CN1868889A - Preparation method of fine calcium carbonate - Google Patents
Preparation method of fine calcium carbonate Download PDFInfo
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- CN1868889A CN1868889A CN 200510045329 CN200510045329A CN1868889A CN 1868889 A CN1868889 A CN 1868889A CN 200510045329 CN200510045329 CN 200510045329 CN 200510045329 A CN200510045329 A CN 200510045329A CN 1868889 A CN1868889 A CN 1868889A
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Abstract
A process for preparing superfine calcium carbonate particles features the reaction between the CO2 contained gas and Ca(OH)2 contained liquid under the action of a magnetic field and/or an electric field.
Description
Technical field
The present invention is a kind of preparation method of fine calcium carbonate, particularly prepares the method for subparticle lime carbonate under electromagnetic field, ultrasonic field synergy condition.
Background technology
Lime carbonate is a kind of important inorganic powder material, progress along with lime carbonate miniaturization and process for treating surface, make calcium carbonate product by single filled-type to customizations, become more meticulous, the functionalization direction develops, people are increasing to the demand of subparticle lime carbonate, for example, people have had increasing needs to nanometer grade calcium carbonate.Nano-calcium carbonate is widely used in coating, plastics, rubber, tackiness agent, papermaking, printing ink, car paint, makeup and medicine and other fields.
At present, generally adopt the bubbling carbonizing legal system to be equipped with subparticle lime carbonate both at home and abroad, it is to contain CO
2Gas feed Ca (OH) be housed
2Slurries with or without finishing carburizing reagent in the bubble tower of agitator or the retort, by the refrigeration control reaction temperature with add the preparation that additives such as dispersion agent, crystal formation control agent are realized fine calcium carbonates.Because the ununiformity that gas phase distributes causes the alternate interface contact area of gas, liquid, solid little, mass transfer velocity is slow, it is poor that microcosmic mixes, product particle is thin inadequately, and generally at 0.1 μ m～several μ m, size distribution is inhomogeneous, dispersiveness and stability are also poor, be difficult to prepare high-grade nano level product, carburizing reagent is for up to a few hours, and batch production efficient is low, small scale, energy consumption is big.
Summary of the invention
The objective of the invention is to: disclose and a kind ofly can realize the lime carbonate production of subparticle and make the product particle super-refinement, size distribution is comparatively even, dispersed, good stability, significantly alleviate product accumulation of salt in the surface soil phenomenon, can shorten carbonization time significantly, the production efficiency height, the preparation method of energy-conservation fine calcium carbonate and equipment thereof.
The present invention adopts and contains CO
2Gas and contain Ca (OH)
2Liquid be raw material, its technical scheme is: the carbonation reaction that above-mentioned two kinds of raw materials generate lime carbonate magnetic field or electric field or magnetic field and electric field is common or the effect of alternating electromagnetic field under carry out.
Electromagnetic field to the influence of carburizing reagent is: crystallization rate increases substantially.Contain Ca (OH)
2Liquid in various ion (Ca
2+, CO
3 2-, OH
-, H
+, HCO
3 -), the effect that will be subjected to lorentz's force when all kinds of charged particle is flowed through magnetic field produces motion (magnetophoresis), in electric field, be subjected to the effect of electrical forces to produce motion (electrophoresis), polar molecule produces in alternating electromagnetic field and rotatablely moves, these motions all have the molecule agitation effects, this has greatly strengthened based on microcosmic diffusion, mixing and mass transfer process on ion, the molecular scale, cause the increase of mass transfer coefficient and interfacial area, accelerated the alternate rate of mass transfer of gas, liquid, solid, improved Ca (OH)
2Dissolution rate in liquid film and CO
2Absorption rate has overcome the influence of liquid-film resistance to reaction whole process speed, makes Ca
2+And CO
3 2-Degree of supersaturation increase, form a lot of reactive centers.
Because the effect of electromagnetic field, the association macromolecular mass structure of water wrecks, be cracked into subset, this energy barrier that helps between two equilibrium theory of tide of ion migration reduces, ionigraphic mobility thereby increase, the interionic reversing motion is (with f change of electromagnetic field frequency direction) violent collision mutually continually repeatedly, has improved Ca
2+And CO
3 2-Realize the probability of " effective collision ", connect the CaCO that forms some amount with enough stability
3" ionic association body ", thus constituted a large amount of crystallization nucleis, and this is similar to the effect that adds crystal seed.
In the carburizing reagent along with the rising of carbonation rate, the viscosity of slurries can increase gradually, when the magnetic flux phi of externally-applied magnetic field is appropriate, the increase of interior energy, surface tension and the viscosity factor of water are reduced, can weaken solution viscosity to a certain extent and increase the disadvantageous effect of bringing, improve crystallization condition, help crystalline material in the metastable phase, thereby accelerate crystallisation process by the transformation of liquid phase to solid phase.
Water molecules and associated complex thereof, microscopic particles such as hydrated ion, all carrying out continual vibratory drive, and corresponding to certain energy level, when the time spent of doing that is subjected to electromagnetic field optimum frequency field, just may resonate the of short duration effect of this resonance effect, the activation energy of crystallisation process in can the reduction system has been strengthened the ability of liquor capacity intercrystalline.
Enter carbonization latter stage, CO in the gas phase
2Concentration constant, Ca in the solution (OH)
2(s) concentration very low (＜1%), Ca (OH)
2The liquid-solid interface area of solid phase is much smaller than CO
2The liquid-gas interface area, add Ca (OH)
2The lytic activity of particle is poor, and dissolution rate significantly reduces, the very fast decline of pH value, and the late phase reaction environment tends to weakly alkaline, CO in addition gradually
2Absorption, dissolving, ionization only depend on the dissociation reaction of hydration reaction and carbonic acid to generate CO
3 2-Speed slower, this all becomes the key (the later stage carbonization time accounts for the over half of total carbonization time) of restriction late phase reaction speed, because Electromagnetic Environmental Effect has improved Ca (OH)
2Dissolution rate in liquid film, OH
-Ion has increased the ability of breaking through liquid-film resistance under the effect of magnetic field, electrical forces, enter in the liquid phase, until entering CO
2Liquid film will advantageously promote CO
2Gas dissolving, ionization, diffusion process, thus the speed of later stage carburizing reagent improved greatly.
Electromagnetic field to another influence of carburizing reagent is: be to make crystal grain through miniaturization, homogenization, product dispersiveness, the accumulation of salt in the surface soil are able to remarkable improvement.
The magnetization of magnetic field, electric field, polarized action can make atomic polarity strengthen, the split pole effect disappears in strong ionisation region, cohesive force weakens, the result has changed these molecules, ionic out-shell electron cloud distributes and the ionic distortion, destroy interionic electrostatic attraction and changed crystallization condition, this effect equals crystallization rived becomes extremely thin thin layer, and then make its ionic arrange axial consistent with magnetic field, to the calcium carbonate crystal particulate influence be the small crystalchecked of formation dispersive float and be dispersed in the solution.
Water is subjected to electric field, the action of a magnetic field during by electromagnetic field, the moment of dipole of water molecules will increase or divide, thereby also increased the polarity of water molecules, the cleaved formation subset of associating macromolecular mass or some single water moleculess, they very easily are adsorbed on the polarity CaCO of harsh one-tenth
3On the nucleus, form water molecules and resultant of reaction CaCO
3The associated molecule group of crystallite.
The solution transverse cutting is in the time in addition, the magnetic field that changes on the space, can cause hysteresis effect to salt quasi-molecule in the aqueous solution and ionic magnetic couple, thereby changed the solvability of salt in water, the mutual affinity of salt quasi-molecule (crystallinity) is weakened, and and the affinity of water molecules increase, this effect has further been strengthened, form the quantity and the stability of the associated molecule group of water molecules and resultant of reaction lime carbonate crystallite, the steric effect of this adsorption layer plays good dissemination to the lime carbonate nucleus, and it is difficult at reactant Ca (OH)
2Surface precipitation (this can effectively alleviate the accumulation of salt in the surface soil phenomenon of calcium carbonate product), and because electrostatic interaction CaCO
3Be difficult to do crystalline ordered arrangement, be difficult for generating heavy crystalline substance, twin and the cohesion of secondary glomerocryst, promptly be difficult to grow into macrocrystal, but, form cotton-shaped polymer suspension in solution in a large number with the loose polymerization of identical static crystallite.
In sum, electromagnetic field is not only highly enriched based on microcosmic diffusion, mixing and mass transfer process on ion, the molecular scale to the influence of carburizing reagent, but also directly influences the formation and the crystalline process of growth of nucleus.Can quicken to generate the nucleus of a large amount of lime carbonate, can not make nucleus grow up to macrocrystal again, and because even, instantaneous each space that occurs in liquid phase of this effect makes growth, the coarsening rate of each nucleus be close to identical, to quickening the homogenization generation and the fine particlesization of lime carbonate nucleus, for control the finished product grain through at 100 μ m with the interior condition of having created.This is very crucial technical measures in nano-calcium carbonate production.Also accelerate simultaneously the speed of carburizing reagent effectively, shortened carbonization time.
If adopt bubbling carbonizing explained hereafter lime carbonate, though magnetic field or electric field or electric field and magnetic field is common or the effect effect of alternating electromagnetic field under carry out carburizing reagent and can generate fine lime carbonate than existing bubbling carbonizing, but in order to give full play to Electromagnetic Environmental Effect, the carburizing reagent of two kinds of raw materials can be adopted at magnetic field or electric field or electric field and the method for the carburizing reagent of carrying out under magnetic field is common or alternating electromagnetic field acts synergistically with ultrasonic field.During concrete enforcement, can CO will be contained
2Gas send into the gas distributor of the bubbling carbonizing device bottom that ultrasonic field mechanism is housed with air pump, effusion contain CO
2Gas at the bottom of by tower in the process that rises and contain Ca (OH)
2Liquid is subjected in electromagnetic field, ultrasonic place to finish carburizing reagent under the synergy of the polarization of electromagnetic field, magnetization and ultrasonic cavitation effect, and this more helps fine particlesization and accelerates carbonization speed, and effect is better than single electromagnetic field or single ultrasonic field.
Why said process of the present invention carries out with the ultrasonic field synergy, this mainly is to utilize ultrasonic cavitation to supervene the intensive shockwave, (1500m/s) reach the 400Km microjet with speed per hour, little acoustic streaming, make the liquid of local tiny area be subjected to violent stirring, mechanical effects such as flow at high speed, the liquid movement transverse cutting is in the time like this, speed during the magnetic field that changes on the space strengthens, thereby the lorentz's force F=qv * B of the action of a magnetic field on moving charge is also big more, obviously the magnetic field effect that electromagnetic field is exerted one's influence to carburizing reagent under the synergy of ultrasonic cavitation effect will greatly be strengthened, and be given full play to.Be embodied in the following aspects:
Negative ions (Ca
2+, CO
3 2-, OH
-, H
+, HCO
3 -) because the lorentz's force that is subjected to strengthens greatly, and its momentum also increases, the ability of breaking through liquid-film resistance respectively also increases thereupon, easier entering in the liquid phase, thereby chemical reaction rate increases severely.
Because Electromagnetic Environmental Effect has improved Ca (OH)
2Dissolution rate in liquid film, OH
-After the lorentz's force that ion is subjected to strengthened, its momentum increased, and the ability of breaking through liquid-film resistance increases, easier entering in the liquid phase,
，
To advantageously promote CO
2Gas dissolving, ionization, diffusion process.This effect can effectively improve the speed of carburizing reagent.
The salt quasi-molecule is (as CaCO in the aqueous solution
3) and the hysteresis effect of ionic magnetic couple, further being enhanced, this effect has further been strengthened, and forms quantity and stability that water molecules and the associated molecule of resultant of reaction lime carbonate crystallite are rolled into a ball.
Charged ion in the aqueous solution, particle flux are when magnetic field, and the lorentz's force that is subjected to will greatly be strengthened, and this effect makes hydrated ion make heterodromous speed to improve greatly, and kinetic energy increases, and negative ions is (as Ca
2+And CO
3 2-) collision is more violent mutually, improved the probability of realization " effective collision ", connect and form the more of " ionic association body ", promptly in the aqueous solution, formed more crystallization nuclei, the homogenization of more having quickened the lime carbonate nucleus generates, for the miniaturization of crystalline particle provides better condition.
Ultrasonic field also has following active influence to carburizing reagent except the above-mentioned auxiliary enhancement to electromagnetic field: the partial high pressure (5 * 10 that produces when the non-linear motion of ultrasonic cavitation bubble and cavitation bubble collapse
7Pa) high temperature (more than the 5000K), the variation of temperature rate is up to 10
9K/s changes the energy of the inner each point of system, causes bigger fluctuation of energy, and Intermolecular Forces is weakened, and has strengthened mass transfer motion and probability of collision between reactant molecule.
The shockwave that ultrasonic cavitation is supervened, microjet, little acoustic streaming, make the liquid of local tiny area be subjected to stirring the mobile mechanical effect that waits, and hyperacoustic cavitation mechanism can make solution inside do the vibration of microcosmic, the diffusion of acceleration molecular, strengthened mass transfer process, all make the huge speed of relative movement of the alternate generation of gas, liquid, solid and the phase interface of fast updating, strengthened the alternate mixing of gas, liquid, solid, improved the volume rate of mass transfer of interphase mass transfer.More than these effects can improve CO
2The microcosmic of gas in liquid phase disperses, and quickens its absorption and dissolving, also can promote Ca (OH) simultaneously
2The dissolving of solid particulate, thus make Ca in the liquid phase
2+And CO
3 2-Degree of supersaturation increases, so ultrasonic wave also can make the microcosmic mixing rate greatly be strengthened effectively, has quickened carburizing reagent.
In addition, carbonization to the nucleus that forms some amount since solution to be in hypersaturated state crystalline growth rate very fast, forms control by nucleus and is converted into crystal growth and controls.When cavitation occurs in than the macrocrystal surface, cavitation bubble is asymmetric when closed, be spherical when it begins, promptly asymmetric then contraction forms a hydrofluidic that points to plane of crystal, this high-speed jet (＞110m/s), can form the huge impact effect to plane of crystal, can make colony, the broken and dispersion of dendrite, the macrocrystal that each is grown up forms many new nucleus, thereby obtains more more uniform close grains.But single ultrasonic field is if will reach above-mentioned effect same then consumes energy greatly, and electromagnetic field and ultrasonic field synergy are had complementary advantages, and be not only effective but also energy-conservation.
In this course, ultrasonic wave adopt continuous wave or pulse wave all can, the ultrasonic transducer ultrasonic frequency is 15～70kHz, sound power is 0.5～10W/cm
2Contain Ca (OH)
2The ultrasonic transducer ultrasonic frequency on liquid fluid column top be 20～50kHz, sound power is 0.5～4W/cm
2, in the fluid column, the ultrasonic transducer ultrasonic frequency of bottom is 15～30kHz, sound power is 4～8W/cm
2
In aforementioned process, if earlier to containing Ca (OH)
2The liquid carbonization that atomizes, then can improve carburizing reagent nucleus in early stage and form quantity, carbonization does not contain Ca (OH)
2Droplet assemble after, make two kinds of raw materials carry out above-mentioned reaction again, can guarantee that then nucleus grows to a certain degree, reach fine and the even purpose of growth, and can also improve speed of response greatly.Atomizing can adopt multiple modes such as existing air-stream spraying, press atomization and centrifugal spraying to realize, if desire to make atomizing effect better, also can utilize method of the present invention to realize with two kinds of raw materials itself, that is: adopt and contain CO
2Gas to containing Ca (OH)
2Liquid carry out the air-flow ultrasonic atomizatio.Concrete grammar is: containing CO
2High pressure gas feed ultrasonic generating unit, then the high velocity air load from air outlet ejection has the ultrasonic wave of certain frequency (40～100) kHz and contains Ca (OH)
2Liquid flow clash, ultrasonic energy is acted on liquid stream, when ultrasonic frequency band elastic vibration is propagated in liquid, the intensive acoustic vibration produces cavatition, make liquid medium generation explosion, turn to drop, drop continues to be subjected to acoustic vibration and is atomized into atomic small droplets (50～500 μ m).The drop of specific pressure spraying, centrifugal spraying is little many, thereby surface-area is bigger, and drop experiences the high condition of alternate speed of relative movement, has prolonged at CO
2The residence time in the gas phase, this knock on effect makes drop pass the impact surface infiltration, be scattered in CO
2In the gas phase, gas, liquid produce fiercer turbulence, shear-mixed mutually, and gas, liquid contact are more abundant, even, have increased gas effectively, the liquid surface in contact is long-pending, has reduced thickness of liquid film, has accelerated the alternate rate of mass transfer of gas, liquid, solid, has improved Ca (OH)
2Dissolution rate in liquid film and CO
2Absorption rate forms a lot of reactive centers, produces a large amount of nucleus, and gas, liquid duration of contact basic identical makes the growth of each nucleus, coarsening rate basic identical, thereby can guarantee that product cut size is even, and narrow distribution range has significantly been accelerated carburizing reagent speed.
Desire to control better the particle grain warp and the accelerated reaction speed of product, on the basis of ultimate principle of the present invention, can also adopt following method: earlier to containing Ca (OH)
2The atomization of liquid after, make and contain Ca (OH)
2Droplet with contain CO
2Gas magnetic field or electric field or magnetic field and electric field is common or the alternating electromagnetism field action under the carburizing reagent that atomizes.And atomising method can adopt aforesaid variety of way.This atomizing carburizing reagent under the Electromagnetic Environmental Effect effect can make speed of reaction further improve, and the carburizing reagent initial stage is with a large amount of CaCO of the instantaneous generation of speed of response faster
3Nucleus, thereby for the more miniaturization of control the finished product particle, homogenization provide condition, for more helping generating grain through having created condition at 100 μ m with interior fine calcium carbonate.Concrete grammar is: the magnetic field or electric field or electric field and magnetic field mechanism common or alternating electromagnetic field of can producing of the present invention is installed in atomizing carburizing reagent zone gets final product.
Equally, adopt this carbonization mode, after the atomizing carburizing reagent not carbonization contain Ca (OH)
2Droplet also it can be assembled after, under ultrasonic field effect separately with contain CO
2Gas carry out bubbling carbonizing reaction, certainly, be preferably in the common or alternating electromagnetic field in magnetic field or electric field or electric field and magnetic field and carry out bubbling carbonizing down with the ultrasonic field synergy and react.Thereby make Ca (OH)
2Reaction more thorough, make the finished product reach production requirement.
On the basis of ultimate principle of the present invention, by synthetic method of the present invention: the electromagnetic field bubbling carbonizing, electromagnetic field, ultrasonic field bubbling carbonizing, electromagnetic field atomizing carbonization, carbonization of air-flow ultrasonic atomizatio and electromagnetic field, the carbonization of air-flow ultrasonic atomizatio etc., or between the synthetic methods such as prior art such as multistage spray carbonation, bubbling carbonizing, can be combined into many multi-form building-up reactions methods mutually.The preparation method of best fine calcium carbonate of the present invention is made up of electromagnetic field, air-flow ultrasonic atomizatio carbonation process and electromagnetic field, ultrasonic field bubbling carbonizing operation, and preceding operation adopts and contains CO
2Gas to containing Ca (OH)
2Liquid carry out air-flow ultrasonic atomizatio or other atomization technique, atomizing time both magnetic field or electric field or electric field and magnetic field is common or the alternating electromagnetism field action under atomizing carbonization technical scheme, back operation adopts magnetic field or electric field or electric field and magnetic field is common or alternating electromagnetic field and act synergistically with ultrasonic field under the bubbling carbonizing technical scheme.Use fine calcium carbonate preparation method of the present invention, the calcium carbonate product particulate grain of production is through in 20～50 μ m, and grain is through narrowly distributing, and the carburizing reagent time is shorter, shortens 5～15 times than traditional method.
The electromagnetic field parameter that adopts during the invention process: if when only selecting magnetic field for use, its magneticstrength H=1 * 10
5 ~ 7A/m; When only selecting electric field for use, electric field strength E=800～1500V/cm; When only selecting electric field and magnetic field acting in conjunction for use, strength of electric field is generally E=800～1000V/cm, and magneticstrength is generally H=1 * 10
6A/m; When only selecting alternating electromagnetic field for use, wave frequency is generally 50～1 * 10
8Hz, its strength of electric field is generally 15～1000V/cm.
Air-flow ultrasonic atomizatio parameter: at this moment contain CO
2Gas may be selected to be 100～350m/s in the speed of ultrasonic generating unit air stream outlet, ultrasonic frequency may be selected to be (40～100) kHz, and contains Ca (OH)
2Flow stream velocity can select 0.5～2.5m/s.
The production unit of fine calcium carbonate of the present invention is to install additional to contain CO on conversion unit
2Gas and contain Ca (OH)
2Liquid both carry out producing magnetic field or electric field or electric field in the zone of carburizing reagent and magnetic field is common or the mechanism of alternating electromagnetic field.Said structure specifically can comprise: conversion unit is a tubular metal hollow tower body, in tower body central authorities the interior electrode of insulating layer coating outside is installed by support, with the metal shell of the co-axial tower of interior electrode be outer electrode, with concentric cable interior electrode and outer electrode, be connected respectively to the output terminal of electromagnetic oscillation producer, connect power supply and promptly form alternating electromagnetic field in the intravital inside and outside interelectrode space of tower, its electric field and magnetic field all are distributed in the cross section of tower body, and electric field has only E
rComponent, magnetic field has only H
ΦComponent; Perhaps replace concentric cable inside and outside electrode be connected to the output terminal of high-voltage D.C. generator, just form radial electric field in the intravital inside and outside interelectrode space of tower with cable; Magnetic field generating means perhaps is installed on device housings, can use coil, magnet or more complicated prior art, simultaneously the electrode that is positioned at tower body central authorities is changed into magnetic core stick (also claiming iron core), outside using during coiling, the two ends of coil are connected to the output terminal of power supply with cable, after connecting power supply, just produce magnetic field at coil with between the magnetic core stick of tower body central authorities, can also adopt the generation mechanism that electric field and magnetic field are installed simultaneously, to produce electric field and the coefficient effect in magnetic field.Mist eliminator is arranged at tower body top, is tail gas relief outlet after the carburizing reagent on the mist eliminator, and there is gas inlet the bottom and links to each other with gas distributor, and discharge nozzle is arranged at the bottom, and overflow port is arranged more than the LCL, and there is fluid inlet the overflow port top.
When the technological process of invention requires to have ultrasonic field to strengthen electromagnetic field effect, in above-mentioned magnetic field or electric field or electric field and magnetic field is common or the outside of the corresponding metal tower body in alternating electromagnetism field-effect district, at least one or more groups (for example three groups) ultrasonic field is installed below metal line, every group of ultrasonic field formed by several ultrasonic transducers are in parallel, drive simultaneously by one or several ultrasonic generator, electric energy is converted to acoustic energy and passes to liquid by transverter, produces the intensive cavitation effect.
When technological process of the present invention required to have the atomizing carbonization process, the present invention was provided with air-flow ultrasonic atomizatio mechanism, and it adopts prior art.With containing CO
2Gas to containing Ca (OH)
2Liquid both carry out carburizing reagent when air-flow ultrasonic atomizatio mechanism atomizes, the Ca that contains not carbonization (OH) that is generated
2Droplet stream can be connected with inlet on electromagnetic field, the ultrasonic field bubbling carbonizing processing apparatus by corresponding outlet on the air-flow ultrasonic atomizatio carbonation process equipment.At this moment, the equipment of electromagnetic field, ultrasonic field bubbling carbonizing operation can be connected by pipeline, pump with the equipment of air-flow ultrasonic atomizatio carbonation process, also can make both adopt same housing, be about to the top that air-flow ultrasonic atomizatio carbonation process equipment is arranged on electromagnetic field, ultrasonic field bubbling carbonizing processing apparatus, and install the cage of garden under the epicone and hollow in the housing of between additional, leave between it and the shell and can make the Ca (OH) that contains not carbonization
2Spray makes between the two-step by passage or annular space that gravity descends, though every and communicate, mist eliminator is housed in the cage, on the cage conical top of mist eliminator top the pneumatic outlet that leads to outside shell is arranged.Mist eliminator is arranged at air-flow ultrasonic atomizatio carbonizing zone tower body top, is tail gas relief outlet after the carburizing reagent on the mist eliminator.
When technological process of the present invention requires to have electromagnetic field to strengthen the atomizing carbonization process, can be above the upper-spraying type shower nozzle of atomising mechanism or the following spray shower nozzle below atomizing carbonization zone in, above-mentioned generation magnetic field or electric field or electric field and magnetic field mechanism common or alternating electromagnetic field is installed gets final product.
Description of drawings
Figure one to figure eight is followed successively by the used device structure synoptic diagram of the embodiment of the invention one to embodiment eight;
Wherein, 1-refining storage tank; 2-refining pump; The ripe slurry discharge nozzle of 3-; The 4-gas distributor; 5-bubbling carbonizing inlet pipe; 6-2
#The internal electrode lead-wire pipe; 7-2
#The outer electrode terminal stud; 8-2
#Interior electrode; 9-2
#Interior electrode suppor; The 10-ultrasonic transducer; The 11-overflow port; The 12-LCL; The 13-mist eliminator; The outlet of 14-bubbling carbonizing tail gas; 15-CO
2Gas transfer pipeline; The 16-high-pressure pump; The 17-air valve; 18-CO
2The gas house steward; 19-air-flow ultrasonic atomizer inlet pipe; 20-1
#The outer electrode terminal stud; 21-1
#Interior electrode; 22-1
#Interior electrode suppor; The 23-mist eliminator; The outlet of 24-atomizing carbonization tail gas; 25-1
#The internal electrode lead-wire pipe; 26-air-flow ultrasonic atomizer; The 27-liquid-inlet pipe; 28-refining pipeline; The 29-cage.
Y-tank level control meter interface, T-thermometer boss, D-conductivitimeter interface.
Embodiment
Embodiment one:
As shown in Figure 1, the equipment that present embodiment uses is a tubular metal hollow tower body, and magnetic field or electric field or electric field are housed below 12 tower middle part LCL and magnetic field is common or the generating mechanism of alternating electromagnetic field.It can be the interior electrode 8 that insulating layer coating outside is installed by support 9 in tower body central authorities, with the metal shell of the co-axial tower of interior electrode be outer electrode 7, with concentric cable interior electrode 8 and outer electrode 7, be connected respectively to the output terminal of electromagnetic oscillation producer, connect power supply and promptly form alternating electromagnetic field in the intravital inside and outside interelectrode space of tower, its electric field and magnetic field all are distributed in the cross section of tower body, and electric field has only E
rComponent, magnetic field has only H
ΦComponent; Perhaps replace concentric cable inside and outside electrode is connected to the output terminal of high-voltage D.C. generator, at the intravital inside and outside interelectrode space formation radial electric field of tower with cable; Magnetic field generating means perhaps is installed on device housings, can use coil, magnet or more complicated prior art, simultaneously the electrode that is positioned at tower body central authorities is changed into magnetic core stick (also claiming iron core), outside using during coiling, the two ends of coil are connected to the output terminal of power supply with cable, after connecting power supply, just produce magnetic field at coil with between the magnetic core stick of tower body central authorities; Can also adopt above-mentioned electric field and magnetic field generation mechanism are installed simultaneously, to produce electric field and the coefficient effect in magnetic field.
The employed equipment of present embodiment comprises the shell of equipment, shell upper has liquid-inlet pipe 27, LCL has overflow port 11 more than 12, mist eliminator 13 is arranged at tower body top, it on the mist eliminator tail gas relief outlet 14 after the carburizing reagent, there is gas inlet pipe 5 bottom and links to each other with gas distributor 4, and ripe slurry discharge nozzle 3 is arranged at the bottom.
Present embodiment electromagnetic field parameter: when selecting alternating electromagnetic field for use, wave frequency is generally 50～1 * 10
5Hz, its strength of electric field is generally 350～450V/cm.When only selecting magnetic field for use, its magneticstrength H=1 * 10
6A/m; When only selecting electric field for use, electric field strength E=1300～1500V/cm; When selecting electric field and magnetic field acting in conjunction for use, strength of electric field is generally E=900～1000V/cm, and magneticstrength is generally H=1 * 10
5A/m.
Processing parameter is as follows:
The above-mentioned CO that contains
2Gas can be commercially pure CO
2Or CO
2The mixed gas of content 25～30%.
Contain CO
2Gas unit cross-sectional area air flow preferably be controlled at 0.2 ~ 0.7m
3/ (m
2S)
Contain Ca (OH)
2Strength of fluid (massfraction) be controlled at 9～10%.
Carbonation reaction temperature does not have particular requirement, is advisable with 10 ~ 90 ℃.
Embodiment two:
The employed equipment of present embodiment removes following liquid-inlet pipe 27 and changes spray inlet pipe, CO into
2 Gas inlet pipe 5 directly feeds in the tower and gets final product, and does not need in addition outside refining pump 2, refining pipeline 28, gas distributor 4 and the overflow port 11, and all the other are with figure one.The method of present embodiment is to feed to contain Ca (OH) in tower
2Spray, droplet fills the air in the CO from tower body lower gas inlet pipe 5
2In the gas phase of gas, gas, liquid two-phase at full contact, evenly and both magnetic field effects of producing in magnetic field generating means, or the electrical effect of electric field generating mechanism generation, or the electric field that produces separately of electric field and magnetic field generating means and the joint effect in magnetic field, or the carburizing reagent that atomizes under the polarization of electromagnetic field that produces of alternating electromagnetism ripple generating mechanism, magnetization effect effect.This has greatly accelerated Ca in reactant such as the droplet (OH)
2With CO in the gas phase
2Speed and reaction product CaCO to the dissolving of liquid level, ionization, diffusion
3Leave the speed of liquid film, significantly accelerated atomizing carburizing reagent speed.The carburizing reagent initial stage is with a large amount of CaCO of the instantaneous generation of speed of response faster like this
3Nucleus.Contain as yet the not Ca of carbonization (OH)
2Droplet stream is under action of gravity, and descending comes together in tower bottom, is flowed out by discharge nozzle 3, carries out the bubbling carbonizing reaction through the pump input as the third-class fluid inlet of embodiment one, embodiment again.Or by the discharge nozzle 3 of bottom through being pumped into the atomizing generating mechanism, after atomizing, feed the carburizing reagent that atomizes in this tower once more, circulation repeatedly reaches 7～8 until the pH value, shows that carburizing reagent enters subsequent processing fully.
Present embodiment electromagnetic field parameter: with embodiment one
Processing parameter is as follows:
Remove the following Ca (OH) that contains
2Strength of fluid (massfraction) be controlled at 5～8% be advisable outside, all the other are with embodiment one.
Embodiment three:
Except that following variation, all the other are with embodiment one.Shown in figure two, the outside of the common or corresponding metal tower body in alternating electromagnetism field-effect district in magnetic field in previous embodiment one or electric field or electric field and magnetic field, from LCL one or more groups (for example three groups) ultrasonic field is installed below 12, every group of ultrasonic field is made up of several ultrasonic transducer 10 parallel connections, drive simultaneously by one or several ultrasonic generator, electric energy is converted to acoustic energy and passes to liquid by transverter, produces the intensive cavitation effect.To contain CO
2Gas send into the gas distributor 4 of electromagnetic field, ultrasonic field bubbling carbonizing tower bottom with air pump through bubbling carbonizing inlet pipe 5, the CO that overflows by the gas distributor micropore
2Gas at the bottom of by tower in the process that rises and tower contain Ca (OH)
2Liquid magnetic field or electric field or electric field and magnetic field is common or the synergy of the cavitation effect of polarization, magnetization and the ultrasonic field of alternating electromagnetic field under carry out carburizing reagent.
Ultrasonic field parameter in the present embodiment: the ultrasonic transducer ultrasonic frequency on fluid column top is 25～28kHz, and sound power is 0.5～4W/cm
2, in the fluid column, the ultrasonic transducer ultrasonic frequency of bottom is 15～18kHz, sound power is 4～8W/cm
2)
Electromagnetic field parameter: with embodiment one
Processing parameter is as follows: except that following carbonation reaction temperature requirement was advisable with 10 ~ 60 ℃, all the other were with embodiment one.
Embodiment four:
Present embodiment is to require to strengthening the carbonization effect when technological process of the present invention, when obtaining the calcium carbonate product of evenly refinement and short carbonization time, can before electromagnetic field, ultrasonic field bubbling carbonizing operation, increase the atomizing carbonation process, the atomising mechanism that is adopted can be existing air-stream spraying, press atomization, centrifugal spraying etc., and corresponding outlet is connected with the inlet of electromagnetic field, ultrasonic field bubbling carbonizing equipment on the atomizing carburizing reagent equipment.Mode of connection can be passed through pipeline, pump connects, perhaps adopt following structure shown in the present embodiment figure three: compare with figure two, make atomizing carburizing reagent processing apparatus be positioned at top, and magnetic field or electric field or electric field with magnetic field is common or alternating electromagnetic field, ultrasonic field bubbling carbonizing reaction process equipment place the bottom, the shared same housing of two-step, among the figure: except that increasing 26-spraying gun and shell increase, all the other are with figure one.Technological process is except that following variation, and all the other are with embodiment three, at the atomizing carbonizing zone according to selected humidifier type, in the bottom or top corresponding spraying gun 26 is installed, contain Ca (OH)
2Liquid communicate through liquid-inlet pipe 27 and spraying gun 26, liquid is atomized the back droplet and fills the air in after the reaction of electromagnetic field, ultrasonic field bubbling carbonizing operation, the effusion liquid level continues the CO that contains that rises
2The gas phase of gas in, gas, liquid two-phase at full contact, the carburizing reagent that atomizes under the condition uniformly.Contain as yet the not Ca of carbonization (OH)
2Droplet stream descends under action of gravity, is gathered into liquid after flowing into electromagnetic field, bubbling carbonizing reaction process, again with by bubbling carbonizing inlet pipe 5, and from gas distributor 4 micropores, overflow contain CO
2Gas, under the cavitation effect effect of polarization, magnetization and the ultrasonic field of electromagnetic field, proceed the bubbling carbonizing reaction.The situation of this partial reaction is identical with embodiment three, repeats no more here.
Atomizing carbonizing zone top of tower is equipped with mist eliminator 23, has above the mist eliminator and leads to outside shell, for containing CO after the atomizing carburizing reagent
2The outlet 24 of tail gas.
Bubbling carbonizing operation electromagnetic field, ultrasonic field parameter: with embodiment three.
Processing parameter is as follows:
Remove the following Ca (OH) that contains
2Strength of fluid (massfraction) be controlled at outside 5～8% differences, all the other are with embodiment three.
Embodiment five:
Except that following variation, all the other are with embodiment four.Present embodiment is to require to be reinforcement atomizing carbonization effect when technological process of the present invention, when requiring droplet more tiny.The present invention adopts air-flow ultrasonic atomizatio mechanism, shown in figure four, spraying gun 26 changes the air-flow ultrasonic atomizer into, the still shared same housing of two-step, upper-spraying type air-flow ultrasonic atomizer is equipped with in bottom at the atomizing carbonizing zone, install a cage 29 in the housing between two-step additional, leave between it and the shell and can make the Ca (OH) that contains not carbonization
2Spray makes between the two-step by passage or annular space that gravity descends, though every and communicate, mist eliminator 13 is housed in the cage, the cage conical top of mist eliminator top has the pneumatic outlet 14 that leads to outside shell, through CO
2Gas transfer pipeline 15, high-pressure pump 16 and atomizing carburizing reagent district shell overdraught ultrasonic atomizer inlet pipe 19 are connected.Contain Ca (OH)
2The fluid flow tube 34 of liquid in liquid-inlet pipe 27 and ultrasonic atomizer communicate, and from electromagnetic field, ultrasonic field bubbling carbonizing reaction process, the effusion liquid level contain CO
2Gas, rise and compile through cage 29, after mist eliminator 13 demists of in covering, being equipped with again, discharge from the pneumatic outlet 14 that the cage conical top is led to outside shell, again through CO
2Gas transfer pipeline 15 and high-pressure pump 16 pressurizations feed atomizing carburizing reagent district shell overdraught ultrasonic atomizer inlet pipe 19, enter the CO of the ultrasonic generating unit (figure 5 31) in the air-flow ultrasonic atomizer
2Gas feed 30, and from its CO
2(280～350m/s), load has the ultrasonic wave of certain frequency (75～100) kHz and from the fluid flow tube 34 effusive Ca of containing (OH) of air-flow ultrasonic atomizer to the high velocity air of pneumatic outlet 32 ejection
2Liquid flow clash, gas, liquid two-phase under more abundant, the uniform condition of embodiment three contacts, have been accelerated the alternate rate of mass transfer of gas, liquid, solid under the effect of clashing mutually, after the atomizing carburizing reagent, contain as yet the Ca (OH) of not carbonization
2Droplet stream descends by gravity, by passage or the annular space between cage and the tower body shell, flow into electromagnetic field, bubbling carbonizing reaction process and by gas main 18 in bubbling carbonizing inlet pipe 5, gas distributor 4 micropores, overflow contain CO
2Gas, under the cavitation effect effect of polarization, magnetization and the ultrasonic field of electromagnetic field, proceed carburizing reagent.The situation of this partial reaction is identical with embodiment three, repeats no more here.
Air-flow ultrasound parameter in the present embodiment: contain CO
2Gas be chosen as 280～350m/s from ultrasonic generating unit velocity of discharge, ultrasonic frequency may be selected to be (75～100) kHz, and contains Ca (OH)
2Flow stream velocity can select 1.5～2.5m/s (to strengthen it and to contain CO
2The speed of relative movement of gas, improve reaction efficiency and also the particle diameter of droplet reduced as far as possible).
Bubbling carbonizing operation electromagnetic field, ultrasonic field parameter: with embodiment three.
Processing parameter is as follows:
Remove the following CO that contains
2Gas can be commercially pure CO
2Or CO
2The mixed gas of content 30～40%, the vapour-liquid ratio of air-flow ultrasonic atomizatio are that all the other are with embodiment three outside 0.3～0.5 differences such as (quality).
Embodiment six:
Present embodiment is to require to improve nucleus formation in early stage quantity when technological process of the present invention, strengthen atomizing carbonization effect, during for the calcium carbonate product that obtains more even refinement and shorter carbonization time, above the upper-spraying type shower nozzle of atomising mechanism or the following spray shower nozzle below atomizing carbonization zone in, can set up as same magnetic field or electric field or the electric field of embodiment one and magnetic field is common or the generating mechanism of alternating electromagnetic field.The present embodiment atomising mechanism adopts air-flow ultrasonic atomizatio mechanism, shown in figure six, compares with figure four, and above upper-spraying type air-flow ultrasonic atomizer 26, removing increases 20-1
#The outer electrode terminal stud; 21-1
#Interior electrode; 22-1
#Interior electrode suppor; 25-1
#Outside the internal electrode lead-wire pipe, all the other tops and bottom construction are with the figure four of embodiment five.Contain Ca (OH) after the atomizing
2Droplet be scattered in CO
2In the gas phase, be subjected to the effect of polarization, the magnetization effect of the common or alternating electromagnetic field in magnetic field or electric field or electric field and the magnetic field carburizing reagent that atomizes this moment under atomizing state, and the situation of this partial reaction is identical with embodiment two, repeats no more here.The present embodiment atomising mechanism also can adopt existing technology such as air-stream spraying, press atomization, centrifugal spraying.
Electromagnetic field parameter: with embodiment one
Processing parameter is as follows: remove the following Ca (OH) that contains
2Strength of fluid (massfraction) be controlled at outside 5～8% differences, all the other with
Embodiment one.
Embodiment seven:
The present embodiment characteristics are that air-flow ultrasonic atomizatio technology is adopted in atomizing, and the atomizing carbonization process be magnetic field or electric field or electric field and magnetic field is common or the alternating electromagnetism field action under carry out, then the Ca that contains not carbonization (OH)
2After droplet compiles, again under the effect of ultrasonic field cavitation effect and contain CO
2Gas proceed carburizing reagent.Shown in figure seven, among the figure: process, equipment, air-flow ultrasonic atomizatio mechanism and the parameter of its electromagnetic field, atomizing carburizing reagent operation and electromagnetic field generating mechanism and parameter are with embodiment six; The process of its ultrasonic field, bubbling carbonizing reaction process, ultrasonic field generating mechanism, ultrasonic frequency and sound intensity parameter are with embodiment three; Processing parameter is with embodiment five.
Embodiment eight:
Present embodiment is that its carbonization process of preparation method of best fine calcium carbonate of the present invention is a bubbling carbonizing after the atomizing carbonization earlier, and the former adopts contains CO
2Gas to containing Ca (OH)
2Liquid carry out the air-flow ultrasonic atomizatio, atomizing time both magnetic field or electric field or electric field and magnetic field is common or the alternating electromagnetism field action under the technical scheme of carburizing reagent, the technical scheme that the latter adopts the common or alternating electromagnetic field of magnetic field or electric field or electric field and magnetic field and reacts with ultrasonic field synergy bubbling carbonizing down is shown in figure eight.Still shared same housing of two-step and employing isolation cover structure, process, equipment, air-flow ultrasonic atomizatio mechanism and the parameter of the air-flow ultrasonic atomizatio carbonization under the electromagnetic field effect and electromagnetic field generating mechanism and parameter are with embodiment six; The process of the bubbling carbonizing under electromagnetic field and the ultrasonic field synergy, equipment, wherein electromagnetic field generating mechanism and parameter and ultrasonic field generating mechanism and parameter be with embodiment three.Use the preparation method and the equipment of present embodiment, has the influence that can apply carburizing reagent by the materialization effect of bringing into play electromagnetic field, ultrasonic field to greatest extent, thereby can obtain that particle is extremely fine, the calcium carbonate product of homogeneous (20～50 μ m), crystallization rate can be greatly improved, therefore carbonization time reduces significantly, shortens 5～15 times than traditional method, no matter be batch production or continuous production, plant factor and production efficiency significantly improve, and energy-conservation again effect.
The electromagnetic field parameter is with embodiment one; Bubbling carbonizing operation ultrasonic field parameter is with embodiment three; Air-flow ultrasonic atomizatio parameter is with embodiment five; Processing parameter is as follows: with embodiment five.
Use preparation method of the present invention and device fabrication fine calcium carbonate, the product cut size I is controlled in the 100 μ m, narrow distribution range, and the quality height, the carburizing reagent time is short, shortens 5～15 times than legacy equipment, and equipment yield is big, the production efficiency height.By adjusting vapour-liquid ratio, gas flow rate, calcium hydroxide concentration, gas concentration lwevel, temperature of reaction, electromagnetic frequency and electromagnetic field amount, frequency of ultrasonic and the sound intensity, the control refining in electromagnetic field, ultrasonic bubble tower the residence time or add dispersion agent, crystal formation control agent etc. and can reach the particle diameter of control calcium carbonate crystal and the purpose of shape.
This processing method and equipment are not only applicable to the production of fine calcium carbonate, and can be widely used in light industry, petrochemical industry and the medicine and other fields of mass transfer limited gas, liquid, solid or liquid, liquid, solid reaction.
Claims (9)
1, a kind of preparation method of fine calcium carbonate, the liquid that employing contains the gas of C02 and contains Ca (OH) 2 is raw material, it is characterized in that: the carbonation reaction that above-mentioned two kinds of raw materials generate lime carbonate magnetic field or electric field or magnetic field and electric field is common or the alternating electromagnetism field action under carry out.
2, the preparation method of fine calcium carbonate according to claim 1 is characterized in that: the carburizing reagent of two kinds of raw materials is at magnetic field or electric field or electric field and the carburizing reagent of carrying out under magnetic field is common or alternating electromagnetic field acts synergistically with ultrasonic field.
3, the preparation method of fine calcium carbonate according to claim 2 is characterized in that: ultrasonic wave is continuous wave or pulse wave, and the ultrasonic transducer ultrasonic frequency is 15～70kHz, and sound power is 0.5～10W/cm
2Contain Ca (OH)
2The ultrasonic transducer ultrasonic frequency on liquid fluid column top be 20～50kHz, sound power is 0.5～4W/cm
2, in the fluid column, the ultrasonic transducer ultrasonic frequency of bottom is 15～30kHz, sound power is 4～8W/cm
2
4, the preparation method of fine calcium carbonate according to claim 2 is characterized in that: earlier with to containing Ca (OH)
2Liquid atomize and carbonization, carbonization does not contain Ca (OH)
2Droplet make two kinds of raw materials carry out carburizing reagent again after assembling at magnetic field or electric field or electric field with under magnetic field is common or alternating electromagnetic field acts synergistically with ultrasonic field.
5, the preparation method of fine calcium carbonate according to claim 1 is characterized in that: will contain Ca (OH)
2The atomization of liquid after, make and contain Ca (OH)
2Droplet with contain CO
2Gas magnetic field or electric field or magnetic field and electric field is common or the alternating electromagnetism field action under carry out carburizing reagent.
6, the preparation method of fine calcium carbonate according to claim 5 is characterized in that: after the atomizing carburizing reagent not carbonization contain Ca (OH)
2Droplet assemble the back under the ultrasonic field effect with contain CO
2Gas carry out carburizing reagent.
7, the preparation method of fine calcium carbonate according to claim 6 is characterized in that: after the atomizing carburizing reagent not carbonization contain Ca (OH)
2Droplet assemble the back magnetic field or electric field or electric field and magnetic field is common or alternating electromagnetic field and with the ultrasonic field synergy under carry out carburizing reagent.
8, according to the preparation method of claim 4 or 5 or 6 or 7 described fine calcium carbonates, it is characterized in that: described atomizing contains CO for adopting
2Gas to containing Ca (OH)
2Liquid carry out the air-flow ultrasonic atomizatio.
9, according to the preparation method of claim 1 or 2 or 3 or 4 or 5 or 6 or 7 described fine calcium carbonates, it is characterized in that: described electromagnetic field adopts alternating electromagnetic field, and hertzian wave is continuous wave or pulse wave, and its wave frequency is 50～1 * 10
8Hz, electromagnetic field strength of electric field is 15～1000V/cm.
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