CN108033475A - A kind of method that micro- reaction prepares nano-calcium carbonate - Google Patents
A kind of method that micro- reaction prepares nano-calcium carbonate Download PDFInfo
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- CN108033475A CN108033475A CN201810109767.6A CN201810109767A CN108033475A CN 108033475 A CN108033475 A CN 108033475A CN 201810109767 A CN201810109767 A CN 201810109767A CN 108033475 A CN108033475 A CN 108033475A
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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Abstract
The present invention provides a kind of method that micro- reaction prepares nano-calcium carbonate, micro- reaction prepares nano-calcium carbonate device and is mainly made of Water Tank with Temp.-controlled, microreactor, temperature controller, constant-flux pump, mixing groove, blender, filtrate regenerator, mixed airflow gauge, nitrogen storage tank, carbon dioxide stream gauge, carbon dioxide storage tank, pH value measuring instrument, dehvery pump, water washed filter to dryer and corresponding connecting pipe；Using the micro- reaction carbonization technique of calcium carbonate；The reaction time can significantly be shortened, lift the yield of nano-calcium carbonate product, particle size distribution range is narrow, and product quality is stablized, it is possible to achieve industrialized production, technique is simple, and energy consumption is low.
Description
Technical field
The present invention relates to technical field of chemical material preparation, relates in particular to a kind of micro- reaction and prepares nano-calcium carbonate
Method.
Background technology
Calcium carbonate is widely used in the fields such as papermaking, plastics, papermaking, rubber, viscose, coating and ink, can play increasing
Amount filling, the effect for reducing processing cost, can also carry out functional modification to filled object.Nano-calcium carbonate, due to its compared with
Small particle diameter, higher specific surface area and special surface treatment, has the incomparable superiority of micron order ordinary calcium carbonate
Energy.
Method currently used for nano-calcium carbonate production mainly has two kinds of double decomposition and carbonizatin method.（1）Double decomposition master
If being reacted using water-soluble Ca salt with water soluble carbonate under appropriate process conditions, precipitation passes through this liquid-solid
Required nano-calcium carbonate calcium product is made in phase reaction.This method can by control the concentration of reactant, temperature, feed rate and and
The degree of supersaturation of product calcium carbonate, add appropriate additive etc., produces the grain such as calcium carbonate is spherical of different-shape and size
Footpath≤0.1 μm, the amorphous calcium carbonate product that specific surface area is big, dissolubility is good, product purity is high, whiteness is good.But double decomposition
Prepare that the product cost of nano-calcium carbonate different crystal forms is higher, be not easy to remove the big of in calcium carbonate forming process its adsorption
Chlorion is measured, it is necessary to take considerable time and washed with water, is rarely employed both at home and abroad.（2）Carbonation method is with high-quality stone
Lime stone is raw material, and calcium oxide and carbonated kiln gas are obtained by calcining, and calcium oxide and water generation calcium hydroxide are suspended
Liquid, then passes to the kiln gas after purified treatment, carbonation reaction generation lime deposit, by being dehydrated, drying, crushing and obtain
Nano-calcium carbonate calcium product.At present the nanometer grade calcium carbonate for preparing both at home and abroad mainly in this way, according to carbon dioxide
With the way of contact of calcium hydroxide suspension, carbonation method can be divided into intermittent bubbling carbonizing method, batch type carbonizatin method,
Continuous multilevel spray carbonization and high-gravity carbonation method etc..
Chinese invention patent CN200410016164.X discloses a kind of preparation method of nanometer grade super fine calcium carbonate, be
The Ca (OH) of high speed machine vibration2It is passed through in suspension containing CO2Kiln gas be carbonized, pass through high speed machine vibrating disk, produce
Violent microturbulent motion, makes Ca (OH)2Suspended particulate and CO2Bubble is fully broken, and height mixes, and greatly improves to transmit as control
The carbonation reaction speed of step processed, can and generate 30~100nm calcium carbonate superfine powder particle；At the same time by tower outer circulation, make
Ca(OH)2Suspension and CO2Back flow of gas contacts, and while " back-mixing " is reduced, preferably realizes micromixing so that
The calcium carbonate particle of generation is relatively more evenly distributed, but this production method complex process, and high energy consumption, production cost is higher, and
The product of acquisition is mostly chain product, it is necessary to add certain crystal control agent, and technique is more complicated.
Chinese invention patent CN02114174.6 prepares nanoscale using rotating bed with helix channel supergravity reactor and surpasses
Thin calcium carbonate.The mass transfer of gas-liquid-solid multiphase is carried out in the helical duct of reactor rotor, is reacted, i.e. carburizing reagent, instead
Emulsion after answering is discharged by revolving bed bottom discharge mouth, obtains nanometer grade super fine calcium carbonate after filtered, dry, but this is anti-
Device design complexity is answered, equipment investment is big, and energy consumption is high, hardly possible cleaning, unfavorable to follow-up continuous production.
The reaction of preparation of nanometer calcium carbonate by carbonization is moment reaction.In nano-calcium carbonate preparation process, mass transport process is
The committed step of synthesis is controlled, ensures that uniform admixture and reactant concentration are synthesizing high purity carbon acid calcium and realize that it is filled
The key of mitogenetic length.From existing preparation method, the interphase mass transfer of gas-liquid must be strengthened by obtaining nanometer grade calcium carbonate, be shortened
In the reaction time, reinforcing particle nucleation, weakens Grain growth.Micro- reaction is chemically reacted in microreactor, reactant
Scattered scale is in micron dimension, so there is the characteristics of reinforcing and the controllability of the change of hydrodynamics rule, transmittance process are high.
Nano-calcium carbonate, Ca (OH) are prepared using micro-reaction device2The flow rate of suspension can accurately be controlled by constant-flux pump, is pumped into
In reactor, so that Ca (OH)2With CO2It is continued for reacting, using the micro-structure system of microreactor material is possessed
Higher mixing efficiency, reaction mass can be accurately mixed with required material ratio, accurate controlling reaction temperature so that
Calcium carbonate favorable dispersibility, particle size distribution range is narrow, and product quality is stablized.
The content of the invention
The present invention provides a kind of method that micro- reaction prepares nano-calcium carbonate, using miniflow field technology as technical support,
Using microreactor as reaction member, the material ratio of reactant is accurately controlled, the reaction time, in reaction temperature and reaction process
The pH value of solution, can significantly shorten the reaction time, lift the yield of nano-calcium carbonate product, particle size distribution range is narrow, product
Stable quality, realizes industrialized production, and technique is simple, and energy consumption is low.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of micro- reaction prepares the preparation facilities of nano-calcium carbonate, as shown in Figure 1, by Water Tank with Temp.-controlled, microreactor, temperature controller,
Constant-flux pump, be mixed groove, blender, filtrate regenerator, mixed airflow gauge, nitrogen storage tank, carbon dioxide stream gauge, temperature
Sensor, carbon dioxide storage tank, pH value measuring instrument, dehvery pump, water washed filter are formed to dryer and corresponding connecting pipe.
A kind of method that micro- reaction prepares nano-calcium carbonate, using the preparation process flow shown in Fig. 1：
（1）The system of reaction is the CO of volume fraction 30%2 -N2Mixed gas and mass percentage concentration are 15%~35%Ca
(OH)2Suspension；
（2）Combi inlet port 0.1~0.2MPa of pressure, the addition of nitrogen, enhances disturbance and strengthens matter, while steady during gas-liquid contact
Determine gaseous pressure；
（3）Gaseous mixture enters microreactor, Ca (OH) through film decentralized system2Suspension is pumped into micro- reaction system by constant-flux pump；
（4）Gas-liquid two-phase is reacted in microreactor and in follow-up pipeline, subsequently into mixing groove；
（5）When the pH value of mixing groove solution reaches 7.0, microreactor stops being passed through gaseous mixture；
（6）Material after the reaction was complete is filtered, is washed, it is dry, obtain nano-calcium carbonate calcium product；
（7）Filtrate adds Ca (OH)2, it is 15%~35%Ca (OH) to be configured to mass percentage concentration2Suspension recycles；
（8）Reaction temperature, is controlled by Water Tank with Temp.-controlled.
A kind of method that micro- reaction prepares nano-calcium carbonate, using following operating procedure and operating parameter：
（1）It is configured to Ca (OH)2Suspension：Ca (OH) is added to being mixed in groove2And water, it is agitated to be configured to Ca (OH)2It is outstanding
Turbid, Ca (OH)2Mass percentage concentration is 15%~35%；
（2）The Gas Mixture Preparation of carbon dioxide and nitrogen：The volume fraction of carbon dioxide and nitrogen is controlled 30% by flowmeter,
The addition of nitrogen, enhances disturbance and strengthens matter, while stablizes gaseous pressure during gas-liquid contact；
（3）Ca(OH)2Suspension carries out carburizing reagent：Mass percentage concentration is 15%~30%Ca (OH)2Suspension, it is and corresponding
The gaseous mixture of carbon dioxide and nitrogen is reacted in microreactor；
（4）Reaction temperature is controlled at 20~45 DEG C by Water Tank with Temp.-controlled；
（4）Calcium Carbonate Filtration washs drying：Filtered after the completion of reaction, precipitation of calcium carbonate is through 2~3 washings, in 110 DEG C~150
Processing is dried between DEG C, obtains the calcium carbonate powder between middle 30~60nm of particle diameter；
（5）Filtrate cycle：Filtrate is mainly water, adds Ca (OH)2, stirring, is configured to 15%~30%Ca (OH)2Suspension.
Beneficial effects of the present invention
The present invention provides a kind of method that micro- reaction prepares nano-calcium carbonate, can preferably solve conventional formula reactor
In mixed performance it is poor, the gas-liquid mass transfer time is longer, distribution of concentration is uneven, product quality is poor, particle agglomeration phenomenon
Seriously with particle heterogeneity the problems such as, obtained calcium carbonate particle diameter is small, and size is more uniform；The micro-structure system of microreactor causes
Material mixing efficiency is high, realizes and reaction mass is accurately mixed with required material ratio, can accurately control react into
Journey and reaction temperature, overcome conventional method during the reaction reactant concentration skewness the shortcomings that.
A kind of micro- reaction that Fig. 1 is the present invention prepares nano-calcium carbonate process flow diagram；
In Fig. 1：1. Water Tank with Temp.-controlled, 2. microreactors, 3. temperature controllers, 4. constant-flux pumps, 5. are mixed groove, 6. stirrings
Device, 7. filtrate regenerators, 8. mixed airflow gauge, 9. nitrogen storage tanks, 10. carbon dioxide stream gauge, 11. temperature sensing
Device, 12 carbon dioxide storage tanks, 13. pH value measuring instruments, 14. dehvery pumps, 15. water washed filters, 16. machines dry machine.
Embodiment
The invention will be further described with embodiment below in conjunction with the accompanying drawings：
A kind of micro- reaction prepares the preparation facilities of nano-calcium carbonate, as shown in Figure 1, by Water Tank with Temp.-controlled 1, microreactor 2, temperature controller
3rd, constant-flux pump 4, mixing groove 5, blender 6, filtrate regenerator 7, mixed airflow gauge 8, nitrogen storage tank 9, carbon dioxide stream
Gauge 10, temperature sensor 11, carbon dioxide storage tank 12, pH value measuring instrument 13, dehvery pump 14, water washed filter 15, dryer
16 form with corresponding connecting pipe.
A kind of method that micro- reaction prepares nano-calcium carbonate, using the preparation process flow shown in Fig. 1：
（1）The system of reaction is the CO of volume fraction 30%2 -N2Mixed gas and mass percentage concentration are 15%~35%Ca
(OH)2Suspension reacts in microreactor 2；
（2）Gaseous mixture CO2 -N2Volume fraction is 30%, 0.1~0.2MPa of mixture pressure, by nitrogen stream gauge 10, gaseous mixture
Flowmeter 8 and respective valves control, the addition of nitrogen, enhance disturbance and strengthen matter, while stablize gaseous pressure during gas-liquid contact；
（3）Film decentralized system of the gaseous mixture through microreactor 2 enters microreactor 2, Ca (OH)2Suspension is by mixing groove 5
Micro- reaction system is pumped into through constant-flux pump 4；
（4）Gas-liquid two-phase is reacted in microreactor 2 and in follow-up pipeline, subsequently into mixing groove 5；
（5）The pH value that 5 solution of groove is mixed is measured by pH value measuring instrument 13, and when pH value reaches 7.0, microreactor 2 stops
It is passed through gaseous mixture；
（6）Then reacting rear material adds water washed filter 15 through product pump 14 by mixing groove 5 and is filtered, water washing,
Drying machine 16 is dried, and obtains nano-calcium carbonate calcium product；
（7）The filtrate of water washed filter 15 and washing lotion, into groove 5 is mixed, add Ca (OH)2, it is dense to be configured to quality percentage
Spend for 15%~35%Ca (OH)2Suspension, recycles；
（8）Reaction temperature, is controlled by Water Tank with Temp.-controlled 1, is measured by temperature sensor 11, is controlled by temperature controller 3.
A kind of method that micro- reaction prepares nano-calcium carbonate, using following operating procedure and operating parameter：
（1）It is configured to Ca (OH)2Suspension：Ca (OH) is added to being mixed in groove 52, water washed filter 15 filtrate and wash
Liquid and supplement water, agitated device 6 are configured to Ca (OH)2Suspension, Ca (OH)2Mass percentage concentration is 15%~35%；
（2）The Gas Mixture Preparation of carbon dioxide and nitrogen：Controlled by nitrogen stream gauge 10 and mixed airflow gauge 8 and respective valves
The volume fraction 30% of carbon dioxide and nitrogen, and when keeping gas-liquid contact gaseous pressure stabilization in 0.1~0.2MPa；
（3）Ca(OH)2Suspension carries out carburizing reagent：Mass percentage concentration is 15%~30%Ca (OH)2Suspension, it is and corresponding
The gaseous mixture of carbon dioxide and nitrogen is reacted in microreactor 2；
（4）Reaction temperature is measured by temperature sensor 11, is controlled by temperature controller 3, is controlled at 20~45 DEG C；
（5）Calcium Carbonate Filtration washs drying：Filtered after the completion of reaction, precipitation of calcium carbonate is through 2~3 washings, in 110 DEG C~150
Processing is dried between DEG C, obtains the calcium carbonate powder between middle 30~60nm of particle diameter；
（6）Filtrate cycle：Filtrate is mainly water, adds Ca (OH)2, stirring, it is 15%~30%Ca (OH) to be configured to mass fraction2
Suspension, recycles.
The present invention is not limited to the above embodiments, and without departing from the spirit and scope of the present invention, the present invention is also
Various changes and modifications are had, these changes and improvements are all within the scope of the present invention.
Claims (3)
1. a kind of method that micro- reaction prepares nano-calcium carbonate, it is characterized in that, micro- reaction prepares nano-calcium carbonate device, such as
Shown in Fig. 1, by Water Tank with Temp.-controlled, microreactor, temperature controller, constant-flux pump, mixing groove, blender, filtrate regenerator, mixing
Air-flow gauge, nitrogen storage tank, carbon dioxide stream gauge, temperature sensor, carbon dioxide storage tank, pH value measuring instrument, dehvery pump,
Water washed filter is formed to dryer and corresponding connecting pipe.
2. the method that a kind of micro- reaction as claimed in claim 1 prepares nano-calcium carbonate, it is characterized in that, using shown in Fig. 1
Preparation process flow：
（1）The system of reaction is the CO of volume fraction 30%2 -N2Mixed gas and mass percentage concentration are 15%~35%Ca
(OH)2Suspension reacts in microreactor；
（2）Gaseous mixture CO2 -N2Volume fraction is 30%, 0.1~0.2MPa of mixture pressure, by nitrogen stream gauge and mixed airflow
Gauge and respective valves control, the addition of nitrogen, enhance disturbance and strengthen matter, while stablize gaseous pressure during gas-liquid contact；
（3）Film decentralized system of the gaseous mixture through microreactor enters microreactor, Ca (OH)2Suspension is by mixing groove through flat
Stream pump is pumped into micro- reaction system；
（4）Gas-liquid two-phase is reacted in microreactor and in follow-up pipeline, subsequently into mixing groove；
（5）The pH value that groove solution is mixed is measured by pH value measuring instrument, and when pH value reaches 7.0, microreactor stops being passed through
Gaseous mixture, reaction are completed；
（6）Material adds water washed filter through product pump by mixing groove and is filtered after the completion of reaction, washes, drying machine
It is dry, obtain nano-calcium carbonate calcium product；
（7）The filtrate of water washed filter and washing lotion, into groove is mixed, add Ca (OH)2, being configured to mass percentage concentration is
15%~35%Ca (OH)2Suspension, recycles；
（8）Reaction temperature, is controlled by Water Tank with Temp.-controlled, by temperature sensor measurement, is controlled by temperature controller.
3. the method that a kind of micro- reaction as described in claim 1 and claim 2 prepares nano-calcium carbonate, it is characterized in that, adopt
With following operating procedure and operating parameter：
（1）It is configured to Ca (OH)2Suspension：Ca (OH) is added to being mixed in groove2, water washed filter filtrate and washing lotion and
Water is supplemented, agitated device is configured to Ca (OH)2Suspension, Ca (OH)2Mass percentage concentration is 15%~35%；
（2）The Gas Mixture Preparation of carbon dioxide and nitrogen：By nitrogen stream gauge and mixed airflow gauge and respective valves control two
The volume fraction 30% of carbonoxide and nitrogen, and when keeping gas-liquid contact gaseous pressure stabilization in 0.1~0.2MPa；
（3）Ca(OH)2Suspension carries out aminating reaction：Mass percentage concentration is 15%~30%Ca (OH)2Suspension, it is and corresponding
The gaseous mixture of carbon dioxide and nitrogen is reacted in microreactor；
（4）Reaction temperature is by temperature sensor measurement, by temperature controller control control at 20~45 DEG C；
（5）Calcium Carbonate Filtration washs drying：Reaction is filtered after completing through washing filtering machine, and calcium carbonate is through 2~3 washings, in 110
DEG C~150 DEG C between processing is dried, obtain the calcium carbonate powder between middle 30~60nm of particle diameter；
（6）Filtrate cycle：Filtrate is mainly water, adds Ca (OH)2, stirring, it is 15%~30%Ca (OH) to be configured to mass fraction2
Suspension, recycles.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503357A (en) * | 2018-12-25 | 2019-03-22 | 维思普新材料（苏州）有限公司 | A kind of continuous preparation method of metal fatty acid salt |
| CN110128851A (en) * | 2019-04-19 | 2019-08-16 | 清华大学 | A kind of preparation method of dewatering nano calcium carbonate |
| CN112705128A (en) * | 2020-12-08 | 2021-04-27 | 永丰县广丰化工有限公司 | Nanoscale calcium carbonate processing device |
| CN115286028A (en) * | 2022-05-12 | 2022-11-04 | 四川大学 | Preparation method and device for synthesizing high-dispersion nano calcium carbonate without using additive |
| CN115608299A (en) * | 2022-10-24 | 2023-01-17 | 贵州大学 | Micro-reaction equipment for preparing nano calcium carbonate and using method |
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| CN1769180A (en) * | 2005-09-09 | 2006-05-10 | 山东海泽纳米材料有限公司 | Method for preparing nanometer calcium carbonate granule |
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| CN105036171A (en) * | 2015-08-06 | 2015-11-11 | 广西碳酸钙产业化工程院有限公司 | Novel technology for continuously producing light calcium carbonate |
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| CN1769180A (en) * | 2005-09-09 | 2006-05-10 | 山东海泽纳米材料有限公司 | Method for preparing nanometer calcium carbonate granule |
| CN202898377U (en) * | 2012-11-13 | 2013-04-24 | 江苏恒创科技有限公司 | Device for methane decarburization and synchronous preparation of nanometer calcium carbonate |
| CN105036171A (en) * | 2015-08-06 | 2015-11-11 | 广西碳酸钙产业化工程院有限公司 | Novel technology for continuously producing light calcium carbonate |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503357A (en) * | 2018-12-25 | 2019-03-22 | 维思普新材料（苏州）有限公司 | A kind of continuous preparation method of metal fatty acid salt |
| CN110128851A (en) * | 2019-04-19 | 2019-08-16 | 清华大学 | A kind of preparation method of dewatering nano calcium carbonate |
| CN110128851B (en) * | 2019-04-19 | 2020-11-03 | 清华大学 | Preparation method of hydrophobic nano calcium carbonate |
| CN112705128A (en) * | 2020-12-08 | 2021-04-27 | 永丰县广丰化工有限公司 | Nanoscale calcium carbonate processing device |
| CN112705128B (en) * | 2020-12-08 | 2022-07-29 | 永丰县广丰化工有限公司 | Nanoscale calcium carbonate processing device |
| CN115286028A (en) * | 2022-05-12 | 2022-11-04 | 四川大学 | Preparation method and device for synthesizing high-dispersion nano calcium carbonate without using additive |
| CN115286028B (en) * | 2022-05-12 | 2023-12-15 | 四川大学 | Preparation method and device for synthesizing high-dispersion nano calcium carbonate without using additive |
| CN115608299A (en) * | 2022-10-24 | 2023-01-17 | 贵州大学 | Micro-reaction equipment for preparing nano calcium carbonate and using method |
| CN115608299B (en) * | 2022-10-24 | 2024-04-12 | 贵州大学 | Micro-reaction equipment for preparing nano calcium carbonate and application method |
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