CN1116185A - Ultra-fine calcium carbonate preparation method - Google Patents
Ultra-fine calcium carbonate preparation method Download PDFInfo
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- CN1116185A CN1116185A CN95105343A CN95105343A CN1116185A CN 1116185 A CN1116185 A CN 1116185A CN 95105343 A CN95105343 A CN 95105343A CN 95105343 A CN95105343 A CN 95105343A CN 1116185 A CN1116185 A CN 1116185A
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- emulsion
- rotating bed
- gas
- calcium carbonate
- bed
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- 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
Abstract
Said invention adopts rotary bed ultragravity field device as the reactor of carbonizing reaction which reacts under ultrogravity field of porous padding layer, the mass-transfer and micromixing process is intensified greatly, the shortage under common gravity field is overcome, the particle diameter on average reaches 10-100 nm and is distributed homogeneously, and the quality and productivity is raised greatly. Said method is easy to be industrialized.
Description
The present invention relates to a kind of method of utilizing the rotating bed super gravity field device to prepare 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 0.1 μ m-several 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 5 page 550-556 of 19 phase); 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, adopt the rotating bed super gravity field device to replace conventional stirring tank or bubble tower reactor as carburizing reagent.To contain CO
2Gas with contain Ca (OH)
2Lime emulsion feed rotating bed by inlet mouth and fluid inlet respectively, carburizing reagent takes place in the protruded packing layer of bed, 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 times 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 2.2K9CaO, 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 (4)
1, a kind of preparation method of calcium carbonate superfine powder comprises it is characterized in that the postprocessing working procedures of carburizing reagent and product: adopt the reactor of rotating bed super gravity field device as carburizing reagent, will contain CO
2Gas and contain Ca (OH)
2Lime emulsion feed rotating bed by inlet mouth and fluid inlet respectively, in the protruded packing layer generation carburizing reagent of bed, emulsion after reaction is discharged through the rotating bed discharge gate, 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.
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.
4, according to the method for claim 1 or 2, it is characterized in that: the emulsion of discharging from discharge gate directly enters and comprises separation, filtration, exsiccant postprocessing working procedures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95105343A CN1038578C (en) | 1995-05-26 | 1995-05-26 | Ultra-fine calcium carbonate preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95105343A CN1038578C (en) | 1995-05-26 | 1995-05-26 | Ultra-fine calcium carbonate preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1116185A true CN1116185A (en) | 1996-02-07 |
| CN1038578C 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 | Ultra-fine calcium carbonate preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1038578C (en) |
Cited By (13)
| 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 |
| CN100417436C (en) * | 2005-07-14 | 2008-09-10 | 中国石油化工股份有限公司 | Catalytic selective hydrogenation |
| DE112007001885T5 (en) | 2006-08-25 | 2009-07-02 | Beijing University Of Chemical Technology | Process for the synthesis of butyl rubber |
| CN1429772B (en) * | 2001-12-31 | 2010-12-08 | 纳米材料科技有限公司 | Method for preparing calcium carbonate with actual forms |
| CN102127223B (en) * | 2010-01-15 | 2012-10-17 | 北京化工大学 | Preparation method of micro/nano polyaniline |
| CN103113947A (en) * | 2013-03-06 | 2013-05-22 | 清华大学 | Methane separation and purification device and method thereof for purifying methane by absorbing CO2 through 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 |
| US9156015B2 (en) | 2009-04-09 | 2015-10-13 | Beijing Univesity Of Chemical Technology | Microchannel double pipe device and usage thereof |
| CN104975168A (en) * | 2014-04-01 | 2015-10-14 | 北京化工大学 | Method for rapidly desulfurizing lead-sulfate-containing substances |
| CN105417564A (en) * | 2015-09-14 | 2016-03-23 | 广西大学 | Preparation method for petal sheet-like calcium carbonate crystals |
| CN109911924A (en) * | 2017-12-13 | 2019-06-21 | 财团法人工业技术研究院 | The preparation method of calcium carbonate granule |
| 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 |
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|---|---|---|---|---|
| CN100441285C (en) * | 2003-09-24 | 2008-12-10 | 北京化工大学 | Hypergravity-supercritical reaction/crystallizing device and application/crystallizing technique |
| CN100448879C (en) | 2004-07-22 | 2009-01-07 | 北京化工大学 | Method for preparing unformed cefuroxime axetil |
| CN101279923B (en) | 2007-04-06 | 2010-08-25 | 宁波万华聚氨酯有限公司 | Preparation of polymethylene polyphenyl polyamine |
Family Cites Families (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
Cited By (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 | Method for preparing calcium carbonate with actual forms |
| CN100417436C (en) * | 2005-07-14 | 2008-09-10 | 中国石油化工股份有限公司 | Catalytic selective hydrogenation |
| DE112007001885T5 (en) | 2006-08-25 | 2009-07-02 | Beijing University Of Chemical Technology | Process for the synthesis of butyl rubber |
| US9156015B2 (en) | 2009-04-09 | 2015-10-13 | Beijing Univesity Of Chemical Technology | Microchannel double pipe device and usage thereof |
| CN102127223B (en) * | 2010-01-15 | 2012-10-17 | 北京化工大学 | Preparation method of micro/nano polyaniline |
| CN103113947A (en) * | 2013-03-06 | 2013-05-22 | 清华大学 | Methane separation and purification device and method thereof for purifying methane by absorbing CO2 through 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 |
| CN105417564A (en) * | 2015-09-14 | 2016-03-23 | 广西大学 | Preparation method for petal sheet-like calcium carbonate crystals |
| CN109911924A (en) * | 2017-12-13 | 2019-06-21 | 财团法人工业技术研究院 | The preparation method of calcium carbonate granule |
| CN109911924B (en) * | 2017-12-13 | 2021-10-01 | 财团法人工业技术研究院 | Process 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 |
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| Publication number | Publication date |
|---|---|
| CN1038578C (en) | 1998-06-03 |
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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 |