CN114455622A - Preparation method of ultra-dispersed functional calcium carbonate - Google Patents
Preparation method of ultra-dispersed functional calcium carbonate Download PDFInfo
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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 141
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 36
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 33
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 33
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000007885 magnetic separation Methods 0.000 claims abstract description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 238000003763 carbonization Methods 0.000 claims abstract description 12
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000006148 magnetic separator Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 8
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000292 calcium oxide Substances 0.000 claims abstract description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000029087 digestion Effects 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 7
- 230000005284 excitation Effects 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 description 52
- 239000004033 plastic Substances 0.000 description 12
- 229920003023 plastic Polymers 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 5
- 239000004743 Polypropylene Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052748 manganese Inorganic materials 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004597 plastic additive Substances 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000006235 reinforcing carbon black Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- 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
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention provides a preparation method of ultra-dispersed functional calcium carbonate, which belongs to the technical field of nano material preparation, wherein the preparation method comprises the steps of taking calcium oxide and water, carrying out digestion reaction on the obtained slurry, carrying out magnetic separation and enrichment on the obtained slurry by a magnetic separator, collecting the flowing-out calcium hydroxide slurry, carrying out aging reaction and sieving on the calcium hydroxide slurry, and adding water to dilute the calcium hydroxide slurry to obtain a calcium hydroxide suspension; and adding 2-amino-2-methyl propanol into the calcium hydroxide suspension, introducing carbon dioxide gas to carry out carbonization reaction, stopping carbonization reaction when the pH value of the reaction system is reduced to 6.5-7.0, and dehydrating, drying, crushing and screening the obtained calcium carbonate slurry to obtain the ultra-dispersed functional calcium carbonate. The cubic ultra-dispersed functional calcium carbonate prepared by adding 2-amino-2-methyl propanol has the advantages of large specific surface area, good dispersibility, difficult agglomeration and low oil absorption value.
Description
Technical Field
The invention relates to a preparation method of calcium carbonate, in particular to a preparation method of ultra-dispersed functional calcium carbonate.
Background
The light calcium carbonate has various shapes such as cubic shape, spindle shape, chain shape, needle shape, sheet shape, spherical shape and the like, and the preparation methods of calcium carbonate with different shapes and crystal forms are different, and the corresponding application fields and the functions are also different. The light calcium carbonate has the advantages of high whiteness, high purity, good dispersibility, high intermiscibility, high rheological property and the like, and can partially replace semi-reinforcing carbon black and white carbon black products. The nano calcium carbonate is used as a filler of plastics, rubber and paper, has a semi-reinforcing effect, has better dispersibility after surface treatment, and has higher performance-to-cost ratio when used for the filler.
The nano calcium carbonate is used as an excellent plastic product additive, so that the volume of the plastic can be increased, and the product cost can be reduced; the dimensional stability, hardness and rigidity of the plastic are improved, and the plastic plays a role of a framework; the processing property of the plastic is improved, the viscosity is controlled, and the properties of the product, such as bending strength, bending elastic modulus, thermal deformation temperature and the like, are improved. And when calcium carbonate with different morphologies is used as a plastic additive, the obtained effect is different. Among them, the cubic nano calcium carbonate particles have good dispersibility and good affinity with high molecules, and are most suitable for preparing high-end plastic products.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of ultra-dispersed functional calcium carbonate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of ultra-dispersed functional calcium carbonate comprises the following steps in sequence:
1) after digestion reaction of calcium oxide and water, carrying out magnetic separation enrichment on the obtained slurry by a magnetic separator, and collecting the flowing-out calcium hydroxide slurry;
2) taking calcium hydroxide slurry, carrying out aging reaction, sieving, and adding water for dilution to obtain a calcium hydroxide suspension;
3) adding the calcium hydroxide suspension into a reactor, adding 2-amino-2-methyl propanol, introducing carbon dioxide gas for carbonization reaction, and stopping the carbonization reaction when the pH value of a reaction system is reduced to 6.5-7.0 to obtain calcium carbonate slurry;
4) and (3) dehydrating, drying, crushing and screening the calcium carbonate slurry to obtain the ultra-dispersed functional calcium carbonate.
Further, in the step 1), the magnetic separation and enrichment comprises the following steps:
opening excitation current, adjusting the magnetic separation intensity of the magnetic separator to 140-160 mT, and starting injecting slurry for magnetic separation and enrichment;
and (3) after the slurry is enriched by magnetic separation, collecting the effluent, injecting the effluent into the magnetic separator again for repeated magnetic separation, and collecting the effluent which is subjected to repeated magnetic separation for more than 2 times to obtain the calcium hydroxide slurry.
Further, the slurry injection speed is 30-40 mL/s.
Further, in the step 3), the addition amount of the 2-amino-2-methylpropanol is 0.7-1.2 wt% of the weight of the calcium hydroxide in the calcium hydroxide suspension.
Further, in the step 3), the temperature of the carbonization reaction is 35-40 ℃.
Further, in the step 3), turbine type stirring is adopted in the carbonization reaction process.
Furthermore, the rotating speed of turbine type stirring is 480-500 r/min.
Further, in the step 3), the volume content of the carbon dioxide gas in the reactor is 25-30%.
Further, in the step 2), the concentration of calcium hydroxide in the calcium hydroxide suspension is 12-15 wt%.
Further, in the step 1), the weight volume ratio of calcium oxide to water is 1: 7-8;
the temperature of the digestion reaction is 80-85 ℃;
in the step 2), the time of the aging reaction is 9-10 h;
the aperture of the sieved sieve is 180-200 meshes.
The preparation method of the ultra-dispersed functional calcium carbonate has the beneficial effects that:
the 2-amino-2-methylpropanol is used as a crystal form control agent, and the structural formula of the crystal form control agent has two groups, namely hydroxyl and amino, wherein the hydroxyl can generate a strong electrostatic matching effect with calcium ions and is combined with the calcium ions to occupy an active center for the growth of calcium carbonate crystals, so that the growth of calcium carbonate particles is inhibited; meanwhile, the amino group has a strong chelating effect and can be chelated with calcium carbonate particles to increase the steric hindrance of the calcium carbonate particles, so that the growth of the calcium carbonate particles is inhibited; the cubic ultra-dispersed functional calcium carbonate is prepared by adding 2-amino-2-methylpropanol, and has the advantages of large specific surface area, good dispersibility, difficult occurrence of agglomeration and low oil absorption value;
according to the invention, the magnetic separation and enrichment method is adopted to adsorb the elements such as magnesium, iron and manganese in the slurry, so that the metal elements contained in the calcium hydroxide slurry are removed fundamentally, the metal content in the prepared ultra-dispersed functional calcium carbonate is effectively reduced, the whiteness of the calcium carbonate is improved, and meanwhile, the cubic crystal form of the calcium carbonate is more favorably formed;
the invention effectively controls the formation of cubic calcium carbonate by selecting proper process parameters, and has better dispersibility; when the cubic calcium carbonate prepared by the invention is used as a filler to prepare plastics, the cubic calcium carbonate can be well dispersed in the plastics and can be used as a stress concentration point to initiate a large amount of silver streaks, so that impact energy is absorbed, and the toughness of the composite material is increased; meanwhile, the cubic calcium carbonate can also play a role of a crosslinking point, when the composite material is subjected to tensile stress, the crosslinking point has a balance effect of stress concentration and stress radiation, and can play a role of uniformly distributing the stress by absorbing external energy and radiation energy, so that the tensile strength of the composite material is not reduced.
Drawings
FIG. 1 is a structural representation of the ultra-dispersed functional calcium carbonate prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Example 1 preparation method of ultra-dispersed functional calcium carbonate
The embodiment is a preparation method of ultra-dispersed functional calcium carbonate, and the specific preparation process comprises the following steps in sequence:
1) adding 1kg of calcium oxide into 7kg of water with the temperature of 85 ℃ for digestion reaction to obtain slurry;
opening excitation current, adjusting the magnetic separation intensity of the magnetic separator to 150mT, and starting injecting slurry for magnetic separation;
and (3) magnetically separating the slurry, collecting the effluent, injecting the effluent into the magnetic separator again for repeated magnetic separation, and collecting the effluent subjected to the repeated magnetic separation for more than 2 times (the slurry is magnetically separated for 2 times) to obtain the calcium hydroxide slurry.
After most elements such as magnesium, iron, manganese and the like are effectively adsorbed by a magnetic separator under specific magnetic separation strength, the obtained calcium hydroxide slurry is almost free of metal elements, so that the subsequent formation of the crystal form of cubic calcium carbonate is facilitated, the metal content in the prepared calcium carbonate can be reduced, and the whiteness of the calcium carbonate is improved.
2) Directly standing and aging the calcium hydroxide slurry for 9h (no heating is performed in the standing and aging process, and the temperature is naturally reduced to room temperature), filtering the calcium hydroxide slurry through a 200-mesh sieve to remove insoluble impurities and agglomerated particles so as to avoid influencing the molding of cubic calcium carbonate crystals, and adding water to prepare a calcium hydroxide suspension with the concentration of 14 wt%.
3) Adding a calcium hydroxide suspension into a reaction kiln, heating to 35 ℃, starting turbine stirring at the rotation speed of 500r/min, adding 1.0 wt% of 2-amino-2-methyl propanol (the addition amount of the 2-amino-2-methyl propanol is 1.0 wt% of the weight of calcium hydroxide in the calcium hydroxide suspension), introducing carbon dioxide gas with the gas flow rate of 16L/h, maintaining the volume content of carbon dioxide in the reaction kiln to be 28%, continuously stirring at the temperature of 35 ℃ and the rotation speed of 500r/min for carbonization reaction, and stopping the carbonization reaction when the pH value of a reaction system is reduced to 6.5 to obtain calcium carbonate slurry;
in the reaction process, a turbine stirring method is adopted, so that the fluid in the reaction kiln can be ensured to be in a radial popular flowing state, the circulation rate is high, and the calcium hydroxide is conveniently and fully contacted with carbon dioxide to form cubic calcium carbonate crystals.
4) And (3) taking out the calcium carbonate slurry, and dehydrating, drying, crushing and screening to obtain the ultra-dispersed functional calcium carbonate, wherein the label is N1, and the structural representation diagram of the ultra-dispersed functional calcium carbonate is shown in figure 1.
The ultra-dispersed functional calcium carbonate prepared in this example was measured according to general Industrial precipitated calcium carbonate (HG/T2226-2010) and had a specific surface area of 38.2m2(ii) a whiteness of 95.3, an iron content of 0.001%, a manganese content of 0.001%, a lead content of 0.0003%, a chromium content of 0.0002%, and an oil absorption value of 15.7%.
Example 2-6 preparation method of ultra-dispersed functional calcium carbonate
Examples 2 to 6 are respectively a method for preparing ultra-dispersed functional calcium carbonate, the steps of which are basically the same as those of example 1, and the differences are only in the amount of raw materials and process parameters, and the details are shown in table 1:
TABLE 1 summary of the process parameters of examples 2 to 6
The contents of the other portions of examples 2 to 6 are the same as those of example 1.
Experimental example 1 Properties of ultra-dispersed functional calcium carbonate
Comparative examples 1 to 4 are comparative tests of the preparation process of the ultra-dispersed functional calcium carbonate in example 1, and the differences are only that:
comparative example 1, in which 2-amino-2-methylpropanol was not added, the obtained ultra-dispersed functional calcium carbonate was identified as DN1 and had a specific surface area of 10.7m2(ii) a whiteness of 95.2, an iron content of 0.001%, a manganese content of 0.002%, a lead content of 0.0002%, a chromium content of 0.0001%, an oil absorption value of 54.9%;
in comparative example 2, the aging reaction was carried out directly without magnetic concentration, and the obtained super-dispersed functional calcium carbonate was designated as DN2, and had a specific surface area of 35.2m2(ii) a whiteness of 93.9, an iron content of 0.07%, a manganese content of 0.008%, a lead content of 0.0010%, a chromium content of 0.0005%, and an oil absorption value of 25.7%.
A cooperative unit is entrusted, the super-dispersed functional calcium carbonates N1-N6, DN 1-DN 2 prepared in examples 1-6 and comparative examples 1-2 and the commercially available nano calcium carbonate are respectively used as additives (the addition amount is 7wt percent) for preparing the polypropylene plastics, and the performance of the corresponding polypropylene plastics is detected according to polypropylene (PP) resin (GB/T12670-2008), and the specific detection results are as follows:
TABLE 2 summary of rubber article Performance test results
| Group of | Impact Strength (kJ/m)2) | Flexural modulus (MPa) | Tensile Strength (MPa) |
| Example 1 | 16.23 | 989.21 | 34.13 |
| Example 2 | 15.74 | 976.31 | 33.87 |
| Example 3 | 15.21 | 962.94 | 34.21 |
| Example 4 | 15.98 | 981.52 | 33.17 |
| Example 5 | 16.02 | 973.96 | 33.62 |
| Example 6 | 15.73 | 969.41 | 34.06 |
| Comparative example 1 | 11.24 | 762.14 | 27.73 |
| Comparative example 2 | 14.47 | 924.92 | 31.89 |
| Commercial nano calcium carbonate | 11.83 | 798.24 | 28.01 |
As can be seen from Table 2, the ultra-dispersed functional calcium carbonate prepared by the invention can obviously improve the impact strength, bending model and tensile strength of polypropylene plastics.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and 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.
Claims (10)
1. The preparation method of the ultra-dispersed functional calcium carbonate is characterized by comprising the following steps of:
1) after digestion reaction of calcium oxide and water, carrying out magnetic separation enrichment on the obtained slurry by a magnetic separator, and collecting the flowing-out calcium hydroxide slurry;
2) taking calcium hydroxide slurry, carrying out aging reaction, sieving, and adding water for dilution to obtain a calcium hydroxide suspension;
3) adding the calcium hydroxide suspension into a reactor, adding 2-amino-2-methyl propanol, introducing carbon dioxide gas for carbonization reaction, and stopping the carbonization reaction when the pH value of a reaction system is reduced to 6.5-7.0 to obtain calcium carbonate slurry;
4) and (3) dehydrating, drying, crushing and screening the calcium carbonate slurry to obtain the ultra-dispersed functional calcium carbonate.
2. The method for preparing the ultra-dispersed functional calcium carbonate according to claim 1, wherein the magnetic separation and enrichment in the step 1) comprises the following steps:
opening excitation current, adjusting the magnetic separation intensity of the magnetic separator to 140-160 mT, and starting injecting slurry for magnetic separation and enrichment;
and (3) after the slurry is enriched by magnetic separation, collecting the effluent, injecting the effluent into the magnetic separator again for repeated magnetic separation, and collecting the effluent which is subjected to repeated magnetic separation for more than 2 times to obtain the calcium hydroxide slurry.
3. The method for preparing ultra-dispersed functional calcium carbonate according to claim 2, wherein the slurry is injected at a rate of 30 to 40 mL/s.
4. The method for preparing ultra-dispersed functional calcium carbonate according to any one of claims 1 to 3, wherein in the step 3), the amount of the 2-amino-2-methylpropanol is 0.7 to 1.2wt% of the weight of the calcium hydroxide in the calcium hydroxide suspension.
5. The method for preparing ultra-dispersed functional calcium carbonate according to any one of claims 1 to 3, wherein the temperature of the carbonization reaction in the step 3) is 35 to 40 ℃.
6. The process for preparing ultra-disperse functional calcium carbonate according to any one of claims 1 to 3, wherein in step 3), turbine stirring is used during the carbonization reaction.
7. The method for preparing the ultra-dispersed functional calcium carbonate according to claim 6, wherein the rotation speed of the turbine type stirring is 480 to 500 r/min.
8. The method for preparing ultra-dispersed functional calcium carbonate according to any one of claims 1 to 3 and 7, wherein the volume content of carbon dioxide gas in the reactor in the step 3) is 25-30%.
9. The method for preparing ultra-dispersed functional calcium carbonate according to any one of claims 1 to 3 and 7, wherein the concentration of calcium hydroxide in the calcium hydroxide suspension in the step 2) is 12 to 15 wt%.
10. The process for preparing a highly dispersed functional calcium carbonate according to any one of claims 1 to 3 and 7,
in the step 1), the weight volume ratio of calcium oxide to water is 1: 7-8;
the temperature of the digestion reaction is 80-85 ℃;
in the step 2), the time of the aging reaction is 9-10 h;
the aperture of the sieved sieve is 180-200 meshes.
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| JP2003137548A (en) * | 2001-10-24 | 2003-05-14 | Nittetsu Mining Co Ltd | Method for manufacturing titanium oxide-calcium carbonate composite grain |
| CN107021515A (en) * | 2017-04-25 | 2017-08-08 | 井陉县天顺钙业有限公司 | Control precipitated calcium carbonate length of particle than method |
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| CN111717929A (en) * | 2020-07-10 | 2020-09-29 | 沈阳鑫博工业技术股份有限公司 | Carbide slag comprehensive utilization device and method |
| CN112299464A (en) * | 2020-10-10 | 2021-02-02 | 浙江省建德市正发药业有限公司 | Preparation method of multipurpose calcium carbonate superfine powder |
| CN113955789A (en) * | 2021-11-22 | 2022-01-21 | 广西东泰实业有限责任公司 | Preparation method of cubic ultrafine light calcium carbonate |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003137548A (en) * | 2001-10-24 | 2003-05-14 | Nittetsu Mining Co Ltd | Method for manufacturing titanium oxide-calcium carbonate composite grain |
| CN107021515A (en) * | 2017-04-25 | 2017-08-08 | 井陉县天顺钙业有限公司 | Control precipitated calcium carbonate length of particle than method |
| CN108017079A (en) * | 2017-12-26 | 2018-05-11 | 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) | A kind of method of lime foam production calcite |
| CN111717929A (en) * | 2020-07-10 | 2020-09-29 | 沈阳鑫博工业技术股份有限公司 | Carbide slag comprehensive utilization device and method |
| CN112299464A (en) * | 2020-10-10 | 2021-02-02 | 浙江省建德市正发药业有限公司 | Preparation method of multipurpose calcium carbonate superfine powder |
| CN113955789A (en) * | 2021-11-22 | 2022-01-21 | 广西东泰实业有限责任公司 | Preparation method of cubic ultrafine light calcium carbonate |
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