CN107986313B - Preparation method of spherical calcium carbonate - Google Patents
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Abstract
The invention discloses a preparation method of spherical calcium carbonate, which comprises the steps of preparing PVP-sodium stearate composite solution with a certain concentration, adding one part of the PVP-sodium stearate solution into calcium chloride solution to form solution A, placing the solution on a constant-speed stirrer after ultrasonic treatment for continuous stirring for 1 hour, adding the other part of the PVP-sodium stearate solution into sodium carbonate solution to form solution B, placing the solution on the constant-speed stirrer for continuous stirring for half an hour after low-frequency ultrasonic treatment, quickly pouring the solution A into the solution B, carrying out suction filtration on slurry, and washing to obtain spherical calcium carbonate particles. The preparation method has the advantages of mild preparation conditions, simple production equipment and environmental protection, and the spherical calcium carbonate prepared by using the PVP-sodium stearate composite solution as the crystal form control agent has the advantages of small particle size and uniform dispersion.
Description
Technical Field
The invention relates to a preparation method of spherical calcium carbonate.
Background
Calcium carbonate is a recognized pollution-free and friendly inorganic filler. The calcium carbonate has wide sources and wide application range, and has three crystal forms, namely an aragonite type, a calcite type and a vaterite type, wherein the most stable crystal form is the calcite type, the aragonite and the vaterite type belong to unstable structures in nature and are easily converted into the calcite type in nature, and the calcite type calcium carbonate is mainly present in marble; the aragonite calcium carbonate mainly exists in shells and marine sedimentary rocks, and can be prepared into whisker-shaped aragonite calcium carbonate with a certain length-diameter ratio under certain experimental control conditions; the vaterite type calcium carbonate is rare in nature, is generally spherical in characteristic appearance and needs to be synthesized through experiments. Currently, scientists have studied calcium carbonate with various morphologies, including cubic, needle, rod, petal, spindle, sheet, etc., and the industrial application field of calcium carbonate with different morphologies is different.
Spherical calcium carbonate has a large specific surface area, good dispersibility, high solubility and a small specific gravity, and the characteristics of the spherical calcium carbonate make the spherical calcium carbonate attract more and more attention in the fields of medicines, catalysis, ink and the like. The dispersibility and isotropy of the spherical calcium carbonate structure endows it with an elastic structure and better plasticity, and has attracted the interest of many researchers. At present, the preparation of spherical calcium carbonate at home and abroad mainly adopts the following method: one is Ca (OH)2And CO2The second method is to prepare CaCl with a certain concentration2Adjusting the pH value with alkaline solution, introducing CO2The gas is carbonized to produce calcium carbonate, and the third method is water-soluble calcium salt (such as CaCl)2Solution, Ca (NO)3)2Solution, etc.) and carbonates (e.g., Na)2CO3Solution, NaHCO3Solution, etc.) under appropriate experimental conditions to form calcium carbonate. The existing method generally regulates and controls the nucleation and crystallization of calcium carbonate by means of organic matters, adopts organic matters extracted from organisms or artificially synthesized organic matter molecules to regulate and control the crystal form and the morphology of the calcium carbonate, and the materials are organic-inorganic repair materials and exceed the performances of common inorganic materials in the aspects of mechanical properties and the like. Therefore, a suitable morphology control agent is found to have important application value for preparing calcium carbonate, and polyvinylpyrrolidone as a synthetic water-soluble high molecular compound has excellent solubility, physiological compatibility and low toxicity. Tantan Jianyun and the like disclose a preparation method of spherical calcium carbonate with low costCMC (sodium carboxymethylcellulose) with viscosity is used as a morphology control agent, and the solid spherical calcium carbonate with smooth surface is successfully prepared, and has the grain diameter of about 5-10 mu m and larger grain diameter.
Disclosure of Invention
The invention provides a preparation method of spherical calcium carbonate, which takes sodium stearate modified PVP as a morphology control agent to prepare the spherical calcium carbonate.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the spherical calcium carbonate is characterized by comprising the following steps:
s1, adding PVP powder and sodium stearate powder into 100mL of water for dissolving to obtain a PVP-sodium stearate composite solution, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer at the temperature of 20-40 ℃, stirring for 30min, and then placing the mixture on a heat collection type magnetic stirrer at the temperature of 35 ℃ for ultrasonic treatment for 30min to obtain a crystal form control agent;
s2, quickly adding 50mL of crystal form control agent into 500mL of calcium chloride solution with the concentration of 0.1-0.4mol/L, performing ultrasonic treatment on an ultrasonic cleaning machine for 20min to uniformly mix, marking as a solution A, transferring the solution A into a constant-temperature water bath kettle, and continuously stirring the solution A on a constant-speed stirrer for 1 hour; adding 50mL of crystal form control agent into 500mL of sodium carbonate solution with the concentration of 0.1-0.4mol/L, carrying out ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into a constant-temperature water bath kettle, placing the constant-temperature water bath kettle on a constant-speed stirrer, continuously stirring for 30min, then quickly adding the solution A into the solution B, and then placing the solution A into the water bath kettle with the reaction temperature of 20-40 ℃ to react at the stirring speed of 600-;
s3, after the slurry is subjected to suction filtration, taking out a precipitate, alternately washing the precipitate for 3 times by using deionized water and absolute ethyl alcohol, drying the precipitate for 8 hours at 60 ℃, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
Further, the PVP adding mass in the step S1 is 1-2g, and the sodium stearate adding mass is 2-4 g.
Further, the dissolving temperature of PVP in the step S1 is 20-40 ℃.
Further, the molar ratio of calcium chloride to sodium carbonate in the step S2 is 1: 1.
Further, the mixing reaction time of the solution A and the solution B in the step S2 is 60-120 min.
The invention has the beneficial effects that:
PVP-sodium stearate is adopted as a shape control agent, the shape control agent has the advantages of wide source and low price, PVP is used as a water-soluble nonionic polymer, sodium stearate is an anionic surfactant, the PVP-sodium stearate composite solution is formed by combining the PVP-sodium stearate and the sodium stearate, sodium stearate micelles are associated to PVP groups to form a chain spherical cluster to form a supermolecule self-assembly structure, and polar groups on the PVP-sodium stearate composite micelles attract Ca through electrostatic action2+Provides nucleation sites for the formation of calcium carbonate, prepares the organic-inorganic composite structure microspheres through layer-by-layer association, and the prepared spherical calcium carbonate has the excellent performances of environmental protection and low toxicity, and the average grain diameter of the spherical calcium carbonate prepared by the invention is 0.5-2 mu m.
In the PVP-sodium stearate system, the main driving force of the supramolecular action between the PVP-sodium stearate system and the sodium stearate system is the electrostatic action or the ion dipole action between polar groups between the sodium stearate and the PVP, and after the sodium stearate is loaded on the PVP structure, a spherical cluster body is formed to attract Ca in the solution from all directions2+Greatly enriches the chelating sites of calcium ions and overcomes the problem of few binding sites in reaction regulation. Because sodium stearate is a surfactant, a microemulsion system is formed in the preparation process, and calcium carbonate particles are distributed more uniformly.
The preparation method takes calcium chloride and sodium carbonate as basic raw materials, takes PVP-sodium stearate as a morphology control agent, overcomes the defects of difficult control of reaction conditions, large product particle size, toxic products and the like in the traditional chemical method for preparing the spherical calcium carbonate, can prepare the spherical calcium carbonate with high sphericity, small particle size and high dispersity under the condition of less addition amount of the morphology control agent, has simple and convenient preparation process and lower requirements on process equipment, and reduces the cost for preparing the spherical calcium carbonate.
Drawings
FIG. 1 is a 2.0K-fold scanning electron micrograph of the spherical calcium carbonate prepared in example 1;
FIG. 2 is a scanning electron micrograph of the spherical calcium carbonate prepared in example 1 at 5.0K times;
FIG. 3 is a scanning electron micrograph of the spherical calcium carbonate prepared in example 1 at a magnification of 10.0K;
FIG. 4 is a 20.0K-fold scanning electron micrograph of the spherical calcium carbonate prepared in example 1;
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 preparation method of spherical calcium carbonate comprises the following steps:
s1, firstly preparing a PVP-sodium stearate composite solution with a certain concentration as a morphology control agent, weighing 1g of PVP powder and 2g of sodium stearate powder, adding the PVP powder and the sodium stearate powder into 100mL of water with the temperature of 20 ℃ for dissolving, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer with the temperature of 35 ℃ for stirring for 30min, placing the solution on an ultrasonic cleaning machine with the temperature of 35 ℃ for ultrasonic treatment for 30min after stirring, enabling the PVP-sodium stearate solution to form a homogeneous solution, and then evenly dividing the solution into two parts, each of which is 50mL, for later use;
s2, preparing 500mL of calcium chloride solution with the concentration of 0.1mol/L, quickly adding one portion of PVP-sodium stearate composite solution into the calcium chloride solution, firstly carrying out low-frequency ultrasonic treatment on an ultrasonic cleaning machine for 20min to ensure that calcium ions, PVP groups and stearate ions are uniformly chelated, uniformly mixing, marking as solution A, transferring the solution A into a constant-temperature water bath kettle, placing the constant-temperature water bath kettle on a constant-speed stirrer for continuously stirring for 1 hour, preparing 500mL of sodium carbonate solution with the concentration of 0.1mol/L, adding the other portion of PVP-sodium stearate solution into the sodium carbonate solution, carrying out low-frequency ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into the constant-temperature water bath kettle, placing the constant-speed stirrer on the constant-speed stirrer for continuously stirring for half an hour, then quickly adding the solution A into the solution B to obtain a mixed solution, reacting the mixed solution in the water bath kettle at the reaction temperature of 35 ℃ and the stirring speed of, obtaining slurry;
and S3, carrying out suction filtration on the slurry in a suction filtration bottle, taking out a precipitate, repeatedly washing the precipitate for three times by using deionized water and absolute ethyl alcohol, drying the precipitate obtained after suction filtration at 60 ℃ for 8 hours, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
The average particle size of the prepared spherical calcium carbonate was 2 μm.
Example 2
S1, firstly preparing a PVP-sodium stearate composite solution with a certain concentration as a morphology control agent, weighing 1g of PVP powder and 2g of sodium stearate powder, adding the PVP powder and the sodium stearate powder into 100mL of water with the temperature of 40 ℃ for dissolving, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer with the temperature of 40 ℃ for stirring for 30min, placing the solution on an ultrasonic cleaning machine with the temperature of 40 ℃ for ultrasonic treatment for 30min after stirring, enabling the PVP-sodium stearate solution to form a homogeneous solution, and then evenly dividing the solution into two parts with the volume of 50mL for later use;
s2, preparing 500mL of calcium chloride solution with the concentration of 0.2mol/L, quickly adding one portion of PVP-sodium stearate composite solution into the calcium chloride solution, firstly carrying out low-frequency ultrasonic treatment on an ultrasonic cleaning machine for 20min to ensure that calcium ions, PVP groups and stearate ions are uniformly chelated, uniformly mixing, marking as solution A, transferring the solution A into a constant-temperature water bath kettle, placing the constant-temperature water bath kettle on a constant-speed stirrer for continuously stirring for 1 hour, preparing 500mL of sodium carbonate solution with the concentration of 0.2mol/L, adding the other portion of PVP-sodium stearate solution into the sodium carbonate solution, carrying out low-frequency ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into the constant-temperature water bath kettle, placing the constant-speed stirrer on the constant-speed stirrer for continuously stirring for half an hour, then quickly adding the solution A into the solution B to obtain a mixed solution, reacting the mixed solution in the water bath kettle at the reaction temperature of 40 ℃ and the stirring speed of, obtaining slurry;
and S3, carrying out suction filtration on the slurry in a suction filtration bottle, taking out a precipitate, repeatedly washing the precipitate for three times by using deionized water and absolute ethyl alcohol, drying the precipitate obtained after suction filtration at 60 ℃ for 8 hours, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
The average particle size of the prepared spherical calcium carbonate was 0.5. mu.m.
Example 3
S1, firstly preparing a PVP-sodium stearate composite solution with a certain concentration as a morphology control agent, weighing 2g of PVP powder and 4g of sodium stearate powder, adding the PVP powder and the sodium stearate powder into 100mL of water with the temperature of 35 ℃ for dissolving, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer with the temperature of 20 ℃ for stirring for 30min, placing the solution on an ultrasonic cleaning machine with the temperature of 35 ℃ for ultrasonic treatment for 30min after stirring, enabling the PVP-sodium stearate solution to form a homogeneous solution, and then evenly dividing the solution into two parts, each of which is 50mL, for later use;
s2, preparing 500mL of calcium chloride solution with the concentration of 0.2mol/L, quickly adding one portion of PVP-sodium stearate composite solution into the calcium chloride solution, firstly carrying out low-frequency ultrasonic treatment on an ultrasonic cleaning machine for 20min to ensure that calcium ions, PVP groups and stearate ions are uniformly chelated, uniformly mixing, marking as solution A, transferring the solution A into a constant-temperature water bath kettle, placing the constant-temperature water bath kettle on a constant-speed stirrer for continuously stirring for 1 hour, preparing 500mL of sodium carbonate solution with the concentration of 0.2mol/L, adding the other portion of PVP-sodium stearate solution into the sodium carbonate solution, carrying out low-frequency ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into the constant-temperature water bath kettle, placing the constant-speed stirrer on the constant-speed stirrer for continuously stirring for half an hour, then quickly adding the solution A into the solution B to obtain a mixed solution, reacting the mixed solution in the water bath kettle at the reaction temperature of 35 ℃ and the stirring speed of, obtaining slurry;
and S3, carrying out suction filtration on the slurry in a suction filtration bottle, taking out a precipitate, repeatedly washing the precipitate for three times by using deionized water and absolute ethyl alcohol, drying the precipitate obtained after suction filtration at 60 ℃ for 8 hours, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
The average particle size of the prepared spherical calcium carbonate was 2 μm.
Example 4
S1, firstly preparing a PVP-sodium stearate composite solution with a certain concentration as a morphology control agent, weighing 2g of PVP powder and 4g of sodium stearate powder, adding the PVP powder and the sodium stearate powder into 100mL of water with the temperature of 40 ℃ for dissolving, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer with the temperature of 40 ℃ for stirring for 30min, placing the solution on an ultrasonic cleaning machine with the temperature of 40 ℃ for ultrasonic treatment for 30min after stirring, enabling the PVP-sodium stearate solution to form a homogeneous solution, and then evenly dividing the solution into two parts, each of which is 50mL, for later use;
s2, preparing 500mL of calcium chloride solution with the concentration of 0.4mol/L, quickly adding one portion of PVP-sodium stearate composite solution into the calcium chloride solution, firstly carrying out low-frequency ultrasonic treatment on an ultrasonic cleaning machine for 20min to ensure that calcium ions, PVP groups and stearate ions are uniformly chelated, uniformly mixing, marking as solution A, transferring the solution A into a constant-temperature water bath kettle, placing the constant-temperature water bath kettle on a constant-speed stirrer for continuously stirring for 1 hour, preparing 500mL of sodium carbonate solution with the concentration of 0.4mol/L, adding the other portion of PVP-sodium stearate solution into the sodium carbonate solution, carrying out low-frequency ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into the constant-temperature water bath kettle, placing the constant-speed stirrer on the constant-speed stirrer for continuously stirring for half an hour, then quickly adding the solution A into the solution B to obtain a mixed solution, reacting the mixed solution in the water bath kettle at the reaction temperature of 40 ℃ and the stirring speed of, obtaining slurry;
and S3, carrying out suction filtration on the slurry in a suction filtration bottle, taking out a precipitate, repeatedly washing the precipitate for three times by using deionized water and absolute ethyl alcohol, drying the precipitate obtained after suction filtration at 60 ℃ for 8 hours, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
The average particle size of the prepared spherical calcium carbonate was 1.5. mu.m.
Example 5
S1, firstly preparing a PVP-sodium stearate composite solution with a certain concentration as a morphology control agent, weighing 2g of PVP powder and 4g of sodium stearate powder, adding the PVP powder and the sodium stearate powder into 100mL of water with the temperature of 40 ℃ for dissolving, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer with the temperature of 40 ℃ for stirring for 30min, placing the solution on an ultrasonic cleaning machine with the temperature of 40 ℃ for ultrasonic treatment for 30min after stirring, enabling the PVP-sodium stearate solution to form a homogeneous solution, and then evenly dividing the solution into two parts, each of which is 50mL, for later use;
s2, preparing 500mL of calcium chloride solution with the concentration of 0.4mol/L, quickly adding one part of PVP-sodium stearate composite solution into the calcium chloride solution, firstly carrying out low-frequency ultrasonic treatment on an ultrasonic cleaning machine for 20min to ensure that calcium ions, PVP groups and stearate ions are uniformly chelated, uniformly mixing, marking as solution A, transferring the solution A into a constant-temperature water bath kettle, continuously stirring for 1 hour on a constant-speed stirrer, preparing 500mL of 0.4mol/L sodium carbonate solution, adding the other part of PVP-sodium stearate solution into the sodium carbonate solution, carrying out low-frequency ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into the constant-temperature water bath kettle, continuously stirring for half an hour on the constant-speed stirrer, then quickly adding the solution A into the solution B to obtain a mixed solution, reacting the mixed solution in the water bath kettle at the reaction temperature of 20 ℃ and the stirring speed of 1000rpm for 120min, obtaining slurry;
and S3, carrying out suction filtration on the slurry in a suction filtration bottle, taking out a precipitate, repeatedly washing the precipitate for three times by using deionized water and absolute ethyl alcohol, drying the precipitate obtained after suction filtration at 60 ℃ for 8 hours, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
The average particle size of the prepared spherical calcium carbonate was 1 μm.
The protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (5)
1. The preparation method of the spherical calcium carbonate is characterized by comprising the following steps:
s1, adding PVP powder and sodium stearate powder into 100mL of water for dissolving to obtain a PVP-sodium stearate composite solution, placing the PVP-sodium stearate composite solution on a heat collection type magnetic stirrer at the temperature of 20-40 ℃, stirring for 30min, and then placing the mixture on a heat collection type magnetic stirrer at the temperature of 35 ℃ for ultrasonic treatment for 30min to obtain a crystal form control agent;
s2, quickly adding 50mL of crystal form control agent into 500mL of calcium chloride solution with the concentration of 0.1-0.4mol/L, performing ultrasonic treatment on an ultrasonic cleaning machine for 20min to uniformly mix, marking as a solution A, transferring the solution A into a constant-temperature water bath kettle, and continuously stirring the solution A on a constant-speed stirrer for 1 hour; adding 50mL of crystal form control agent into 500mL of sodium carbonate solution with the concentration of 0.1-0.4mol/L, carrying out ultrasonic treatment for 20min, uniformly mixing, marking as solution B, transferring the solution B into a constant-temperature water bath kettle, placing the constant-temperature water bath kettle on a constant-speed stirrer, continuously stirring for 30min, then quickly adding the solution A into the solution B, and then placing the solution A into the water bath kettle with the reaction temperature of 20-40 ℃ to react at the stirring speed of 600-;
s3, after the slurry is subjected to suction filtration, taking out a precipitate, alternately washing the precipitate for 3 times by using deionized water and absolute ethyl alcohol, drying the precipitate for 8 hours at 60 ℃, and finally taking out the precipitate and grinding the precipitate into powder to obtain the spherical calcium carbonate.
2. The method for preparing spherical calcium carbonate according to claim 1, wherein the PVP is added in an amount of 1-2g and the sodium stearate is added in an amount of 2-4g in step S1.
3. The method for preparing spherical calcium carbonate according to claim 1, wherein the PVP dissolution temperature in the step S1 is 20-40 ℃.
4. The method for preparing spherical calcium carbonate according to claim 1, wherein the molar ratio of calcium chloride to sodium carbonate in step S2 is 1: 1.
5. The method for preparing spherical calcium carbonate according to claim 1, wherein the mixing reaction time of the solution A and the solution B in the step S2 is 60-120 min.
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