CN110577232A - Preparation method of nano calcium carbonate - Google Patents
Preparation method of nano calcium carbonate Download PDFInfo
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- CN110577232A CN110577232A CN201911019741.3A CN201911019741A CN110577232A CN 110577232 A CN110577232 A CN 110577232A CN 201911019741 A CN201911019741 A CN 201911019741A CN 110577232 A CN110577232 A CN 110577232A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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- 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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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a preparation method of nano calcium carbonate, which obtains CaCl based on steel slag2‑NH4Cl‑NH3‑H2The method comprises the steps of adding cane sugar into the leachate of an O system, introducing carbon dioxide into the leachate, simultaneously starting ultrasonic waves with the power of 1500 ~ 1800W, and sieving to obtain the nano calcium carbonate.
Description
Technical Field
The invention relates to the technical field of preparation of calcium carbonate, in particular to a preparation method of nano calcium carbonate.
Background
The nano calcium carbonate is generally calcium carbonate particles with characteristic dimension size of nano magnitude (1-100 nm), and comprises ultrafine calcium carbonate (particle size of 0.02-0.1 mu m) and ultrafine calcium carbonate (particle size of less than or equal to 0.02 mu m) which are generally called in light calcium carbonate industry, and due to the ultrafine property of the nano calcium carbonate, the particle crystal structure and the surface electronic structure of the nano calcium carbonate are changed, so that the quantum size effect, small size effect, surface effect and macroscopic quantum effect which are not possessed by common calcium carbonate are generated, and the nano calcium carbonate has superior performance compared with the conventional materials in the aspects of magnetism, catalyst, photo-thermal resistance, melting point and the like. The product filled in rubber and plastic has bright surface, good elongation, high tensile strength, strong tearing resistance, good bending resistance and good anti-cracking performance, and is an excellent white reinforcing material. The product has good gloss, transparency, stability, quick drying and other characteristics in high-grade printing ink and coating.
The preparation method of calcium carbonate materials mainly comprises three main categories: solid phase method, liquid phase method, gas phase method, the nano calcium carbonate mainly adopts the liquid phase method. According to the difference of the synthesis mechanism, the method can be divided into three reaction systems: ca (OH)2-H2O-CO2The reaction system, namely the traditional carbonization method, mainly comprises production methods such as an intermittent carbonization method, a continuous spray carbonization method, a supergravity carbonization method and the like, the reaction systems of the methods are simple, the reaction process is usually controlled by utilizing the conductivity and the pH value, but the preparation process of the system usually needs processes such as mining, transporting, calcining, digesting and the like on limestone, so that the environmental pollution is large, the preparation method is complicated and the cost is high; ca2+-H2O-CO3 2-Reaction system, i.e. containing Ca2+With a solution containing CO3 2-The solution is mixed and reacted under certain conditions to prepare the nano calcium carbonate; ca2+-R-CO3 2-Reaction systems (R is an organic medium), namely a microemulsion method and a gel method. The latter two methods have not been used in actual production for a while. For example, patent CN201811350972.8 discloses a spherical nano calcium carbonate and a preparation method thereof, which comprises the following steps: dissolving sodium carbonate, potassium carbonate or ammonium bicarbonate in water to prepare CO3 2-The concentration is 0.25-1mol/L solution A; dissolving calcium acetate monohydrate or calcium chloride monohydrate in water to form Ca2+Solution B with the concentration of 0.25-1 mol/L; respectively adding a certain amount of glycerol into different containers, and then respectively adding deionized water according to the volume ratio of 4:5-8:1 to prepare a solution C; respectively adding the solution A into the solution C, stirring for 3-5 minutes, then adding the solution B while stirring, and continuing stirring for 4-5 hours after the solution becomes turbid; the resulting white precipitate was centrifuged, washed repeatedly with deionized water, and dried in an oven at 60 ℃ under vacuum overnight. The invention patent CN201910012324.X discloses a preparation method of nano calcium carbonate for MS glue, which comprises the steps of mixing calcium oxide (CaO) with water (H)2O) digestion of the resulting calcium hydroxide (Ca (OH)2) Removing impurities from the slurry, aging under constant temperature, adding crystal form control agent, and washing with carbon dioxide (CO)2) The kiln gas is subjected to a primary carbonization synthesis reaction, and then an after-treatment agent is added, aged for a certain time and then mixed with the washed carbon dioxide (CO)2) The kiln gas is subjected to secondary carbonization synthesis reaction to obtain calcium carbonate (CaCO)3) And (3) curing the slurry, namely adding a modifier into the cured slurry, and performing filter pressing, dehydration, drying, crushing and classification after the reaction is finished to obtain the nano calcium carbonate for the MS glue. However, the method has complex process and high cost. In CaCl2-NH4Cl-NH3-H2the research of preparing the nano calcium carbonate under the O system has not been reported so far.
With the continuous mass production of steel enterprises in China for decades, the accumulation of steelmaking slag is gradually increased year by year, and at present, no ideal steel slag treatment technology is developed in China, and the utilization rate is only about 10%. A large amount of steel slag is stacked, which not only occupies land, but also easily causes salinization of the land, and causes a large amount of resource waste and serious environmental pollution. Meanwhile, the steel-making process is accompanied by the generation of a large amount of carbon dioxide, and the greenhouse effect brought by the carbon dioxide has obvious influence on the global climate: so that glaciers melt, natural ecological degeneration and natural disasters frequently occur, and the survival and development of human beings in partial regions are directly threatened. Therefore, how to realize the resource utilization of the steelmaking slag and the carbon dioxide becomes a problem which needs to be solved urgently.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of nano calcium carbonate, which solves the problems of complex process, high cost, great environmental pollution and the like of the existing preparation method and improves the resource utilization of steel slag.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of nano calcium carbonate comprises the following steps:
1) Adding ammonium chloride solution into the steel slag for reaction to obtain CaCl2-NH4Cl-NH3-H2Standing the leaching solution of the O system overnight for later use;
2) Adding cane sugar into the leachate obtained in the step 1), introducing carbon dioxide into the leachate, starting ultrasonic waves with the power of 1500-1800W, stopping the reaction when the pH value of the leachate is 7.1, immediately screening by using a 250-mesh screen, rinsing the screened product by using absolute ethyl alcohol, and drying in a vacuum drying oven to obtain the nano calcium carbonate.
Preferably, CaCl is contained in the leachate2Is 0.4mol/L, NH4Cl concentration of 1mol/L, NH4The concentration of HO was 0.8 mol/L.
Preferably, the temperature in the leaching reaction in the step 1) is 40-60 ℃.
Preferably, the temperature of the leachate obtained in the step 2) in the reaction process is 15-25 ℃.
Preferably, the adding amount of the sucrose is 2% of the mass of the calcium chloride in the leaching solution.
Preferably, the flow rate of the carbon dioxide is 45 ml/min.
Preferably, the drying temperature is 80-125 ℃, and the drying time is 1-18 h.
The action mechanism of the invention is as follows: in CaCl2-NH4Cl-NH3-H2In the O solution system, the sucrose and the ultrasonic wave prolong the induction period in the early stage of the preparation of the calcium carbonate, which is beneficial to quickly and uniformly forming calcium carbonate crystal nuclei, thereby reducing the particle size of calcium carbonate particles. At the same timeThe ultrasonic cavitation generates local high temperature and high pressure, which provides the required energy for the formation of crystal nucleus, so that the forming speed of the crystal nucleus can be increased by several orders of magnitude, when the ultrasonic power is larger (1500-1800W), the local high temperature caused by the ultrasonic cavitation dominates, along with the preparation of calcium carbonate, a large amount of tiny cavitation bubbles generated in the reaction by ultrasonic waves can form the flushing effect on the surface of calcium carbonate particles, and transient holes are generated on the surface of the generated calcium carbonate particles, so that the erosion effect is generated, the surface area of mass transfer contact is increased, the specific surface free energy of tiny crystal grains is reduced, the coalescence and the growth of the crystal nucleus are inhibited, calcium carbonate crystals can grow rapidly and uniformly, and the crystal density is reduced. And by compounding sucrose, the particle size of calcium carbonate crystals can be further reduced, and calcium carbonate crystal nuclei can be rapidly and uniformly formed. Because the surface energy of the nano calcium carbonate is high and the nano calcium carbonate is easy to agglomerate, the nano calcium carbonate is immediately filtered and dried after the reaction reaches 7.1, the agglomeration probability caused by mutual collision of the nano calcium carbonate during dissolution and recrystallization in an aging stage can be reduced, and meanwhile, a part of nano calcium carbonate aggregates generated can be screened out by sieving with a 250-mesh sieve, which is beneficial to ensuring the granularity and quality of products. Thus in CaCl2-NH4Cl-NH3-H2Under the system of O, the preparation of the nano calcium carbonate product is promoted under the synergistic action and the flow of the preparation process.
Compared with the prior art, the invention has the following beneficial effects:
1. The invention realizes the comprehensive utilization of the steel slag in CaCl2-NH4Cl-NH3-H2The O system can fix a large amount of carbon dioxide which is generated along with the steelmaking process, the ammonium chloride solution can be regenerated and recycled, and the prepared nano calcium carbonate has good shape, narrow particle size distribution, uniform appearance and good repeatability, and is easy for large-scale production.
2. The method has the characteristics of simple process, low cost, green and environment-friendly preparation process, short production period, simple process, resource saving, environmental friendliness and low cost, is simple and controllable in experimental operation process, is easy for industrial production, and has good application prospect.
3. The invention improves the resource utilization of the industrial steel slag to realize high added value, avoids environmental pollution and resource waste, and realizes a process approach of treating wastes with processes of wastes against one another and changing wastes into valuables. And put forward for the first time based on CaCl2-NH4Cl-NH3-H2The O system is used for preparing the nano calcium carbonate, and provides a new idea and a new choice for preparing the nano calcium carbonate.
drawings
FIG. 1 shows CaCl2-NH4Cl-NH3-H2The change curves of calcium content, pH value and conductivity in the reaction liquid along with the reaction time under the O system;
FIG. 2 is an SEM image of a crude product prepared by aging reaction in comparative examples 1-4; (a) comparative example 1; (b) comparative example 2; (c) comparative examples 3 and (d) comparative example 4;
FIG. 3 is a TEM image of nano calcium carbonate in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples. The calcium ion content in the solution in the following examples was determined by the EDTA titration method, which is a chinese national standard. The particle size of the calcium carbonate is detected by a laser particle size analyzer (German fly, analysis 22MicroTec plus) and a national standard particle size analysis-laser diffraction method, and the appearance of the prepared calcium carbonate is detected by a field emission electron microscope (FEI, Nova 400Nano, USA) and a telephoto electron microscope (JEOL, JEOL-JEM-1005, USA). The steel slag used in the following examples was calcium silicate as a main component.
Preparation method of nano calcium carbonate
In order to judge the end point of the carbonation reaction of the system, firstly, the CaCl leached based on the steel slag ammonium chloride under the action of ultrasonic waves is researched2-NH4Cl-NH3-H2The conductivity and pH value of the O system during the reaction change with the reaction time and the content of calcium ions, and the result is shown in FIG. 1.
As can be seen from FIG. 1, the conductivity of the reaction solution was substantially constant throughout the reaction, while the pH value decreased slowly, and began to decrease rapidly when the pH value was about 7.5, until the pH value was atThe balance is reached when the pH value is about 6.3, and the pH value of the system is reduced in an inverse S shape in the whole process. With conventional Ca (OH)2-H2compared with the bubbling method under the O system, the pH value and the conductivity of the system are obviously different along with the change of the reaction time. This is probably because the dissolution reaction of formula (1) occurs when the solution is charged with carbon dioxide, that is, carbon dioxide is dissolved in the aqueous solution, and the dissolved carbon dioxide reacts with water to release hydrogen ions, bicarbonate ions, and carbonate ions (formulas (2) and (3)), and the amount of calcium carbonate precipitates due to the reaction of carbonate ions with calcium ions decreases (formula (4)), so that formulas (2) and (3) move to the right of the equation, and the hydrogen ion content in the system increases and the pH decreases. Meanwhile, because the buffer balance of ammonium chloride and ammonia exists in the system, the continuously increased hydrogen ions enable the reaction (5) to move towards the right continuously, so that the pH value in the system is slowly reduced at the beginning, and after all the amino in the system is converted into ammonium ions, the continuously increased hydrogen ions enable the pH value of the system to be rapidly reduced. The final reaction equation for producing calcium carbonate by precipitation is shown in formula (6), and one divalent calcium ion is consumed while two monovalent hydrogen ions are produced. In addition, the hydrogen radical ion can react with ammonia (5) to form an ammonium radical ion, and the divalent calcium ion can also form a complex with ammonia, so that the electrical conductivity does not change much in the carbonation reaction that occurs in the system. Since the crystallization rate of calcium is already very high when the reaction is carried out to a pH of about 7 and the reaction system is maintained for a while if bubbling is stopped, the present invention fixes the reaction end point to a pH of about 7.1.
It can be seen that carbon dioxide is dissolved in an aqueous solution, and the dissolved carbon dioxide reacts with water to release hydrogen ions, bicarbonate ions and carbonate ions, which are in CaCl2-NH4Cl-NH3-H2In the O system, the hydrogen radical ions and ammonia and ammonium radical ions exist in balance, so that the solution system can rapidly absorb and contain more carbon dioxide to form high-concentration carbonate ions, and the conductivity and pH value of the system are equal to those of the conventional Ca (OH) due to the existence of ammonium chloride-ammonia buffer balance in the system2-H2Compared with calcium carbonate prepared by a bubbling method under an O system, the calcium carbonate prepared by the bubbling method has great difference, and the reaction mechanisms of the two preparation processes are completely different.
Example 1
1) Adding an ammonium chloride solution into the steel slag, and carrying out leaching reaction at 40-60 ℃ to obtain CaCl2-NH4Cl-NH3-H2Leachate of O system, wherein CaCl2Is 0.4mol/L, NH4Cl concentration of 1mol/L, NH4HO concentration of 0.8mol/L, standing overnight, standby.
2) Controlling the temperature of the leachate obtained in the step 1) to be 20 ℃, adding sucrose, wherein the adding amount of the sucrose is 2% of the mass of calcium chloride, introducing 45ml/min of carbon dioxide into the leachate, starting ultrasonic treatment with the power of 1620W, stopping the reaction when the pH value of the leachate is 7.1, immediately screening by using a 250-mesh screen, subsequently rinsing the filtered calcium carbonate by using absolute ethyl alcohol, and drying in a vacuum drying oven at 100 ℃ for 15 hours to obtain the product, namely the nano-scale calcium carbonate.
example 2
1) Adding ammonium chloride solution into the steel slag at 40-60 DEG CLeaching reaction to obtain CaCl2-NH4Cl-NH3-H2And (4) leaching solution of an O system. Wherein, CaCl2Is 0.4mol/L, NH4Cl concentration of 1mol/L, NH4HO concentration of 0.8mol/L, standing overnight, standby.
2) Controlling the temperature of the leachate obtained in the step 1) to be 20 ℃, adding sucrose, wherein the adding amount of the sucrose is 2% of the mass of calcium chloride, introducing 45ml/min of carbon dioxide into the leachate, starting ultrasonic treatment with the power of 1500W, stopping reaction when the pH value of the leachate is 7.1, immediately screening by using a 250-mesh screen, subsequently rinsing the filtered calcium carbonate by using absolute ethyl alcohol, and drying in a vacuum drying oven at 100 ℃ for 15h to obtain the product, namely the nano-scale calcium carbonate.
Example 3
1) Adding an ammonium chloride solution into the steel slag, and carrying out leaching reaction at 40-60 ℃ to obtain CaCl2-NH4Cl-NH3-H2Leachate of O system, wherein CaCl2Is 0.4mol/L, NH4Cl concentration of 1mol/L, NH4HO concentration of 0.8mol/L, standing overnight, standby.
2) Controlling the temperature of the leachate obtained in the step 1) to be 20 ℃, adding sucrose, wherein the adding amount of the sucrose is 2% of the mass of calcium chloride, introducing 45ml/min of carbon dioxide into the leachate, starting ultrasonic treatment with the power of 1800W, stopping the reaction when the pH value of the leachate is 7.1, immediately screening by using a 250-mesh screen, subsequently rinsing the filtered calcium carbonate by using absolute ethyl alcohol, and drying in a vacuum drying oven at 100 ℃ for 15 hours to obtain the product, namely the nano-scale calcium carbonate.
Comparative example 1
And (3) carrying out ageing reaction for 3 hours after the reaction is stopped without ultrasonic waves, then carrying out vacuum filtration, subsequently rinsing the filtered calcium carbonate with absolute ethyl alcohol, and drying, wherein other steps and parameters are the same as those in example 1.
Comparative example 2
The ultrasonic power is 540W, the aging reaction is carried out for 3h after the reaction is stopped, then the vacuum filtration is carried out, then the calcium carbonate after the filtration is rinsed by absolute ethyl alcohol and dried, and other steps and parameters are the same as those of the example 1.
Comparative example 3
The ultrasonic power is 1080W, the aging reaction is carried out for 3h after the reaction is stopped, then the vacuum filtration is carried out, then the calcium carbonate after the filtration is rinsed by absolute ethyl alcohol and dried, and other steps and parameters are the same as those of the example 1.
Comparative example 4
After the reaction was stopped, an aging reaction was carried out for 3 hours, followed by vacuum filtration, followed by rinsing the filtered calcium carbonate with anhydrous ethanol, and drying, and the other steps and parameters were the same as in example 1.
Secondly, product detection
1. Scanning electron microscope observation is carried out on the crude products prepared in comparative examples 1-4, and the result is shown in figure 2.
As can be seen from the figure, regardless of whether the ultrasonic treatment is carried out or not in the reaction process, after the aging reaction is carried out after the reaction is finished, the crystal grains of the product calcium carbonate are mutually agglomerated to form an aggregate, so that the particle is coarse. The particle size of the calcium carbonate particles is further reduced with the increase of the ultrasonic power, which is mainly due to the fact that a large number of nucleation sites are generated by high-power ultrasonic, and the interaction with the sucrose can delay the induction period of the reaction, so that the outline of the calcium carbonate particles is obvious, the agglomeration degree is further reduced, but the particle size of the calcium carbonate is still micron or submicron. In addition, because sound microflow and shock waves generated by ultrasonic waves have double effects of breaking crystal grains and increasing the collision probability among particles, when the ultrasonic power is too high (more than 1800W), the calcium carbonate particles have the tendency of not only not having the effect of refining the crystal grains but also becoming aggregates.
2. The product prepared in example 1 was observed under a transmission electron microscope, and the result is shown in fig. 3.
As can be seen from FIG. 3, the nano calcium carbonate obtained by the invention has uniform particle size distribution, regular appearance and spherical shape. Because the nano calcium carbonate has high surface energy and is easy to agglomerate, the nano calcium carbonate is immediately filtered and dried after the reaction reaches 7.1, the agglomeration probability caused by mutual collision of the nano calcium carbonate during dissolution and recrystallization in the aging stage can be reduced, and meanwhile, a part of the nano calcium carbonate can be screened out by a 250-mesh sieveThe nano calcium carbonate aggregate is produced, which is beneficial to ensuring the granularity and quality of the product. Thus in CaCl2-NH4Cl-NH3-H2Under the system of O, the preparation process of the invention is beneficial to the preparation of the nano calcium carbonate product under the synergistic effect and the flow.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The preparation method of the nano calcium carbonate is characterized by comprising the following steps:
1) Adding ammonium chloride solution into the steel slag for reaction to obtain CaCl2-NH4Cl-NH3-H2Standing the leaching solution of the O system overnight for later use;
2) adding cane sugar into the leachate obtained in the step 1), introducing carbon dioxide into the leachate, simultaneously starting ultrasonic waves with the power of 1500 ~ 1800W, stopping the reaction when the pH value of the leachate is 7.1, immediately screening by using a 250-mesh screen, and then rinsing the screened product by using absolute ethyl alcohol and drying in a vacuum drying oven to obtain the nano calcium carbonate.
2. The method for preparing nano calcium carbonate according to claim 1, wherein CaCl in the leaching solution is2Is 0.4mol/L, NH4Cl concentration of 1mol/L, NH4The concentration of HO was 0.8 mol/L.
3. The method for preparing nano calcium carbonate according to claim 1, wherein the reaction temperature in the step 1) is 40 ~ 60 ℃.
4. The method for preparing nano calcium carbonate according to claim 1, wherein the temperature of the leachate in the step 2) is 15 ~ 25 ℃ during the reaction.
5. The method for preparing nano calcium carbonate according to claim 1, wherein the amount of the sucrose added is 2% of the mass of the calcium chloride in the leachate.
6. The method for preparing nano calcium carbonate according to claim 1, wherein the flow rate of the carbon dioxide is 45 ml/min.
7. The method for preparing nano calcium carbonate according to claim 1, wherein the drying temperature is 80 ~ 125 ℃ and the drying time is 1 ~ 18 h.
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