CN111874933A - Quick preparation process of rice-grain light calcium carbonate - Google Patents
Quick preparation process of rice-grain light calcium carbonate Download PDFInfo
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- CN111874933A CN111874933A CN202010816224.5A CN202010816224A CN111874933A CN 111874933 A CN111874933 A CN 111874933A CN 202010816224 A CN202010816224 A CN 202010816224A CN 111874933 A CN111874933 A CN 111874933A
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- C—CHEMISTRY; METALLURGY
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- 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
Abstract
The invention discloses a rapid preparation process of rice-grain-shaped light calcium carbonate, belonging to the technical field of preparation of light calcium carbonate powder of inorganic nonmetallic materials. The quick preparation process of the rice-shaped light calcium carbonate comprises the steps of adding alkali metal ions before carbonation reaction, fully mixing the alkali metal ions with calcium hydroxide slurry, introducing carbon dioxide mixed gas with a certain concentration for quick carbonation reaction to obtain calcium carbonate slurry, and dehydrating, drying and crushing the calcium carbonate slurry to obtain the rice-shaped light calcium carbonate. The invention solves the problems of long carbonation reaction time of the light calcium carbonate, irregular appearance of product particles, uneven particle size and unstable quality of the product in the prior art.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic non-metallic material calcium carbonate powder, and particularly relates to a rapid preparation process of rice-shaped light calcium carbonate.
Background
The precipitated calcium carbonate for domestic industry is divided into two types according to the appearance: one is conventional spindle light calcium carbonate, which is called light calcium for short in China, and mainly divides the product quality and grade by the settlement volume; the other is cubic nano calcium carbonate which is called nano calcium for short in China, and the classification of the nano calcium carbonate is distinguished by the difference of specific surface area and modification process. The foreign refining production process is mainly used for improving and perfecting the crystal morphology of calcium carbonate and dividing calcium carbonate products by different regular crystal morphologies. The light calcium product has spindle crystal form, rice grain crystal form, rod crystal form or crystal whisker; the nano calcium carbonate can be in an orthorhombic crystal particle shape with clear water caltrops at 100-150nm, and the high-specific-surface-area nano calcium carbonate is in a cubic shape without water caltrops or with unobvious water caltrops but good dispersibility. The foreign advanced nano calcium carbonate technology is worthy of learning, and the refinement of the production technology and the fine division of the product types of domestic calcium carbonate production enterprises are yet to be enhanced.
The refinement of the production process technology needs to be improved in two aspects, namely the refinement of production equipment on one hand and the refinement of the production process on the other hand. The main process influencing the crystal morphology and the crystal grain size of the product is the carbonation reaction of calcium hydroxide, and the precise regulation and control of the carbonation process are the premise of ensuring the crystal morphology of calcium carbonate. The carbonation reaction process is somewhat dependent on the carbonation reactor. At present, the carbonation reactors for preparing the nano calcium carbonate in China are various and comprise a traditional bubbling carbonation reactor, an intermittent bubbling stirring carbonation reactor, a novel spraying carbonation reactor, a hypergravity carbonation reactor, a Venturi tube spraying carbonation reactor and the like. The production process comprises pure process regulation and control and crystal form control agent regulation and control. The domestic production technology is mainly based on pure process regulation, and a small number of enterprises regulate and control the crystal morphology by combining process regulation and control with a crystal form control agent. In view of various data such as comprehensive production process and product performance, the regulation and control production process of the domestic crystal form control agent is supported by further research and breakthrough.
Disclosure of Invention
The invention provides a rapid preparation process of rice-grain-shaped light calcium carbonate, which aims to solve the problems of long carbonation reaction time, irregular product particle appearance, uneven particle size and unstable quality in the existing light calcium carbonate preparation technology.
In order to solve the technical problems, the invention adopts the following technical scheme:
a process for quickly preparing the rice-shaped light calcium carbonate includes such steps as adding alkali metal ions to the calcium hydroxide slurry, mixing, introducing the mixture of carbon dioxide and water, quick carbonating reaction to obtain calcium carbonate slurry, dewatering, baking and pulverizing.
Further, the calcium hydroxide slurry is obtained by adding normal temperature water or hot water into light-burned or medium-burned lime for slaking, sieving and refining, wherein the ratio of lime slaking ash water is 1: 4-9; refining the lime slurry through a 40-200 mesh screen for multiple times to obtain calcium hydroxide slurry, and refining the calcium hydroxide slurry through combination of screens with different meshes from low to high; the solid content of the calcium hydroxide obtained by refining is regulated and controlled to be 8-20%, and the calcium hydroxide can be aged or not aged.
Furthermore, the carbonation reaction has no special requirements on the reactor, and the requirements of the carbonation reaction can be met by an intermittent bubbling carbonation reactor, an intermittent bubbling stirring carbonation reactor, a super-gravity carbonation reactor and a venturi tube jet reaction kettle.
Further, the alkali metal ions can be one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate; the dosage of the alkali metal ions is 0.5-5mol/L, and the carbonation reaction time is shorter when the dosage is larger.
Further, the concentration of the carbon dioxide mixed gas is 10-40%, the initial carbonation temperature of the calcium hydroxide slurry is 30-68 ℃, the rapid carbonation reaction is started after the carbon dioxide is introduced, and the reaction can be judged to be finished if the pH value of the slurry is lower than 8 or the alcoholic phenolphthalein solution is not red in the experiment.
Further, in the carbonation reaction process, when the initial carbonation temperature of the calcium hydroxide slurry is low, the temperature is rapidly increased, and when the initial temperature is high, the temperature rise speed is not obvious because the slurry and air have large temperature difference and the gas takes away more heat.
Furthermore, the carbonation reaction time is obviously reduced, and compared with the reaction process without adding alkali metal ions, the carbonation reaction time is reduced by more than 5 percent, and the production efficiency can be effectively improved.
Further, calcium carbonate slurry obtained by the rapid carbonation reaction is centrifuged or filter-pressed to obtain a calcium carbonate filter cake, and the filter-pressing process can be used for cleaning the filter cake or not; filtrate obtained by dehydration can be used for lime digestion to realize recycling.
Furthermore, the rice-grain light calcium carbonate has regular shape, uniform particle size, the particle size range of 200-900nm, good dispersibility, no need of surface modification and no need of adding a dispersing agent to improve the split dispersion performance.
The invention has the following beneficial effects:
(1) the invention can effectively increase the utilization rate of carbon dioxide in the mixed gas, effectively reduce the production cost and simultaneously reduce the emission of carbon dioxide, thereby being beneficial to the green production of products.
(2) The method can effectively reduce the carbonation reaction time of the light calcium carbonate, improve the production efficiency and reduce the time cost.
(3) The grain-shaped light calcium carbonate has larger grain diameter than nano calcium carbonate (within 100 nanometers), and agglomeration can not be formed without strong cohesive force of nano calcium carbonate particles.
(4) The grain-shaped light calcium carbonate has smaller grain diameter than spindle light calcium carbonate (larger than 1 micron), has the service performance closer to that of nano calcium carbonate, has certain characteristics of nano calcium carbonate, has better functional filling effect than the spindle light calcium carbonate in the filling application of downstream products, and has better mechanical properties such as reinforcement, toughness and the like.
(5) The method has the characteristics of simple process, low energy consumption, short reaction time and easy operation and control, and the rice grain-shaped light calcium carbonate produced by the method has uniform and stable quality.
Drawings
FIG. 1 is a scanning electron microscope analysis chart of the rice-shaped light calcium carbonate product prepared in example 1;
FIG. 2 is the scanning electron microscope analysis chart of the rice-shaped light calcium carbonate product prepared in example 2.
Detailed Description
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
Example 1
A rapid preparation process of rice-shaped light calcium carbonate belongs to a carbonization method of calcium hydroxide solution for preparing rice-shaped light calcium carbonate, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and water at the mass ratio of 1:4 at room temperature, aging and cooling properly, sieving the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adjusting the solid content of calcium hydroxide to be 15% after the calcium hydroxide slurry is cooled to the room temperature;
(2) alkali metal ion addition: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding sodium carbonate as alkali metal ions, adjusting the concentration of sodium ions in the slurry to be 2.8mol/L, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 35 ℃, opening a gas valve, introducing mixed gas with the carbon dioxide concentration of 33% to carry out carbonization reaction, closing the gas valve when the pH of the reaction liquid is 7.0 after carbonization, stopping the reaction, and stopping stirring;
(4) dehydrating, drying and crushing: the rice grain-shaped light calcium carbonate with the average grain diameter of 600 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Example 2
A rapid preparation process of rice-shaped light calcium carbonate belongs to a carbonization method of calcium hydroxide solution for preparing rice-shaped light calcium carbonate, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and water at the mass ratio of 1:6 at room temperature, aging and cooling properly, sieving the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adjusting the solid content of calcium hydroxide to 12% after the calcium hydroxide slurry is cooled to room temperature;
(2) alkali metal ion addition: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding sodium hydroxide serving as alkali metal ions, adjusting the concentration of sodium ions in the slurry to be 2.0mol/L, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 38 ℃, opening a gas valve, introducing mixed gas with the carbon dioxide concentration of 28% to carry out carbonization reaction, closing the gas valve when the pH of the reaction liquid is 7.2 after carbonization, stopping the reaction, and stopping stirring;
(4) dehydrating, drying and crushing: the rice grain-shaped light calcium carbonate with the average grain diameter of 630 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Example 3
A rapid preparation process of rice-shaped light calcium carbonate belongs to a carbonization method of calcium hydroxide solution for preparing rice-shaped light calcium carbonate, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and water at the mass ratio of 1:8 at room temperature, aging and cooling properly, sieving the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adjusting the solid content of calcium hydroxide to 13% after the calcium hydroxide slurry is cooled to the room temperature;
(2) alkali metal ion addition: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding sodium bicarbonate serving as alkali metal ions, adjusting the concentration of sodium ions in the slurry to be 1.8mol/L, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 42 ℃, opening a gas valve, introducing mixed gas with the carbon dioxide concentration of 28% to carry out carbonization reaction, closing the gas valve when the pH of the reaction liquid is 7.6 after carbonization, stopping the reaction, and stopping stirring;
(4) dehydrating, drying and crushing: the rice grain-shaped light calcium carbonate with the average grain diameter of 500 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
(5) Example 3 was repeated by changing the amount of sodium bicarbonate added to adjust the molar concentration to 0mlol/L, 2.3mol/L, 2.8mol/L, 3.3mol/L, and the carbonation times obtained were as follows:
| alkali concentration (mol/L) | 0 | 1.8 | 2.3 | 2.8 | 3.3 |
| Carbonization time (min) | 45 | 38 | 34 | 31 | 27 |
(6) Example 3 illustrates that an increased amount of alkali metal ions can effectively reduce the carbonation reaction time and effectively reduce the production cost.
Example 4
A rapid preparation process of rice-shaped light calcium carbonate belongs to a carbonization method of calcium hydroxide solution for preparing rice-shaped light calcium carbonate, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and water at the mass ratio of 1:7 at room temperature, aging and cooling properly, sieving the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adjusting the solid content of calcium hydroxide to 8% after the calcium hydroxide slurry is cooled to room temperature;
(2) alkali metal ion addition: pumping the debugged calcium hydroxide slurry into an intermittent bubble carbonization tower with a stirring device by using a pump, adding potassium hydroxide serving as alkali metal ions, adjusting the concentration of sodium ions in the slurry to be 1.2mol/L, and uniformly stirring;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 32 ℃, opening a gas valve, introducing mixed gas with the carbon dioxide concentration of 36% to carry out carbonization reaction, closing the gas valve when the pH of the reaction liquid is 6.8 after carbonization, stopping the reaction, and stopping stirring;
(4) dehydrating, drying and crushing: the rice grain-shaped light calcium carbonate with the average grain diameter of 400 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Example 5
A rapid preparation process of rice-shaped light calcium carbonate belongs to a carbonization method of calcium hydroxide solution for preparing rice-shaped light calcium carbonate, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and water at the mass ratio of 1:5 at room temperature, aging and cooling properly, sieving the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adjusting the solid content of calcium hydroxide to 11% after the calcium hydroxide slurry is cooled to the room temperature;
(2) alkali metal ion addition: pumping the adjusted calcium hydroxide slurry into an intermittent bubbling carbonization tower with a stirring device by using a pump, and adding sodium hydroxide and potassium bicarbonate with the molar ratio of 1: 1 is taken as alkali metal ions, the concentration of sodium ions in the slurry is adjusted to be 3.2mol/L, and the slurry is stirred uniformly;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 45 ℃, opening a gas valve, introducing mixed gas with the carbon dioxide concentration of 31% to carry out carbonization reaction, closing the gas valve when the pH of the reaction liquid is 7.0 after carbonization, stopping the reaction, and stopping stirring;
(4) dehydrating, drying and crushing: the rice grain-shaped light calcium carbonate with the average grain diameter of 650 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Example 6
A rapid preparation process of rice-shaped light calcium carbonate belongs to a carbonization method of calcium hydroxide solution for preparing rice-shaped light calcium carbonate, and the preparation method comprises the following steps:
(1) lime slaking and calcium hydroxide slurry preparation: sufficiently stirring and digesting lime and water at the mass ratio of 1:8 at room temperature, aging and cooling properly, sieving the obtained lime slurry to remove large particles of insoluble matters and impurities to obtain refined calcium hydroxide slurry, adjusting the solid content of calcium hydroxide to 13% after the calcium hydroxide slurry is cooled to the room temperature;
(2) alkali metal ion addition: pumping the adjusted calcium hydroxide slurry into an intermittent bubbling carbonization tower with a stirring device by using a pump, and adding sodium carbonate and sodium hydroxide according to the molar ratio of 1: 1 is taken as alkali metal ions, the concentration of sodium ions in the slurry is adjusted to be 2.5mol/L, and the slurry is stirred uniformly;
(3) carbonizing: adjusting the initial carbonization temperature of the calcium hydroxide slurry to 55 ℃, opening a gas valve, introducing mixed gas with the carbon dioxide concentration of 33% to carry out carbonization reaction, closing the gas valve when the pH of the reaction liquid is 7.3 after carbonization, stopping the reaction, and stopping stirring;
(4) dehydrating, drying and crushing: the rice grain-shaped light calcium carbonate with the average grain diameter of 700 nanometers is obtained after the procedures of dehydration, drying, crushing, sieving and the like.
Claims (10)
1. A process for quickly preparing the rice-shaped light calcium carbonate includes such steps as adding alkali metal ions to the calcium hydroxide slurry, mixing, introducing the mixture of carbon dioxide and water, quick carbonating reaction to obtain calcium carbonate slurry, dewatering, baking and pulverizing.
2. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the calcium hydroxide slurry is obtained by adding normal-temperature water or hot water into light-burned or medium-burned lime for digestion, and the lime digestion gray-water ratio is 1: 4-9; refining the lime slurry through a 40-200 mesh screen for multiple times to obtain calcium hydroxide slurry, wherein the calcium hydroxide slurry can be refined through combination of screens with different meshes from low to high; the solid content of the calcium hydroxide obtained by refining is regulated and controlled to be 8-20%, and the calcium hydroxide can be aged or not.
3. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the carbonation reaction has no special requirement on a reactor, and comprises a batch bubbling carbonation reactor, a batch bubbling stirring carbonation reactor, a super-gravity carbonation reactor and a venturi tube spray reactor which can meet the carbonation reaction requirement.
4. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the alkali metal ions can be one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate; the dosage of the alkali metal ions is 0.5-5mol/L, and the carbonation reaction time is shorter when the dosage is larger.
5. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the concentration of the carbon dioxide mixed gas is 10-40%, the initial carbonation temperature of the calcium hydroxide slurry is 30-68 ℃, the rapid carbonation reaction is started after the carbon dioxide is introduced, and the reaction can be judged to be finished if the pH value of the slurry is lower than 8 or the alcoholic phenolphthalein solution is not red in a test.
6. The process for rapid preparation of rice-shaped light calcium carbonate according to claim 1, wherein the carbonation reaction process is characterized in that the temperature of the calcium hydroxide slurry is rapidly increased at a low initial carbonation temperature, and the temperature is increased at a low initial temperature due to the large temperature difference between the slurry and the air, and the gas takes away more heat at a low temperature.
7. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the carbonation reaction time is significantly reduced, and the carbonation reaction time is reduced by more than 5% compared with the reaction process without adding alkali metal ions, so that the production efficiency can be effectively improved.
8. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the calcium carbonate slurry obtained by the rapid carbonation reaction is centrifuged or filter-pressed to obtain a calcium carbonate filter cake, and the filter-pressing process can be performed without cleaning the filter cake; the filtrate obtained by filter pressing can be used for lime digestion to realize recycling.
9. The rapid preparation process of the rice-shaped light calcium carbonate as claimed in claim 1, wherein the rice-shaped light calcium carbonate has regular morphology and uniform particle size, and the particle size range is 200-900 nm.
10. The process for rapidly preparing rice-shaped light calcium carbonate according to claim 1, wherein the rice-shaped light calcium carbonate has good dispersibility, does not need surface modification, and does not need to add a dispersant to improve the powder dispersibility.
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