CN114684840A - Method for preparing nano rod-shaped calcium carbonate by self-induction of impurities - Google Patents
Method for preparing nano rod-shaped calcium carbonate by self-induction of impurities Download PDFInfo
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- CN114684840A CN114684840A CN202210340770.5A CN202210340770A CN114684840A CN 114684840 A CN114684840 A CN 114684840A CN 202210340770 A CN202210340770 A CN 202210340770A CN 114684840 A CN114684840 A CN 114684840A
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 170
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000012535 impurity Substances 0.000 title claims abstract description 29
- 239000002893 slag Substances 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 14
- 238000003763 carbonization Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 9
- 239000002910 solid waste Substances 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 239000000945 filler Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000007796 conventional method Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000005997 Calcium carbide Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- 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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention belongs to the technical field of functional material preparation, and provides a method for preparing nano rod-shaped calcium carbonate by impurity self-induction, aiming at solving the problems of complex process and high cost caused by impurity removal of carbide slag and addition of a crystal form control agent in the conventional method for preparing rod-shaped nano calcium carbonate by using carbide slag. Directly uses the self-induction of impurities in the carbide slag to directly mix the carbide slag and CO2And carrying out gas-liquid-solid three-phase continuous reaction to prepare the nano calcium carbonate with a rod-shaped crystal form. The method can consume 0.58 ton of CO for treating 1 ton of carbide slag2And generating 1.5 tons of rod-shaped nano calcium carbonate. Because of the influence of ferric oxide impurities in the carbide slag, the induced product is self-assembled into a rod-shaped crystal form, can be used as a paper making filler and a paper coating material, has simple production process and lower production cost, and can realize industrial production. The invention consumes a large amount of industrial solid wastes such as carbide slag and the like, reduces the cost of raw materials, protects the ecological environment and realizes solidificationAnd comprehensively utilizing waste resources.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a method for preparing nano rod-shaped calcium carbonate by self-induction of impurities.
Background
The carbide slag is calcium carbide and waterThe waste residue of acetylene gas is prepared by reaction, and about 1.5 tons of carbide slag are generated by one ton of carbide. The carbide slag has low water content, small particle size and higher reactivity, is strongly alkaline after being dissolved in water (pH is more than 12), can cause salinization of land by random stacking, pollutes underground water, causes flying dust and the like, and threatens environmental safety and human health. In the presence of CO2In the storage and utilization technique of (1), CO2Mineralization is also considered to be one of the most potential directions. The nano calcium carbonate has high thermodynamic stability and high mechanical strength, and is an important inorganic non-metallic material. Compared with heavy calcium carbonate and light calcium carbonate, the rod-shaped nano calcium carbonate can be used as a filler in paper, rubber and plastics to enhance the strength and toughness of the paper, the rubber and the plastics.
In recent years, researchers at home and abroad have made a great deal of research on the preparation of the rod-shaped nano calcium carbonate. For example, the Chinese patent CN101570344A discloses a method for preparing aragonite crystal form calcium carbonate, which is to digest lime and water and then perform slaking treatment, and prepare rodlike calcium carbonate with the grain diameter of 1-2 um by taking needle-shaped magnesium hydroxide crystals as seed crystals. In the invention, the slaking time after lime and water are slaked is long, the process is complex, and the production cost is high. Chinese patent CN106517285B discloses a method for preparing rod-like nano calcium carbonate, which comprises mixing lime with hot water, grinding, removing residue to obtain calcium hydroxide emulsion, adding crystal form control agent, and mixing with CO2Reacting in a reaction tower to finally obtain the rod-shaped nano calcium carbonate. The process is complicated and tedious, and additionally uses additives, so that the cost is increased.
Therefore, the research and development of the technology for exploring simpler process and the rodlike nano calcium carbonate with lower cost and higher quality have good economic and social benefits.
Disclosure of Invention
The invention provides a method for preparing nano rodlike calcium carbonate by impurity self-induction, aiming at overcoming the problems of complex process and high cost caused by impurity removal of carbide slag and addition of a crystal form control agent in the prior method for preparing rodlike nano calcium carbonate by using carbide slag, and the method does not need to add other additives, prepares rodlike nano calcium carbonate by researching the induction of ferric oxide impurities in the carbide slag on products, and has simple process and high economic benefit; not only solves the problem of environmental pollution caused by accumulation of solid wastes, realizes comprehensive utilization of solid waste resources, but also obtains the rod-shaped nano calcium carbonate with high practical value.
The invention is realized by the following technical scheme: a method for preparing nanometer rod-shaped calcium carbonate by self-induction of impurities utilizes self-induction of impurities in carbide slag to directly mix carbide slag and CO2And carrying out gas-liquid-solid three-phase continuous reaction to prepare the nano calcium carbonate with a rod-shaped crystal form.
The method comprises the following specific steps:
(1) preparing carbide slag slurry: sieving the carbide slag with a 200-mesh sieve to obtain powder; adding distilled water according to the solid-to-liquid ratio of 1-10:100, and stirring for 10min to uniformly disperse the distilled water to obtain carbide slag slurry;
(2) and (3) carbonization reaction: introducing CO into the carbide slag slurry obtained in the step (1) while stirring2，CO2The flow rate of the stirring device is 200-500 mL/min, and the stirring speed range is 400-800 rpm/min; measuring pH with pH meter in the whole course of reaction, and stopping CO when pH of carbonization reaction reaches 6.5-7.52Stopping stirring with gas, and finishing the reaction to obtain a calcium carbonate suspension;
(3) and (3) standing, filtering and drying the calcium carbonate suspension obtained in the step (2) to obtain a rod-shaped nano calcium carbonate product.
The solid-to-liquid ratio in the step (1) is 1:100, 3:100, 5:100, 7:100 or 10: 100.
CO in the carbonation reaction process in the step (2)2The flow rate of (A) is 200, 300 or 500 mL/min; in the carbonization reaction process, the material mixing time is controlled for 10 minutes, and the stirring speed is 400-600 rpm/min.
The carbide slag is waste slag generated in the preparation of acetylene gas through the reaction of carbide and water, has low water content, small particle size and higher reactivity, is strongly alkaline after being dissolved in water (pH is greater than 12), can cause salinization of land, pollutes underground water, causes dust emission and the like, and threatens environmental safety and human health. In CO2In the storage and utilization technique of (1), CO2Mineralization is also considered to be one of the most prominentThe direction of the potential.
The invention directly uses the self-induction of impurities in the carbide slag slurry to prepare the rod-shaped nano calcium carbonate, and the method can consume 0.58 ton of CO when used for treating 1 ton of carbide slag2And generating 1.5 tons of rod-shaped nano calcium carbonate. On one hand, the purposes of simplifying the process and reducing the cost are achieved, and the Fe element is utilized to induce the granular calcium carbonate to be assembled into a rod-shaped structure, thereby providing a new way for preparing the rod-shaped nano calcium carbonate. On the other hand, a large amount of industrial solid wastes such as carbide slag and the like are consumed, the raw material cost is reduced, the comprehensive utilization of solid waste resources and CO are realized2The discharge reduction is realized, and the rodlike nano calcium carbonate with high practical value is obtained.
Compared with the prior art, the invention has the advantages and beneficial effects that: the rod-shaped nano calcium carbonate is mainly prepared from industrial solid waste-carbide slag, reduces the cost of raw materials, and embodies ecological environmental protection and comprehensive utilization of solid waste resources.
According to the invention, no crystal form control agent is additionally added in the process, the crystal form of the nano calcium carbonate can be controlled by utilizing the self-induction of the iron oxide impurities in the carbide slag, the production cost is low, the product stability is good, and the nano calcium carbonate can be used for plastic fillers and papermaking fillers. The invention has the advantages of gas-liquid-solid one-step mineralization reaction, simple process and stable performance, and is suitable for large-scale production.
Drawings
FIG. 1 is an SEM representation of the rod-like nano calcium carbonate product obtained in step (3) of example 1;
FIG. 2 is an SEM representation of rod-like nano calcium carbonate after stirring at a stirring speed of 800 r/min for 10min and ultrasonic processing for 30min in step (4) of example 1;
FIG. 3 is an SEM representation of the rod-shaped nano calcium carbonate obtained in example 2;
FIG. 4 is an SEM representation of the rod-like nano calcium carbonate obtained in example 3;
FIG. 5 is a TEM representation of the rodlike nano-calcium carbonate obtained in example 3;
FIG. 6 is an SEM representation of the lamellar calcium carbonate obtained in example 4;
FIG. 7 is an SEM representation of the granular nano calcium carbonate obtained in example 5;
FIG. 8 is an SEM representation of nano calcium carbonate prepared in example 6 without the addition of iron oxide impurities;
FIG. 9 is an SEM representation of the nano calcium carbonate rods prepared in example 6 with the addition of iron oxide impurities.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs and the disclosures and references cited herein and the materials to which they refer are incorporated by reference.
Those skilled in the art will recognize that equivalents to the specific embodiments described, as may be learned by routine experimentation, are intended to be encompassed by the present application.
The experimental procedures in the following examples are conventional unless otherwise specified. The instruments used in the following examples are, unless otherwise specified, laboratory-standard instruments; the experimental materials used in the following examples were purchased from a conventional biochemical reagent store unless otherwise specified.
Example 1: a method for preparing rod-shaped calcium carbonate by self-induction of impurities comprises the following steps:
(1) and sieving the carbide slag with a 200-mesh sieve to obtain powder. Accurately weighing the powder according to the solid-liquid ratio of 10:100, placing the powder in a beaker, adding distilled water, and stirring for ten minutes to uniformly disperse the powder to obtain the carbide slag slurry.
(2) Introducing CO into the carbide slag slurry obtained in the step (1) while stirring2，CO2The flow rate of (2) was 200 mL/min, and the stirring speed was 400 rpm/min. Full range measurement with pH meterMeasuring the pH value in the reaction process, and closing CO when the pH value of the carbonization reaction reaches about 72Stopping stirring by gas, and finishing the reaction to obtain the calcium carbonate suspension.
(3) And (3) standing, filtering and drying the calcium carbonate suspension obtained in the step (2) to obtain a rod-shaped nano calcium carbonate product.
(4) And (4) re-dissolving the rodlike nano calcium carbonate obtained in the step (3) in water, stirring at a stirring speed of 800 r/min for 10min, then dispersing by using ultrasonic waves for 30min, and standing, filtering and drying to obtain the treated rodlike nano calcium carbonate.
In this embodiment, the calcium carbonate product obtained in step (3) is detected by a scanning electron microscope and a transmission electron microscope, and the detection result is shown in fig. 1. It can be seen from the figure that the nano calcium carbonate is in a rod-shaped structure and has uniform particle size distribution. And (5) performing scanning electron microscope detection on the calcium carbonate product subjected to stirring and ultrasonic treatment in the step (4), wherein the detection result is shown in figure 2. It can be seen from the figure that the nano calcium carbonate has stable structure and still presents a rod-like structure.
Example 2: a method for preparing rod-shaped calcium carbonate by impurity self-induction comprises the following steps: stirring the carbide slag slurry and introducing CO2The stirring speed was 500 rpm/min. When the pH value of the carbonization reaction reaches about 7, CO is closed2Stopping stirring by gas, and finishing the reaction to obtain the calcium carbonate suspension. The other methods were the same as those described in example 1.
The calcium carbonate product obtained in this example is detected by a scanning electron microscope, and the detection result is shown in fig. 3. It can be seen from the figure that the nano calcium carbonate is in a rod-shaped structure and has uniform particle size distribution.
Example 3: a method for preparing rod-shaped calcium carbonate by impurity self-induction comprises the following steps: stirring the carbide slag slurry and introducing CO2The stirring speed was 600 rpm/min. When the pH value of the carbonization reaction reaches about 7, CO is closed2Stopping stirring by gas, and finishing the reaction to obtain the calcium carbonate suspension. The other methods were the same as those described in example 1.
The calcium carbonate product obtained in this example was detected by a scanning electron microscope and a transmission electron microscope, and the detection results are shown in fig. 4 and 5. It can be seen from the figure that the nano calcium carbonate is in a rod-shaped structure and has uniform particle size distribution.
Example 4: a method for preparing rod-shaped calcium carbonate by self-induction of impurities comprises the following steps: and (3) mixing the solid-liquid ratio of 1:100 carbide slag slurry is stirred while introducing CO2The stirring speed was 600 rpm/min. When the pH value of the carbonization reaction reaches about 7, CO is closed2Stopping stirring by gas, and finishing the reaction to obtain the calcium carbonate suspension. The other methods were the same as those described in example 1.
The calcium carbonate product obtained in this example was detected by a scanning electron microscope, and the detection result is shown in fig. 6. It can be seen from the figure that calcium carbonate is in lamellar and blocky structures, and the particle size distribution is not uniform.
Example 5: a method for preparing rod-shaped calcium carbonate by self-induction of impurities comprises the following steps: and (3) setting the solid-liquid ratio as 5:100 carbide slag slurry is stirred while introducing CO2The stirring speed was 600 rpm/min. When the pH value of the carbonization reaction reaches about 7, CO is closed2Stopping stirring by gas, and finishing the reaction to obtain the calcium carbonate suspension. The other methods were the same as those described in example 1.
The calcium carbonate product obtained in this example was detected by scanning electron microscopy, and the detection result is shown in fig. 7. It can be seen from the figure that the nano calcium carbonate is in the form of small particles and lamellar, the particle size distribution is not uniform, and the appearance is uncontrollable.
Example 6: a method for preparing rod-shaped calcium carbonate by self-induction of impurities comprises the following steps: preparing two parts of solid-liquid ratio of 10:100 Ca (OH)2A certain amount of iron oxide is added into one part of the slurry, and the stirring speed is 600 rpm/min. When the pH value of the carbonization reaction reaches about 7, CO is closed2Stopping stirring by gas, and finishing the reaction to obtain the calcium carbonate suspension. The other methods were the same as those described in example 1.
The calcium carbonate product obtained in this example was detected by a scanning electron microscope, and the detection results are shown in fig. 8 and 9. As can be seen from the figure, the nano calcium carbonate without the ferric oxide is in a small granular shape, the nano calcium carbonate with the ferric oxide impurity is in a rod-shaped structure, the grain size distribution is uniform, and the appearance is controllable.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A method for preparing nano rod-shaped calcium carbonate by self-induction of impurities is characterized by comprising the following steps: directly uses the self-induction of impurities in the carbide slag to directly mix the carbide slag and CO2And carrying out gas-liquid-solid three-phase continuous reaction to prepare the nano calcium carbonate with a rod-shaped crystal form.
2. The method for preparing nano rod-shaped calcium carbonate by impurity self-induction according to claim 1, which is characterized in that: the method comprises the following specific steps:
(1) preparing carbide slag slurry: sieving the carbide slag with a 200-mesh sieve to obtain powder; adding distilled water according to the solid-to-liquid ratio of 1-10:100, and stirring for 10min to uniformly disperse the distilled water to obtain carbide slag slurry;
(2) and (3) carbonization reaction: introducing CO into the carbide slag slurry obtained in the step (1) while stirring2，CO2The flow rate of the stirring device is 200-500 mL/min, and the stirring speed range is 400-800 rpm/min; measuring pH with pH meter in the whole course of reaction, and stopping CO when pH of carbonization reaction reaches 6.5-7.52Stopping stirring with gas, and finishing the reaction to obtain a calcium carbonate suspension;
(3) and (3) standing, filtering and drying the calcium carbonate suspension obtained in the step (2) to obtain a rod-shaped nano calcium carbonate product.
3. The method for preparing nano rod-shaped calcium carbonate by impurity self-induction according to claim 2, which is characterized in that: and (4) re-dissolving the rodlike nano calcium carbonate obtained in the step (3) in water, stirring at a stirring speed of 800 r/min for 10min, then dispersing by using ultrasonic waves for 30min, and standing, filtering and drying to obtain the treated rodlike nano calcium carbonate.
4. The method for preparing nano rod-shaped calcium carbonate by impurity self-induction according to claim 2, which is characterized in that: the solid-to-liquid ratio in the step (1) is 1:100, 3:100, 5:100, 7:100 or 10: 100.
5. The method for preparing nano rod-shaped calcium carbonate by impurity self-induction according to claim 2, which is characterized in that: CO in the carbonation reaction process in the step (2)2The flow rate of (A) is 200, 300 or 500 mL/min; in the carbonization reaction process, the material mixing time is controlled for 10 minutes, and the stirring speed is 400-600 rpm/min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738997A (en) * | 2013-12-17 | 2014-04-23 | 柳州东风化工股份有限公司 | Method for preparing nano calcium carbonate by taking carbide slag as raw material |
| CN106517285A (en) * | 2016-11-21 | 2017-03-22 | 广西华纳新材料科技有限公司 | Method for preparing bar-shaped nanometer calcium carbonate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738997A (en) * | 2013-12-17 | 2014-04-23 | 柳州东风化工股份有限公司 | Method for preparing nano calcium carbonate by taking carbide slag as raw material |
| CN106517285A (en) * | 2016-11-21 | 2017-03-22 | 广西华纳新材料科技有限公司 | Method for preparing bar-shaped nanometer calcium carbonate |
Non-Patent Citations (2)
| Title |
|---|
| ONIMISI A. JIMOH等: "Utilization of milk of lime(MOL) originated from carbide lime waste and operating parameters optimization study for potential precipitated calcium carbonate(PCC) production", 《ENVIRON EARTH SCI》 * |
| 曹春霞等: "电石渣及二氧化碳资源化利用现状与展望", 《化工矿物与加工》 * |
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