CN114314628A - Process for preparing regular spherical calcium carbonate by double decomposition method - Google Patents
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Abstract
The invention discloses a preparation process of regular spherical calcium carbonate by a double decomposition method, which comprises the following steps: the soluble calcium salt solution and the soluble carbonate solution react quickly under the action of the calcium carbonate crystal form stabilizer to generate a vaterite crystal form, the primary particles of the vaterite crystal form calcium carbonate are overlapped for the second time under the action of the crystal morphology control agent to form spherical calcium carbonate, and the obtained calcium carbonate slurry is dehydrated, washed and dried to obtain the spherical calcium carbonate. The spherical calcium carbonate obtained by the invention does not need surface treatment, has regular sphere, good dispersibility, simple preparation process and low production cost, and the particle size of the prepared spherical calcium carbonate can be adjusted and controlled within the range of 0.1-5 microns. The spherical calcium carbonate has good processing fluidity as a downstream product filler, has good characteristics of removing a template by acid dissolution as a template material of hollow particles, and can be widely applied to the field.
Description
Technical Field
The invention belongs to the technical field of preparation of regular spherical calcium carbonate powder by a double decomposition method of inorganic nonmetallic materials, and particularly relates to calcium carbonate with spherical vaterite crystal form crystal morphology prepared by double decomposition of soluble calcium salt and soluble carbonate and a process thereof.
Background
In recent years, researches show that the hollow particles are a novel material with a special cavity structure, due to the special geometric structure and the physical and chemical properties such as high internal space, low density, large specific surface area, good stability, strong surface permeability and the like, the hollow particles have attracted attention in the field of scientific research, and have good application prospects in the fields of medicine, catalysis, materials and the like. Different templates have different advantages and disadvantages, the calcium carbonate raw material is cheap and easy to obtain, the preparation method is simple, and the calcium carbonate is easy to remove, so that the spherical calcium carbonate is considered as a template material with great potential.
The preparation research of the domestic spherical calcium carbonate has made some progress, the CaCO is prepared3The conventional methods for particles are mainly a double decomposition method and a carbonization method. The double decomposition method has the advantages that the preparation method is simple and is easy to prepare the sphero-star calcium carbonate particles, but the morphology and the particle size of the spherical calcium carbonate particles are difficult to control, the spherical calcium carbonate with uniform particle size is difficult to prepare, the production efficiency of the method is low, and the large-scale industrial production cannot be realized at present. The invention prepares regular spherical calcium carbonate by using a soluble calcium salt and soluble carbonate double decomposition method, and provides a technical process solution for preparing the regular spherical calcium carbonate. The method for preparing regular spherical calcium carbonate with different specifications and particle sizes by developing a soluble calcium salt and a soluble carbonate double decomposition method is used for preparing spherical calcium carbonate products with stable performance and meeting different requirements so as to meet the ever-increasing market demands and has positive significance for improving the added value of the calcium carbonate products.
Disclosure of Invention
The invention provides a preparation process of regular spherical calcium carbonate by a double decomposition method, belongs to the technical field of preparation of calcium carbonate powder of inorganic nonmetallic materials, and particularly relates to a preparation process of calcium carbonate with spherical vaterite crystal form crystal morphology by a soluble calcium salt and soluble carbonate double decomposition method; solves the technical problem of the preparation process for preparing the spherical calcium carbonate particles with uniform and regular particle size.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation process of regular spherical calcium carbonate by a double decomposition method belongs to the technical field of rapid reaction of soluble calcium salt and soluble carbonate under the action of an organic solvent as a calcium carbonate crystal form stabilizer to generate vaterite crystal form calcium carbonate particles, and the vaterite crystal form calcium carbonate particles are agglomerated under the action of a calcium carbonate crystal form control agent to form the regular spherical calcium carbonate; carrying out double decomposition reaction to obtain calcium carbonate slurry, and dehydrating, washing, drying, crushing and screening to obtain spherical calcium carbonate; the preparation method comprises the following steps:
1) dissolving soluble calcium salt in water to prepare calcium salt solution, and dissolving soluble carbonate in water to prepare carbonate solution;
2) adding a crystal form stabilizer into the double decomposition reactant solution;
3) adding a crystal form control agent into the metathesis reactant solution;
4) carrying out double decomposition reaction under stirring, dehydrating, drying, crushing and screening the calcium carbonate slurry obtained by the reaction to obtain the spherical calcium carbonate.
Furthermore, the crystal form is a mixed crystal form of a vaterite crystal form and a calcite crystal form, the crystal morphology is spherical calcium carbonate, the vaterite crystal form accounts for the main part of the mixed crystal form, the calcite crystal form accounts for a small amount, and the particle size of the spherical calcium carbonate is 0.1-5 microns.
Furthermore, the preparation process of the regular spherical calcium carbonate by the double decomposition method can be regular, complete and uniform spherical calcium carbonate, irregular and nonuniform spherical calcium carbonate or spherical calcium carbonate containing part of crushed ball calcium, which is formed because the reaction conditions and process parameters are not controlled in place, or spherical calcium carbonate containing a certain amount of cubic crystal particles.
Further, in the step 1), the soluble calcium salt can be one of calcium chloride, calcium nitrate and calcium chlorate, and the soluble carbonate can be one of sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and ammonium carbonate; the molar ratio of calcium ions to carbonate ions in the soluble calcium salt and the soluble carbonate is 1:1, and the concentration of the calcium ions is 0.4-4 mol/L.
Further, in the step 2), the organic solvent can be at least one of methanol, ethanol, methyl acetate, diethyl ether, acetone and toluene, and the amount of the organic solvent is 10-70% of that of the soluble calcium salt solution and the soluble carbonate solution; part of the double decomposition reactant solution can form complex precipitation with an organic solvent, little or no organic solvent is added for generating the complex precipitation, and the organic solvent with higher proportion is added into the other double decomposition reactant solution which can not generate the precipitation, so that enough calcium carbonate crystal form stabilizer can be ensured in the solution; the organic solvent has a good function of a vaterite crystal form stabilizer, and can effectively prevent the vaterite crystal form from being converted into a calcite crystal form.
Further, at least one of inorganic polymer polyaluminium chloride and polyaluminium sulfate is added into the soluble calcium salt and the soluble carbonate solution in the step 3) as a crystal morphology control agent, and the amount of the added crystal morphology control agent is 0-9% of the content of the soluble calcium salt; at least one crystal morphology control agent is added into at least one metathesis reactant before the metathesis reaction and is stirred evenly.
Further, in the step 3), adding a crystal morphology control agent into the reaction solution with better solubility in a stirring reaction device, uniformly stirring, and adjusting the initial reaction temperature to 2-50 ℃; adding a double decomposition reactant with better solubility and no precipitation into a reaction device with stirring, and adding a double decomposition reactant with low solubility or precipitation under stirring for reaction to obtain spherical calcium carbonate slurry; the addition of the slurry with the complex precipitate to a metathesis reactant solution having a relatively high solubility can reduce the influence of the precipitate on the reaction rate.
Furthermore, the crystal form control agent can be added into at least one of double decomposition reaction solutions, the effect of adding the reaction solution with better solubility is better, and the dosage can be reduced.
Further, stirring is required for the metathesis reactor in the step 4) for dissolving the reaction solution and uniformly mixing the reaction auxiliary agent in the reaction solution, and stirring and mixing reaction during the metathesis reaction.
Further, filtering and dehydrating the calcium carbonate slurry obtained in the step 4) to obtain a calcium carbonate filter cake, and drying, washing, crushing and screening the filter cake to obtain the spherical calcium carbonate.
The invention has the following beneficial effects:
1. soluble calcium salt and carbonate are used as raw materials for preparing the spherical calcium carbonate, the raw materials are wide in source, calcium chloride solution can be prepared by adding hydrochloric acid after dissolving carbide slag, and calcium-containing minerals or waste residues in other forms can be used for preparing the spherical calcium carbonate after being calcined and dissolved. Provides feasible technology for utilizing the calcium-containing slag and the calcium-containing solid waste.
2. The raw materials for preparing the spherical calcium carbonate by the double decomposition reaction are soluble calcium salt and carbonate which can be dissolved in water to form ions, and the calcium ions and the carbonate ions can quickly react in the solution to generate calcium carbonate precipitates, so that the formation of the vaterite crystal form calcium carbonate is more facilitated.
3. The vaterite crystal form calcium carbonate has better stability in a solution taking an organic solvent as a crystal form stabilizer, and the vaterite is more favorable for forming the spherical calcium carbonate under the action of the crystal form control agent under the condition that the vaterite is not converted into the calcite crystal form.
4. The invention has the advantages of simple process design, easy implementation of mass production, low process cost, short reaction time and easy operation and control, and the spherical calcium carbonate produced by the invention has uniform and stable quality.
5. The spherical calcium carbonate prepared by the method has controllable particle size, has good processing fluidity as a downstream product filler, and has good template removing characteristic by acid washing as a template material of hollow particles.
Drawings
FIG. 1 is a scanning electron microscope analysis chart of the spherical calcium carbonate product prepared in example 1;
FIG. 2 is a scanning electron microscope analysis chart of the spherical 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 regular spherical calcium carbonate preparation process belongs to a soluble calcium salt and soluble carbonate double decomposition method for preparing spherical calcium carbonate, and the preparation method comprises the following steps:
(1) preparing soluble calcium salt and carbonate solution: fully stirring and dissolving calcium chloride with minimum water at room temperature to prepare a solution, and fully stirring and dissolving sodium carbonate with minimum water at room temperature to prepare a solution according to the molar ratio of 1:1 of sodium carbonate to calcium chloride;
(2) adding a crystal form stabilizer: adding methanol and water into the calcium chloride solution to adjust the concentration of the calcium chloride to be 12 percent, wherein the adding amount of the methanol is 50 percent of the mass of the adjusted calcium chloride slurry; adding methanol and water into the sodium carbonate solution to adjust the concentration of the sodium carbonate to be 11.6 percent, wherein the adding amount of the methanol is 50 percent of the mass of the adjusted sodium carbonate solution.
(3) Adding a crystal morphology control agent: pumping the adjusted sodium carbonate solution into a reactor with a stirring device by using a pump, adding polyaluminium sulfate with the mass of 1.0 percent of the mass of calcium chloride as a crystal morphology control agent, and uniformly stirring;
(4) double decomposition reaction: regulating the temperature of the solution of the double decomposition reactant to 25 ℃, adding the calcium chloride slurry into the sodium carbonate solution under the stirring action to perform double decomposition reaction to obtain calcium carbonate slurry;
(5) and (3) dehydrating and drying: the calcium carbonate slurry obtained by the double decomposition reaction is dehydrated, washed, dried, crushed, sieved and the like to obtain the regular spherical calcium carbonate with the average grain diameter of 900 nanometers.
Example 2
A regular spherical calcium carbonate preparation process belongs to a soluble calcium salt and soluble carbonate double decomposition method for preparing spherical calcium carbonate, and the preparation method comprises the following steps:
(1) preparing soluble calcium salt and carbonate solution: fully stirring and dissolving calcium nitrate with minimum water at room temperature to prepare a solution, and fully stirring and dissolving sodium carbonate with minimum water at room temperature to prepare a solution according to the molar ratio of 1:1 of sodium carbonate to calcium nitrate;
(2) adding a crystal form stabilizer: adding methanol and water into the calcium nitrate solution to adjust the concentration of the calcium nitrate to be 10 percent, wherein the adding amount of the methanol is 40 percent of the mass of the adjusted calcium nitrate slurry; adding methanol and water into the sodium carbonate solution to adjust the concentration of the sodium carbonate to be 9.6 percent, wherein the adding amount of the methanol is 40 percent of the mass of the adjusted sodium carbonate solution.
(3) Adding a crystal morphology control agent: pumping the adjusted sodium carbonate solution into a reactor with a stirring device by using a pump, adding polyaluminium chloride with the mass of 1.2 percent of the mass of calcium nitrate as a crystal morphology control agent, and uniformly stirring;
(4) double decomposition reaction: regulating the temperature of the solution of the double decomposition reactant to be 30 ℃, adding calcium nitrate slurry into the sodium carbonate solution under the stirring action to perform double decomposition reaction to obtain calcium carbonate slurry;
(5) and (3) dehydrating and drying: the calcium carbonate slurry obtained by the double decomposition reaction is dehydrated, washed, dried, crushed, screened and the like to obtain the regular spherical calcium carbonate with the average grain diameter of 1.2 microns.
Example 3
A regular spherical calcium carbonate preparation process belongs to a soluble calcium salt and soluble carbonate double decomposition method for preparing spherical calcium carbonate, and the preparation method comprises the following steps:
(1) preparing soluble calcium salt and carbonate solution: fully stirring and dissolving calcium chloride with minimum water at room temperature to prepare a solution, and fully stirring and dissolving potassium carbonate with minimum water at room temperature to prepare a solution according to the molar ratio of 1:1 of potassium carbonate to calcium chloride;
(2) adding a crystal form stabilizer: adding ethanol and water into the calcium chloride solution to adjust the calcium chloride concentration to be 8.0%, wherein the adding amount of the ethanol is 55% of the mass of the adjusted calcium chloride slurry; adding ethanol and water into the potassium carbonate solution to adjust the concentration of the potassium carbonate to be 8.0 percent, wherein the adding amount of the ethanol is 60 percent of the mass of the prepared potassium carbonate solution.
(3) Adding a crystal morphology control agent: pumping the adjusted potassium carbonate solution into a reactor with a stirring device by using a pump, adding polyaluminium sulfate with the mass being 1.3 percent of the mass of calcium chloride as a crystal morphology control agent, and uniformly stirring;
(4) double decomposition reaction: regulating the temperature of the solution of the double decomposition reactant to 35 ℃, adding the calcium chloride slurry into the potassium carbonate solution under the stirring action to perform double decomposition reaction to obtain calcium carbonate slurry;
(5) and (3) dehydrating and drying: the calcium carbonate slurry obtained by the double decomposition reaction is dehydrated, washed, dried, crushed, sieved and the like to obtain the regular spherical calcium carbonate with the average particle size of 700 nanometers.
Example 4
A regular spherical calcium carbonate preparation process belongs to a soluble calcium salt and soluble carbonate double decomposition method for preparing spherical calcium carbonate, and the preparation method comprises the following steps:
(1) preparing soluble calcium salt and carbonate solution: fully stirring and dissolving calcium nitrate with minimum water at room temperature to prepare a solution, and fully stirring and dissolving potassium carbonate with minimum water at room temperature to prepare a solution according to the molar ratio of 1:1 of potassium carbonate to calcium nitrate;
(2) adding a crystal form stabilizer: adding methyl acetate and water into the calcium nitrate solution to adjust the calcium nitrate concentration to 9 percent, wherein the adding amount of the methyl acetate is 45 percent of the mass of the adjusted calcium nitrate slurry; methyl acetate and water are added into the potassium carbonate solution to adjust the concentration of the calcium nitrate to be 10 percent, and the adding amount of the methyl acetate is 60 percent of the mass of the adjusted calcium nitrate slurry.
(3) Adding a crystal morphology control agent: pumping the adjusted potassium carbonate solution into a reactor with a stirring device by using a pump, adding polyaluminium chloride with the mass of 0.7 percent of the mass of calcium nitrate as a crystal morphology control agent, and uniformly stirring;
(4) double decomposition reaction: regulating the temperature of the solution of the double decomposition reactant to be 30 ℃, and adding calcium nitrate slurry into the potassium carbonate solution under the stirring action to perform double decomposition reaction to obtain calcium carbonate slurry;
(5) and (3) dehydrating and drying: the calcium carbonate slurry obtained by the double decomposition reaction is dehydrated, washed, dried, crushed, screened and the like to obtain the regular spherical calcium carbonate with the average particle size of 600 nanometers.
Example 5
A regular spherical calcium carbonate preparation process belongs to a soluble calcium salt and soluble carbonate double decomposition method for preparing spherical calcium carbonate, and the preparation method comprises the following steps:
(1) preparing soluble calcium salt and carbonate solution: fully stirring and dissolving calcium chlorate with minimum water at room temperature to prepare solution, and fully stirring and dissolving sodium carbonate with minimum water at room temperature to prepare solution according to the molar ratio of 1:1 of sodium carbonate to calcium chlorate;
(2) adding a crystal form stabilizer: adding ethanol and water into the calcium chlorate solution to adjust the calcium chloride concentration to be 14 percent, wherein the adding amount of the ethanol is 40 percent of the mass of the adjusted calcium chlorate slurry; adding ethanol and water into the sodium carbonate solution to adjust the concentration of the sodium carbonate solution to 13 percent, wherein the adding amount of the ethanol is 60 percent of the mass of the adjusted sodium carbonate solution.
(3) Adding a crystal morphology control agent: pumping the adjusted sodium carbonate solution into a reactor with a stirring device by using a pump, adding polyaluminium sulfate with the mass being 1.1 percent of the mass of the calcium chlorate as a crystal morphology control agent, and uniformly stirring;
(4) double decomposition reaction: regulating the temperature of the solution of the double decomposition reactant to 35 ℃, adding the calcium chlorate slurry into the sodium carbonate solution under the stirring action to perform double decomposition reaction to obtain calcium carbonate slurry;
(5) and (3) dehydrating and drying: the calcium carbonate slurry obtained by the double decomposition reaction is dehydrated, washed, dried, crushed, sieved and the like to obtain the regular spherical calcium carbonate with the average grain diameter of 900 nanometers.
Example 6
A regular spherical calcium carbonate preparation process belongs to a soluble calcium salt and soluble carbonate double decomposition method for preparing spherical calcium carbonate, and the preparation method comprises the following steps:
(1) preparing soluble calcium salt and carbonate solution: fully stirring and dissolving calcium chlorate with minimum water at room temperature to prepare a solution, and fully stirring and dissolving sodium bicarbonate with minimum water at room temperature to prepare a solution according to the molar ratio of 1:1 of sodium bicarbonate to calcium chlorate;
(2) adding a crystal form stabilizer: adding acetone and water into the calcium chlorate solution to prepare the calcium chlorate with the concentration of 9 percent, wherein the adding amount of the acetone is 50 percent of the mass of the prepared calcium chlorate slurry; methanol and water are added into the sodium bicarbonate solution to adjust the concentration of the sodium bicarbonate to be 11.6 percent, and the adding amount of acetone is 50 percent of the mass of the prepared sodium bicarbonate solution.
(3) Adding a crystal morphology control agent: pumping the adjusted sodium bicarbonate solution into a reactor with a stirring device by using a pump, adding polyaluminium sulfate with the mass of 1.5 percent of the mass of the calcium chlorate as a crystal morphology control agent, and uniformly stirring;
(4) double decomposition reaction: regulating the temperature of the solution of the double decomposition reactant to 38 ℃, and adding the calcium chlorate slurry into the sodium bicarbonate solution under the stirring action to perform double decomposition reaction to obtain calcium carbonate slurry;
(5) and (3) dehydrating and drying: the calcium carbonate slurry obtained by the double decomposition reaction is dehydrated, washed, dried, crushed, screened and the like to obtain regular spherical calcium carbonate with the average particle size of 1.5 microns.
Claims (10)
1. A preparation process of regular spherical calcium carbonate by a double decomposition method is characterized by comprising the following steps: soluble calcium salt and soluble carbonate react rapidly under the action of an organic solvent as a calcium carbonate crystal form stabilizer to generate vaterite crystal form calcium carbonate particles, and the vaterite crystal form calcium carbonate particles are agglomerated under the action of a calcium carbonate crystal form control agent to form regular spherical calcium carbonate; carrying out double decomposition reaction to obtain calcium carbonate slurry, and dehydrating, washing, drying, crushing and screening to obtain spherical calcium carbonate; the preparation method comprises the following steps:
1) respectively dissolving soluble calcium salt and soluble carbonate in water to prepare salt forming solution;
2) adding a crystal form stabilizer into the double decomposition reactant solution;
3) adding a crystal form control agent into the metathesis reactant solution;
4) carrying out double decomposition reaction under stirring, dehydrating, washing, drying, crushing and screening the calcium carbonate slurry obtained by the reaction to obtain the spherical calcium carbonate.
2. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: the crystal form is a mixed crystal form of a vaterite crystal form and a calcite crystal form, the crystal form is spherical calcium carbonate, the vaterite crystal form accounts for more than 50% of the mixed crystal form, the calcite crystal form accounts for less than 50%, and the particle size of the spherical calcium carbonate is 0.1-5 microns.
3. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: the calcium carbonate can be regular, complete and uniform spherical calcium carbonate, irregular, non-uniform or spherical calcium carbonate containing partial crushed ball calcium formed because the reaction conditions and process parameters are not controlled well, and the spherical calcium carbonate containing a certain amount of cubic crystal particles.
4. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: in the step 1), the soluble calcium salt can be one of calcium chloride, calcium nitrate and calcium chlorate, and the soluble carbonate can be one of sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and ammonium carbonate. The molar ratio of calcium ions to carbonate ions in the soluble calcium salt and the soluble carbonate is 1:1, and the concentration of the calcium ions is 0.4-4 mol/L.
5. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: the organic solvent in the step 2) can be at least one of methanol, ethanol, methyl acetate, diethyl ether, acetone and toluene, and the dosage of the organic solvent is 10-70% of that of the soluble calcium salt solution and the soluble carbonate solution; part of the double decomposition reactant solution can form complex precipitation with an organic solvent, little or no organic solvent is added for generating the complex precipitation, and the organic solvent with higher proportion is added into the other double decomposition reactant solution which can not generate the precipitation, so that enough calcium carbonate crystal form stabilizer can be ensured in the solution; the organic solvent has a good function of a vaterite crystal form stabilizer, and can effectively prevent the vaterite crystal form from being converted into a calcite crystal form.
6. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: adding at least one of inorganic polymer polyaluminium chloride and polyaluminium sulfate into the soluble calcium salt and soluble carbonate solution in the step 3) as a crystal morphology control agent, wherein the amount of the added crystal morphology control agent is 0-9% of the content of the soluble calcium salt; at least one crystal morphology control agent is added into at least one metathesis reactant before the metathesis reaction and is stirred evenly.
7. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: in a reaction device with stirring in the step 3), adding a crystal morphology control agent into the reaction solution with better solubility, uniformly stirring, and adjusting the initial reaction temperature to 2-50 ℃; adding a double decomposition reactant with better solubility and no precipitation into a reaction device with stirring, and adding a double decomposition reactant with low solubility or precipitation under stirring for reaction to obtain spherical calcium carbonate slurry; the addition of the slurry with the complex precipitate to a metathesis reactant solution having a relatively high solubility can reduce the influence of the precipitate on the reaction rate.
8. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 7, wherein: the crystal form control agent can be added into at least one of double decomposition reaction solutions, the effect of adding the reaction solution with better solubility is better, and the dosage can be reduced.
9. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: in the step 4), the double decomposition reactor needs to be stirred, and the double decomposition reactor is used for dissolving the reaction liquid, uniformly mixing the reaction auxiliary agent in the reaction liquid and stirring and mixing the reaction liquid in the double decomposition reaction process.
10. The process for preparing regular spherical calcium carbonate by double decomposition method according to claim 1, which is characterized in that: and 4) filtering and dehydrating the calcium carbonate slurry obtained in the step 4) to obtain a calcium carbonate filter cake, and drying, washing, crushing and screening the filter cake to obtain the spherical calcium carbonate.
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