CN100545092C - A kind of preparation method of submicron grade superfine calcium carbonate dispersion particle - Google Patents
A kind of preparation method of submicron grade superfine calcium carbonate dispersion particle Download PDFInfo
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- CN100545092C CN100545092C CNB2005100271269A CN200510027126A CN100545092C CN 100545092 C CN100545092 C CN 100545092C CN B2005100271269 A CNB2005100271269 A CN B2005100271269A CN 200510027126 A CN200510027126 A CN 200510027126A CN 100545092 C CN100545092 C CN 100545092C
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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 47
- 239000002245 particle Substances 0.000 title claims abstract description 20
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 19
- 239000006185 dispersion Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 31
- 238000003763 carbonization Methods 0.000 claims description 14
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 11
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 150000002016 disaccharides Chemical class 0.000 claims description 2
- 150000004676 glycans Chemical class 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052816 inorganic phosphate Inorganic materials 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229920001282 polysaccharide Polymers 0.000 claims description 2
- 239000005017 polysaccharide Substances 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 229960004418 trolamine Drugs 0.000 claims description 2
- 230000005587 bubbling Effects 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 238000010000 carbonizing Methods 0.000 abstract description 6
- 239000000049 pigment Substances 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 238000005255 carburizing Methods 0.000 abstract description 2
- 238000002050 diffraction method Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 239000012744 reinforcing agent Substances 0.000 abstract description 2
- 239000012763 reinforcing filler Substances 0.000 abstract description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 25
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 208000004434 Calcinosis Diseases 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a kind of preparation method of submicron grade superfine calcium carbonate dispersion particle.The present invention draws the advantage of bubbling carbonizing method, again according to the ultimate principle of crystallography, adopt specific crystal structure adjusting agent, the growth velocity of control crystalline nucleation and each crystal face, particularly add dispersion agent to regulate particle surface electric charge and space resistance latter stage, make particle have good dispersiveness in carburizing reagent.Not only be suitable as the paper stopping composition and paper coating pigment has gloss height and low viscosity characteristics, and be suitable for application scenarios such as coating, plastics as semi-reinforcing agent and filler.
Description
Technical field
The present invention relates to a kind of preparation method who is applicable to the calcium carbonate granule in the paper, specifically, relate to submicron grade superfine calcium carbonate particulate preparation method.
Background technology
The submicron grade superfine calcium carbonate particle of indication of the present invention is meant the calcium carbonate granule of median size between 0.1～1.0 μ m, and its pattern can be cube, the mixing of prismatic, grain of rice shape or above several patterns.
Along with the development of paper-making technique, precipitated chalk has become the indispensable important source material of paper-making industry.The fine precipitated chalk need possess apparent characteristics such as high whiteness, high covering power, printing ink anchorage and excellent in optical properties.Plastic working requires pearl filler to have lower oil-absorption(number) (bigger loading level), high brightness and is easy to mix and carry.From powdered material physical chemistry angle, require precipitated chalk: 1) thus the low high whiteness of high purity that embodies of contained foreign pigment content such as ferrimanganic; 2) have the particle scale and the homogeneous granules degree thereof that are complementary with the pigment requirement and distribute, under the single particle dispersion state, embody excellent pigment optical characteristics and filling intensity; 3) have regular granule-morphology, make the user be easy to disperse, minimum apparent hardness (low abrasion), minimum oil-absorption(number) and increase loading level embodies excellent coating rheological properties such as highly filled low viscosity; 4) lower manufacturing cost.
With the Wingdale mineral is initial feed, become unslaked lime and carbonated kiln gas through thermolysis, the digestion of unslaked lime water obtains containing calcium hydroxide solid slaked lime suspension (hereinafter referred to as milk of lime), carbonated clean kiln gas and milk of lime contact reacts carbonate synthesis calcium deposit, this type of relates to gas-liquid-solid heterogeneous reaction and produces the main stream approach that the method for precipitated chalk remains the industry member employing at present.
Difference according to the technical scheme that adopts, the way of contact of milk of lime and carbon dioxide containing gas mainly contains the bubbling hybrid mode, the mechanical stirring hybrid mode, and gas phase is the milk of lime spraying way of contact of external phase, and wherein the specific energy consumption of first kind of mode is saved the most.But, in the tradition bubble tower, if do not add the crystal formation control agent, the product that obtains mostly is spindle-type, two-dimensional projection's maximum length of primary particle is 2 μ m～6 μ m, above coacervates of 10 particles normally between the primary particle, the yardstick of coacervate is generally 15 μ m～40 μ m, and oil-absorption(number) is more than 60DOPg/100g.For improve traditional technology produce precipitated chalk dispersiveness and and satisfy of the requirement of different application field to particle scale, various Technological improvement plans have been proposed.
For example, the open CN1330039A of Chinese patent application, in order to obtain certain products granularity and size-grade distribution thereof, adding under sugar and the cold condition, adopt the mechanical stirring hybrid mode, synthesize 0.02 μ m～0.09 μ m cube calcium carbonate superfine powder, deal with the cohesion of nano-scale particle by soap or titanate coupling agent.But the nano level precipitated chalk after handling like this has hydrophobic surface and is not suitable for as the pigment of paper grade (stock) weighting agent with the coating paper.
The open CN1348428A of Chinese patent application has announced the preparation method who is suitable for as the precipitated chalk of paper weighting agent and coating paper colors.Adding under 0.5～3% and 30～80 ℃ of temperature of sugar, adopt the mechanical stirring hybrid mode, by control reaction temperature and carbohydrate additive add-on, the discrete particle precipitated chalk of synthetic 0.1 μ m～3 μ m.
U.S. Pat P5811070 has announced the method for the precipitated chalk of preparation granularity 0.1 μ m～1 μ m.This method adopts lower lime milk concentration, multistep operation repeatedly, and the technology controlling and process complexity, the unit volume productive rate is not high.
Chinese patent application numbers 200410025155.7 has been announced the method that a kind of two step carborizations are produced the calcium carbonate superfine powder particle dispersion, this method at first needs synthesis of nano lime carbonate as crystal seed, again this crystal seed is added in the milk of lime slurry, and in the presence of additive the dispersed calcium carbonate granule of controlled 0.1～1 μ m of the synthetic particle diameter of two step carbonizations, this technological process control relative complex.
Summary of the invention
The problem that the present invention need solve provides a kind of preparation method of submicron grade superfine calcium carbonate dispersion particle, to overcome the above-mentioned defective that prior art exists.
Technical conceive of the present invention is such:
The present invention draws the advantage of bubbling carbonizing method, again according to the ultimate principle of crystallography, adopt specific crystal structure adjusting agent, the growth velocity of control crystalline nucleation and each crystal face, particularly add dispersion agent to regulate particle surface electric charge and space resistance latter stage, make particle have good dispersiveness in carburizing reagent.
Method of the present invention may further comprise the steps:
(1) crystal structure adjusting agent is added calcium hydroxide slurry (hereinafter to be referred as milk of lime), feed the gas that the carbonated volumetric concentration is 10-100% then, Ventilation Rate is 2～50m
3/ (h m
3Milk of lime), preferred 2～25m
3/ (h m
3Can use bigger bubbling speed when milk of lime), adopting lower density of carbon dioxide gas; When adopting higher density of carbon dioxide gas, can adopt less bubbling speed; Can adopt higher bubbling speed when the content of milk of lime is high, otherwise milk of lime content can adopt lower bubbling speed when low, the starting temperature of reaction is 30～55 ℃, lower starting temperature needs more cooling energy and uneconomical, and too high temperature broadens size distribution and is prone to as undesirable particle shapes such as fusiforms;
It is 18～40% gas that carbonated gas is preferably formed the carbonated volumetric concentration similar to actual lime burner furnace gas mixture;
The weight concentration of calcium hydroxide slurry is 5～23% suspension, and is preferred 10～15%, and lower lime milk concentration will make reaction yield reduce, and too high concentration can make the whole reaction system viscosity become big and make reaction be difficult to carry out;
Said crystal structure adjusting agent is selected from the inorganic phosphate of EDTA or its alkaline metal salt, trolamine, ammonia, ammonium salt, alkaline carbonate, solubility, a kind of or its mixture in alkali metal sulfates or alkaline earth metal sulphate, disaccharides or the polysaccharide, preferred ammonium chloride, sucrose, sodium polyphosphate, sodium sulfate or sodium bicarbonate, the amount of crystal structure adjusting agent is 0.1～10% of a gained lime carbonate quality, preferred 0.5-3%;
(2) carbonization to carbonation rate is 90～100% o'clock, adds surface potential and the space resistance of dispersion agent with regulation system, and this is necessary for the powder that obtains favorable dispersity;
It is one or two or more kinds mixture in 600～10000 polyoxyethylene glycol, sodium laurylsulfonate, sodium lauryl sulphate, the fatty alcohol-polyoxyethylene ether that said dispersion agent is selected from polycarboxylate sodium, polyacrylic acid sodium salt, molecular weight, preferred poly carboxylic acid sodium, sodium laurylsulfonate, sodium polyacrylate, the add-on of dispersion agent is 0.1～5%, preferred 0.25～2% of a gained lime carbonate quality;
(3) when the pH of suspension value reduces to 6.5～7.0, ventilated 10～30 minutes, collecting reaction product from reaction product then, promptly obtain the said submicron order calcium carbonate granule of the present invention, its particle diameter is 0.1～1.0 μ m, and its pattern is cube, the mixing of prismatic, grain of rice shape or above several patterns.
By the detailed description of technique scheme as can be seen, the method for preparing the calcium carbonate superfine powder particle dispersion provided by the invention, be suitable for existing all kinds of conversion unit, almost need not increase equipment, just can implement in various intermittent type precipitator method lime carbonate factory, not only be suitable as the paper stopping composition and paper coating pigment has gloss height and low viscosity characteristics, and be suitable for application scenarios such as coating, plastics as semi-reinforcing agent and filler.
Description of drawings
Fig. 1 is the electromicroscopic photograph of finished product.
Embodiment
Embodiment 1
The preparation weight concentration is 10% earlier, and temperature is 30 ℃ calcium hydroxide milk of lime 15L, adds 9.6g ammonium chloride again, and after stirring, this slurry being placed aspect ratio then is 8: 1, and internal diameter is in the bubbling carbonizing tower of 140mm, with 25m
3/ h.m
3It is that 20% carbon dioxide carries out carbonization that the speed of milk of lime feeds volume content, when carbonation rate to 90%, adds 4.8g polypropylene sodium, when carbonization when the pH value is 7, continue ventilation 20 minutes, stop the carbonization of ventilating, then products therefrom is filtered, dries, pulverizes, transmission electron microscope is observed down, electromicroscopic photograph such as Fig. 1, gained shape and appearance of calcium carbonate are cube or prism-shaped that median size is 0.2 μ m, narrow diameter distribution, specific surface area are 16m
2/ g (adopting GB/T2922-1982 " measuring method of chemical reagent chromosorb specific surface area " method to detect), oil-absorption(number) is 56DOPg/100g.
Embodiment 2
Preparation concentration is 10% earlier, and temperature is 55 ℃ calcium hydroxide milk of lime 15L, adds 38.8g sodium sulfate again, and after stirring, this slurry being placed aspect ratio then is 8: 1, and internal diameter is in the bubbling carbonizing tower of 140mm, with 2m
3/ h.m
3It is that 40% carbon dioxide carries out carbonization when carbonation rate to 95% that the speed of milk of lime feeds volume content, add 38.4g polypropylene sodium, when carbonization when the pH value is 6.5, continue ventilation 30 minutes, stop the carbonization of ventilating, then products therefrom is filtered, dries, pulverizes, transmission electron microscope is observed down, and the gained shape and appearance of calcium carbonate is cube or prism-shaped that median size is 0.4 μ m, narrow diameter distribution, specific surface area are 13m
2/ g, oil-absorption(number) are 50DOPg/100g.
Embodiment 3
The preparation weight concentration is 12% earlier, and temperature is 40 ℃ calcium hydroxide milk of lime 15L, adds the 15g sodium bicarbonate again, and after stirring, this slurry being placed aspect ratio then is 8: 1, and internal diameter is in the bubbling carbonizing tower of 140mm, with 15m
3/ h.m
3It is that 30% carbon dioxide carries out carbonization when carbonation rate to 90% that the speed of milk of lime feeds volume content, add the 57.6g sodium laurylsulfonate, when carbonization when the pH value is 6.5, continue ventilation 20 minutes, stop the carbonization of ventilating, then products therefrom is filtered, dries, pulverizes, transmission electron microscope is observed down, and the gained shape and appearance of calcium carbonate is cube or prism-shaped that median size is 0.5 μ m, narrow diameter distribution, specific surface area are 10.3m
2/ g, oil-absorption(number) are 48DOPg/100g.
Embodiment 4
The preparation weight concentration is 15% earlier, and temperature is 40 ℃ calcium hydroxide milk of lime 15L, adds the 86.5g sodium polyphosphate again, and after stirring, this slurry being placed aspect ratio then is 8: 1, and internal diameter is in the bubbling carbonizing tower of 140mm, with 15m
3/ h.m
3It is that 30% carbon dioxide carries out carbonization that the speed of milk of lime feeds volume content, when carbonation rate to 100%, add 10g sodium laurylsulfonate and 6g poly carboxylic acid sodium, continue ventilation 20 minutes, stop the carbonization of ventilating, then products therefrom is filtered, dries, pulverizes, transmission electron microscope is observed down, and the gained shape and appearance of calcium carbonate is cube or prism-shaped that median size is 0.8 μ m, narrow diameter distribution, specific surface area are 7.8m
2/G, oil-absorption(number) are 46DOPg/100g.
Claims (5)
1. the preparation method of a submicron grade superfine calcium carbonate dispersion particle is characterized in that, may further comprise the steps:
(1) crystal structure adjusting agent is added calcium hydroxide slurry, feed the gas that the carbonated volumetric concentration is 10-100% then, Ventilation Rate is 2～50m
3/ (hm
3Milk of lime), the starting temperature of reaction is 30～55 ℃;
The weight concentration of calcium hydroxide slurry is 5～23% suspension;
Said crystal structure adjusting agent is selected from a kind of in inorganic phosphate, disaccharides or the polysaccharide of trolamine, ammonia, ammonium salt, alkaline carbonate, solubility; It perhaps is 0.1～10% sodium bicarbonate of gained lime carbonate quality;
(2) carbonization to carbonation rate is 90～100% o'clock, adds dispersion agent;
It is one or two or more kinds mixture in 600～10000 polyoxyethylene glycol, sodium laurylsulfonate, sodium lauryl sulphate, the fatty alcohol-polyoxyethylene ether that said dispersion agent is selected from poly carboxylic acid sodium, sodium polyacrylate, molecular weight;
(3) when the pH of suspension value reduces to 6.5～7.0, ventilated 10～30 minutes, collecting reaction product from reaction product promptly obtains the submicron order calcium carbonate granule then.
2. method according to claim 1 is characterized in that, Ventilation Rate is 2～25m
3/ (hm
3Milk of lime).
3. method according to claim 1 is characterized in that, the weight concentration of calcium hydroxide slurry is 10～15%.
4. method according to claim 1 is characterized in that said crystal structure adjusting agent is selected from ammonium chloride, sucrose or sodium polyphosphate, and the amount of crystal structure adjusting agent is 0.1～10% of a gained lime carbonate quality.
5. method according to claim 1 is characterized in that said dispersion agent is selected from poly carboxylic acid sodium, sodium laurylsulfonate, sodium polyacrylate, and the add-on of dispersion agent is 0.1～5% of a gained lime carbonate quality.
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| CNB2005100271269A CN100545092C (en) | 2005-06-24 | 2005-06-24 | A kind of preparation method of submicron grade superfine calcium carbonate dispersion particle |
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| CN100545092C true CN100545092C (en) | 2009-09-30 |
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| US9902652B2 (en) | 2014-04-23 | 2018-02-27 | Calera Corporation | Methods and systems for utilizing carbide lime or slag |
| US11377363B2 (en) | 2020-06-30 | 2022-07-05 | Arelac, Inc. | Methods and systems for forming vaterite from calcined limestone using electric kiln |
| US11577965B2 (en) | 2020-02-25 | 2023-02-14 | Arelac, Inc. | Methods and systems for treatment of lime to form vaterite |
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| CN100341786C (en) * | 2006-06-08 | 2007-10-10 | 上海东升新材料有限公司 | Monodispersion cubic light calcium carbonate and its preparation method and application |
| CN100418617C (en) * | 2006-10-11 | 2008-09-17 | 上海东升新材料有限公司 | Dispersant in use for fibroid light calcium, preparation method and application |
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