CN116692916A - Method for efficiently preparing high-activity nano calcium carbonate suspension - Google Patents
Method for efficiently preparing high-activity nano calcium carbonate suspension Download PDFInfo
- Publication number
- CN116692916A CN116692916A CN202310913762.XA CN202310913762A CN116692916A CN 116692916 A CN116692916 A CN 116692916A CN 202310913762 A CN202310913762 A CN 202310913762A CN 116692916 A CN116692916 A CN 116692916A
- Authority
- CN
- China
- Prior art keywords
- calcium carbonate
- nano calcium
- reaction
- activity
- carbon dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 254
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 127
- 239000000725 suspension Substances 0.000 title claims abstract description 62
- 230000000694 effects Effects 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 35
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 120
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000292 calcium oxide Substances 0.000 claims abstract description 75
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 60
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 230000007613 environmental effect Effects 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 35
- 239000007789 gas Substances 0.000 claims description 29
- 239000002440 industrial waste Substances 0.000 claims description 28
- 238000001914 filtration Methods 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000002912 waste gas Substances 0.000 claims description 15
- 239000011148 porous material Substances 0.000 claims description 13
- 238000011084 recovery Methods 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000000354 decomposition reaction Methods 0.000 claims description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000005265 energy consumption Methods 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 238000010669 acid-base reaction Methods 0.000 claims description 3
- 239000004568 cement Substances 0.000 claims description 3
- 238000012824 chemical production Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000003546 flue gas Substances 0.000 claims description 3
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 claims description 3
- 238000011069 regeneration method Methods 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 3
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to the technical field of preparation of calcium carbonate suspension, in particular to a method for efficiently preparing high-activity nano calcium carbonate suspension, which comprises the following steps: adding calcium oxide with purity higher than 99.9% into a reaction container, and stirring at room temperature to make the calcium oxide fully uniform; adding carbon dioxide with purity higher than 99.9% into another reaction container, and decomposing the carbon dioxide into elemental carbon and oxygen; reacting the elemental carbon and oxygen obtained in the second step with the calcium oxide in the first step to generate nano calcium carbonate; stirring the nano calcium carbonate under ultrasonic equipment to enhance the activity, and adding a proper amount of distilled water after the reaction is finished to generate nano calcium carbonate suspension. The invention provides a method for preparing high-activity nano calcium carbonate suspension with high efficiency, environmental protection and economy, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of preparation of calcium carbonate suspension, in particular to a method for efficiently preparing high-activity nano calcium carbonate suspension.
Background
Nano calcium carbonate is a commonly used inorganic nano material, and is widely applied to various fields of paint, plastic, paper, rubber, ink, medicine, food and the like due to the special physical and chemical properties. However, the conventional nano calcium carbonate preparation method has some problems such as severe reaction conditions, low reaction efficiency, low product activity, negative influence on the environment and the like. Therefore, it is urgent to develop a method capable of preparing high-activity nano calcium carbonate under mild conditions.
In the prior art, complicated equipment is usually required for preparing nano calcium carbonate, and the reaction conditions are severe, such as high temperature, high pressure and the like, which not only lead to high equipment cost and high operation difficulty, but also can have negative influence on the environment. In addition, the nano calcium carbonate obtained by the traditional method is not high in activity, and the application performance is required to be improved. Moreover, conventional methods often fail to achieve precise control of the particle size and shape of nano calcium carbonate, which limits its application in certain fields.
In addition, existing nano calcium carbonate preparation methods mostly use commercial chemicals such as calcium oxide and carbon dioxide as raw materials. However, the production of these commercial chemicals is often accompanied by the emission of large amounts of industrial waste gases, such as carbon dioxide, sulfur oxides, etc., which cause serious environmental pollution. Therefore, how to use the compounds in the industrial waste gas, such as carbon dioxide and calcium oxide, to prepare high-activity nano calcium carbonate becomes an important research direction.
In summary, the existing nano calcium carbonate preparation method has a plurality of defects, and a new preparation method needs to be found to improve the reaction efficiency and the product activity, reduce the influence on the environment and reduce the production cost.
Disclosure of Invention
Based on the above purpose, the invention provides a method for efficiently preparing high-activity nano calcium carbonate suspension.
A method for efficiently preparing high-activity nano calcium carbonate suspension comprises the following steps:
step one: adding calcium oxide with purity higher than 99.9% into a reaction container, and stirring at room temperature to make the calcium oxide fully uniform;
step two: adding carbon dioxide with purity higher than 99.9% into another reaction container, and decomposing the carbon dioxide into elemental carbon and oxygen;
step three: reacting the elemental carbon and oxygen obtained in the second step with the calcium oxide in the first step to generate nano calcium carbonate;
step four: stirring the nano calcium carbonate under ultrasonic equipment to enhance the activity of the nano calcium carbonate;
step five: after the reaction is finished, adding a proper amount of distilled water to generate nano calcium carbonate suspension.
The method can rapidly prepare the high-activity nano calcium carbonate suspension in a short time, not only improves the yield, but also greatly reduces the energy consumption, and has higher practicability and industrial application value.
Further, the stirring time in the first step is 5-10 minutes, the stirring speed is 500-1000 rpm, and the uniformity of the calcium oxide is ensured.
Further, the decomposition of the carbon dioxide in the second step is carried out by adopting ultrasonic equipment with the ultrasonic frequency of 20-40kHz and the power of 100-200W.
Further, the specific reaction steps of the step three are as follows:
placing the calcium oxide obtained in the first step into a reaction container provided with a heating device, starting the heating device, and heating the calcium oxide to a preset reaction temperature, wherein the reaction temperature is 80-120 ℃ and the reaction time is 2-4 hours;
simultaneously, the elemental carbon and oxygen obtained by decomposition in the second step are slowly introduced into a reaction vessel containing calcium oxide through an inlet with adjustable flow, so that the elemental carbon and oxygen are fully contacted and mixed with the calcium oxide;
in the reaction process, the ultrasonic equipment is turned on, and the reactant is stirred and heated by ultrasonic waves so as to ensure that the reaction is fully carried out and the activity of the generated nano calcium carbonate particles is improved;
monitoring the reaction process, and detecting the pH value, color and concentration indexes of the reaction solution by an analytical instrument when the reaction of calcium oxide, elemental carbon and oxygen tends to be completed, so as to confirm that the reaction is completed;
after the reaction is completed, the heating device and the ultrasonic equipment are closed, and the mixture in the reaction vessel is cooled to room temperature, so that the mixture containing the high-activity nano calcium carbonate is obtained.
The steps can ensure the smooth progress of the reaction, the produced nano calcium carbonate has high activity, and the particle size can be controlled by adjusting the reaction conditions, which is of great significance for the subsequent application.
Further, the distilled water in the fifth step is added in an amount which is 2 to 5 times the volume of the nano calcium carbonate.
Further, the nano calcium carbonate suspension in the fifth step is purified through steps of filtering, washing and drying, and the method specifically comprises the following steps:
and (3) filtering: filtering the nano calcium carbonate suspension by using a filter with proper pore size, filtering out large particle impurities, unreacted calcium oxide and the like in the suspension, and obtaining nano calcium carbonate suspension with uniform particle size after filtering, wherein the pore size of the filter is 0.2-0.8 microns;
washing: washing the filtered nano calcium carbonate suspension by using distilled water to remove impurities or residual reactants, and ensuring that the nano calcium carbonate is fully contacted and mixed with a washing solution by stirring and oscillating in the washing process, so that the washing effect is improved;
and (3) drying: the washed nano calcium carbonate suspension removes redundant water through a drying step, and can be subjected to vacuum drying, freeze drying or spray drying, and the obtained nano calcium carbonate particles have higher purity after drying, so that the nano calcium carbonate particles are convenient for subsequent storage and use;
through the steps, the purity of the nano calcium carbonate suspension can be effectively improved, and the activity and application performance of the nano calcium carbonate are improved.
Furthermore, the calcium oxide and the carbon dioxide are recovered from the industrial waste gas, so that the production cost is reduced, the environment is protected, and the specific recovery steps comprise:
and (3) collecting industrial waste gas: firstly, collecting industrial waste gas containing calcium oxide and carbon dioxide, wherein the industrial waste gas comprises cement production, chemical production and electric power production, and the flue gas contains a large amount of carbon dioxide and partial calcium oxide;
pretreatment of waste gas: pretreating the collected industrial waste gas, wherein the pretreatment comprises cooling and dust removal so as to reduce dust and moisture in the waste gas;
and (3) carbon dioxide recovery: the pretreated industrial waste gas passes through an absorption tower, carbon dioxide in the waste gas is absorbed by sodium hydroxide solution, the carbon dioxide is converted into bicarbonate which can be dissolved in water through reaction, and then the bicarbonate is converted into carbon dioxide and water through a regeneration step, and the carbon dioxide with high purity is separated;
and (3) calcium oxide recovery: the calcium oxide in the waste gas generally exists in the form of particles, is separated from the waste gas through filtration and sedimentation, and is further purified through a chemical method (such as acid-base reaction) if the purity of the calcium oxide does not reach the standard;
through the steps, calcium oxide and carbon dioxide in industrial waste gas can be effectively recovered, so that the production cost is reduced, and the environmental protection is contributed.
Further, the surfactant is added in each step to improve the dispersibility of the nano calcium carbonate.
Further, the decomposition in the second step is performed by electrochemical, pyrolysis or photocatalysis, so as to improve the efficiency of the reaction and the purity of the product.
Further, the particle size of the nano calcium carbonate suspension is 10nm-100nm, and the particle shape of the nano calcium carbonate suspension comprises a sphere, a flake and a rod.
The invention has the beneficial effects that:
1. the method of the invention takes calcium oxide and carbon dioxide as raw materials, prepares the high-activity nano calcium carbonate suspension by a solution method, has mild reaction conditions, is simple and convenient to operate, is easy to realize large-scale production, and can obviously improve the reaction efficiency and the product activity.
2. The method can realize the precise control of the particle size and shape of the nano calcium carbonate, thereby meeting the application requirements of different fields, for example, the nano calcium carbonate with the particle size of 10nm-100nm and the particle shape of sphere, sheet, bar and the like can be prepared by adjusting the reaction conditions.
3. The method can realize the effective recovery and utilization of calcium oxide and carbon dioxide in the industrial waste gas, and convert the industrial waste gas into valuable products, thereby reducing the production cost and reducing the influence on the environment.
4. The method adopts proper steps of filtering, washing, drying and the like to purify the nano calcium carbonate suspension, improves the purity of the nano calcium carbonate, and improves the application performance of the nano calcium carbonate in the fields of paint, plastics, paper, rubber, ink, medicine, food and the like.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a preparation method according to an embodiment of the invention;
FIG. 2 is a schematic diagram of a purification step according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of exhaust gas recovery according to an embodiment of the present invention.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
As shown in fig. 1-3, a method for efficiently preparing a high-activity nano calcium carbonate suspension comprises the following steps:
step one: adding calcium oxide with purity higher than 99.9% into a reaction container, and stirring at room temperature to make the calcium oxide fully uniform;
step two: adding carbon dioxide with purity higher than 99.9% into another reaction container, and decomposing the carbon dioxide into elemental carbon and oxygen;
step three: reacting the elemental carbon and oxygen obtained in the second step with the calcium oxide in the first step to generate nano calcium carbonate;
step four: stirring the nano calcium carbonate under ultrasonic equipment to enhance the activity of the nano calcium carbonate;
step five: after the reaction is finished, adding a proper amount of distilled water to generate nano calcium carbonate suspension.
The method can rapidly prepare the high-activity nano calcium carbonate suspension in a short time, not only improves the yield, but also greatly reduces the energy consumption, and has higher practicability and industrial application value.
The stirring time of the first step is 5-10 minutes, the stirring speed is 500-1000 rpm, and the uniformity of the calcium oxide is ensured.
In the second step, the decomposition of carbon dioxide is carried out by adopting ultrasonic equipment with the ultrasonic frequency of 20-40kHz and the power of 100-200W.
The third specific reaction steps are as follows:
placing the calcium oxide obtained in the first step into a reaction container provided with a heating device, starting the heating device, and heating the calcium oxide to a preset reaction temperature, wherein the reaction temperature is 80-120 ℃ and the reaction time is 2-4 hours;
simultaneously, the elemental carbon and oxygen obtained by decomposition in the second step are slowly introduced into a reaction vessel containing calcium oxide through an inlet with adjustable flow, so that the elemental carbon and oxygen are fully contacted and mixed with the calcium oxide;
in the reaction process, the ultrasonic equipment is turned on, and the reactant is stirred and heated by ultrasonic waves so as to ensure that the reaction is fully carried out and the activity of the generated nano calcium carbonate particles is improved;
monitoring the reaction process, and detecting the pH value, color and concentration indexes of the reaction solution by an analytical instrument when the reaction of calcium oxide, elemental carbon and oxygen tends to be completed, so as to confirm that the reaction is completed;
after the reaction is completed, the heating device and the ultrasonic equipment are closed, and the mixture in the reaction vessel is cooled to room temperature, so that the mixture containing the high-activity nano calcium carbonate is obtained.
The steps can ensure the smooth progress of the reaction, the produced nano calcium carbonate has high activity, and the particle size can be controlled by adjusting the reaction conditions, which is of great significance for the subsequent application.
And step five, the adding amount of distilled water is 2-5 times of the volume of the nano calcium carbonate.
The nano calcium carbonate suspension in the fifth step is purified by the steps of filtering, washing and drying, and the method comprises the following steps:
and (3) filtering: filtering the nano calcium carbonate suspension by using a filter with proper pore diameter, filtering out large particle impurities, unreacted calcium oxide and the like in the suspension, and obtaining the nano calcium carbonate suspension with uniform particle size after filtering, wherein the pore diameter of the filter is 0.2-0.8 microns;
washing: washing the filtered nano calcium carbonate suspension by using distilled water to remove impurities or residual reactants, and ensuring that the nano calcium carbonate is fully contacted and mixed with a washing solution by stirring and oscillating in the washing process, so that the washing effect is improved;
and (3) drying: the washed nano calcium carbonate suspension removes redundant water through a drying step, and can be subjected to vacuum drying, freeze drying or spray drying, and the obtained nano calcium carbonate particles have higher purity after drying, so that the nano calcium carbonate particles are convenient for subsequent storage and use;
through the steps, the purity of the nano calcium carbonate suspension can be effectively improved, and the activity and application performance of the nano calcium carbonate are improved.
The calcium oxide and the carbon dioxide are recovered from the industrial waste gas, so that the production cost is reduced, the environment is protected, and the specific recovery steps comprise:
and (3) collecting industrial waste gas: firstly, collecting industrial waste gas containing calcium oxide and carbon dioxide, wherein the industrial waste gas comprises cement production, chemical production and electric power production, and the flue gas contains a large amount of carbon dioxide and partial calcium oxide;
pretreatment of waste gas: pretreating the collected industrial waste gas, wherein the pretreatment comprises cooling and dust removal so as to reduce dust and moisture in the waste gas;
and (3) carbon dioxide recovery: the pretreated industrial waste gas passes through an absorption tower, carbon dioxide in the waste gas is absorbed by sodium hydroxide solution, the carbon dioxide is converted into bicarbonate which can be dissolved in water through reaction, and then the bicarbonate is converted into carbon dioxide and water through a regeneration step, and the carbon dioxide with high purity is separated;
and (3) calcium oxide recovery: the calcium oxide in the waste gas generally exists in the form of particles, is separated from the waste gas through filtration and sedimentation, and is further purified through a chemical method (such as acid-base reaction) if the purity of the calcium oxide does not reach the standard;
through the steps, calcium oxide and carbon dioxide in industrial waste gas can be effectively recovered, so that the production cost is reduced, and the environmental protection is contributed.
The surfactant is added in each step to improve the dispersibility of the nano calcium carbonate.
The decomposition in the second step is performed by electrochemical, thermal pyrolysis or photocatalysis to improve the efficiency of the reaction and the purity of the product.
The particle size of the nano calcium carbonate suspension is 10nm-100nm, and the particle shape of the nano calcium carbonate suspension comprises a sphere, a flake and a rod.
The following describes the embodiments of the present invention in further detail with reference to specific examples, but is not intended to limit the scope of the present invention:
example 1:
first, a 0.1M solution of calcium oxide was reacted with a 0.1M solution of carbon dioxide at a temperature of 30℃and a pressure of 1atm to obtain a nano calcium carbonate suspension. In the reaction process, calcium oxide and carbon dioxide react according to a molar ratio of 1:1. The reaction time was 2 hours. Then, the nano calcium carbonate solid was obtained by filtration through a filter having a pore size of 0.5 μm, and then purified by washing and drying steps. Finally, the high-activity nano calcium carbonate is obtained by heat treatment at 300 ℃ for 1 hour.
Example 2:
the 0.1M solution of calcium oxide and the 0.1M solution of carbon dioxide are reacted at a temperature of 50 ℃ and a pressure of 1atm to obtain a nano calcium carbonate suspension. In the reaction process, calcium oxide and carbon dioxide react according to a molar ratio of 1:1. The reaction time was 3 hours. Then, the nano calcium carbonate solid was obtained by filtration through a filter having a pore size of 0.6 μm, and then purified by washing and drying steps. Finally, the high-activity nano calcium carbonate is obtained by heat treatment for 1.5 hours at 350 ℃.
Example 3:
and (3) collecting calcium oxide and carbon dioxide in the industrial waste gas, and obtaining a calcium oxide and carbon dioxide solution through pretreatment and absorption reaction. Then, the two solutions were reacted at a temperature of 40 ℃ and a pressure of 1atm to obtain a nano calcium carbonate suspension. In the reaction process, calcium oxide and carbon dioxide react according to a molar ratio of 1:1. The reaction time was 2.5 hours. Then, the nano calcium carbonate solid was obtained by filtration through a filter having a pore size of 0.7 μm, and then purified by washing and drying steps. Finally, the high-activity nano calcium carbonate is obtained by heat treatment at 320 ℃ for 1 hour.
Example 4:
and (3) collecting calcium oxide and carbon dioxide in the industrial waste gas, and obtaining a calcium oxide and carbon dioxide solution through pretreatment and absorption reaction. Then, the two solutions were reacted at a temperature of 60 ℃ and a pressure of 1atm to obtain a nano calcium carbonate suspension. In the reaction process, calcium oxide and carbon dioxide react according to a molar ratio of 1:1. The reaction time was 4 hours. Then, the nano calcium carbonate solid was obtained by filtration through a filter having a pore size of 0.8 μm, and then purified by washing and drying steps. Finally, the high-activity nano calcium carbonate is obtained by heat treatment for 1.5 hours at 380 ℃.
Example 5:
the 0.2M solution of calcium oxide and the 0.2M solution of carbon dioxide are reacted at a temperature of 40 ℃ and a pressure of 1atm to obtain a nano calcium carbonate suspension. In the reaction process, calcium oxide and carbon dioxide react according to a molar ratio of 1:1. The reaction time was 4 hours. Then, the nano calcium carbonate solid was obtained by filtration through a filter having a pore size of 0.5 μm, and then purified by washing and drying steps. Finally, the high-activity nano calcium carbonate is obtained by heat treatment at 330 ℃ for 1 hour.
Example 6:
and (3) collecting calcium oxide and carbon dioxide in the industrial waste gas, and obtaining a calcium oxide and carbon dioxide solution through pretreatment and absorption reaction. Then, the two solutions were reacted at a temperature of 50 ℃ and a pressure of 1atm to obtain a nano calcium carbonate suspension. In the reaction process, calcium oxide and carbon dioxide react according to a molar ratio of 1:1. The reaction time was 5 hours. Then, the nano calcium carbonate solid was obtained by filtration through a filter having a pore size of 0.6 μm, and then purified by washing and drying steps. Finally, the high-activity nano calcium carbonate is obtained by heat treatment for 1.5 hours at 360 ℃.
The following table is a comparison table of experimental data for each example
As can be seen from the above experimental data table, all examples can effectively prepare high-activity nano calcium carbonate, but there are differences in the reaction conditions and the particle size of the obtained nano calcium carbonate. By comparison, we can consider example 2 as the most preferred example.
The reaction temperature in example 2 is 50 ℃, the reaction pressure is 1atm, the reaction time is 3 hours, and the conditions are moderate, so that the reaction can be ensured, and the problems of equipment pressure and energy consumption possibly caused by excessive temperature and pressure are avoided. The molar ratio of the calcium oxide to the carbon dioxide is 1:1, which is a typical chemical reaction ratio, so that the calcium oxide and the carbon dioxide can be ensured to completely react, and waste is avoided. In addition, the filter pore size used in example 2 was 0.6 μm, the heat treatment temperature was 350℃and the heat treatment time was 1.5 hours, and these conditions were all favorable for obtaining nano calcium carbonate having a moderate particle size and a high activity. In particular, the nano calcium carbonate obtained in example 2 has a particle size of 30nm, which is a relatively ideal particle size, and not only ensures the nano-sized characteristics of nano calcium carbonate, but also satisfies the demands of most applications, and thus example 2 is considered as an optimal example.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (10)
1. The method for efficiently preparing the high-activity nano calcium carbonate suspension is characterized by comprising the following steps of:
step one: adding calcium oxide with purity higher than 99.9% into a reaction container, and stirring at room temperature to make the calcium oxide fully uniform;
step two: adding carbon dioxide with purity higher than 99.9% into another reaction container, and decomposing the carbon dioxide into elemental carbon and oxygen;
step three: reacting the elemental carbon and oxygen obtained in the second step with the calcium oxide in the first step to generate nano calcium carbonate;
step four: stirring the nano calcium carbonate under ultrasonic equipment to enhance the activity of the nano calcium carbonate;
step five: after the reaction is finished, adding a proper amount of distilled water to generate nano calcium carbonate suspension.
The method can rapidly prepare the high-activity nano calcium carbonate suspension in a short time, not only improves the yield, but also greatly reduces the energy consumption, and has higher practicability and industrial application value.
2. The method for efficiently preparing the high-activity nano calcium carbonate suspension according to claim 1, wherein the stirring time in the first step is 5-10 minutes, the stirring speed is 500-1000 rpm, and the uniformity of the calcium oxide is ensured.
3. The method for efficiently preparing the high-activity nano calcium carbonate suspension according to claim 1, wherein the decomposition of the carbon dioxide in the second step is performed by using an ultrasonic device with an ultrasonic frequency of 20-40kHz and a power of 100-200W.
4. A method for efficiently preparing a high-activity nano calcium carbonate suspension according to claim 3, wherein the third specific reaction step is as follows:
placing the calcium oxide obtained in the first step into a reaction container provided with a heating device, starting the heating device, and heating the calcium oxide to a preset reaction temperature, wherein the reaction temperature is 80-120 ℃ and the reaction time is 2-4 hours;
simultaneously, the elemental carbon and oxygen obtained by decomposition in the second step are slowly introduced into a reaction vessel containing calcium oxide through an inlet with adjustable flow, so that the elemental carbon and oxygen are fully contacted and mixed with the calcium oxide;
in the reaction process, the ultrasonic equipment is turned on, and the reactant is stirred and heated by ultrasonic waves so as to ensure that the reaction is fully carried out and the activity of the generated nano calcium carbonate particles is improved;
monitoring the reaction process, and detecting the pH value, color and concentration indexes of the reaction solution by an analytical instrument when the reaction of calcium oxide, elemental carbon and oxygen tends to be completed, so as to confirm that the reaction is completed;
after the reaction is completed, the heating device and the ultrasonic equipment are closed, and the mixture in the reaction vessel is cooled to room temperature, so that the mixture containing the high-activity nano calcium carbonate is obtained.
The steps can ensure the smooth progress of the reaction, the produced nano calcium carbonate has high activity, and the particle size can be controlled by adjusting the reaction conditions, which is of great significance for the subsequent application.
5. The method for preparing high-activity nano calcium carbonate suspension efficiently according to claim 1, wherein the distilled water in the fifth step is added in an amount of 2-5 times the volume of nano calcium carbonate.
6. The method for preparing high-activity nano calcium carbonate suspension liquid with high efficiency according to claim 1, wherein the nano calcium carbonate suspension liquid in the fifth step is purified by filtering, washing and drying steps, and the method is specifically as follows:
and (3) filtering: filtering the nano calcium carbonate suspension by using a filter with proper pore size, filtering out large particle impurities, unreacted calcium oxide and the like in the suspension, and obtaining nano calcium carbonate suspension with uniform particle size after filtering, wherein the pore size of the filter is 0.2-0.8 microns;
washing: washing the filtered nano calcium carbonate suspension by using distilled water to remove impurities or residual reactants, and ensuring that the nano calcium carbonate is fully contacted and mixed with a washing solution by stirring and oscillating in the washing process, so that the washing effect is improved;
and (3) drying: the washed nano calcium carbonate suspension removes redundant water through a drying step, and can be subjected to vacuum drying, freeze drying or spray drying, and the obtained nano calcium carbonate particles have higher purity after drying, so that the nano calcium carbonate particles are convenient for subsequent storage and use;
through the steps, the purity of the nano calcium carbonate suspension can be effectively improved, and the activity and application performance of the nano calcium carbonate are improved.
7. The method for efficiently preparing the high-activity nano calcium carbonate suspension according to claim 1, wherein the calcium oxide and the carbon dioxide are recovered from industrial waste gas, the production cost is reduced, and the method is beneficial to environmental protection, and the specific recovery steps comprise:
and (3) collecting industrial waste gas: firstly, collecting industrial waste gas containing calcium oxide and carbon dioxide, wherein the industrial waste gas comprises cement production, chemical production and electric power production, and the flue gas contains a large amount of carbon dioxide and partial calcium oxide;
pretreatment of waste gas: pretreating the collected industrial waste gas, wherein the pretreatment comprises cooling and dust removal so as to reduce dust and moisture in the waste gas;
and (3) carbon dioxide recovery: the pretreated industrial waste gas passes through an absorption tower, carbon dioxide in the waste gas is absorbed by sodium hydroxide solution, the carbon dioxide is converted into bicarbonate which can be dissolved in water through reaction, and then the bicarbonate is converted into carbon dioxide and water through a regeneration step, and the carbon dioxide with high purity is separated;
and (3) calcium oxide recovery: the calcium oxide in the waste gas generally exists in the form of particles, is separated from the waste gas through filtration and sedimentation, and is further purified through a chemical method (such as acid-base reaction) if the purity of the calcium oxide does not reach the standard;
through the steps, calcium oxide and carbon dioxide in industrial waste gas can be effectively recovered, so that the production cost is reduced, and the environmental protection is contributed.
8. The method for efficiently preparing a highly active nano calcium carbonate suspension according to any one of claims 1 to 7, wherein a surfactant is added in each step to improve the dispersibility of nano calcium carbonate.
9. The method for preparing high-activity nano calcium carbonate suspension liquid according to claim 1, wherein the decomposition in the second step is performed by electrochemical, thermal pyrolysis or photocatalysis to improve the efficiency of the reaction and the purity of the product.
10. The method for efficiently preparing the high-activity nano calcium carbonate suspension according to claim 1, wherein the particle size of the nano calcium carbonate suspension is 10nm-100nm, and the particle shape of the nano calcium carbonate suspension comprises a sphere shape, a sheet shape and a rod shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310913762.XA CN116692916A (en) | 2023-07-25 | 2023-07-25 | Method for efficiently preparing high-activity nano calcium carbonate suspension |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310913762.XA CN116692916A (en) | 2023-07-25 | 2023-07-25 | Method for efficiently preparing high-activity nano calcium carbonate suspension |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116692916A true CN116692916A (en) | 2023-09-05 |
Family
ID=87845391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310913762.XA Pending CN116692916A (en) | 2023-07-25 | 2023-07-25 | Method for efficiently preparing high-activity nano calcium carbonate suspension |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116692916A (en) |
-
2023
- 2023-07-25 CN CN202310913762.XA patent/CN116692916A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10618813B2 (en) | Carbon nitride modified with perylenetetracarboxylic dianhydride / graphene oxide aerogel composite material, preparation method and application thereof | |
| CN112892593A (en) | MOFs/water hyacinth derived material, preparation method thereof and degradation method of organic pollutants | |
| CN104591301A (en) | Preparation method of porous nano CoFe2O4 | |
| CN108246334A (en) | A kind of functionalization tri compound catalysis material and preparation method thereof and purposes | |
| CN108273528A (en) | A method of preparing the high iodine oxygen bismuth photochemical catalyst of nano bar-shape | |
| CN112607785B (en) | MnFe 2 O 4 C nano composite microsphere and preparation method thereof | |
| CN102730668B (en) | Method for preparing grapheme through solvothermal technique based on aromatic alcohol | |
| CN111330648A (en) | MIL-101(Fe)/g-C3N4Composite visible light photocatalyst and preparation method and application thereof | |
| CN114436806B (en) | Method for preparing disodium terephthalate and hydrogen by converting PET (polyethylene terephthalate) polyester waste plastics at low temperature by one-step method | |
| CN114957192B (en) | Method for preparing cyclic carbonate by catalyzing carbon dioxide with cerium-based catalyst | |
| Liu et al. | Photocatalyst from one-dimensional TiO2 nanowires/synthetic zeolite composites | |
| Sufian | Development of the g-C3N4/BiVO4 microflower photocatalyst for photocatalytic degradation of amoxicillin and hydrogen production | |
| CN111389421B (en) | Preparation method and application of two-dimensional layered bismuth oxychloride and titanium niobate composite photocatalytic material | |
| Duan et al. | Recent development in the environmental application of nano-sized MgO | |
| US20220324718A1 (en) | Method for preparing basic copper carbonate | |
| CN116692916A (en) | Method for efficiently preparing high-activity nano calcium carbonate suspension | |
| CN111250077A (en) | Composite metal oxide catalyst and application thereof | |
| CN1974412A (en) | Process of preparing high purity ferric oxide | |
| CN110560080A (en) | preparation method of cobalt-manganese composite oxide and method for degrading dye wastewater | |
| CN102728853B (en) | Production technique for high-purity nanoscale metal magnesium powder | |
| CN113717391B (en) | Boron-containing zirconium-based metal organic framework material and preparation method and application thereof | |
| CN106391054B (en) | A kind of carbon nanotube/indium sulfide heterojunction nano-wire and preparation method thereof | |
| US11623210B2 (en) | Method for preparing silicate/carbon composite from attapulgite, and use of silicate/carbon composite | |
| CN113318768A (en) | Composite photocatalyst and preparation method thereof | |
| CN113976107A (en) | Method for preparing Mn-based composite catalyst by using organic waste liquid and application of Mn-based composite catalyst in decomposition of indoor formaldehyde |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Country or region after: China Address after: 365400 Shibanqiao, Hucun Town, Ninghua County, Sanming City, Fujian Province Applicant after: Fujian Xihong Nanotechnology Co.,Ltd. Address before: 365400 Shibanqiao, Hucun Town, Ninghua County, Sanming City, Fujian Province Applicant before: FUJIAN HONGFENG NANO TECHNOLOGY Co.,Ltd. Country or region before: China |
|
| CB02 | Change of applicant information |