CN105836781A - Carbonization and activation integration device and method for producing nano calcium carbonate - Google Patents
Carbonization and activation integration device and method for producing nano calcium carbonate Download PDFInfo
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- CN105836781A CN105836781A CN201610409055.7A CN201610409055A CN105836781A CN 105836781 A CN105836781 A CN 105836781A CN 201610409055 A CN201610409055 A CN 201610409055A CN 105836781 A CN105836781 A CN 105836781A
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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 invention relates to a carbonization and activation integration device and method for producing nano calcium carbonate. The carbonization and activation integration device comprises parts such as a heat conduction oil jacket, a refrigerating coil pipe, an acidometer, a thermocouple, a gas distributor, a variable-frequency speed regulation stirrer and a carbon dioxide buffer tank. The method comprises the steps: pumping calcium hydroxide refining plasma with mass percentage of 6 to 15 percent into the carbonization and activation integration device, stirring, cooling, introducing carbon dioxide-air mixed gas of a variable concentration, performing the carbonization at 10 to 50 DEG C, ending the carbonization when pH is lowered to 6 to 7, opening the jacket to heat by virtue of the heat conduction oil, increasing the stirring rotation speed, adding additives equivalent to 1 to 5 percent of a dry matrix amount of the calcium hydroxide, controlling the activation temperature at 60 to 90 DEG C, activating and modifying for 20 to 40 minutes, stopping heating and stirring, and ending the activation modification; and moving the carbonized and activated slurry out of the integration device, press filtering, dehydrating, and sufficiently drying at 110 to 130 DEG C to obtain a nano calcium carbonate product of different crystal forms.
Description
Technical field
The present invention relates to a kind of production nano-calcium carbonate carbonization-activation integrated apparatus and method, belong to inorganic chemical industry powder body material field.
Background technology
Calcium carbonate is the inorganic powder material that a kind of consumption is big, purposes is wide, owing to its raw material is wide, price is low, avirulence, whiteness are high
Feature, is widely used as the row such as rubber, plastics, papermaking, coating, paint, electric wire, cable, ink, food, daily use chemicals, feedstuff
The filler of industry or additive.Nano-calcium carbonate has obtained the most widely should as a kind of novel high-grade functional inorganic powder body material
With, but there is also the problem that some product crystal formation concordance, integrity, product dispersibility and quality stability are poor, product granularity divides
Cloth is uniform not, and product settling volume controllability is the best, and parcel accumulation of salt in the surface soil phenomenon happens occasionally.Produce now that nano-calcium carbonate is common to be done
Method is to carry out carburizing reagent in carbonization kettle, and the gas distributor gas distributed effect of tradition carbonisation is undesirable, there is carbonization dead angle,
Cause the product accumulation of salt in the surface soil, carburizing reagent complete after gained ripe slurry needs carry out standing, are aged, cool down, the operation such as enrichment processes, retransfer
Carrying out activation processing in wet-process activation still, activation modification needs heating, but at this moment the ripe slurry of calcium carbonate has been cooled to room temperature, and heating needs
Consuming more energy, this not only needs to take a long time more than 24 hours, reduce production efficiency, also consumes energy more,
Add production cost.
For overcoming above-mentioned carbonization kettle and producing the defect of nano-calcium carbonate technique, a kind of carbonization-activation producing nano-calcium carbonate of the present invention
Integrated apparatus and method, simplify and produce the device of nano-calcium carbonate and flow process, it is to avoid the standing of serosity, is aged, cools down, increases
Dense process procedure such as grade, improves the seriality of technique, is effectively utilized carbonation reaction partial reaction heat, the most energy-conservation and raising
Constant product quality.
Summary of the invention
It is an object of the invention to provide a kind of carbonization-activation integrated apparatus producing nano-calcium carbonate and method.
The technical scheme is that
1. produce a carbonization-activation integrated apparatus for nano-calcium carbonate, by conduction oil chuck, cooling coil, carbon dioxide gas
Body distributor, frequency-control blender, outer barrel wall are constituted, and built with acidometer and thermocouple, cooling coil coolant is used
In controlling carbonation reaction temperature, conduction oil chuck is heating when activation modification, so constitutes the integrated apparatus of carbonization-activation；
Described carbonization-activation integrated apparatus is also connected with carbon dioxide-air mixing surge tank system, this surge tank system
Can be with regulation of carbon dioxide and the mixed proportion of air and the flow of carbon dioxide-air Mixture and pressure；
Described carbon dioxide distributor is made up of an empty circles and coupled logical hollow center cross, empty
Passage is had, for avoiding gas distributor underlying space that gas occurs on heart circle and coupled logical hollow center cross
The dead angle that can not arrive and avoid clogging deposits passage, adjacent vent holes dislocation 15～30 the most in opposite directions inwards in empty circles
Degree diagonal cut joint down, on hollow center cross adjacent vent holes misplace in opposite directions to both sides 15～30 degree of diagonal cut joints down, passage
A diameter of 3～9mm, passage spacing is 5～10cm, and passage is symmetric, and circle distribution is closeer and central distribution relatively
Dilute, to meet carbon dioxide equally distributed needs in carbonization-activation integrated apparatus.
2. the method producing nano-calcium carbonate according to carbonization-activation integrated apparatus described in 1, is by the matter through the refinement treatment that removes the gred
Amount percentage concentration 6～the calcium hydroxide slip of 15%, squeeze into carbonization-activation integrated apparatus, low rate mixing, cooler pan with starching pump
Being passed through cooling water cooling in pipe, controlling carbonation reaction temperature is 10～50 DEG C, is passed through carbonated concentration expressed in percentage by volume 30～100%
Carbon dioxide-air Mixture carry out carbonization, when carbodiimide solution pH value reaches 6～7, stop being passed through the mixing of carbon dioxide-air
Gas, stops refrigeration, terminates carburizing reagent, restarts heat-conducting oil heating, quickly stir, when slurry temperature reaches 60～90 DEG C,
Add and be equivalent to calcium hydroxide butt quality 1～the additive of 5%, activation modification 20～after 40 minutes, stop heating and stirring,
Terminate activation modification, slip is removed integrated apparatus, filter-press dehydration, at 110～130 DEG C the most after drying, i.e. obtains nanometer
Calcium carbonate product；
The rotating speed of described carbonisation low rate mixing is 100～300 turns per minute, and described carbonisation is passed through carbon dioxide body
Long-pending percentage concentration is gradually lowered from 100% to 30%, is gradually lowered Tong Bus change with calcium hydroxide water oar concentration, and carburizing temperature
Then gradually rise from 10 DEG C to 50 DEG C, the most both realized the adaptation of carbon dioxide and calcium hydroxide carburizing reagent concentration, ensured again two
Carbon oxide gas obtains fully dispersed and utilizes, and maintains certain time of staying, to realize efficient carbonization；
The rotating speed that described activation process quickly stirs is 310～600 turns per minute, utilizes the particle encounter that quickly stirring kinetic energy brings,
Activation modification is carried out under Action of Surfactant；
Described additive be zinc sulfate, Polyethylene Glycol, stearic acid, sodium stearate, sodium polyacrylate at least one or one with
On.
3. the method producing nano-calcium carbonate according to carbonization-activation integrated apparatus described in 2, when calcium hydroxide pulp quality percentage is dense
When degree is 6～10%, controls to be passed through carbon dioxide concentration expressed in percentage by volume in carbon dioxide-air Mixture and be gradually lowered to from 80%
30%, controlling carbonization final temperature is 30～40 DEG C, is sodium stearate at surfactant added by calcium carbonate activation stage, stearic acid
Sodium addition is the 1～3.5% of calcium hydroxide butt quality, and gained nano-calcium carbonate calcium product pattern is Spindle, and product granularity is
40～60 nanometers.
The method that the most according to claim 2, carbonization-activation integrated apparatus produces nano-calcium carbonate, when calcium hydroxide slurry is dense
When degree is 11～15%, adds and be equivalent to 0.3～the zinc sulfate of 0.5% of calcium hydroxide butt quality, control to be passed through carbonated-
In air Mixture, carbon dioxide concentration expressed in percentage by volume is gradually lowered to 50% from 100%, controls carbonization final temperature 40～50 DEG C,
It is Polyethylene Glycol and stearic acid composite surface activator, Polyethylene Glycol and stearic acid at surfactant added by calcium carbonate activation stage
The quality addition of the two is respectively the 1.5～2.5% and 0.5～1% of calcium hydroxide butt quality, gained nano-calcium carbonate calcium product pattern
For cube, product granularity is 70～90 nanometers.
The method that the most according to claim 2, carbonization-activation integrated apparatus produces nano-calcium carbonate, gained nano-calcium carbonate produces
The basicity of product controls at pH 9～10, product activation grade >=98%.
The present invention has following technical advantage and a beneficial effect:
1. the present invention produces the device of nano-calcium carbonate, collects carbonization, activation integral, simple in construction, reasonable energy utilization, behaviour
Facilitating, low cost, practical, product quality is controlled, can produce the nano-calcium carbonate calcium product of different crystal forms structure.
2. by special gas distributor, it is passed through adjustable density of carbon dioxide gas and speed-regulating mechanical stirring, improves dioxy
Change carbon gas distributed effect, avoid carbonization dead angle and product parcel accumulation of salt in the surface soil phenomenon, add a small amount of additive, control calcium carbonate product crystal formation
And product granularity, it is ensured that the concordance of product and integrity, improve the stability of product quality.
Accompanying drawing explanation
Fig. 1 is the carbonization-activation integrated apparatus producing nano-calcium carbonate: 1-additive entrance is held concurrently air vent；2-acidometer；3
-thermocouple；4-cooling water inlet；5-wall；6-cooling coil；7-shaft；8-gas distributor；9-frequency conversion
Speed stirrer；10-CO2Entrance；11-calcium hydroxide slurry inlet；12-coolant outlet；13-conduction oil exports；
14-stirring paddle；15-conduction oil chuck；16-heat conductive oil inlet；17-drain hole.
Fig. 2 is gas distributor.
Detailed description of the invention
The present invention is further illustrated with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Under room temperature, by the calcium hydroxide slip of the mass percentage concentration 8% through slagging-off refinement treatment, squeeze into carbonization-activation with starching pump
Integrated apparatus, opens stirring, and mixing speed is 150 turns per minute, is passed through cooling water cooling in cooling coil, controls carbonization
Reaction temperature is less than 40 DEG C, is passed through carbon dioxide-air Mixture and carries out carburizing reagent, by thermocouple temperature measurement, passes through acidity
Meter detection pH characterizes carburizing reagent process, along with the carrying out of carburizing reagent, regulates be passed through carbon dioxide concentration expressed in percentage by volume
It is gradually decrease to 30% by initial 80%, when carbodiimide solution pH value reaches 6, stops being passed through carbon dioxide-air Mixture,
Stopping refrigeration, terminate carburizing reagent, restart heat-conducting oil heating, quickly stir, mixing speed is 350 turns per minute, works as material
When slurry temperature reaches 70 DEG C, adding the sodium stearate being equivalent to calcium hydroxide butt quality 2%, activation modification, after 30 minutes, stops
Only heating and stirring, terminate activation modification, the slip after carbonization-activation removed integrated apparatus, and filter-press dehydration, at 120 DEG C
The most dried, i.e. obtain nano-calcium carbonate calcium product, nano-calcium carbonate crystal formation is Spindle, and draw ratio is about 3～4: 1, average particle
Footpath 45nm, the basicity of gained nano-calcium carbonate calcium product is pH 9, and product activation grade is 98.5%.
Embodiment 2
Under room temperature, by the calcium hydroxide slip of the mass percentage concentration 13% through slagging-off refinement treatment, squeeze into carbonization with starching pump and live
Changing integrated apparatus, add the zinc sulfate of be equivalent to calcium hydroxide butt quality 0.5%, open stirring, mixing speed is every point
250 turns of clock, is passed through cooling water cooling in cooling coil, control carbonation reaction temperature less than 50 DEG C, be passed through carbonated-
Air gas mixture carries out carburizing reagent, by thermocouple temperature measurement, is detected by acidometer and characterizes carburizing reagent process, along with
The carrying out of carburizing reagent, regulates be passed through carbon dioxide concentration expressed in percentage by volume and is gradually decrease to 50% by initial 100%, work as carbon
When change solution ph reaches 7, stop being passed through carbon dioxide-air Mixture, stop refrigeration, terminate carburizing reagent, restart
Heat-conducting oil heating, quickly stirs, and mixing speed is 400 turns per minute, when slurry temperature reaches 80 DEG C, adds and is equivalent to hydrogen
The Polyethylene Glycol of calcium oxide butt quality 2% activates with the composite surface of the stearic acid composition being equivalent to calcium hydroxide butt quality 1%
Agent, after carrying out activation modification 40 minutes, stops heating and stirring, terminates activation modification, then removed by the slip after carbonization-activation
Integrated apparatus, filter-press dehydration, fully dried at 130 DEG C, i.e. obtain nano-calcium carbonate calcium product, nano-calcium carbonate crystal formation in
Cube, mean diameter is pH 9.5 in 75nm, the basicity of gained nano-calcium carbonate calcium product, and product activation grade is 99%.
Claims (5)
1. the carbonization-activation integrated apparatus producing nano-calcium carbonate, it is characterised in that by conduction oil chuck, cooling coil,
Carbon dioxide distributor, frequency-control blender, outer barrel wall are constituted, built with acidometer and thermocouple, cooling coil
Coolant is used for controlling carbonation reaction temperature, and conduction oil chuck is heating when activation modification, so constitutes the one of carbonization-activation
Body gasifying device；
Described carbonization-activation integrated apparatus is also connected with carbon dioxide-air mixing surge tank system, this surge tank system
Can be with regulation of carbon dioxide and the mixed proportion of air and the flow of carbon dioxide-air Mixture and pressure；
Described carbon dioxide distributor is made up of an empty circles and coupled logical hollow center cross, empty
Passage is had, for avoiding gas distributor underlying space that gas occurs on heart circle and coupled logical hollow center cross
The dead angle that can not arrive and avoid clogging deposits passage, adjacent vent holes dislocation 15～30 the most in opposite directions inwards in empty circles
Degree diagonal cut joint down, on hollow center cross adjacent vent holes misplace in opposite directions to both sides 15～30 degree of diagonal cut joints down, passage
A diameter of 3～9mm, passage spacing is 5～10cm, and passage is symmetric, and circle distribution is closeer and central distribution relatively
Dilute, to meet carbon dioxide equally distributed needs in carbonization-activation integrated apparatus.
The method that the most according to claim 1, carbonization-activation integrated apparatus produces nano-calcium carbonate, it is characterised in that: will
Through mass percentage concentration 6～the calcium hydroxide slip of 15% of slagging-off refinement treatment, squeeze into carbonization-activation integrated apparatus with starching pump,
Low rate mixing, cooling coil are passed through cooling water cooling, control carbonation reaction temperature 10～50 DEG C, are passed through carbonated volume
Percentage concentration 30～100% carbon dioxide-air Mixture carry out carbonization, when carbodiimide solution pH value reaches 67, stop being passed through
Carbon dioxide-air Mixture, stops refrigeration, terminates carburizing reagent, restarts heat-conducting oil heating, quickly stir, when slip temperature
Degree reaches 60～90 DEG C, adds and is equivalent to calcium hydroxide butt quality 1～the additive of 5%, activation modification 20～after 40 minutes, stops
Only heating and stirring, terminate activation modification, the slip after carbonization-activation removed integrated apparatus, and filter-press dehydration, at 110～130 DEG C
The most dried, i.e. obtain nano-calcium carbonate calcium product；
The rotating speed of described carbonisation low rate mixing is 100～300 turns per minute, and described carbonisation is passed through carbon dioxide body
Long-pending percentage concentration is gradually lowered from 100% to 30%, is gradually lowered Tong Bus change with calcium hydroxide water oar concentration, and carburizing temperature
Then gradually rise from 10 DEG C to 50 DEG C, the most both realized the adaptation of carbon dioxide and calcium hydroxide carburizing reagent concentration, ensured again two
Carbon oxide gas obtains fully dispersed and utilizes, and maintains certain time of staying, to realize efficient carbonization；
The rotating speed that described activation process quickly stirs is 310～600 turns per minute, utilizes the particle encounter that quickly stirring kinetic energy brings,
Activation modification is carried out under Action of Surfactant；
Described additive be zinc sulfate, Polyethylene Glycol, stearic acid, sodium stearate, sodium polyacrylate at least one or one with
On.
The method that the most according to claim 2, carbonization-activation integrated apparatus produces nano-calcium carbonate, it is characterised in that: work as hydrogen
When calcium oxide pulp quality percentage concentration is 6～10%, control to be passed through carbon dioxide volume basis in carbon dioxide-air Mixture dense
Spending and be gradually lowered to 30% from 80%, controlling carbonization final temperature is 30～40 DEG C, in surface activity added by calcium carbonate activation stage
Agent is sodium stearate, and sodium stearate addition is the 1～3.5% of calcium hydroxide butt quality, and gained nano-calcium carbonate calcium product pattern is
Spindle, product granularity is 40～60 nanometers.
The method that the most according to claim 2, carbonization-activation integrated apparatus produces nano-calcium carbonate, it is characterised in that: work as hydrogen
When calcium oxide concentration of slurry is 11～15%, add 0.3～the zinc sulfate of 0.5% being equivalent to calcium hydroxide butt quality, control logical
Enter carbon dioxide concentration expressed in percentage by volume in carbonated-air Mixture and be gradually lowered to 50% from 100%, control carbonization final
Temperature 40～50 DEG C, be Polyethylene Glycol and stearic acid composite surface activator at surfactant added by calcium carbonate activation stage, poly-
The quality addition of both ethylene glycol and stearic acid is respectively the 1.5～2.5% and 0.5～1% of calcium hydroxide butt quality, gained nanometer
Calcium carbonate product pattern is cube, and product granularity is 70～90 nanometers.
The method that the most according to claim 2, carbonization-activation integrated apparatus produces nano-calcium carbonate, it is characterised in that: gained
The basicity of nano-calcium carbonate calcium product controls at pH 9～10, product activation grade >=98%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106673043A (en) * | 2017-01-06 | 2017-05-17 | 石家庄学院 | Toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate for filling polyethersulfone resin as well as preparation method and application of toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate |
| 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 |
| CN107827138A (en) * | 2017-12-08 | 2018-03-23 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of superfine active calcium carbonate |
| 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 |
| CN111013521A (en) * | 2019-12-25 | 2020-04-17 | 广西华纳新材料科技有限公司 | Nano calcium carbonate pressurized carbonation and surface modification integrated reaction kettle and application |
| CN114380315A (en) * | 2021-09-22 | 2022-04-22 | 湖南新绿方药业有限公司 | Purification method and production equipment of medicinal calcium carbonate |
| CN115041125A (en) * | 2022-06-21 | 2022-09-13 | 耒阳市百汇粉体有限公司 | Activation treatment equipment for calcium carbonate powder production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106673043A (en) * | 2017-01-06 | 2017-05-17 | 石家庄学院 | Toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate for filling polyethersulfone resin as well as preparation method and application of toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate |
| 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 |
| CN107827138A (en) * | 2017-12-08 | 2018-03-23 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of superfine active calcium carbonate |
| 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 |
| CN111013521A (en) * | 2019-12-25 | 2020-04-17 | 广西华纳新材料科技有限公司 | Nano calcium carbonate pressurized carbonation and surface modification integrated reaction kettle and application |
| CN114380315A (en) * | 2021-09-22 | 2022-04-22 | 湖南新绿方药业有限公司 | Purification method and production equipment of medicinal calcium carbonate |
| 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 |
| CN115041125A (en) * | 2022-06-21 | 2022-09-13 | 耒阳市百汇粉体有限公司 | Activation treatment equipment for calcium carbonate powder production |
| 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 |
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