CN105836781B - A kind of carbonization-activation integrated apparatus and method for producing nano-calcium carbonate - Google Patents
A kind of carbonization-activation integrated apparatus and method for producing nano-calcium carbonate Download PDFInfo
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- CN105836781B CN105836781B CN201610409055.7A CN201610409055A CN105836781B CN 105836781 B CN105836781 B CN 105836781B CN 201610409055 A CN201610409055 A CN 201610409055A CN 105836781 B CN105836781 B CN 105836781B
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- activation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to one kind production nano-calcium carbonate carbonization-activation integrated apparatus and method, including heat conduction oil lagging, refrigeration coil, acidometer, thermocouple, gas distributor, frequency-control blender, the parts such as carbon dioxide buffer tank, mass percentage concentration is squeezed into carbonization-activation integrated apparatus for 6~15% calcium hydroxide refining, stirring, cooling, the carbon dioxide air gaseous mixture for being passed through Variable Composition is carbonized, 10~50 DEG C of carburizing temperature, when pH is down to 6~7, terminate carbonization, it is then turned on chuck heat-conducting oil heating, increase speed of agitator, add the additive equivalent to calcium hydroxide butt quality 1~5%, it is 60~90 DEG C to control activation temperature, after activation modification 20~40 minutes, stop heating and stirring, terminate activation modification.Slurry after carbonization-activation is removed into integrated apparatus, filter-press dehydration, after 110~130 DEG C are fully dried, you can obtain the nano-calcium carbonate calcium product of different crystal forms.
Description
Technical field
The present invention relates to one kind production nano-calcium carbonate carbonization-activation integrated apparatus and method, belong to inorganic chemical industry powder
Material Field.
Background technology
Calcium carbonate is the inorganic powder material that a kind of consumption is big, purposes is wide, because its raw material is wide, price is low, non-toxic, white
The features such as spending high, is widely used as the row such as rubber, plastics, papermaking, coating, paint, electric wire, cable, ink, food, daily use chemicals, feed
The filler or additive of industry.Nano-calcium carbonate has obtained more and more extensive as a kind of novel high-grade functional inorganic powder body material
Application, but also exist some product crystal formation uniformity, integrality, product dispersiveness and quality stability it is poor the problem of, production
Product size distribution is not uniform enough, and product settling volume controllability is not good, and parcel accumulation of salt in the surface soil phenomenon happens occasionally.Nano-sized carbon is produced now
Sour calcium common practice is that carburizing reagent is carried out in carbonization kettle, and the gas distributor gas distributed effect of traditional carbonisation is not
, there is carbonization dead angle in ideal, cause the product accumulation of salt in the surface soil, after the completion of carburizing reagent the ripe slurry of gained need to be stood, be aged, cool down,
The processing of the processes such as enrichment, is then transferred in wet-process activation kettle and carries out activation process, and activation modification needs heating, but at this moment calcium carbonate
Ripe slurry has been cooled to normal temperature, and heating needs to consume more energy, and this not only needs to take a long time more than 24 hours, reduction
Production efficiency, it is also to consume energy more, add production cost.
To overcome above-mentioned carbonization kettle and its producing the defect of nano-calcium carbonate technique, a kind of production nano-calcium carbonate of the present invention
Carbonization-activation integrated apparatus and method, simplify the device and flow of production nano-calcium carbonate, it is to avoid the standings of slurries,
The process procedures such as ageing, cooling, enrichment, improve the continuity of technique, are effectively utilized carbonation reaction partial reaction heat,
Be conducive to saving and improve product quality stability.
The content of the invention
It is an object of the invention to provide a kind of carbonization-activation integrated apparatus and method for producing nano-calcium carbonate.
The technical scheme is that：
1. a kind of carbonization-activation integrated apparatus for producing nano-calcium carbonate, by heat conduction oil lagging, cooling coil, titanium dioxide
Carbon gas distributor, frequency-control blender, outer barrel wall are constituted, built with acidometer and thermocouple, the logical cooling of cooling coil
Agent is used to control carbonation reaction temperature, and heat conduction oil lagging is used to heat during activation modification, so constitutes the integration of carbonization-activation
Device；
Described carbonization-activation integrated apparatus is also connected with carbon dioxide-air mixing buffering can system, the buffering
Can system can be with the flow and pressure of the mixed proportion and carbon dioxide-air Mixture of regulation of carbon dioxide and air；
Described carbon dioxide distributor is by an empty circles and coupled logical hollow center cross
Passage is provided with composition, empty circles and coupled logical hollow center cross, it is empty below gas distributor to avoid
Between there is dead angle that gas can not reach and avoid in clogging deposits passage, empty circles adjacent vent holes inwards to foreign minister
To 15~30 degree of diagonal cut joints of dislocation down, adjacent vent holes misplace 15~30 degree and tiltedly opened in opposite directions to both sides on hollow center cross
Mouth down, a diameter of 3~9mm of passage, ventilation pitch of holes is 5~10cm, and passage is symmetric, and circle distribution is closeer
And central distribution is diluter, to meet the need for carbon dioxide is uniformly distributed in carbonization-activation integrated apparatus.
2. the method that the carbonization-activation integrated apparatus according to 1 produces nano-calcium carbonate, is by through the refinement treatment that removes the gred
Mass percentage concentration 6~15% calcium hydroxide slurry, carbonization-activation integrated apparatus is squeezed into starching pump, mix slowly,
Cooling water cooling is passed through in cooling coil, it is 10~50 DEG C to control carbonation reaction temperature, is passed through carbonated volume basis dense
Carbon dioxide-air Mixture of degree 30~100% is carbonized, when carbodiimide solution pH value reaches 6~7, and stopping is passed through dioxy
Change carbon-air Mixture, stop refrigeration, terminate carburizing reagent, restart heat-conducting oil heating, quick stirring, when slurry temperature reaches
To 60~90 DEG C, the additive equivalent to calcium hydroxide butt quality 1~5% is added, activation modification stops after 20~40 minutes
Heating and stirring, terminate activation modification, slurry are removed into integrated apparatus, filter-press dehydration, after 110~130 DEG C are fully dried,
Obtain nano-calcium carbonate product；
The rotating speed that the carbonisation is mixed slowly is 100~300 turns per minute, and the carbonisation is passed through carbon dioxide
Gas volume percentage concentration is gradually reduced from 100% to 30%, and synchronous change is gradually reduced with calcium hydroxide water oar concentration, and carbon
Change temperature then to gradually rise from 10 DEG C to 50 DEG C, so both realize being adapted to for carbon dioxide and calcium hydroxide carburizing reagent concentration,
Ensure that carbon dioxide is obtained fully dispersed and utilized again, and maintain certain residence time, to realize efficient carbonization；
The rotating speed that the activation process is quickly stirred is 310~600 turns per minute, the grain brought using quick stirring kinetic energy
Son collision, carries out activation modification under Action of Surfactant；
The additive is at least one or one of zinc sulfate, polyethylene glycol, stearic acid, Sodium stearate, Sodium Polyacrylate
More than kind.
3. the method that the carbonization-activation integrated apparatus according to 2 produces nano-calcium carbonate, when calcium hydroxide pulp quality
When percentage concentration is 6~10%, control be passed through in carbon dioxide-air Mixture carbon dioxide concentration expressed in percentage by volume from 80% by
30% is gradually reduced to, it is 30~40 DEG C to control carbonization final temperature, is hard ester in surfactant added by calcium carbonate activation stage
Sour sodium, Sodium stearate addition is the 1~3.5% of calcium hydroxide butt quality, and gained nano-calcium carbonate calcium product pattern is spinning Duo
Body, product granularity is 40~60 nanometers.
4. the method that carbonization-activation integrated apparatus produces nano-calcium carbonate according to claim 2, works as calcium hydroxide
When concentration of slurry is 11~15%, 0.3~0.5% zinc sulfate equivalent to calcium hydroxide butt quality is added, control is passed through
Carbon dioxide concentration expressed in percentage by volume is gradually lowered to 50% from 100% in carbonated-air Mixture, and control carbonization is final
40~50 DEG C of temperature, surfactant added by calcium carbonate activation stage be polyethylene glycol and stearic acid composite surface activator,
The quality addition of both polyethylene glycol and stearic acid is respectively the 1.5~2.5% and 0.5~1% of calcium hydroxide butt quality,
Gained nano-calcium carbonate calcium product pattern is cube, and product granularity is 70~90 nanometers.
5. the method that carbonization-activation integrated apparatus produces nano-calcium carbonate according to claim 2, gained nano-sized carbon
The basicity of sour calcium product is controlled in pH 9~10, product activation grade >=98%.
The present invention has following technical advantage and beneficial effect：
1. the device of present invention production nano-calcium carbonate, collection carbonization, activation integral, simple in construction, reasonable energy utilization,
Easy to operate, cost is low, practical, and product quality is controllable, can produce the nano-calcium carbonate calcium product of different crystal forms structure.
2. by special gas distributor, being passed through adjustable density of carbon dioxide gas and speed-regulating mechanical stirring, come
Improve carbon dioxide distributed effect, avoid carbonization dead angle and product parcel accumulation of salt in the surface soil phenomenon, add a small amount of additive, control carbon
Sour calcium product crystal formation and product granularity, it is ensured that the uniformity and integrality of product, improve the stability of product quality.
Brief description of the drawings
Fig. 1 is the carbonization-activation integrated apparatus of production nano-calcium carbonate：1- additives entrance and exhaust outlet；2- acidity
Meter；3- thermocouples；4- cooling water inlets；5- walls；6- cooling coils；7- agitating shafts；8- gas distributors；9- frequency controls are stirred
Mix machine；10-CO2Entrance；11- calcium hydroxide slurry inlets；12- coolant outlets；13- conduction oil outlets；14- agitating paddles；15-
Heat conduction oil lagging；16- heat conductive oil inlets；17- drain holes.
Fig. 2 is gas distributor.
Embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples.
Embodiment 1
Under normal temperature, by the calcium hydroxide slurry of the mass percentage concentration 8% through the refinement treatment that removes the gred, carbon is squeezed into starching pump
Change activation integral makeup to put, open stirring, mixing speed is 150 turns per minute, and cooling water cooling is passed through in cooling coil, is controlled
Carbonation reaction temperature is no more than 40 DEG C, is passed through carbon dioxide-air Mixture and carries out carburizing reagent, by thermocouple temperature measurement, leads to
Cross acidometer detection pH to characterize carburizing reagent process, with the progress of carburizing reagent, regulation is passed through carbon dioxide volume hundred
Point concentration is gradually decrease to 30% by initial 80%, when carbodiimide solution pH value reaches 6, and stopping is passed through carbon dioxide-air and mixed
Gas is closed, stops refrigeration, terminates carburizing reagent, restarts heat-conducting oil heating, quick stirring, mixing speed is 350 turns per minute, when
When slurry temperature reaches 70 DEG C, the Sodium stearate equivalent to calcium hydroxide butt quality 2% is added, activation modification is after 30 minutes,
Stop heating and stirring, terminate activation modification, the slurry after carbonization-activation is removed into integrated apparatus, filter-press dehydration, at 120 DEG C
After fully drying, that is, nano-calcium carbonate product is obtained, nano-calcium carbonate crystal formation is in Spindle, and draw ratio is about 3~4: 1, average
Particle diameter 45nm, the basicity of gained nano-calcium carbonate calcium product is pH 9, and product activation grade is 98.5%.
Embodiment 2
Under normal temperature, the calcium hydroxide slurry of the mass percentage concentration 13% through the refinement treatment that removes the gred is squeezed into starching pump
Carbonization-activation integrated apparatus, adds 0.5% zinc sulfate equivalent to calcium hydroxide butt quality, opens stirring, stirring speed
Spend for 250 turns per minute, cooling water cooling is passed through in cooling coil, control carbonation reaction temperature is no more than 50 DEG C, is passed through containing two
Carbonoxide-air gas mixture carries out carburizing reagent, enters by thermocouple temperature measurement, by acidometer detection to characterize carburizing reagent
Journey, with the progress of carburizing reagent, regulation is passed through carbon dioxide concentration expressed in percentage by volume and is gradually decrease to by initial 100%
50%, when the solution ph that is carbonized reaches 7, stopping is passed through carbon dioxide-air Mixture, stops refrigeration, terminates carburizing reagent,
Restart heat-conducting oil heating, quick stirring, mixing speed is 400 turns per minute, when slurry temperature reaches 80 DEG C, is added suitable
It is compound that polyethylene glycol in calcium hydroxide butt quality 2% and the stearic acid equivalent to calcium hydroxide butt quality 1% are constituted
Surfactant, carries out activation modification after 40 minutes, stops heating and stirring, terminate activation modification, then by after carbonization-activation
Slurry removes integrated apparatus, and filter-press dehydration after 130 DEG C are fully dried, that is, obtains nano-calcium carbonate product, nano-calcium carbonate
Crystal formation is in cube, and average grain diameter is in 75nm, and the basicity of gained nano-calcium carbonate calcium product is pH 9.5, and product activation grade is
99%.
Claims (5)
1. a kind of carbonization-activation integrated apparatus for producing nano-calcium carbonate, it is characterised in that by heat conduction oil lagging, cooling coil,
Carbon dioxide distributor, frequency-control blender, outer barrel wall are constituted, built with acidometer and thermocouple, cooling coil
Coolant is used to control carbonation reaction temperature, and heat conduction oil lagging is used to heat during activation modification, so constitutes carbonization-activation
Integrated apparatus；
Described carbonization-activation integrated apparatus is also connected with carbon dioxide-air mixing buffering can system, the surge tank system
System can be with the flow and pressure of the mixed proportion and carbon dioxide-air Mixture of regulation of carbon dioxide and air；
Described carbon dioxide distributor is made up of an empty circles and coupled logical hollow center cross,
Passage is provided with empty circles and coupled logical hollow center cross, to avoid gas distributor underlying space from occurring
Dead angle and avoid adjacent vent holes outwards opposite dislocation inwards in clogging deposits passage, empty circles that gas can not be reached
Down, adjacent vent holes misplace 15~30 degree of diagonal cut joint courts 15~30 degree of diagonal cut joints in opposite directions to both sides on hollow center cross
Under, a diameter of 3~9mm of passage, ventilation pitch of holes is 5~10cm, and passage is symmetric, and circle distribution it is closeer and in
Heart distribution is diluter, to meet the need for carbon dioxide is uniformly distributed in carbonization-activation integrated apparatus.
2. the method that carbonization-activation integrated apparatus produces nano-calcium carbonate according to claim 1, it is characterised in that：Will be through
The calcium hydroxide slurry of the mass percentage concentration 6~15% for the refinement treatment that removes the gred, carbonization-activation integrally makeup is squeezed into starching pump
Put, mix slowly, cooling water cooling is passed through in cooling coil, control 10~50 DEG C of carbonation reaction temperature, be passed through carbon dioxide body
Product percentage concentration is more than 30%, carbon dioxide-air Mixture less than 100% and is carbonized, 6 are reached when carbodiimide solution pH value~
When 7, stopping is passed through carbon dioxide-air Mixture, stops refrigeration, terminates carburizing reagent, restarts heat-conducting oil heating, quickly stir
Mix, when slurry temperature reaches 60~90 DEG C, add the additive equivalent to calcium hydroxide butt quality 1~5%, activation modification 20
After~40 minutes, stop heating and stirring, terminate activation modification, the slurry after carbonization-activation is removed into integrated apparatus, press filtration
Dehydration, after 110~130 DEG C are fully dried, that is, obtains nano-calcium carbonate product；
The rotating speed that the carbonisation is mixed slowly is 100~300 turns per minute, and the carbonisation is passed through carbon dioxide
Concentration expressed in percentage by volume is gradually reduced from 100% to 30%, and synchronous change is gradually reduced with calcium hydroxide slurry density, and it is warm to be carbonized
Degree then gradually rises from 10 DEG C to 50 DEG C, has so both realized being adapted to for carbon dioxide and calcium hydroxide carburizing reagent concentration, again guarantor
Card carbon dioxide is obtained fully dispersed and utilized, and maintains certain residence time, to realize efficient carbonization；
The rotating speed that the activation process is quickly stirred is 310~600 turns per minute, and the particle brought using quick stirring kinetic energy is touched
Hit, activation modification is carried out under Action of Surfactant；
The additive is at least one of zinc sulfate, polyethylene glycol, stearic acid, Sodium stearate, Sodium Polyacrylate.
3. the method that carbonization-activation integrated apparatus produces nano-calcium carbonate according to claim 2, it is characterised in that：Work as hydrogen
When calcium oxide pulp quality percentage concentration is 6~10%, control is passed through carbon dioxide volume hundred in carbon dioxide-air Mixture
Point concentration is gradually lowered to 30% from 80%, and it is 30~40 DEG C to control carbonization final temperature, in table added by calcium carbonate activation stage
Face activating agent is Sodium stearate, and Sodium stearate addition is the 1~3.5% of calcium hydroxide butt quality, gained nano-calcium carbonate
Product pattern is Spindle, and product granularity is 40~60 nanometers.
4. the method that carbonization-activation integrated apparatus produces nano-calcium carbonate according to claim 2, it is characterised in that：Work as hydrogen
When calcium oxide pulp quality percentage concentration is 11~15%, 0.3~0.5% sulphur equivalent to calcium hydroxide butt quality is added
Sour zinc, control is passed through in carbon dioxide-air Mixture carbon dioxide concentration expressed in percentage by volume from more than 80%, less than 100% model
50% is gradually lowered in enclosing, control 40~50 DEG C of final temperature of carbonization is in surfactant added by calcium carbonate activation stage
Polyethylene glycol and stearic acid composite surface activator, the quality addition of both polyethylene glycol and stearic acid is respectively calcium hydroxide
The 1.5~2.5% of butt quality and 0.5~1%, gained nano-calcium carbonate calcium product pattern be cube, product granularity be 70~
90 nanometers.
5. the method that carbonization-activation integrated apparatus produces nano-calcium carbonate according to claim 2, it is characterised in that：Gained
The basicity of nano-calcium carbonate calcium product is controlled in pH9~10, product activation grade >=98%.
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| CN106277016A (en) * | 2016-09-29 | 2017-01-04 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of equipment for calcium carbonate activation |
| CN106673043B (en) * | 2017-01-06 | 2017-11-14 | 河北立信化工有限公司 | Polyethersulfone resin filling anti-oxidant nano-calcium carbonate of toughness reinforcing uvioresistant and its production and use |
| CN106861409A (en) * | 2017-04-11 | 2017-06-20 | 山西大学 | A kind of carbon dioxide mineralising reaction device |
| CN107445189A (en) * | 2017-09-30 | 2017-12-08 | 广西华洋矿源材料有限公司 | A kind of preparation method of needle-like nano calcium carbonate |
| CN107555461A (en) * | 2017-09-30 | 2018-01-09 | 广西华洋矿源材料有限公司 | A kind of Nano calcium carbonate dedicated preparation method of plastics |
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| CN110817921A (en) * | 2019-10-24 | 2020-02-21 | 湖南金箭新材料科技有限公司 | Nano calcium carbonate aging, homogenizing and surface treatment integrated production process |
| CN111013521B (en) * | 2019-12-25 | 2022-06-14 | 广西华纳新材料股份有限公司 | Nano calcium carbonate pressurized carbonation and surface modification integrated reaction kettle and application |
| CN114380315B (en) * | 2021-09-22 | 2024-01-26 | 湖南新绿方药业有限公司 | Purification method and production equipment of medicinal calcium carbonate |
| CN115041125B (en) * | 2022-06-21 | 2024-04-16 | 耒阳市百汇粉体有限公司 | Activation treatment equipment for calcium carbonate powder production |
| CN118579786B (en) * | 2024-07-18 | 2024-10-18 | 山西龙清环保新材料有限公司 | Carbonization-activation integrated active carbon sintering equipment |
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