CN106219586A - A kind of be raw material production nanometer grade calcium carbonate with carbide slag device and method - Google Patents
A kind of be raw material production nanometer grade calcium carbonate with carbide slag device and method Download PDFInfo
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- CN106219586A CN106219586A CN201610624402.8A CN201610624402A CN106219586A CN 106219586 A CN106219586 A CN 106219586A CN 201610624402 A CN201610624402 A CN 201610624402A CN 106219586 A CN106219586 A CN 106219586A
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- calcium carbonate
- groove
- carbide slag
- digestion reaction
- carburizing reagent
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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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- 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
Abstract
The invention discloses a kind of device and method being raw material production nanometer grade calcium carbonate with carbide slag, including for making carbide slag and the digestion reaction groove of water generation digestion reaction, the port of export of digestion reaction groove connects automatic back-washing surface filter, the slurry outlet of automatic back-washing surface filter is connected to slurry groove, purified liquor outlet is connected to dashpot, the port of export of dashpot is connected to molten solid/liquid/gas reactions device, connect on molten solid/liquid/gas reactions device and have carbon dioxide pipeline, the port of export of molten solid/liquid/gas reactions device connects carburizing reagent groove, the port of export of carburizing reagent groove connects dry slag filter, the dry slag port of export of dry slag filter connects hig h-speed centrifugal spray drying system, the purified liquor outlet end of dry slag filter is connected to the arrival end of digestion reaction groove.Flow process of the present invention is simple, consersion unit configuration is simple, floor space is little, simple to operation, and carburizing reagent speed is fast, and production efficiency is high.
Description
Technical field
The present invention relates to nanometer grade calcium carbonate production field, be specifically related to a kind of with carbide slag for raw material production nano-scale carbon
The device and method of acid calcium.
Background technology
Carbide slag is carbide (CaC2) hydrolysis acquisition acetylene gas (C2H2The waste residue with calcium oxide as main component after), mesh
The carbide slag of front China only has minimal amount of for concrete with cement mortar, most does not obtain as solid slag fully
Utilization.Carbide slag not only takies substantial amounts of soil and stacks, and pollutes the water resource stacked near place, easily air-dries and is formed
Dust environmental pollution is serious, and traditional carbide slag processing mode can not meet the requirement of environment and economy, and carbide slag is
The trade waste with priority treatment and utilization must be paid attention to.
Traditional calcium carbonate produces all with limestone as raw material, works the mischief environment in the recovery process of raw material,
Produce substantial amounts of energy consumption simultaneously.Utilizing carbide slag to produce nano-calcium carbonate is a good selection, and nano-calcium carbonate is a kind of
Novel solid materials, owing to super-refinement, the whiteness of calcium carbonate particle are high, loading is big and has the features such as reinforcing effect, rubber
The industrial circles such as glue, plastics, papermaking, ink have a wide range of applications.The market potential of domestic nano-calcium carbonate is huge, market price
Lattice differ bigger because of performance and the difference of application.Along with solid waste resource recovery utilizes the development of technology, with
Replacing carbide slag with lime stone produces that nano-calcium carbonate becomes a kind of novel, environmental protection, economic carbide slag processes and nano-calcium carbonate
Production technology, not only can eliminate the carbide slag impact on environment, additionally it is possible to save the production cost of nano-calcium carbonate, " becomes useless
For treasured " realize the doulbe-sides' victory of environmental improvement and economic interests.
The technology of existing carbide slag production nano-calcium carbonate also exists production equipment complexity, response time length, equipment
Floor space is big waits shortcomings.
Summary of the invention
It is an object of the invention to provide a kind of device and method being raw material production nanometer grade calcium carbonate with carbide slag, with
Overcoming the defect that above-mentioned prior art exists, flow process of the present invention is simple, consersion unit configuration is simple, floor space is little, operation is simple
Just, carburizing reagent speed is fast for folk prescription, and production efficiency is high.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of be raw material production nanometer grade calcium carbonate with carbide slag device, including for making carbide slag and water digest
The digestion reaction groove of reaction, the port of export of digestion reaction groove connects automatic back-washing surface filter, automatic back-washing surface filtration
The slurry outlet of device is connected to slurry groove, and purified liquor outlet is connected to dashpot, and the port of export of dashpot is connected to molten solid/liquid/gas reactions dress
Putting, molten solid/liquid/gas reactions device connects carbon dioxide pipeline, and the port of export of molten solid/liquid/gas reactions device connects carburizing reagent groove,
The port of export of carburizing reagent groove connects dry slag filter, and the dry slag port of export of dry slag filter connects high speed centrifugation spray dried
Drying system, the purified liquor outlet end of dry slag filter is connected to the arrival end of digestion reaction groove.
Further, digestion reaction groove includes the one-level digestion reaction groove that is arranged in series and two grades of digestion reaction grooves, and one
Level digestion reaction groove and two grades of digestion reaction grooves are equipped with agitating device.
Further, carburizing reagent groove includes the one-level carburizing reagent groove being arranged in series, two grades of carburizing reagent grooves and three grades
Carburizing reagent groove, and one-level carburizing reagent groove, two grades of carburizing reagent grooves and tertiary carbon reactive tank are equipped with agitating device.
Further, between digestion reaction groove and automatic back-washing surface filter and dashpot and molten solid/liquid/gas reactions device it
Between be all connected with anti-interference hydrotreater and elevator pump in turn.
Further, between carburizing reagent groove and dry slag filter, connection has elevator pump.
A kind of with carbide slag for the method for raw material production nanometer grade calcium carbonate, comprise the following steps:
1) in carbide slag, addition water for industrial use carries out digestion and obtains digestion mixed liquor；
2) digestion mixed liquor is carried out solid-liquid separation, obtain saturated calcium hydroxide aqueous solution；
3) in saturated calcium hydroxide aqueous solution, add chemical additives and dispersant, obtain buffer；
4) in buffer, add carbon dioxide generation carburizing reagent, obtain carbonization mixed liquor；
5), after being filtered by carbonization mixed liquor, calcium carbonate filter cake and clear liquid are obtained；
6) by clear liquid and step 1) in water for industrial use mixing reuse, calcium carbonate filter cake is carried out hig h-speed centrifugal spray drying i.e.
Obtain nano-calcium carbonate calcium powder.
Further, step 1) middle employing two-stage digests and carries out digestion reaction, and addition in every 580L water for industrial use
1.65kg carbide slag.
Further, step 3) in the addition of chemical additives and dispersant be saturated calcium hydroxide aqueous solution quality
1‰。
Further, step 4) in carbon dioxide be by the liquid carbon dioxide of purity ＞ 99% by decompressor and
Obtain after air temperature gasifier gasification, and the pH=7 of carburizing reagent～8, temperature is room temperature.
Further, step 5) in the moisture content of calcium carbonate filter cake that obtains be 40～60%, step 6) in nano-calcium carbonate
The moisture content ＜ 0.5% of calcium powder.
Compared with prior art, the present invention has a following useful technique effect:
Apparatus of the present invention arrange digestion reaction groove and are dissolved by the calcium hydroxide in carbide slag, and then by automatic back-washing surface
Filter carries out solid-liquid separation and obtains saturated calcium hydroxide aqueous solution, saturated calcium hydroxide aqueous solution in molten solid/liquid/gas reactions device with
Carbon dioxide is fully contacted and reacts, and molten solid/liquid/gas reactions device can improve the contact surface of carbon dioxide and aqua calcis
Long-pending, accelerate reaction rate, save carbonization time, subsequently enter carburizing reagent groove and the most fully react, complete through carburizing reagent
Rear mixed liquor is delivered to dry slag filter and carries out solid-liquid separation, and dry slag filter is equipped with compressed air piping carbon in system
Drying up of acid calcium filter cake, the clear liquid after the filtration of the most dry slag filter arranges reflux line and is directly back to carbide slag digestion reaction
Groove recycles, and finally uses hig h-speed centrifugal spray drying system to be dried, to improve drying efficiency, and need not any pulverize
And screening plant can directly obtain powder body calcium carbonate product, automatic back-washing surface filter and dry slag used in it filter
Device all can automatic discharge, and carry backwash function, personnel demand amount greatly reduces, and consersion unit of the present invention configuration is simple, take up an area
Area is little, simple to operation, and carburizing reagent speed is fast, and production efficiency is high.
Further, digestion reaction groove uses two-stage digestion reaction groove to be arranged in series, and can be effectively improved carbide slag digestion
Efficiency.
Further, carburizing reagent groove uses tertiary carbon reactive tank to be arranged in series, and can be effectively improved carburizing reagent effect
Rate.
Further, arrange in digestion reaction groove and carburizing reagent groove agitating device be prevented from calcium carbonate deposition and
Response speed can be accelerated.
Further, prevent because of calcium to strengthen the activity of solution flowing in pipeline by arranging anti-interference hydrotreater
The pipeline scale etc. that ion exists and causes.
Calcium hydroxide in carbide slag is dissolved by the inventive method, and then carries out solid-liquid separation and obtain saturated calcium hydroxide water
Solution, adds chemical additives and dispersant to reach to obtain the calcium carbonate particle of specific morphology in the carbonized and can have
The purpose that effect suppression calcium carbonate particle is reunited, makes that final products particle diameter is less, is more evenly distributed, have better processability
Can, then pass to carbon dioxide and make saturated calcium hydroxide aqueous solution and carbon dioxide be fully contacted and carburizing reagent occurs,
After carburizing reagent completely, mixed liquor carries out solid-liquid separation, filter cake is finally dried process and i.e. obtains nano-calcium carbonate calcium powder
End, the present invention is without other raw materials, with carbide slag for main material production calcium carbonate and the pollution problem that solves carbide slag,
Make its recycling, the most also produce high value-added product, generate without other by-products in the middle of production process, and produce use
Water can be recycled, and rate of water make-up is few, simple to operation, and carburizing reagent speed is fast, and production efficiency is high.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of the present invention.
Wherein: 1-one-level digestion reaction groove；Bis-grades of digestion reaction grooves of 2-；The anti-interference hydrotreater of 3-；4-elevator pump；5-is certainly
Dynamic backwash surface filter；6-dashpot；7-molten solid/liquid/gas reactions device；8-carburizing reagent groove；9-dry slag filter；10-at a high speed from
Heart spray drying system.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is described in further detail:
See Fig. 1, a kind of be raw material production nanometer grade calcium carbonate with carbide slag device, including for making carbide slag and water
The digestion reaction groove of digestion reaction occurs, and digestion reaction groove includes that the one-level digestion reaction groove 1 that is arranged in series and two grades of digestion are anti-
Answering groove 2, and be equipped with agitating device in one-level digestion reaction groove 1 and two grades of digestion reaction grooves 2, the port of export of digestion reaction groove leads to
Cross the anti-interference hydrotreater 3 being sequentially connected with and elevator pump 4 is connected to automatic back-washing surface filter 5, automatic back-washing surface mistake
The slurry outlet of filter 5 is connected to slurry groove, and purified liquor outlet is connected to dashpot 6, and the port of export of dashpot 6 is by being sequentially connected with
Anti-interference hydrotreater 3 and elevator pump 4 be connected to molten solid/liquid/gas reactions device 7, on molten solid/liquid/gas reactions device 7 connect have carbon dioxide to enter
Feed channel, the port of export of molten solid/liquid/gas reactions device 7 connects has carburizing reagent groove 8, carburizing reagent groove 8 to include the one-level carbon being arranged in series
Change reactive tank, two grades of carburizing reagent grooves and tertiary carbon reactive tank, and one-level carburizing reagent groove, two grades of carburizing reagent grooves and three grades
Being equipped with agitating device in carburizing reagent groove, the port of export of carburizing reagent groove 8 is connected to dry slag filter 9 by elevator pump 4, dry
The dry slag port of export of slag filter 9 connects hig h-speed centrifugal spray drying system 10, and the purified liquor outlet end of dry slag filter 9 connects
Arrival end to digestion reaction groove.
A kind of with carbide slag for the method for raw material production nanometer grade calcium carbonate, comprise the following steps:
1) in carbide slag, add water for industrial use, use two-stage digestion to carry out digestion and obtain digesting mixed liquor, wherein, often
580L water for industrial use adds 1.65kg carbide slag；
2) digestion mixed liquor is carried out solid-liquid separation, obtain saturated calcium hydroxide aqueous solution；
3) in saturated calcium hydroxide aqueous solution, add chemical additives and dispersant, obtain buffer, wherein, crystal formation control
The addition of preparation and dispersant is the 1 ‰ of saturated calcium hydroxide aqueous solution quality；
4) in buffer, add carbon dioxide, control pH=7～8, carburizing reagent at room temperature occurs, obtain carbonization and mix
Closing liquid, wherein carbon dioxide is by obtaining after decompressor and air temperature gasifier gasification by the liquid carbon dioxide of purity ＞ 99%
Arrive；
5), after carbonization mixed liquor being dried filtration, clear liquid and calcium carbonate filter cake that moisture content is 40～60% are obtained；
6) by clear liquid and step 1) in water for industrial use mixing reuse, calcium carbonate filter cake is carried out hig h-speed centrifugal spray drying i.e.
Obtain the nano-calcium carbonate calcium powder of moisture content ＜ 0.5%.
Below in conjunction with the accompanying drawings the implementation process of the present invention is further described:
As it can be seen, carbide slag and water carry out digestion reaction (opening stirring), carbide in one-level digestion reaction groove 1 simultaneously
In slag, calcium hydroxide is dissolved in other insoluble matters of water and contamination precipitation, and after digestion reaction completes, mixed liquor passes through one-level digestion reaction
Groove 1 upper isopipe overflow is to two grades of digestion reaction grooves 2 (band stirring), and the boosted pump of Digestive system 4 is delivered to automatic back-washing subsequently
Surface filter 5 carries out solid-liquid separation, and impurity in solution and other insoluble matters are gone divided by obtaining saturated calcium hydroxide aqueous solution
(this aqueous solution pH is more than 12) is standby.Calcium hydroxide clear liquid gravity flow after filtration enters in dashpot 6 and (if desired obtains specific shape
The calcium carbonate of looks and particle diameter can add dispersant and the chemical additives of saturated calcium hydroxide aqueous solution quality 1 ‰ at this), subsequently
Boosted pump 4 is delivered to that molten solid/liquid/gas reactions device 7 is full and uniform with carbon dioxide to be mixed, and in pressure air-dissolving reactor 7
Fully reaction is completely, and this process controls addition and the stream of calcium hydroxide saturated solution of carbon dioxide with solution ph after reaction
Amount.The pressurized molten reacted calcium carbonate serosity of solid/liquid/gas reactions device 7 (reaction end pH controls 7～8) is from molten solid/liquid/gas reactions device 7
Bottom gravity flow enters carburizing reagent groove 8, and the most boosted pump 4 is delivered in dry slag filter 9 carry out solid-liquid separation and contains to obtain
Water rate 40～the calcium carbonate filter cake of 60% and in neutral clear liquid, clear liquid gravity flow returns digestion reaction groove and recycles, calcium carbonate
Filter cake eventually passes through hig h-speed centrifugal spray drying system 10 drying and dehydrating to obtain the moisture content nano-calcium carbonate calcium powder less than 5%
End.
Prepare nano-calcium carbonate device based on above-mentioned carbide slag, be embodied as comprising the following steps:
(1) saturated calcium hydroxide aqueous solution is produced in the digestion of carbide slag: by calcium hydroxide content analysis in carbide slag
And calcium hydroxide the considering of dissolubility in water, according to every 580L water for industrial use adding the ratio of 1.65kg carbide slag by two
Person is mixed and stirred for reaction, and after reaction, obtaining saturated calcium hydroxide aqueous solution through solid-liquid separation, (this solution ph is more than
12)。
(2) chemical additives and the input of dispersant: according to the feature of target product and require before carburizing reagent or anti-
Add in should saturated calcium hydroxide aqueous solution quality 1 ‰ chemical additives and dispersant to obtain specific morphology and particle diameter
Calcium carbonate product.
(3) carburizing reagent: make calcium hydroxide saturated aqueous solution and carbon dioxide be sufficiently mixed all by molten solid/liquid/gas reactions device 7
Even, in carburizing reagent groove 8, reaction is completely to obtain calcium carbonate serosity simultaneously, and this process is adjusted by the pH value of mixed liquor after reaction
The addition of whole carbon dioxide and the flow of aqua calcis ensure that carburizing reagent is completely, thoroughly.
(4) separate, be dried: the calcium carbonate serosity after carburizing reagent carries out separating obtaining through overdrying slag filter 9 aqueous
The calcium carbonate filter cake of rate 40%～60% and the clear liquid in neutrality, clear liquid returns digestion reaction groove and continues cycling through use, and filter cake leads to
Cross high speed centrifugal spray drying system 10 and carry out dehydrate to obtain the moisture content calcium carbonate powder less than 0.5%.
Claims (10)
1. the device that a kind is raw material production nanometer grade calcium carbonate with carbide slag, it is characterised in that include for make carbide slag and
The digestion reaction groove of water generation digestion reaction, the port of export of digestion reaction groove connects has automatic back-washing surface filter (5), automatically
The slurry outlet of backwash surface filter (5) is connected to slurry groove, and purified liquor outlet is connected to dashpot (6), going out of dashpot (6)
Mouth end is connected to molten solid/liquid/gas reactions device (7), and the upper connection of molten solid/liquid/gas reactions device (7) has carbon dioxide pipeline, and molten solid/liquid/gas reactions fills
The port of export connection putting (7) has carburizing reagent groove (8), and the port of export of carburizing reagent groove (8) connects dry slag filter (9), dry
The dry slag port of export of slag filter (9) connects hig h-speed centrifugal spray drying system (10), the purified liquor outlet of dry slag filter (9)
End is connected to the arrival end of digestion reaction groove.
The most according to claim 1 a kind of be raw material production nanometer grade calcium carbonate with carbide slag device, it is characterised in that
Digestion reaction groove includes one-level digestion reaction groove (1) that is arranged in series and two grades of digestion reaction grooves (2), and one-level digestion reaction groove
(1) and two grades of digestion reaction grooves (2) are equipped with agitating device.
The most according to claim 1 a kind of be raw material production nanometer grade calcium carbonate with carbide slag device, it is characterised in that
Carburizing reagent groove (8) includes the one-level carburizing reagent groove being arranged in series, two grades of carburizing reagent grooves and tertiary carbon reactive tank, and one
Level carburizing reagent groove, two grades of carburizing reagent grooves and tertiary carbon reactive tank are equipped with agitating device.
The most according to claim 1 a kind of be raw material production nanometer grade calcium carbonate with carbide slag device, it is characterised in that
Between digestion reaction groove and automatic back-washing surface filter (5) and between dashpot (6) and molten solid/liquid/gas reactions device (7) the most successively
Connect and have anti-interference hydrotreater (3) and elevator pump (4).
The most according to claim 1 a kind of be raw material production nanometer grade calcium carbonate with carbide slag device, it is characterised in that
Connect between carburizing reagent groove (8) and dry slag filter (9) and have elevator pump (4).
6. the method that a kind is raw material production nanometer grade calcium carbonate with carbide slag, it is characterised in that comprise the following steps:
1) in carbide slag, addition water for industrial use carries out digestion and obtains digestion mixed liquor；
2) digestion mixed liquor is carried out solid-liquid separation, obtain saturated calcium hydroxide aqueous solution；
3) in saturated calcium hydroxide aqueous solution, add chemical additives and dispersant, obtain buffer；
4) in buffer, add carbon dioxide generation carburizing reagent, obtain carbonization mixed liquor；
5), after being filtered by carbonization mixed liquor, calcium carbonate filter cake and clear liquid are obtained；
6) by clear liquid and step 1) in water for industrial use mixing reuse, calcium carbonate filter cake is carried out hig h-speed centrifugal spray drying and i.e. obtains
Nano-calcium carbonate calcium powder.
The most according to claim 6 a kind of be raw material production nanometer grade calcium carbonate with carbide slag method, it is characterised in that
Step 1) middle employing two-stage digests and carries out digestion reaction, and addition 1.65kg carbide slag in every 580L water for industrial use.
The most according to claim 6 a kind of be raw material production nanometer grade calcium carbonate with carbide slag method, it is characterised in that
Step 3) in chemical additives and addition is saturated calcium hydroxide aqueous solution quality the 1 ‰ of dispersant.
The most according to claim 6 a kind of be raw material production nanometer grade calcium carbonate with carbide slag method, it is characterised in that
Step 4) in carbon dioxide be by after decompressor and air temperature gasifier gasification by the liquid carbon dioxide of purity ＞ 99%
Obtain, and the pH=7 of carburizing reagent～8, temperature is room temperature.
The most according to claim 6 a kind of be raw material production nanometer grade calcium carbonate with carbide slag method, its feature exists
In, step 5) in the moisture content of calcium carbonate filter cake that obtains be 40～60%, step 6) in the moisture content of nano-calcium carbonate calcium powder
＜ 0.5%.
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|---|---|---|---|---|
| CN110342558A (en) * | 2019-08-15 | 2019-10-18 | 张旭 | Prepare the device and technique of high-purity calcium carbonate |
| CN110589862A (en) * | 2019-09-09 | 2019-12-20 | 建德华明科技有限公司 | Multistage series method for producing nano-grade calcium carbonate by carbonization method with liquid phase as continuous phase |
| CN110615458A (en) * | 2019-10-08 | 2019-12-27 | 张旭 | Device and process for preparing high-purity calcium carbonate |
| CN111330435A (en) * | 2020-03-18 | 2020-06-26 | 福建龙净脱硫脱硝工程有限公司 | Carbide slag absorbent and preparation method thereof |
| CN112897561A (en) * | 2021-05-10 | 2021-06-04 | 中国科学院过程工程研究所 | System device and method for preparing calcium carbonate by using micro-nano bubbles |
| CN113087004A (en) * | 2021-04-14 | 2021-07-09 | 上海抚翌科技有限公司 | Production method of calcium carbonate in cigarette paper |
| CN113104875A (en) * | 2021-03-31 | 2021-07-13 | 陕西金禹科技发展有限公司 | Process for preparing superfine or nano calcium carbonate from carbide slag and treatment system thereof |
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