CN110510650A - The preparation method and nanometer calcium carbonate of nanometer calcium carbonate - Google Patents
The preparation method and nanometer calcium carbonate of nanometer calcium carbonate Download PDFInfo
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- CN110510650A CN110510650A CN201910784544.4A CN201910784544A CN110510650A CN 110510650 A CN110510650 A CN 110510650A CN 201910784544 A CN201910784544 A CN 201910784544A CN 110510650 A CN110510650 A CN 110510650A
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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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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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
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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
-
- 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
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2/00—Lime, magnesia or dolomite
- C04B2/02—Lime
- C04B2/04—Slaking
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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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
- C01P2006/80—Compositional purity
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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
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a kind of preparation methods of nanometer calcium carbonate and nanometer calcium carbonate prepared therefrom.The preparation method comprises the following steps: calcining carbide slag at 600~700 DEG C;Calcined carbide slag is added in 80~90 DEG C of hot water with the weight ratio of 1:5~7 and is digested, digestion mixture is obtained;The digestion mixture is filtered, slurry is obtained;The slurry and water are configured to the calcium hydroxide suspension that mass percent is 3~10%, Xiang Suoshu calcium hydroxide suspension is passed through the carbonated gas of packet, the slurries after reaction is carbonized at 20~50 DEG C.Nanometer calcium carbonate prepared according to the methods of the invention has high whiteness and high-purity.
Description
Technical field
The present invention relates to a kind of preparation methods of nanometer calcium carbonate, belong to field of nanometer material technology.
Background technique
Nanometer calcium carbonate has in coating, plastics, electronics and Material Field and is widely applied as inorganic filler.Conventional
The preparation method of nanometer calcium carbonate includes the carbonizatin method that carbon dioxide gas is passed through into calcium hydroxide solution, and makes solubility
Calcium salt and carbonate directly mix double decomposition.
Carbide slag is the waste material generated during producing acetylene as raw material using calcium carbide, and main component is calcium hydroxide.
Generally included using the preparation method that carbide slag produces nanometer calcium carbonate as raw material: carbide slag leaches and the step of synthetic calcium carbonate.
In the leaching step of this method, ammonium chloride solution is generallyd use as leaching agent, carbide slag is made to be converted to calcium chloride solution, then
Ammonium chloride and calcium carbonate are formed through carbonization.The reaction equation of the technical process is as follows:
Ca(OH)2+2NH4Cl═CaCl2+NH3·H2O
CaCl2+H2O+CO2+2NH3═CaCO3↓+2NH4Cl
The shortcomings that technique is as follows: 1, equipment investment is larger.2, due to there is ammonium chloride generation, ammonium chloride is volatile, environmental protection
Pressure is larger.Therefore, low and technical process environmentally friendly synthesis nanometer calcium carbonate method is put into there is an urgent need to develop a kind of.
Summary of the invention
For this purpose, the present invention provides a kind of preparation method of nanometer calcium carbonate, using carbide slag as raw material, disappeared by calcining, acid
Change liquid nitrification and carbonization treatment, the nanometer calcium carbonate that average particle size is 50~150nm can be made, this method is easy to operate, to setting
It is low for requiring, and nanometer calcium carbonate product whiteness obtained is high, purity is high.
According to an aspect of the present invention, a kind of preparation method of nanometer calcium carbonate is provided, comprising the following steps:
Calcining step calcines carbide slag at 600~700 DEG C;
Calcined carbide slag is added in 80~90 DEG C of hot water with the weight ratio of 1:5~7 and is digested by digestion step,
Obtain digestion mixture;
Filtration step filters the digestion mixture, obtains digestion slurry;
The digestion slurry and water are configured to the calcium hydroxide suspension that mass percent is 3~10% by synthesis step,
It is passed through the carbonated gas of packet to the calcium hydroxide suspension, the slurries after reaction is carbonized at 20~50 DEG C.
Specifically, auxiliary agent is added in the digestion step, the auxiliary agent is selected from hydrochloric acid, citric acid, acetic acid, propylene
One of acid, sulfuric acid and phosphoric acid are a variety of.The additive amount of the auxiliary agent is the 0.1~1% of the digestion mixture weight.
Preferably, dispersing agent is added in the synthesis step, the dispersing agent is selected from Sodium Polyacrylate, phosphoric acid, coke
One of phosphoric acid is a variety of.The additive amount of the dispersing agent is the 0.1~1% of calcium hydroxide solid content.
In the synthesis step, the volume content of the carbon dioxide in the gas is 30~90%.Two in the gas
The flow of carbonoxide is 20~40m3/min。
Preferably, the preparation method further comprises brightening step, and the carbon is added into the slurries after the carbonization
The sodium dithionite of 0.05~1% EDTA and 0.01~1% of slurry weight after change.
It is further preferred that the preparation method further comprises surface-coating step, the increasing is added into the slurries after brightening
2~5% modifying agent of the slurry weight after white is modified at 50~90 DEG C, and the modifying agent is selected from stearic acid, phosphorus
One of acid esters coupling agent, titanate coupling agent, aluminate coupling agent are a variety of.
According to another aspect of the present invention, a kind of nanometer calcium carbonate prepared according to the above method, the nano-sized carbon are provided
Sour calcium has the average grain diameter of 50~150nm, and >=90% whiteness.
Detailed description of the invention
With reference to the attached drawing of accompanying, the more purposes of the present invention, function and advantage are by the as follows of embodiment through the invention
Description is illustrated, in which:
Fig. 1 is the scanning electron microscopic picture of the nanometer calcium carbonate prepared according to embodiment 1.
Specific embodiment
The preparation method of nanometer calcium carbonate according to the present invention, comprising the following steps:
Calcining step calcines carbide slag at 600~700 DEG C;
Calcined carbide slag is added in 80~90 DEG C of hot water with the weight ratio of 1:5~7 and is digested by digestion step,
Obtain digestion mixture;
Filtration step filters the digestion mixture, obtains digestion slurry;
The digestion slurry and water are configured to the calcium hydroxide suspension that mass percent is 3~10% by synthesis step,
It is passed through the carbonated gas of packet to the calcium hydroxide suspension, the slurries after reaction is carbonized at 20~50 DEG C.
Specifically, high-temperature calcination is carried out to carbide slag to be used to remove the carbon slag in carbide slag.In general, containing in carbide slag
2% or so carbon slag is such as directly carbonized to produce calcium carbonate product, will affect calcium carbonate quality, especially seriously
Influence product whiteness.The ignition temperature of carbon slag is 600 DEG C or so, Ca (OH)2Decomposition temperature is 450~680 DEG C, therefore uses and forge
Firing method can not only remove carbon elimination slag, moreover it is possible to promote Ca (OH)2It is converted to the CaO of high activity, the stone of high quality can be obtained through digesting
Grey cream, is more conducive to prepare nanometer grade calcium carbonate.Slurry temperature is increased since a large amount of heat can be released when CaO is digested with water,
The more big then slurries adiabatic temperature rise of CaO activity is faster, and the maximum temperature point reached is also bigger.
Calcination temperature is too low, and calcium carbonate present in carbide slag does not decompose completely, so that the activity of CaO is low;But calcining temperature
Height is spent, with inorganic impurity sintering can occur again for CaO causes temperature rise to reduce.From the aspect of CaO activity and energy consumption, present invention choosing
The optimum calcinating temperature selected is 600~700 DEG C.The high-temperature burning process carries out usually in rotary kiln.
In above-mentioned digestion step, preferably addition auxiliary agent is to become soluble for calcium carbonate a small amount of in carbide slag, calcium oxide
Calcium ion, consequently facilitating subsequent calcium carbonate synthesis step.The auxiliary agent be selected from hydrochloric acid, citric acid, acetic acid, acrylic acid, sulfuric acid,
One of phosphoric acid is a variety of, and additive amount is the 0.1-1% of mixture weight to be digested.
In above-mentioned postdigestive filtration step, digestion mixture is passed through to the screen filtration of 100-500 mesh.The purpose of filtering
It is the impurity in removing slurry to get the calcium hydroxide slurry digested.Sieve residue main component be silica, calcium carbonate,
The products such as aluminium oxide, carbon black can be used when construction material.
Preferably, above-mentioned digestion mixture preferably uses the vibration of 100-300 mesh by being sieved twice for the first time
Sieve, second of sieve using 300-500 mesh.
In above-mentioned synthesis step, the calcium hydroxide suspension that mass fraction is about 3-10% is made by slurry is digested with water.
Preferably, calcium hydroxide suspension is added in high shear reaction kettle, the size of reaction kettle is 20-60m3.To above-mentioned hydroxide
Calcium suspension is passed through the gas that carbon dioxide volume content is 30-90%, and the flow of carbon dioxide is preferably 20-40m3/min。
Synthetic reaction usually carries out under normal pressure, and carbonation reaction temperature is between 20-50 DEG C.Preferably, which is divided to two
Secondary carbonization carries out.First time carbonation rate is to 90% or so, second of carbonation rate to 100%.The purpose being carbonized in two times is to improve
The conversion ratio of nanoparticle reduces the pH value of product.
During above-mentioned carburizing reagent, add dispersing agent, such as one of Sodium Polyacrylate, phosphoric acid, pyrophosphoric acid or
A variety of, the amount of addition is the 0.1-1% of calcium hydroxide solid content.It is reacted between terminal point control PH=7-10.
Since the nanometer calcium carbonate whiteness of carbide slag preparation is not high, it usually needs carry out brightening step again after carburising step
Suddenly.Preferably, the step that brightens in preparation method of the invention includes that carbonization rear slurry is added in slurries after above-mentioned carbonization
The sodium dithionite of 0.05~1% EDTA and 0.01~1% of weight is preferably stirred 20~60 minutes.
Since Nano particles of calcium carbonate surface lacks adjacent atom, interaction force is big between particle, easily reunites.It is excellent
Selection of land, it is above-mentioned brighten step after, preparation method of the invention further includes surface-coating step, to improve nanoparticle poly-
Close the dispersibility and compatibility in object.The surface-coating step includes being added to brighten rear slurry weight in slurries after brightening
2~5% modifying agent is modified at 50~90 DEG C, is preferably carried out 30~100 minutes.The modifying agent be selected from stearic acid,
One of phosphate coupling agent, titanate coupling agent, aluminate coupling agent are a variety of.
According to actual needs, preparation method of the invention can also further comprise filters pressing, washing, drying, crushing and packaging
And etc..
Specifically, filters pressing is carried out to by the nanometer calcium carbonate slurry after above-mentioned modification procedure.The filters pressing step is usual
It is carried out using plate and frame type filter-press.
Filter cake after filters pressing is washed in sheet frame with water, to remove chloride ion, sulfate ion, iron ion, aluminium
The impurity such as ion.Further, the filter cake after washing be dried, crushed, being packaged to be finished product Nano particles of calcium carbonate.
A specific embodiment according to the present invention, according to nanometer calcium carbonate prepared by the above method, the nano-sized carbon
Sour calcium has the average grain diameter of 50~150nm, and >=90% whiteness.
The present invention is further illustrated by way of the following example, the scope of the invention is not limited to following implementations
Example.
Embodiment
Embodiment 1
1. carbide slag is placed in rotary kiln, 1h is calcined at 900 DEG C;
2. calcined carbide slag is added in 90 DEG C of hot water with the weight ratio of 1:7, wherein adding electricity into hot water
The acrylic acid of rock ballast weight 1% digests 30min, obtains digestion mixture;
3. above-mentioned digestion mixture is passed through 200 mesh screens, digestion slurry is obtained;
4. above-mentioned digestion slurry and water are configured to the calcium hydroxide suspension that mass percent is 10%, hydroxide is added
1% Sodium Polyacrylate of calcium solid content is passed through as dispersing agent, and to the calcium hydroxide suspension comprising carbon dioxide volume
The gas that content is 90%, the flow of carbon dioxide is preferably 20m3/ min, the slurries after reaction is carbonized at 50 DEG C;
5. adding the sodium dithionite of 1% EDTA and 1% of its weight into above-mentioned carbonization rear slurry, 60 points are stirred
Clock, the slurries after being brightened;
6. adding the modifying agent phosphate coupling agent of the 5% of the slurry weight to the slurries after brightening, it is modified 100 points
Clock obtains modified slurries;
7. a pair modified slurries carry out plate-frame filtering, it is washed with water, dry, pulverize and pack, obtain nanometer calcium carbonate
Particle.
The nanometer calcium carbonate prepared according to embodiment 1 is detected with scanning electron microscope, particle morphology picture is such as
Shown in Fig. 1, and the performances such as average grain diameter, whiteness, activation grade and oil factor for measuring particle, test result, which summarizes, to be shown in Table 1.
Embodiment 2
1. carbide slag is placed in rotary kiln, 1h is calcined at 800 DEG C;
2. calcined carbide slag is added in 80 DEG C of hot water with the weight ratio of 1:5, wherein adding electricity into hot water
The acrylic acid of rock ballast weight 0.1% digests 30min, obtains digestion mixture;
3. above-mentioned digestion mixture is passed through 200 mesh screens, digestion slurry is obtained;
4. above-mentioned digestion slurry and water are configured to the calcium hydroxide suspension that mass percent is 10%, hydroxide is added
0.1% Sodium Polyacrylate of calcium solid content is passed through as dispersing agent, and to the calcium hydroxide suspension comprising carbon dioxide body
The gas that product content is 50%, the flow of carbon dioxide is preferably 40m3/ min, the slurries after reaction is carbonized at 50 DEG C;
5. adding the sodium dithionite of 0.05% EDTA and 0.01% of its weight into above-mentioned carbonization rear slurry, stir
It mixes 60 minutes, the slurries after being brightened;
6. adding the modifying agent aluminate coupling agent of the 2% of the slurry weight to the slurries after brightening, it is modified 100 points
Clock obtains modified slurries;
7. a pair modified slurries carry out plate-frame filtering, it is washed with water, dry, pulverize and pack, obtain nanometer calcium carbonate
Particle.
The performances such as average grain diameter, whiteness, activation grade and the oil factor of particle are measured, test result, which summarizes, to be shown in Table 1.
Comparative example 1
Nanometer calcium carbonate is prepared in the same manner as in Example 1, and difference is without calcining step 1.
The performances such as average grain diameter, whiteness, activation grade and the oil factor of particle are measured, test result, which summarizes, to be shown in Table 1.
Comparative example 2
Nanometer calcium carbonate is prepared in the same manner as in Example 1, and difference is to be added without acrylic acid in digestion step 2.
The performances such as average grain diameter, whiteness, activation grade and the oil factor of particle are measured, test result, which summarizes, to be shown in Table 1.
Comparative example 3
Nanometer calcium carbonate is prepared in the same manner as in Example 1, and difference is without brightening step 5.
The performances such as average grain diameter, whiteness, activation grade and the oil factor of particle are measured, test result, which summarizes, to be shown in Table 1.
Table 1
It can be seen that by the above table 1, nanometer calcium carbonate average grain diameter prepared according to the methods of the invention is small, size distribution
It is narrow, and moisture content is low (≤0.5), whiteness≤0.5 is 92% or more, and activation grade is 95% or more.Contrastingly, comparative example 1,
2 and 3, due to not carrying out one of the method for the present invention processing step, lead to whiteness, the carbonic acid of final nanometer calcium carbonate product
The activation grade of calcium content and product has significant decrease.
Claims (10)
1. a kind of preparation method of nanometer calcium carbonate, which comprises the following steps:
Calcining step calcines carbide slag at 600~700 DEG C;
Calcined carbide slag is added in 80~90 DEG C of hot water with the weight ratio of 1:5~7 and is digested, obtained by digestion step
Digestion mixture;
Filtration step filters the digestion mixture, obtains digestion slurry;
The digestion slurry and water are configured to the calcium hydroxide suspension that mass percent is 3~10%, to institute by synthesis step
It states calcium hydroxide suspension and is passed through the carbonated gas of packet, the slurries after reaction is carbonized at 20~50 DEG C.
2. preparation method according to claim 1, wherein auxiliary agent is added in the digestion step, the auxiliary agent is choosing
From one of hydrochloric acid, citric acid, acetic acid, acrylic acid, sulfuric acid and phosphoric acid or a variety of.
3. preparation method according to claim 2, wherein the additive amount of the auxiliary agent is the digestion mixture weight
0.1~1%.
4. preparation method according to any one of claim 1 to 3, wherein dispersing agent is added in the synthesis step,
The dispersing agent is selected from one of Sodium Polyacrylate, phosphoric acid, pyrophosphoric acid or a variety of.
5. the preparation method according to claim 4, wherein the additive amount of the dispersing agent is calcium hydroxide solid content
0.1~1%.
6. preparation method according to any one of claim 1 to 3, wherein in the synthesis step, in the gas
The volume content of carbon dioxide is 30~90%.
7. preparation method according to any one of claim 1 to 3 further comprises brightening step, to after the carbonization
Slurries in be added the slurry weight after the carbonization 0.05~1% EDTA and 0.01~1% sodium dithionite.
8. preparation method according to claim 7 further comprises surface-coating step, is added into the slurries after brightening
It is described brighten after 2~5% modifying agent of slurry weight be modified at 50~90 DEG C, the modifying agent is selected from tristearin
One of acid, phosphate coupling agent, titanate coupling agent, aluminate coupling agent are a variety of.
9. preparation method according to any one of claim 1 to 3, wherein in synthesis step, titanium dioxide in the gas
The flow of carbon is 20~40m3/min。
10. nanometer calcium carbonate made from preparation method according to any one of claim 1 to 9, with 50~150nm
Average grain diameter, and >=90% whiteness.
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