CN103466678B - Preparation method of special-shaped calcium carbonate - Google Patents
Preparation method of special-shaped calcium carbonate Download PDFInfo
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Abstract
The invention discloses a preparation method of special-shaped calcium carbonate. Through a high shear rate, high pressure and high-temperature reaction of a screw extruder, carbonization is fast completed so that the special-shaped calcium carbonate having a sheet structure is produced continuously, fast and efficiently. The preparation method comprises the following steps of dispersing a crystal form inducer in a calcium hydrate suspension liquid having a high concentration of 20-40%, flocculating the calcium hydrate suspension liquid by a flocculant to obtain pasty slurry, carrying out forced directed extrusion transportation on the pasty slurry to screws by a homodromous twin-screw extruder under the conditions of a rotation rate of 500-800rpm and a screw temperature of 80-120 DEG C so that by crystal form inducer induction, under the action of a high shear rate, high pressure and a high-temperature, the special-shaped calcium carbonate having a sheet structure is fast produced by carbonization, and carrying out two-stage vacuum devolatilization drying and eddy machine-based crushing on the material at a material outlet to obtain the special-shaped calcium carbonate having a sheet structure, radial particle sizes of 1.5-3 microns, sheet thickness of 0.01-0.02 microns and a radius-thickness ratio greater than or equal to 75: 1. The preparation method finishes feeding, a shear reaction and devolatilization drying in one step, realizes continuous operation, can be implemented and controlled easily, has a low cost and is conducive to industrial production.
Description
Technical field
The present invention relates to other shaped calcium carbonate field, be specifically related to a kind of preparation method with the other shaped calcium carbonate of chip architecture.
Background technology
Calcium carbonate is a kind of natural resource, and it mainly comes from calcite, Wingdale and marble, and molecular formula is CaCO
3.Traditional mode of utilizing is to adopt Mechanical Crushing to grind to form calcium carbonate superfine powder after exploitation again, is mainly used in the common fillers of coating, plastics, rubber, papermaking, food, medicine and other fields.Development along with inorganic non-metallic technology, calcium carbonate develops rapidly towards diversification, specialization, the direction that becomes more meticulous, because cuboidal calcium carbonate surface can be lower, the most stable at nature, so in normal circumstances, no matter be directly grind or react by carborization, obtaining crystal structure of calcium carbonate is generally cuboidal structure, its application is subject to certain restrictions, and single super-refinement cannot meet the application needs of calcium carbonate.At present, calcium carbonate is just towards abnormally-structured development, such as the calcium carbonate of sheet, spindle, needle-like, the crystal formation such as spherical, because its special structure makes it, gives material special functional in application.
Flaky calcium carbonate is a kind of functional calcium carbonate with level and smooth sheet structure, its slickness is high, glossiness is high, shading power is strong, in industries such as lubricated, papermaking, coating, paint, have high using value, therefore, flaky calcium carbonate had obtained developing fast and applying in recent years.Due to its good sheet structure and sliding, can be used as antifriction material for all kinds of lubricating grease; In papermaking, flaky calcium carbonate is conducive in page, retain and improve paper opaqueness, smoothness and printability, prevents printing-ink infiltration page; In Paper Coating, flaky calcium carbonate orderly arrangement in coating, coating structure is closely knit, thereby can improve print gloss, reduce coating Gas permeability, gives fiber-covered rate that paper coating is good and higher smoothness; In paint, the alternative Rutile type Titanium Dioxide of flaky calcium carbonate is given whiteness, the gloss and opacifying property that coating is good, well being applied of the senior paint of automobile.
Flaky calcium carbonate technology has two kinds of routes conventionally at present: a kind of is that calcium carbonate is fired, digested for Ca (OH)
2suspension liquid passes into CO in carbonating tower
2gas carries out carbonization, by chemical additives, can control calcium carbonate crystal formation, obtains flaky calcium carbonate.As the patent of notification number CN100400422C discloses a kind of preparation technology of tabular light calcium carbonate, the method will digest Ca (OH)
2slurries are put into jacket reactor, and stirring is also cooling, makes the temperature of slurries be reduced to 10-40 degree, open carbonic acid gas carbonization, add chemical additives, carbonization finishes rear carbonization 10 minutes of crossing, then continue to stir 1-3h, finally wash, dewater, be dried, sieving obtains flake light calcium carbonate.Although be controlled in carbonating tower and can obtain flaky calcium carbonate by crystal formation, but because the reaction times surpasses more than 1 hour, energy consumption is high, cost is high, has limited the application of flaky calcium carbonate, and flaky calcium carbonate chemical additives inducibility is limited especially at present, the flaky calcium carbonate radius-thickness ratio obtaining is lower, be generally 5:1-10:1, therefore, using value limitation is very large.Another kind is that calcium carbonate is directly ground and obtained, as the patent of notification number CN101514533B discloses a kind of flaky calcium carbonate and its preparation method and application, the method is added to the water fibrous light cakium carbonate, and Xiang Shuizhong adds composite grinding aids to grind slurry, make flaky calcium carbonate slurry.The patent of publication number CN101514028 discloses the method for flaky ground calcium carbonate powder, and the method be take calcite ore as raw material, by horizontal ball mill, grinds, and obtains flaky ground calcium carbonate powder.By polishing, prepare flaky calcium carbonate more than half an hour consuming time, belong to batch production, not only efficiency is low, energy consumption is high, and owing to there is powerful grinding, radius-thickness ratio loss is serious, and general footpath is thick only has 5:1.
According to above-mentioned, the flaky calcium carbonate that technical qualification obtain is at present owing to being subject to the restriction of crystal formation inductor and reaction conditions, not only length consuming time, energy consumption is high, cost is high, and the radius-thickness ratio of flaky calcium carbonate is lower, fail to give full play to the characteristic of flaky calcium carbonate smoothness, high gloss, high covering power.
Summary of the invention
For prior art, prepare the defect that the flaky calcium carbonate time is long, energy consumption is high, crystal formation inductor inducibility is limited, the invention provides a kind of preparation method of other shaped calcium carbonate, specifically a kind of preparation method with chip architecture other shaped calcium carbonate.
For achieving the above object, the present invention proposes a kind of preparation method of other shaped calcium carbonate, it is characterized in that high-shear, high pressure, the pyroreaction by screw extruder completes carbonization fast, thereby rapidly and efficiently generates continuously the other shaped calcium carbonate of chip architecture.
The preparation method of a kind of other shaped calcium carbonate that the present invention proposes, comprises following concrete steps:
(1) calcium hydroxide and water are mixed with by weight to the suspension of 20-40% in high-speed mixer, in suspension, add crystal formation inductor, and constantly stir 1-3 minute with the speed of 100-200rpm, crystal formation inductor is dispersed in suspension completely, and crystal formation inductor add-on is the 1-3% of calcium hydroxide weight;
(2) flocculation agent, release of carbonate dioxide agent, pore forming material are added in step (1), and constantly stir 5-10 minute with the speed of 50-80rpm, finally flocculate to paste slurry, flocculant addition is the 2-5% of calcium hydroxide weight, release of carbonate dioxide agent add-on is 3% of calcium hydroxide weight, and pore forming material add-on is the 0.2-0.5% of calcium hydroxide weight;
(3) the paste slurry obtaining in step (2) is pumped into screw extruder, screw extruder is by carrying screwing element, thread engagement element, compression screwing element is arranged on mandrel with cord wood, form transportation section, shear section section, compression section three parts, control extruder temperature 80-120 ℃, under the high speed rotating condition of 500-800rpm, produce and shear, screw extruder delivers into screw rod by the enforceable directed extruding of slurry, slurry is axially being sheared and is being cut into slices, and in compression section, produce the high pressure of 15-20MPa, the continuous carbon dioxide gas of release of carbonate dioxide agent, by the strong shearing of screw extruder and high pressure, strengthening carbonic acid gas osmosis, by crystal formation inductor, induce, in high-shear, under the effect of high pressure and high temperature, complete fast the other shaped calcium carbonate that carbonization forms chip architecture, the last other shaped calcium carbonate of dry chip architecture that obtains by vacuum volatilization at discharge port,
(4) the other shaped calcium carbonate obtaining in step (3) is dropped into eddy airstream pulverizer, obtain radially particle diameter 1.5-3 μ m, the thick 0.01-0.02 μ of sheet m, the chip architecture other shaped calcium carbonate of radius-thickness ratio >=75:1.
Screw extruder described in above-mentioned preparation method is that parallel dual-screw is forced extrusion machine, and screw diameter is 120-180mm.
Screw extruder described in above-mentioned preparation method, wherein said thread engagement element oblique angle is 60 ° and 90 °, during bolt rotary, paste slurry produces the exchange of axial material and moves back and forth, carbonic acid gas generation carburizing reagent with continuous release, slurry is constantly sheared, is orientated, cuts, folds, reorientation, thereby flash carbonization obtains shearing section.
Screw extruder described in above-mentioned preparation method has stable transport efficiency and the residence time of material of stable and uniform, and slurry stops 10-15min in screw extruder.The temperature that screw extruder transportation section described in above-mentioned preparation method, shearing section section, compression section are set is followed successively by 80 ℃, 120 ℃, 100 ℃, 120 ℃ of discharge port design temperatures, at material outlet, secondary vacuum volatilization device is set, be less than-1.5Mpa of vacuum volatilization pressure, guarantees flaky calcium carbonate water content≤0.5%.
Crystal formation inductor described in above-mentioned preparation method is a kind of in stratiform calcium sulfate, lamina sodium silicate, layered magnesium silicate.
Flocculation agent described in above-mentioned preparation method is a kind of in polyaluminium sulfate, polyacrylamide, alum.
Release of carbonate dioxide agent described in above-mentioned preparation method is sodium bicarbonate.
Pore forming material described in above-mentioned preparation method is a kind of in polyvinyl alcohol, polyoxyethylene sorbitan monooleate, glyceryl monostearate, Tween-20, this pore forming material is a kind of interfacial agent, can in flocculation paste slurry, form micro bubble, for the carbonic acid gas of follow-up release provides space, increase carburizing reagent interface.
The preparation method of a kind of other shaped calcium carbonate of the present invention, its outstanding feature is:
1, the present invention has realized continuous high-efficient carbonization by high-shear section, high pressure, the high temperature of screw extruder and has prepared other shaped calcium carbonate, has obtained the other shaped calcium carbonate of high radius-thickness ratio chip architecture, has solved the limited defect of current crystal formation inductor inducibility;
2, the present invention has realized flash carbonization under High Concentration Situation by flocculation agent, built-in release of carbonate dioxide agent and has prepared other shaped calcium carbonate;
3, disposable in screw extruder to complete conveying, cleavage reaction, devolatilization dry in the present invention, can continuous operation, easy to implement with control, with low cost, be beneficial to suitability for industrialized production;
The other shaped calcium carbonate of the chip architecture that 4, the present invention obtains has excellent radius-thickness ratio, glossiness, smoothness, whiteness, shading performance, can be widely used in the fields such as lubricated, papermaking, coating, paint;
5, the chip architecture other shaped calcium carbonate that the preparation method of a kind of other shaped calcium carbonate of the present invention makes has excellent performance, and the key technical indexes is as following table 1:
| Project | Test condition | Other shaped calcium carbonate of the present invention |
| Size distribution | Laser particle size analyzer | Particle diameter 1.5-3 μ m is greater than 97% |
| Median size | Laser particle size analyzer | 2.3μm |
| Average diameter thickness rate | ? | ≥150：1 |
| Whiteness | 457nm place | ≥96% |
Table 1
The chip architecture other shaped calcium carbonate that the preparation method of a kind of other shaped calcium carbonate of the present invention makes has excellent performance, and the paper coating the key technical indexes of preparing with it is as following table 2:
| Project | Test condition | The coating of other shaped calcium carbonate of the present invention |
| Smoothness | GB/T456 | ≥800s |
| Glossiness | GB/T8941 | ≥75% |
| Opaqueness | GB/T1541 | ≥97% |
| Whiteness | GB/T7949 | ≥91% |
Table 2.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that the preparation method of a kind of other shaped calcium carbonate of the present invention adopts.
Embodiment
Following embodiment, is described in further detail foregoing of the present invention again.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following example.Without departing from the idea case in the present invention described above, various replacements or the change according to ordinary skill knowledge and customary means, made, all should comprise within the scope of the invention.
embodiment 1
(1) in SL300 high-speed mixer, 40kg calcium hydroxide and 60kg water are mixed with to 40% suspension, in suspension, add 0.8kg lamina sodium silicate, and constantly stir 3 minutes with the speed of 200rpm, make lamina sodium silicate be dispersed in suspension completely;
(2) 0.8k polyacrylamide, 1.2kg sodium bicarbonate, 0.08kg polyvinyl alcohol 2488 are added in step (1), and constantly stir 10 minutes with the speed of 50rpm, finally flocculate to paste;
(3) the paste slurry obtaining in step (2) is pumped into screw extruder, control extruder temperature 80-120 ℃, under the high speed rotating condition of 800rpm, produce and shear, screw extruder delivers into screw rod by the enforceable directed extruding of slurry, slurry is axially being sheared and is being cut into slices, and in compression section, produce the high pressure of 20MPa, the continuous carbon dioxide gas of release of carbonate dioxide agent, by the strong shearing of screw extruder and high pressure, strengthening carbonic acid gas osmosis, by crystal formation inductor, induce, in high-shear, under the effect of high pressure and high temperature, complete fast the other shaped calcium carbonate that carbonization forms chip architecture, finally at discharge port, by vacuum volatilization, obtain dry chip architecture other shaped calcium carbonate,
(4) the chip architecture other shaped calcium carbonate obtaining in step (3) is dropped into eddy airstream pulverizer, obtain chip architecture other shaped calcium carbonate fine powder.
By detecting: the other shaped calcium carbonate obtaining is white powder crystal, and crystal more than 97% is oval sheet, average radial particle diameter 2.3 μ m, the thick 0.01-0.02 μ of sheet m, average diameter thickness rate 150:1, BET specific surface area 7.5m2/g, whiteness 96%.
70 parts of other shaped calcium carbonate of the present invention and 30 parts of china clay are prepared into Paper Coating material to be detected: during glue spread 20g/m2, and glossiness 75.6%, smoothness 822s, opaqueness 97%.
embodiment 2
(1) in SL300 high-speed mixer, 30kg calcium hydroxide and 70kg water are mixed with to 30% suspension, in suspension, add 0.6kg layered magnesium silicate, and constantly stir 3 minutes with the speed of 200rpm, make layered magnesium silicate be dispersed in suspension completely;
(2) 1.2kg alum, 0.9kg sodium bicarbonate, 0.12kg glyceryl monostearate are added in step (1), and constantly stir 5 minutes with the speed of 50rpm, finally flocculate to paste;
(3) the paste slurry obtaining in step (2) is pumped into screw extruder, control extruder temperature 80-120 ℃, under the high speed rotating condition of 800rpm, produce and shear, screw extruder delivers into screw rod by the enforceable directed extruding of slurry, slurry is axially being sheared and is being cut into slices, and in compression section, produce the high pressure of 20MPa, the continuous carbon dioxide gas of release of carbonate dioxide agent, by the strong shearing of screw extruder and high pressure, strengthening carbonic acid gas osmosis, by crystal formation inductor, induce, in high-shear, under the effect of high pressure and high temperature, complete fast the other shaped calcium carbonate that carbonization forms chip architecture, finally at discharge port, by vacuum volatilization, obtain dry chip architecture other shaped calcium carbonate,
(4) the chip architecture other shaped calcium carbonate obtaining in step (3) is dropped into eddy airstream pulverizer, obtain chip architecture other shaped calcium carbonate fine powder.
By detecting: the other shaped calcium carbonate obtaining is white powder crystal, and crystal more than 97% is oval sheet, average radial particle diameter 2.2 μ m, the thick 0.01-0.02 μ of sheet m, average diameter thickness rate 200:1, BET specific surface area 7.8m2/g, whiteness 97%.
70 parts of other shaped calcium carbonate of the present invention and 30 parts of china clay are prepared into Paper Coating material to be detected: during glue spread 16g/m2, and glossiness 75%, smoothness 1100s, opaqueness 97%.
embodiment 3
(1) in SL300 high-speed mixer, 20kg calcium hydroxide and 80kg water are mixed with to 20% suspension, in suspension, add 0.2kg stratiform calcium sulfate, and constantly stir 2 minutes with the speed of 100rpm, make stratiform calcium sulfate be dispersed in suspension completely;
(2) 0.4kg polyaluminum sulfate al alum, 0.6kg sodium bicarbonate, 0.04kg polyoxyethylene sorbitan monooleate are added in step (1), and constantly stir 8 minutes with the speed of 80rpm, finally flocculate to paste;
(3) the paste slurry obtaining in step (2) is pumped into screw extruder, control extruder temperature 80-120 ℃, under the high speed rotating condition of 800rpm, produce and shear, screw extruder delivers into screw rod by the enforceable directed extruding of slurry, slurry is axially being sheared and is being cut into slices, and in compression section, produce the high pressure of 20MPa, the continuous carbon dioxide gas of release of carbonate dioxide agent, by the strong shearing of screw extruder and high pressure, strengthening carbonic acid gas osmosis, by crystal formation inductor, induce, in high-shear, under the effect of high pressure and high temperature, complete fast the other shaped calcium carbonate that carbonization forms chip architecture, finally at discharge port, by vacuum volatilization, obtain dry chip architecture other shaped calcium carbonate,
(4) the chip architecture other shaped calcium carbonate obtaining in step (3) is dropped into eddy airstream pulverizer, obtain chip architecture other shaped calcium carbonate fine powder.
By detecting: the other shaped calcium carbonate obtaining is white powder crystal, and crystal more than 98% is oval sheet, average radial particle diameter 2.5 μ m, the thick 0.01-0.02 μ of sheet m, average diameter thickness rate 180:1, BET specific surface area 7.3m2/g, whiteness 96%.
70 parts of other shaped calcium carbonate of the present invention and 30 parts of china clay are prepared into Paper Coating material to be detected: during glue spread 25g/m2, and glossiness 77%, smoothness 960s, opaqueness 98%.
Claims (4)
1. a preparation method for other shaped calcium carbonate, is characterized in that utilizing high-shear, high pressure, the pyroreaction of screw extruder, under crystal formation inductor inducing action, completes fast the other shaped calcium carbonate that carbonization forms chip architecture, and concrete preparation process is as follows:
(1) calcium hydroxide and water are mixed with by weight to the suspension of 20-40% in high-speed mixer, in suspension, add crystal formation inductor, and constantly stir 1-3 minute with the speed of 100-200rpm, make crystal formation inductor be dispersed in suspension completely, crystal formation inductor add-on is the 1-3% of calcium hydroxide weight, and described crystal formation inductor is a kind of in stratiform calcium sulfate, lamina sodium silicate, layered magnesium silicate;
(2) flocculation agent, release of carbonate dioxide agent, pore forming material are added in step (1), and constantly stir 5-10 minute with the speed of 50-80rpm, finally flocculate to paste slurry, flocculant addition is the 2-5% of calcium hydroxide weight, release of carbonate dioxide agent add-on is 3% of calcium hydroxide weight, pore forming material add-on is the 0.2-0.5% of calcium hydroxide weight, and described flocculation agent is a kind of in polyaluminium sulfate, polyacrylamide, alum; Described release of carbonate dioxide agent is sodium bicarbonate; Described pore forming material is a kind of in polyvinyl alcohol, polyoxyethylene sorbitan monooleate, glyceryl monostearate, Tween-20;
(3) the paste slurry obtaining in step (2) is pumped into screw extruder, screw extruder is by carrying screwing element, thread engagement element, compression screwing element is arranged on mandrel with cord wood, form transportation section, shear section section, compression section three parts, control extruder temperature 80-120 ℃, under the high speed rotating condition of 500-800rpm, produce and shear, screw extruder delivers into screw rod by the enforceable directed extruding of paste slurry, slurry is axially being sheared and is being cut into slices, and in compression section, produce the high pressure of 15-20MPa, the continuous carbon dioxide gas of release of carbonate dioxide agent, by the strong shearing of screw extruder and high pressure, strengthening carbonic acid gas osmosis, by crystal formation inductor, induce, in high-shear, under the effect of high pressure and high temperature, complete fast the other shaped calcium carbonate that carbonization forms chip architecture, finally at discharge port, by vacuum volatilization, obtain dry chip architecture other shaped calcium carbonate,
(4) the other shaped calcium carbonate obtaining in step (3) is dropped into eddy airstream pulverizer, obtain radially particle diameter 1.5-3 μ m, the thick 0.01-0.02 μ of sheet m, the chip architecture other shaped calcium carbonate of radius-thickness ratio >=75:1.
2. the preparation method of a kind of other shaped calcium carbonate as described in claim 1, is characterized in that the described screw extruder of step (3) is that parallel dual-screw is forced extrusion machine, and screw diameter is 120-180mm.
3. the preparation method of a kind of other shaped calcium carbonate as described in claim 1, it is characterized in that the described thread engagement element oblique angle of step (3) is 60 ° and 90 °, during bolt rotary, paste slurry produces the exchange of axial material and moves back and forth, carbonic acid gas generation carburizing reagent with continuous release, slurry is constantly sheared, is orientated, cuts, folds, reorientation, thereby flash carbonization obtains shearing section.
4. the preparation method of a kind of other shaped calcium carbonate as described in claim 1, the temperature of it is characterized in that the described screw extruder transportation section of step (3), shear section section, compression section being set is followed successively by 80 ℃, 120 ℃, 100 ℃, 120 ℃ of discharge port design temperatures, and secondary vacuum volatilization device is set, be less than-1.5Mpa of vacuum volatilization pressure, guarantees other shaped calcium carbonate water content≤0.5%.
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| US9902652B2 (en) | 2014-04-23 | 2018-02-27 | Calera Corporation | Methods and systems for utilizing carbide lime or slag |
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| CN107881840A (en) * | 2017-11-02 | 2018-04-06 | 洪飞飞 | A kind of preparation method of the antibacterial foam wallpaper with lasting health-care efficacy |
| CN107642004A (en) * | 2017-11-02 | 2018-01-30 | 洪飞飞 | A kind of preparation method of the antibacterial foam wallpaper with durable antibiotic effect |
| WO2021173790A1 (en) | 2020-02-25 | 2021-09-02 | Arelac, Inc. | Methods and systems for treatment of lime to form vaterite |
| CA3182421A1 (en) | 2020-06-30 | 2022-01-06 | Ryan J. Gilliam | Methods and systems for forming vaterite from calcined limestone using electric kiln |
| CN112142087A (en) * | 2020-09-29 | 2020-12-29 | 王权广 | Process for preparing regular spherical calcium carbonate by calcium chloride and ammonia water solution carbonization method |
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| CN100542965C (en) * | 2007-06-28 | 2009-09-23 | 上海东升新材料有限公司 | Calcium carbonate for cigarette paper and its production and application |
| CN100542964C (en) * | 2007-06-28 | 2009-09-23 | 上海东升新材料有限公司 | A kind of preparation method of calcium carbonate for cigarette paper |
| JP5673176B2 (en) * | 2010-06-28 | 2015-02-18 | 王子ホールディングス株式会社 | Slaked lime particles, method for producing light calcium carbonate, and paper and coated paper using light calcium carbonate obtained thereby |
| CN101967000B (en) * | 2010-07-14 | 2013-04-24 | 山东海泽纳米材料有限公司 | Method for preparing high-solid-content and low-viscosity suspended nano calcium carbonate slurry |
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Effective date of registration: 20180427 Address after: 318000 1055 Gaoxin Road, Taizhou Economic Development Zone, Zhejiang Patentee after: ZHEJIANG LINXIANG PLASTIC CO., LTD. Address before: 610091 Donghai Road, Jiao long industrial port, Qingyang District, Chengdu, Sichuan 4 Patentee before: Chengdu Xinkeli Chemical Sci-Tech Co., Ltd. |
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