CN107456931A - A kind of device and method for generating unstable calcium carbonate mineral phase - Google Patents
A kind of device and method for generating unstable calcium carbonate mineral phase Download PDFInfo
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- CN107456931A CN107456931A CN201710671410.2A CN201710671410A CN107456931A CN 107456931 A CN107456931 A CN 107456931A CN 201710671410 A CN201710671410 A CN 201710671410A CN 107456931 A CN107456931 A CN 107456931A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2455—Stationary reactors without moving elements inside provoking a loop type movement of the reactants
- B01J19/2465—Stationary reactors without moving elements inside provoking a loop type movement of the reactants externally, i.e. the mixture leaving the vessel and subsequently re-entering it
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a kind of device and method for generating unstable calcium carbonate mineral phase, and device is by lower reaction zone, middle part fluidization regions and top settling zone composition;The equimolar Na of configuration2CO3And CaCl2Solution enters from the both sides of reactor lower part respectively, and CaCO is generated after mixing3Crystal;Overhead reflux is passed through with faster flow velocity from bottom, has certain diluting effect to entering the aqueous solution, and it, which rises active force, makes CaCO3Crystallization process is in fluidized state;The CaCO of generation3Crystal occurs to precipitate and separate with solution in settling zone, and reacted solution is discharged from top delivery port;The present invention is acted on to CaCO by backflow3The influence of crystallization process, CaCO can be suppressed3The generation of stable phase calcite, promote the generation of unstable phase such as aragonite and aragonite, not only improve and solve the problems, such as the reaction fouling caused by calcite generates, be also beneficial to carry out unstable CaCO3The research that mineral facies utilize;Compared with other method, have the characteristics that operation is simple, cost is low, easy to operate and control.
Description
Technical field
It is more particularly to a kind of to generate unstable calcium carbonate mineral phase the invention belongs to mineral synthesis processing engineering technology field
Device and method.
Background technology
In real life and engineering field, there is different degrees of fouling problem in most heat transmission equipments, to equipment
Harmfulness it is very big.Industrially developed country every year because of dirt and caused by industrial loss account for the 0.3% of its gross national product.
China is developing country, is also energy resource consumption big country, comparatively, Anti-fouling Technology fall behind, because dirt and caused by pass through
The ratio regular meeting that Ji loss accounts for GNP is higher.
CaCO3It is the main component in dirt, there is three kinds of different mineral facies, i.e. calcite, aragonite and aragonite.Fang Xie
Stone generally existing in nature, is the most stable of calcium carbonate mineral phase of thermodynamics, and it is the main component of hard scale, it is more difficult to clear
Remove;Aragonite and aragonite category CaCO3Unstable phase, what they were generated is precipitated as soft dirt, is easily eliminated.Conventional preventing fouling includes
Chemical method and Physical.The essence of chemical scale inhibition is that addition chemical reagent prevents calcium carbonate from growing, and currently used reagent has
Machine phosphoric acid and polymer, CaCO is mainly controlled by effects such as chelating, distortion of lattice, Coulomb repulsions3The habit of crystal, resistance
Only unstable CaCO3Conversion of the mineral facies (aragonite and aragonite) to stable phase calcite, makes aragonite and aragonite be stabilized presence,
The generation of stable phase calcite is but inhibited simultaneously.Physical oil production method, it is mainly purposeful using technology and equipments such as sound, electricity, magnetic
Ground changes Ca2+、CO3 2-And the motion state of hydrone etc., to maintain unstable CaCO3Mineral facies provide dynamics energy, from
And suppress the generation of stable phase calcite.
Above-mentioned chemically and physically antiscaling method is all by controlling CaCO3Crystallization process, prevent CaCO3It is unstable opposite steady
The transformation of phase is determined to realize.The former needs to add chemical reagent, and cost is high, and easily causes secondary pollution to environment;The latter needs
Light, electricity, magnetic dependence device are equipped with, investment is big, and treatment effect is typically not so good as chemical method.In addition, unstable CaCO3Mineral facies have
There are good application prospect, such as aragonite, be widely used in personal care product's additive, medical carrier, photoelectric material, top grade
The fields such as ink, catalyst carrier;Preparation of aragonite whisker as a kind of novel inorganic reinforcing material, be widely used in papermaking, rubber,
Plastics, medicine and other fields.Therefore, simple, inexpensive, environment-friendly unstable CaCO is probed into3Mineral facies generating means and side
Method has important reality and scientific meaning.
The content of the invention
The shortcomings that in order to overcome above-mentioned prior art, it is an object of the invention to provide one kind to generate unstable calcium carbonate ore deposit
The device and method of thing phase, by the operation of reactor itself, suppress CaCO3The generation of stable phase, promote the life of unstable phase
Into to eliminate influence of the dirt to equipment, and development CaCO3A kind of simple, low cost of comprehensive utilization offer of unstable phase,
Environment-friendly apparatus and method.
To achieve these goals, the technical solution adopted by the present invention is:
A kind of device for generating unstable calcium carbonate mineral phase, including reaction zone 1, fluidization regions 2 and settling zone 3, it is described anti-
The both sides of area 1 are answered to be provided with Na2CO3Solution water inlet 5 and CaCl2Solution water inlet 8, bottom are provided with phegma water inlet 15, and middle part is set
There is water-locator 4;The coupled reaction area 1 of fluidization regions 2 and settling zone 3;The settling zone 3 is provided with phegma delivery port 11 and draining
Mouth 13, the phegma delivery port 11 is connected with phegma water inlet 15 by the pipeline with reflux pump 12.
The reaction zone 1, fluidization regions 2 and settling zone 3 are set gradually from bottom to top, wherein reaction zone 1 and the internal diameter of fluidization regions 2
Than for 1, highly than for 0.1-0.2, the internal diameter ratio of the settling zone 3 and fluidization regions 2 be 2-4, and the height of settling zone 3 is that device is total
High 18%-25%.
The 15%-30% of the height of lower inner diameter transition region accounting settling zone 3 of the settling zone 3.
The Na2CO3Solution water inlet 5 connects Na by the pipeline with intake pump 12CO3Solution intake pool 7, it is described
CaCl2Solution water inlet 8 connects CaCl by the pipeline with intake pump 292Solution intake pool 10, the discharge outlet 13 is through pipe
Road connects collecting-tank 14.
The water-locator 4 is located in reaction zone 1 at 3/4 height, the limbers containing 8-16 aperture 1.5mm, water-locator 4
In Na2CO3Solution water inlet 5 and CaCl2The lower section of solution water inlet 8.
Present invention also offers a kind of method of the unstable calcium carbonate mineral phase of generation based on described device, including it is following
Several steps:
Step 1, the Na of equimolar high concentration2CO3And CaCl2Solution is separately stored in Na2CO3The He of solution intake pool 7
CaCl2In solution intake pool 10, by intake pump 1 and intake pump 29 by Na2CO3Solution water inlet 5 and CaCl2Solution is intake
Mouth 8 enters reaction zone 1, and CaCO is generated after mixing3Crystal;
Step 2, enter the aqueous solution and mixed in reaction zone 1, the settling zone 3 become larger via fluidization regions 2 into diameter,
Due to the decrease of effect of increasing power, and the transformation of solution flow direction, CaCO3Crystallized product slowly deposits in settling zone 3, realizes
Solid, liquid two-phase is separated, and a part of liquid phase is flowed back via phegma delivery port 11, and another part liquid phase is discharged via discharge outlet 13,
Into collecting-tank 14;
Step 3, phegma is entered from phegma delivery port 11 by reflux pump 12 by phegma water inlet 15, through water distribution
Device 4 realizes the water distribution uniformity of backflow, under the active force that flows back, CaCO in reaction zone 13Crystallization process is in fluidized state, and
Accelerate the dilution into the aqueous solution to a certain extent, play a part of reducing reaction system degree of supersaturation.
Wherein, hydraulic detention time 40-90min, upflow velocity of the phegma in fluidization regions 2 are 1.5-15m/h.
To the CaCO generated3Mineral characteristic analysis shows, improve device capacity of returns be advantageous to suppress CaCO3Stable phase
The generation of calcite, so as to promote unstable CaCO3The generation of crystal;In unstable phase based on aragonite, with capacity of returns
Increase, there is a small amount of aragonite to occur.Calcite be mostly rule it is square, aragonite with rose shape it is spherical based on, aragonite using pin column as
It is main.
The technical principle of the present invention:
A) by way of solution backflow, using the dilution effect of reflux solution flow control water inlet in systems, so that
The degree of supersaturation in solution is reduced, slows down CaCO3The crystallization process of mineral, be advantageous to the control to crystallization process;
B) as shown in Fig. 2 in CaCO3In crystallization process, never it is settled out first in the supersaturated solution of crystal seed
CaCO3It is amorphous phase, it is to be changed into CaCO3Polycrystalline predecessor, a part are converted into metastable phase aragonite and aragonite, separately
A part is converted into stable phase calcite, and under the conditions of the inhibitory action without external force and additive, metastable phase passes through dissolving-weight
Crystallization mechanism is converted into the most stable of calcite of thermodynamics, and backflow hydraulic disturbance effect can effectively improve solute molecule to meta-stable
The migration of plane of crystal, to CaCO3The dissolve-repreparation mechanism of metastable phase plays inhibitory action, so as to suppress stable phase
The generation of calcite.In addition, there are some researches show external force effect can change CaCO3The enthalpy of formation, be advantageous to meta-stable mineral facies
Be stabilized.
Compared with prior art, the present invention by being intake to system, the continuous operation of water outlet, and solution backflow to crystallization
The disturbance of process and fluidisation, it is suppressed that CaCO3The generation of stable phase, while the yield of unstable mineral facies is improved, can be effective
Solves CaCO3Scale problems, promote to unstable CaCO3The comprehensive utilization of mineral facies.In addition, the present invention need not add other changes
Learn reagent or be equipped with light, electricity, magnetic dependence device, have the characteristics that simple to operate, cost of investment is low and environment-friendly.
Brief description of the drawings
Fig. 1 is the installation drawing of the embodiment of the present invention.
Fig. 2 is the calcium carbonate mineral crystallization process figure of the embodiment of the present invention.
Fig. 3 is the XRD analysis figure that the embodiment of the present invention generates calcium carbonate mineral phase.
Fig. 4 is the electronic microscope photos figure that the embodiment of the present invention generates calcium carbonate mineral phase.
Embodiment
Describe embodiments of the present invention in detail with reference to the accompanying drawings and examples, described embodiment is only
The part example of the present invention, rather than whole examples.Those skilled in the art are obtained under the premise of not making creative work
Every other example, belong to protection scope of the present invention.
As shown in figure 1, a kind of device for generating unstable calcium carbonate mineral phase, is made up, effective volume 1L of lucite,
High 727mm, main reaction zone 1, fluidization regions 2 and the settling zone 3 included from bottom to top.Reaction zone 1 and the internal diameter ratio of fluidization regions 2 are 1,
Highly ratio is 0.1-0.2, and the internal diameter that reaction zone 1 and fluidization regions 2 are selected in the present embodiment is 31mm, highly than for 0.13.Precipitation
The internal diameter ratio of area 3 and fluidization regions 2 be 2-4, and the height of settling zone 3 is the always high 18%-25% of device, the lower inner diameter of settling zone 3
Less than upper inner diameter, the 15%-30% of the height of lower inner diameter transition region accounting settling zone 3, in the present embodiment selective precipitation area 3 with
The internal diameter ratio of fluidization regions 2 is 3, and the height of settling zone 3 is always high 22% of device, and lower inner diameter transition region accounting settling zone 3 is high
The 19% of degree.
The Na of reaction zone 12CO3Solution water inlet 5 connects Na by the pipeline with intake pump 12CO3Solution intake pool
7, the CaCl of reaction zone 12Solution water inlet 8 connects CaCl by the pipeline with intake pump 292Solution intake pool 10.Water-locator
4 are located in reaction zone 1 at 3/4 height, the limbers containing 8-16 aperture 1.5mm, and selection water-locator 4 contains 12 in the present embodiment
Individual aperture 1.5mm limbers.
The discharge outlet 13 of settling zone 3 is connected with collecting-tank 14, the phegma delivery port 11 and reaction zone of settling zone 3 through pipeline
The phegma water inlet 15 of 1 bottom is connected by the pipeline with reflux pump 12.The device of the present invention, its hydraulic detention time are
40-90min, upflow velocity of the recirculation water in recirculating zone 2 are 1.5-15m/h, selected in the present embodiment hydraulic detention time for
60min, upflow velocity of the recirculation water in fluidization regions 2 be 1.5,4.2,8,10m/h.
In the embodiment of the present invention, a kind of method for generating unstable calcium carbonate mineral phase, comprise the following steps:
Step 1, the Na of equimolar high concentration2CO3And CaCl2Solution is separately stored in Na2CO3The He of solution intake pool 7
CaCl2In solution intake pool 10, by intake pump 1 and intake pump 29 by Na2CO3Solution water inlet 5 and CaCl2Solution is intake
Mouth 8 enters reactor, and CaCO is generated after mixing3Crystal.The Na configured in the present embodiment2CO3And CaCl2Solution is 0.05mol/
L, i.e. Ca ion concentrations are 2000mg/L.
Step 2, phegma are entered, through water distribution from phegma delivery port 11 by reflux pump 12 by phegma water inlet 15
Device 4 realizes the water distribution uniformity of backflow, under the active force that flows back, CaCO in reaction zone 13Crystallization process is in fluidized state, and
Accelerate the dilution into the aqueous solution to a certain extent, play a part of reducing reaction system degree of supersaturation.
Step 3, enter the aqueous solution and mixed in reaction zone 1, the settling zone 3 become larger via fluidization regions 2 into diameter,
Due to the decrease of effect of increasing power, and the transformation of solution flow direction, CaCO3Crystallized product slowly deposits in settling zone 3, realizes
Solid, liquid two-phase is separated, and a part of liquid phase flows back via phegma delivery port 11, and another part liquid phase is entered by the discharge of outlet 13
Collecting-tank 14.
Be advantageous to suppress square CaCO test result indicates that improving device capacity of returns3The generation of stable phase calcite, so as to
Promote unstable CaCO3The generation of crystal;In unstable phase based on the spherical aragonite of rose shape, as capacity of returns increases, have
A small amount of needle-shaped aragonite occurs.Under conditions of upflow velocity of the recirculation water in recirculating zone 2 is 10m/h, CaCO3Stable phase side solves
The generation of stone is substantially suppressed, and content is less than 10%, CaCO3Unstable phase aragonite and aragonite proportion up to more than 90%,
Mineralogical characteristic under the experiment condition is as shown in Figures 3 and 4.
Claims (7)
1. a kind of device for generating unstable calcium carbonate mineral phase, it is characterised in that including reaction zone (1), fluidization regions (2) and sink
Shallow lake area (3), reaction zone (1) both sides are provided with Na2CO3Solution water inlet (5) and CaCl2Solution water inlet (8), bottom is provided with
Phegma water inlet (15), middle part are provided with water-locator (4);Fluidization regions (2) the coupled reaction area (1) and settling zone (3);It is described
Settling zone (3) is provided with phegma delivery port (11) and discharge outlet (13), the phegma delivery port (11) and phegma water inlet
(15) connected by the pipeline with reflux pump (12).
2. the device of unstable calcium carbonate mineral phase is generated according to claim 1, it is characterised in that the reaction zone (1),
Fluidization regions (2) and settling zone (3) are set gradually from bottom to top, and wherein reaction zone (1) and fluidization regions (2) internal diameter ratio are 1, height ratio
For 0.1-0.2, the internal diameter ratio of the settling zone (3) and fluidization regions (2) is 2-4, and the height of settling zone (3) is total high for device
18%-25%.
3. the device of unstable calcium carbonate mineral phase is generated according to claim 1, it is characterised in that the settling zone (3)
Lower inner diameter transition region accounting settling zone (3) height 15%-30%.
4. the device of unstable calcium carbonate mineral phase is generated according to claim 1, it is characterised in that the Na2CO3Solution
Water inlet (5) connects Na by the pipeline with intake pump one (6)2CO3Solution intake pool (7), the CaCl2Solution water inlet
(8) CaCl is connected by the pipeline with intake pump two (9)2Solution intake pool (10), the discharge outlet (13) connect through pipeline
Collecting-tank (14).
5. the device of unstable calcium carbonate mineral phase is generated according to claim 1, it is characterised in that the water-locator (4)
Located at 3/4 height, the limbers containing 8-16 aperture 1.5mm, water-locator (4) is located at Na in reaction zone (1)2CO3Solution is intake
Mouth (5) and CaCl2The lower section of solution water inlet (8).
A kind of 6. method of the unstable calcium carbonate mineral phase of generation based on claim 1 described device, it is characterised in that including
Following steps:
Step 1, the Na of equimolar high concentration2CO3And CaCl2Solution is separately stored in Na2CO3Solution intake pool (7) and CaCl2
In solution intake pool (10), by intake pump one (6) and intake pump two (9) by Na2CO3Solution water inlet (5) and CaCl2Solution
Water inlet (8) enters reaction zone (1), and CaCO is generated after mixing3Crystal;
Step 2, enter the aqueous solution and mixed in reaction zone (1), the settling zone become larger via fluidization regions (2) into diameter
(3), due to the decrease of effect of increasing power, and the transformation of solution flow direction, CaCO3Crystallized product slowly sinks in settling zone (3)
Product, realize that solid, liquid two-phase separates, a part of liquid phase flows back via phegma delivery port (11), and another part liquid phase is via draining
Mouth (13) discharge, into collecting-tank (14);
Step 3, phegma is entered from phegma delivery port (11) by reflux pump (12) by phegma water inlet (15), through cloth
Hydrophone (4) realizes the water distribution uniformity of backflow, under the active force that flows back, CaCO in reaction zone (1)3Crystallization process is in fluidisation shape
State, and accelerate the dilution into the aqueous solution to a certain extent, play a part of reducing reaction system degree of supersaturation.
7. the method for unstable calcium carbonate mineral phase is generated according to claim 6, it is characterised in that hydraulic detention time is
40-90min, upflow velocity of the phegma in fluidization regions (2) are 1.5-15m/h.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2022083376A1 (en) * | 2020-10-23 | 2022-04-28 | 中国科学院城市环境研究所 | Sewage treatment device capable of controlling product crystallization granularity and sewage treatment method |
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CN101817581A (en) * | 2010-04-08 | 2010-09-01 | 同济大学 | Integrated nitrogen and phosphorus recovery device in struvite method |
CN201971689U (en) * | 2011-01-18 | 2011-09-14 | 清华大学 | Device for removing and recovering heavy metal by crystallization |
CN106830034A (en) * | 2017-02-09 | 2017-06-13 | 武汉工程大学 | A kind of utilization fluoride waste prepares the method and device of sand like synthetic cryolite |
CN207169666U (en) * | 2017-08-08 | 2018-04-03 | 刘晓吉 | A kind of device for generating unstable calcium carbonate mineral phase |
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2017
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US20010033820A1 (en) * | 2000-03-06 | 2001-10-25 | Isaac Yaniv | Precipitated aragonite and a process for producing it |
CN101817581A (en) * | 2010-04-08 | 2010-09-01 | 同济大学 | Integrated nitrogen and phosphorus recovery device in struvite method |
CN201971689U (en) * | 2011-01-18 | 2011-09-14 | 清华大学 | Device for removing and recovering heavy metal by crystallization |
CN106830034A (en) * | 2017-02-09 | 2017-06-13 | 武汉工程大学 | A kind of utilization fluoride waste prepares the method and device of sand like synthetic cryolite |
CN207169666U (en) * | 2017-08-08 | 2018-04-03 | 刘晓吉 | A kind of device for generating unstable calcium carbonate mineral phase |
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Publication number | Priority date | Publication date | Assignee | Title |
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WO2022083376A1 (en) * | 2020-10-23 | 2022-04-28 | 中国科学院城市环境研究所 | Sewage treatment device capable of controlling product crystallization granularity and sewage treatment method |
US11629077B2 (en) | 2020-10-23 | 2023-04-18 | Institute Of Urban Environment, Chinese Academy Of Sciences | Sewage treatment device capable of controlling product crystallization granularity and sewage treatment method |
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