CN1038578C - Preparation method of superfine calcium carbonate - Google Patents
Preparation method of superfine calcium carbonate Download PDFInfo
- Publication number
- CN1038578C CN1038578C CN95105343A CN95105343A CN1038578C CN 1038578 C CN1038578 C CN 1038578C CN 95105343 A CN95105343 A CN 95105343A CN 95105343 A CN95105343 A CN 95105343A CN 1038578 C CN1038578 C CN 1038578C
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- China
- Prior art keywords
- rotating bed
- emulsion
- reaction
- calcium carbonate
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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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 32
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000005484 gravity Effects 0.000 claims abstract description 10
- 238000012856 packing Methods 0.000 claims abstract description 5
- 239000000839 emulsion Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 10
- 238000005255 carburizing Methods 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/30—Micromixers
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明为一种超细碳酸钙的制备方法。本发明采用在旋转床超重力场条件下的碳化反应，碳化反应在床层的多孔填料层超重力场下进行，极大强化了反应的传质过程及微观混合过程，有效地克服了常重力场下颗粒不够超细化、粒度分布不均匀、反应时间长等缺点，使碳酸钙的平均粒径达到10-100nm，且分布均匀，大幅度地提高了生产效率及产品的品位。本发明的方法易于工业化。
The invention relates to a preparation method of superfine calcium carbonate. The present invention adopts the carbonization reaction under the condition of the rotating bed supergravity field, and the carbonization reaction is carried out under the supergravity field of the porous packing layer of the bed, which greatly strengthens the mass transfer process and the microscopic mixing process of the reaction, and effectively overcomes the constant gravity The off-site particles are not ultra-fine enough, the particle size distribution is uneven, and the reaction time is long. The average particle size of calcium carbonate reaches 10-100nm, and the distribution is uniform, which greatly improves the production efficiency and product quality. The method of the present invention is easy to industrialize.
Description
The present invention relates under the rotating bed super gravity condition, prepare the method for calcium carbonate superfine powder.
Lime carbonate is widely used in many industries such as coating, printing ink, medicine, rubber, plastics, papermaking, microelectronics, automobile.In recent years, the development along with super-refinement, structure complicated and the sufacing of lime carbonate makes the using value of calcium carbonate superfine powder improve significantly.
At present, the common method for preparing calcium carbonate superfine powder in the world is normal gravity field carborization, adopt usually earth gravity after the match stirring tank or bubble tower as carbonization reactor, with CO
2Be passed into and fill Ca (OH)
2Carry out carburizing reagent in the carbonization still of emulsion or the tower, generally finish the preparation of calcium carbonate superfine powder by adding additives such as crystal control agent.Because the rate of mass transfer between the gas-liquid solid phase is slower in stirring tank or bubble tower, it is poor that microcosmic mixes, thereby there is following shortcoming in prepared particulate product: 1, particle diameter generally at the several μ m of 0.1 μ m-(referring to Chinese patent 93108625.6, Japanese Patent 93,228,730 and 93,221,634); 2, carbonization time is long, often needs several hrs, and production efficiency is low, energy consumption big (referring to Chinese patent 93108625.6, the Huadong Chemical College journal is rolled up 19 phases, 5 pages of 550-556); 3, size-grade distribution is even inadequately.The raising and the industrial applications of calcium carbonate product grade and quality have been hindered.Stirring tank or bubble tower take up space also bigger in addition.
Purpose of the present invention: the microcosmic of strengthening carbonization process under super gravity field mixes and the microcosmic mass transfer process, under not additivated situation, can reach the purpose that makes calcium carbonate granule ultramicronising, even particle size distribution, shortening carbonization time.
The invention main points: calcium carbonate superfine powder preparation method of the present invention, comprise the postprocessing working procedures of carburizing reagent and product, carburizing reagent is carried out under the rotating bed super gravity condition, and concrete step is: will contain CO
2Gas with contain Ca (OH)
2Lime emulsion feed the rotating bed super gravity field device by inlet mouth and fluid inlet respectively.In the protruded packing layer of rotating bed carburizing reagent takes place, emulsion after reaction is discharged by the rotating bed discharge gate.Wherein, the rotating speed of rotating bed rotor is 100-10000rpm, and the flow of gas is with the clean CO of standard state
2Meter is controlled at 0.1-10m
3/ hKgCaO.
The above-mentioned CO that contains
2Gas can be commercially pure CO
2Or CO
2The mixed gas of content 〉=10%.
Method of the present invention does not have particular requirement to the temperature of carburizing reagent, but with 10-90 ℃ for well.
The rotating speed of rotating bed rotor is 200-2000rpm preferably.
The flow of gas is with the clean CO of standard state
2Meter preferably is controlled at 0.2-4.8m
3/ hKgCaO.
Emulsion from discharge gate is discharged turns back to rotating bed through the circulation storage tank, continues reaction, through 5-30min (minute), the pH value of emulsion becomes 7-8, shows that carbonization is complete, product enters postprocessing working procedures such as filtration, drying, obtains calcium carbonate superfine powder.This is semi-batch preparation technology of the present invention.
Emulsion from discharge gate is discharged also can directly enter postprocessing working procedures such as separation, filtration, drying, obtains calcium carbonate superfine powder.This is continous way preparation technology of the present invention.
In carbonation reaction, add dispersion agent, crystal control agent, can make the further refinement of particle, the size distribution that narrows, and control CaCO
3The crystalline shape.
The calcium carbonate superfine powder that makes through method of the present invention, median size can be controlled in 10-100nm, and size distribution is even, and carbonization time shortens 5-30 doubly than the method for normal gravity field, improve the grade of production efficiency and product greatly, dwindled the shared space of reactor simultaneously.
Below in conjunction with drawings and Examples method of the present invention is described further.
Fig. 1, semi-batch process flow sheet of the present invention.
Fig. 2, continuous process schema of the present invention.
Embodiment 1:
Adopt semi-batch technical process of the present invention (Fig. 1).Claim 2.2KgCaO, with the digestion of 20l water, form lime emulsion, remove impurity after filtration, place circulation storage tank 13, be heated to 40 ℃, by pump 12, emulsion through sparger 9, enters protruded packing layer 8 from rotating bed fluid inlet 6; CO
2Gas from the steel cylinder source of the gas through the decompression after, with 3m
3The flow of/h feeds rotating bed, CO continuously from inlet mouth 4
2With contain Ca (OH)
2Emulsion in the protruded packing layer 8 of bed, carburizing reagent takes place under the situation of high turbulence, generate the calcium carbonate superfine particle.Controls revolution bed rotor speed is 720rpm, and emulsion after reaction enters circulation storage tank 13 by rotating bed discharge gate 7, constantly by pump circulation and CO
2React in rotating bed, through 18min, the pH value of emulsion becomes 7-8, and carbonization is complete, and after filtration, after the drying, X TEM (transmission electron microscope) analysis, the ultra-fine CaCO that obtains are made in sampling
3Median size is about 50nm.
Embodiment 2:
Except that following variation, all the other are with embodiment 1.
Logical water coolant, control reaction temperature is between 20-30 ℃, and rotating bed rotor speed is 900rpm, CO
2Initial flow is 5m
3/ h.After reaction for some time, CO is arranged at the rotating bed gas outlet
2When gas is emerged, control CO
2Flow is 1m
3/ h.Complete through the 15min carbonization, as to obtain CaCO
3Median size is about 40nm.
Embodiment 3:
Except that following variation, all the other are with embodiment 1.
Rotating bed rotor speed is 1400rpm, CO
2The flow of gas is 5m
3/ h, complete through the 10min carbonization, the lime carbonate median size that obtains is 30nm.
Embodiment 4:
Except that following variation, all the other are with embodiment 1.
CO
2Source of the gas adopts and contains 40%CO
2Air gas mixture, by CO
2Air behind steel cylinder gas and the compressed machine is mixed and forms, and the control mixed gas flow is 7.5m
3/ h.
Embodiment 5:
Except that following variation, all the other are with embodiment 1.
Adopt continuous process flow of the present invention (Fig. 2).Claim 0.2KgCaO.Keep CO
2Gas is with 5m
3/ h feeds rotating bed continuously, and the rotating speed of rotating bed rotor is 1800rpm, and emulsion after reaction is discharged from discharge gate 7, through separation, filtration, drying, and the CaCO that obtains
3Median size be about 30nm.
Claims (3)
1, a kind of preparation method of calcium carbonate superfine powder comprises the postprocessing working procedures of carburizing reagent and product, and it is characterized in that: carburizing reagent is carried out under the rotating bed super gravity condition, and concrete step is: will contain CO
2Gas and contain Ca (OH)
2Lime emulsion feed the rotating bed super gravity field device by inlet mouth and fluid inlet respectively, in the protruded packing layer generation carburizing reagent of rotating bed, the rotating speed of rotating bed rotor is 100-10000rpm, with the clean CO of standard state
2Meter, the flow control of gas is at 0.1-10m
3/ hKgCaO.Emulsion after reaction is discharged through the rotating bed discharge gate, directly enters to comprise separation, filtration, exsiccant postprocessing working procedures.
2, method according to claim 1 is characterized in that: the rotating speed of rotating bed rotor is 200-2000rpm, with the clean CO of standard state
2Meter, the flow control of gas is at 0.2-4.8m
3/ hKgCaO, temperature of reaction is controlled at 10-90 ℃.
3, according to the method for claim 1 or 2, it is characterized in that: from the emulsion that discharge gate is discharged, circulation is returned rotating bed and is continued reaction, and until the pH=7-8 of emulsion, emulsion enters the postprocessing working procedures of product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95105343A CN1038578C (en) | 1995-05-26 | 1995-05-26 | Preparation method of superfine calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95105343A CN1038578C (en) | 1995-05-26 | 1995-05-26 | Preparation method of superfine calcium carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1116185A CN1116185A (en) | 1996-02-07 |
| CN1038578C true CN1038578C (en) | 1998-06-03 |
Family
ID=5075490
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95105343A Expired - Lifetime CN1038578C (en) | 1995-05-26 | 1995-05-26 | Preparation method of superfine calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1038578C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441285C (en) * | 2003-09-24 | 2008-12-10 | 北京化工大学 | A kind of supergravity-supercritical reaction/crystallization device and its application |
| US7507813B2 (en) | 2004-07-22 | 2009-03-24 | Nanomaterials Technology Pte Ltd. | Amorphous cefuroxime axetil and preparation process therefore |
| US7893301B2 (en) | 2007-04-06 | 2011-02-22 | Ningbo Wanhua Polyurethanes Co., Ltd. | Method of preparing polymethylene-polyphenyl-polyamine |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112320C (en) * | 2000-01-18 | 2003-06-25 | 北京化工大学 | Process for preparing calcium carbonate deposit by continuous method |
| WO2003055804A1 (en) * | 2001-12-31 | 2003-07-10 | Nanomaterials Technology Pte Ltd. | Calcium carbonate of different shapes and the preparing process thereof |
| CN1429772B (en) * | 2001-12-31 | 2010-12-08 | 纳米材料科技有限公司 | Process for preparing calcium carbonate with specific morphology |
| CN100417436C (en) * | 2005-07-14 | 2008-09-10 | 中国石油化工股份有限公司 | A method for catalytic selective hydrogenation |
| CN101130585B (en) | 2006-08-25 | 2010-11-10 | 北京化工大学 | Method for preparing isobutylene isoprene rubber |
| CN101507908B (en) | 2009-04-09 | 2010-12-01 | 北京化工大学 | Microchannel Sleeve Device and Its Application |
| CN102127223B (en) * | 2010-01-15 | 2012-10-17 | 北京化工大学 | A kind of preparation method of micro/nanometer polyaniline |
| CN103113947A (en) * | 2013-03-06 | 2013-05-22 | 清华大学 | A biogas separation and purification device and its method for absorbing CO2 and purifying biogas by alkaline method |
| CN103521160A (en) * | 2013-09-29 | 2014-01-22 | 北京化工大学 | Multifunctional and multipurpose multistage rotary packed bed reactor device and method for performing multiphase and multicomponent reaction by using device |
| CN104975168A (en) * | 2014-04-01 | 2015-10-14 | 北京化工大学 | Method for rapidly desulfurizing lead-sulfate-containing substances |
| CN105417564B (en) * | 2015-09-14 | 2017-12-15 | 广西大学 | A kind of preparation method of petal flaky calcium carbonate crystal |
| TWI636957B (en) * | 2017-12-13 | 2018-10-01 | 財團法人工業技術研究院 | Method for preparing calcium carbonate particles |
| CN113753932A (en) * | 2021-09-16 | 2021-12-07 | 乌海市创美佳新材料科技有限公司 | Nano-scale light calcium carbonate carbonization reaction system |
| GR1010709B (en) | 2023-05-12 | 2024-06-19 | Εθνικο Κεντρο Ερευνας Και Τεχνολογικης Αναπτυξης (Ε.Κ.Ε.Τ.Α.), | One-step hydromagnesite nanoparticles production method performed in an intensified rotating bed arrangement furnished with filler |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3669620A (en) * | 1969-09-08 | 1972-06-13 | Tate & Lyle Ltd | Manufacture of aragonite |
| CN1023029C (en) * | 1992-04-03 | 1993-12-08 | 北京化工学院 | Method for deoxidizing water to be filled in oil field |
-
1995
- 1995-05-26 CN CN95105343A patent/CN1038578C/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3669620A (en) * | 1969-09-08 | 1972-06-13 | Tate & Lyle Ltd | Manufacture of aragonite |
| CN1023029C (en) * | 1992-04-03 | 1993-12-08 | 北京化工学院 | Method for deoxidizing water to be filled in oil field |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441285C (en) * | 2003-09-24 | 2008-12-10 | 北京化工大学 | A kind of supergravity-supercritical reaction/crystallization device and its application |
| US7507813B2 (en) | 2004-07-22 | 2009-03-24 | Nanomaterials Technology Pte Ltd. | Amorphous cefuroxime axetil and preparation process therefore |
| US7893301B2 (en) | 2007-04-06 | 2011-02-22 | Ningbo Wanhua Polyurethanes Co., Ltd. | Method of preparing polymethylene-polyphenyl-polyamine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1116185A (en) | 1996-02-07 |
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Owner name: SINGAPORE NANO MATERIAL TECHNOLOGY CO.,LTD. Free format text: FORMER OWNER: BEIJING CHEMICAL ENGINEERING UNIV. Effective date: 20020208 |
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Effective date of registration: 20020208 Address after: No. 336 Smith Road, Singapore, 06-308 Patentee after: Nanomaterials Technology Pte L. Address before: 100029, No. 15 East Third Ring Road, Chaoyang District, Beijing Patentee before: Beijing University of Chemical Technology |
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Expiration termination date: 20150526 Granted publication date: 19980603 |