtain calcium carbonate particles;
and 4, putting the calcium carbonate particles into a grinding machine for secondary grinding to obtain calcium carbonate superfine powder.
In the step 2, the ventilation of the carbon dioxide gas is not less than 0.3 cubic meter per second based on 1000L of calcium hydroxide slurry, and the ventilation after the ventilation is reduced is 10 percent of the normal value.
Example 3, in the drying, firstly, spraying and drying are carried out to obtain calcium carbonate particles with the particle size of 3-10 microns and the water content of 1-3%, and then the calcium carbonate particles are placed in a dryer to be continuously dried until the water content is 0.15-0.5%.
Spray drying adopts atomization spraying, and the temperature is 90-100 ℃; the secondary drying temperature in the dryer is 60-90 ℃, and the drying degree is determined according to the use requirement and is at most below 0.3%.
Example 4, example 2 product testing, see table 1.
TABLE 1
Product(s) Content of impurities Water content Average particle diameter μm Cost of 100kg Whiteness degree
Example 2 ≤0.3% 0.25% 0.29 24.5 yuan 96
Prior Art ≤0.5% 0.3% 0.05-10 27-31 Yuan 94-97
As can be seen from the above table, the product of this example meets the requirements in terms of various indexes, wherein the impurity content is lower than that of the prior art, and the cost is lower.
Example 5 a method for preparing multipurpose calcium carbonate ultra-fine powder, comprising the steps of 1, preparing calcium hydroxide slurry, 2, carbonizing, 3, filtering and drying, and 4, grinding the finished product.
Specifically, step 1, calcined quicklime with impurity content less than 4% is selected, and water and the quicklime are mixed according to the mass ratio of 6: 1, carrying out digestion reaction, then aging for 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 8 percent;
step 2, adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, raising the temperature to 40 ℃, introducing mixed gas of carbon dioxide and nitrogen, continuously stirring at the stirring speed of 180r/min, and carrying out carbonization reaction; when the PH value is reduced to 8.5, adding the crystal form control agent, accelerating the stirring, wherein the stirring speed is 240r/min, the ventilation volume is unchanged, and continuing the carbonization reaction; when the PH value is reduced to 7, the stirring speed is reduced to 120r/min, the ventilation volume is reduced, and the stirring and carbonization are continued for 2 hours to obtain calcium carbonate slurry;
in the mixed gas, the volume ratio of carbon dioxide to nitrogen is 2:5, the ventilation volume is not less than 0.8 cubic meter per second calculated by 1000L of calcium hydroxide slurry, and the ventilation volume after the ventilation volume is reduced is 10 percent of the normal value;
3, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid matter, controlling the water content ratio to be below 60% to obtain wet calcium carbonate, cleaning and filtering by using an ethanol solution with the mass fraction of 30%, repeating for 3 times, then performing pressure filtration until the water content is less than 25%, and then drying until the water content is less than 0.5% to obtain a calcium carbonate cake;
and 4, placing the calcium carbonate cake into a grinding machine for secondary grinding to obtain calcium carbonate superfine powder.
The calcium carbonate superfine powder prepared by the method has the characteristics of simple process and high product purity, and effectively solves the defects of the prior art.
The embodiments described above are some, but not all embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (6)

1. The preparation method of the calcium carbonate superfine powder comprises the steps of 1, preparing calcium hydroxide slurry, 2, carrying out carbonization reaction, 3, filtering and drying, and 4, grinding to obtain the finished product.
2. The method for preparing the multipurpose calcium carbonate superfine powder as claimed in claim 1, wherein in the step 1, calcined quicklime with the impurity content less than 4% is selected, and water and the quicklime are mixed according to the mass ratio of 5-6: 1, carrying out digestion reaction, then aging for at least 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 6-8%;
step 2, adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, heating to 40 ℃, adding a crystal form control agent, and continuously stirring at the stirring speed of 240-300 r/min; introducing carbon dioxide gas to carry out carbonization reaction, reducing the stirring rotation speed to 120-180r/min, reducing the ventilation volume when the PH value is reduced to 7, and continuing stirring and carbonizing for 3-5 hours to obtain calcium carbonate slurry;
3, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing pressure filtration on the solid matter, controlling the water content ratio to be below 60% to obtain wet calcium carbonate, cleaning and filtering by using an ethanol solution with the mass fraction of 30%, repeating for 2-3 times, and then drying at the drying temperature of 90-100 ℃ to obtain calcium carbonate particles;
and 4, putting the calcium carbonate particles into a grinding machine for secondary grinding to obtain calcium carbonate superfine powder.
3. The method for preparing multipurpose calcium carbonate submicron powder as claimed in claim 2, wherein in the step 2, the ventilation of carbon dioxide gas is not less than 0.2 cubic meter per second based on 1000L of calcium hydroxide slurry, and the ventilation after reducing the ventilation is 5-10% of the normal value.
4. The method for preparing multipurpose calcium carbonate superfine powder as claimed in claim 2, wherein in the step 3, the washed calcium carbonate slurry is centrifuged again, the centrifuged solid is sprayed and dried, and then the dried particles are placed in a dryer to be dried until the water content is less than 0.3%.
5. The method for preparing multipurpose calcium carbonate submicron powder as claimed in claim 2, wherein in the step 4, the particle size of the calcium carbonate submicron powder obtained by grinding is less than 0.5 μm.
6. The preparation method of the multipurpose calcium carbonate superfine powder as claimed in claim 1, which is characterized by comprising the step 1 of selecting calcined quicklime with the impurity content of less than 4%, and mixing water and the quicklime according to a mass ratio of 6: 1, carrying out digestion reaction, then aging for 18 hours, sieving by a 200-mesh sieve to obtain calcium hydroxide coarse pulp, adding water into the calcium hydroxide coarse pulp, and continuously stirring the mixture in the water to prepare calcium hydroxide slurry with the concentration of 8 percent;
step 2, adding the calcium hydroxide slurry obtained in the step 1 into a reaction kettle, raising the temperature to 40 ℃, introducing carbon dioxide gas, continuously stirring at the stirring speed of 180r/min, and carrying out carbonization reaction; when the PH value is reduced to 8.5, adding the crystal form control agent, accelerating the stirring, wherein the stirring speed is 240r/min, the ventilation volume is unchanged, and continuing the carbonization reaction; when the PH value is reduced to 7, the stirring speed is reduced to 120r/min, the ventilation volume is reduced, and the stirring and carbonization are continued for 2 hours to obtain calcium carbonate slurry;
3, filtering and drying the calcium carbonate slurry, performing centrifugal filtration, then performing filter pressing on a solid substance, controlling the water content ratio to be below 60% to obtain wet calcium carbonate, cleaning and filtering by using an ethanol solution with the mass fraction of 30%, repeating for 3 times, and then drying until the water content is less than 0.5% to obtain calcium carbonate particles;
and 4, putting the calcium carbonate particles into a grinding machine for secondary grinding to obtain calcium carbonate superfine powder.
CN202011076617.3A 2020-10-10 2020-10-10 Preparation method of multipurpose calcium carbonate superfine powder Pending CN112299464A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114455622A (en) * 2022-02-23 2022-05-10 河北立信新材料科技有限公司 Preparation method of ultra-dispersed functional calcium carbonate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114455622A (en) * 2022-02-23 2022-05-10 河北立信新材料科技有限公司 Preparation method of ultra-dispersed functional calcium carbonate
CN114455622B (en) * 2022-02-23 2024-01-23 河北立信新材料科技有限公司 Preparation method of super-dispersed functional calcium carbonate

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Application publication date: 20210202