CN109179471A - A kind of preparation method with resistance to settling precipitated calcium carbonate - Google Patents
A kind of preparation method with resistance to settling precipitated calcium carbonate Download PDFInfo
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- CN109179471A CN109179471A CN201811139372.7A CN201811139372A CN109179471A CN 109179471 A CN109179471 A CN 109179471A CN 201811139372 A CN201811139372 A CN 201811139372A CN 109179471 A CN109179471 A CN 109179471A
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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
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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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
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The present invention relates to precipitated calcium carbonate technical fields, specifically disclose a kind of preparation method with resistance to settling precipitated calcium carbonate.The preparation method comprises the following steps: calcium oxide being reacted to obtain Ca (OH) with water2Slurry;By Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, and polycarboxylic acid salt's dispersing agent is added in carbonisation and is once coated, and stops carbonization when reaction system pH is 6.5-7.5, obtains clinker slurry;It is 18-22 ' Be that clinker slurry, which is concentrated into Baume degrees, and polycarboxylic acid salt's dispersing agent is added again into the clinker slurry after concentration, takes turbine agitator to carry out secondary cladding, obtains slurry;The material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.The precipitated calcium carbonate that the present invention obtains is fusiform crystal form, and partial size reaches 1.4 μm, and monodisperse rate reaches 56%, and sedimentation volumn ratio reaches 70% or more.
Description
Technical field
The present invention relates to precipitated calcium carbonate technical field more particularly to a kind of preparations with resistance to settling precipitated calcium carbonate
Method.
Background technique
Precipitated calcium carbonate is usually to obtain being purification calcium carbonate by calcining, emulsification, carbonating by lime stone.Due to passing through
There are three decomposition of limestone, lime emulsifying, carbonating phase transition process, the purity of product, density, view specific volume, activity, absorption
The indexs such as property, index of refraction, whiteness, impurity content have a very big difference compared with lime stone (calcium carbonate), apparent density especially
Very little, so being precipitated calcium carbonate.It is the important filler in the fields such as plastics, rubber, papermaking, coating, sealing material, ink or
Additive, the dosage in the whole nation is about 6,000,000 tons at present.
All contain a certain proportion of precipitated calcium carbonate in most of coating, ink, used as white pigments and fillers, it can be with
Part replaces the other materials such as expensive titanium dioxide.Since the true specific gravity of precipitated calcium carbonate is about 2.70 or so, particle is larger,
Agglomeration keeps its settleability big again than more serious.Although using various measures in formulation for coating material and production technology,
Many problems still are brought because of the sedimentation of precipitated calcium carbonate filler in storage and use process, reduce the preservability of coating,
Influence construction and product quality.Currently, mostly using dispersing agent, thickener, antisettling agent or cellulose ether, gas phase two greatly both at home and abroad
The thixotropic agent of silica, bentonite etc lowers its settleability.But for these additives often because expensive, dosage is big, effect
Fruit is undesirable or versatility is not wide and is restricted.
Summary of the invention
For the big problem of the settleability of existing precipitated calcium carbonate, the present invention provides a kind of with resistance to settling lightweight carbonic acid
The preparation method of calcium.
To achieve the above object of the invention, the embodiment of the present invention uses the following technical solution:
A kind of preparation method with resistance to settling precipitated calcium carbonate, the preparation method at least include the following steps:
Step a, it is reacted by calcium oxide with water and Ca (OH) is made2Slurry;
Step b, by the Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carbonized, and in carbonisation
Polycarboxylic acid salt's dispersing agent is added once to be coated, stops carbonization when reaction system pH is 6.5-7.5, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 18-22 ' Be, under agitation, to the clinker after concentration
Polycarboxylic acid salt's dispersing agent is added in slurry again and carries out secondary cladding, obtains slurry;
Step d, the slurry dewatering, drying, crushing, screening are obtained with resistance to settling precipitated calcium carbonate.
Compared with the existing technology, preparation method provided by the invention has the advantage that
(1) precipitated calcium carbonate that the present invention obtains is fusiform crystal form, and partial size reaches 1.4 μm, and monodisperse rate reaches 56%,
Sedimentation volumn ratio reaches 70% or more;
(2) present invention passes through the coating function of polycarboxylic acid salt's dispersing agent, reduces the reunion of fine particle to the maximum extent,
Obtain the activated calcium carbonate powder of high dispersive;
(3) present invention takes coats twice, and when once coating in the carburizing reagent stage, the dispersion dosage of addition is fewer,
Concentration in system is lower, they preferentially coat the relatively large particle of those partial sizes, to newly-generated nucleus and subtle
Grain influences less, they can continue to grow larger, and since larger particles have been wrapped by, new product is not easy to reunite with it, i.e.,
Make have agglomeration, and be easier " soft-agglomerated " of depolymerization, can be broken safely in subsequent crushing process, so
The dispersing agent that carbonation stage is first added, which not only improves, prevents the particle formed earliest from excessively growing up, and does not influence subsequent new formation and produce
The growth of object nucleus, works well;Larger amount of dispersing agent is being added after clinker slurry concentration, and is passing through turbine agitator
Strong stirring can effectively realize cladding and prevent the phenomenon that reuniting again, and it is made to gather around the permanent performance for keeping high dispersive, add
Enter to have after coating and significantly has antisolvent precipitation effect.
Specifically, it is preferable that in step b and step c, total covering amount of polycarboxylic acid salt's dispersing agent are as follows: calcium oxide butt
Quality 0.4-0.8%.
Preferably, in step b, the 30-35% of polycarboxylic acid salt's dispersing agent total amount is once added when cladding.
Preferably, in step c, the 65-70% of polycarboxylic acid salt's dispersing agent total amount is added when secondary cladding.
Preferably, polycarboxylic acid salt's dispersing agent is made into the solution that mass concentration is 10-20%, by polycarboxylate by step b
Class dispersing agent passes through simultaneously with kiln gas to react the venthole in kiln bottom portion and enters reaction kiln.
Preferably, polycarboxylic acid salt's dispersing agent is made into the solution that mass concentration is 10-20%, by polycarboxylate by step c
Class dispersing agent enters reaction kiln in the venthole that nitrogen passes through reaction kiln bottom portion simultaneously.
Dispersing agent as a solution, using the air-flow of kiln gas or nitrogen leads to polycarboxylic acid salt's dispersant solution from bottom
Enter, so that the dispersibility of dispersing agent in the solution is more preferable, and kiln gas enters from bottom so that carburizing reagent progress is more abundant.
Preferably, in step c, using turbine agitator, stirring rate 500-800rpm, mixing time 15-
25min。
With the extension of mixing time, the average grain diameter of calcium carbonate reduces, and monodisperse degree increases, this is because turbine type
The strong stirring of blender is a redisperse and broken process, is generated in those carbonization later periods and concentration process during this
Agglomerated particle " can be smashed ", and monodisperse status can be kept in the presence of dispersants, therefore the average grain diameter of product
It reduces, monodispersity improves.But upon agitation between more than 25min when, mixing time is too long, occurs between calcium carbonate granule
Reunite again, product average grain diameter increases, and monodisperse degree reduces instead, and excessive agitation reduces particle also while crushing
There is " decortication " phenomenon, cause to occur between particle more serious in the covered effect of dispersing agent, the particle that those originals are wrapped by
Reunite.
Preferably, carbonation reaction temperature is 25-30 DEG C in the step b, and kiln gas flow is 14-18L/hLCa (OH)2
Lotion.
Preferably, CO in kiln gas in the step b2Volume content is 25-31%.It is preferred that CO in kiln gas2Volume content is
29-31%.
With CO in kiln gas2The increase of content, CaCO3Partial size is gradually reduced, and monodisperse degree gradually increases, calcium carbonate
Partial size can achieve 1.4 μm or less even hundreds of nanometers, product one pack system settling heights reach 70% or more.Work as CO2Contain
When amount is more than 31%, nucleus is excessive, and nucleus, which is reunited, influences covered effect, and monodisperse rate can decline instead, therefore selects CO2Volume
Content is 25-31%, preferably 29-31%.
Preferably, in step b, mixing speed 300-500rpm.
Preferably, the Ca (OH)2The average grain diameter of slurry is 1.8-2.3 μm.
The average grain diameter of 1.8-2.3 μm of selection, Ca (OH)2The small easy carbonization of partial size forms more nucleus and crystal grain, this
The dispersant-coated that a little crystal grain are added at first forms lesser monodispersed calcium carbonate granule, while short grained calcium carbonate
It is coated by surfactant, the anti-agglomeration energy in subsequent process such as continues to carbonate, be concentrated, be separated by filtration, dry, crush
Power is stronger, and the calcium carbonate granule finally obtained is tiny.If calcium hydroxide particle is bigger in lotion, carbonation is opposite
Slowly, the carbonating rate and between particle is difficult to unanimously, " the vacation carbonating " of " interlayer type " not only easy to form, and carbon
Acidificatoin time is longer, leads to secondary agglomeration between product, and particle size is inconsistent, and causes the uneven even appearance packet of cladding naked
Phenomenon.
Preferably, the Ca (OH)2The mass concentration of slurry is 10-14%.
Preferably, calcium oxide and 55-65 DEG C of water are subjected to digestion reaction in the step a, it is close after digestion reaction
Envelope, and 22-26h is aged at 75-85 DEG C, it crosses 200-300 mesh and obtains Ca (OH)2Slurry.
During digestion reaction, there are the reactions of following two situation: one is calcium oxide particle surface hydrations to generate hydrogen
Calcium oxide, calcium hydroxide are detached from calcium oxide particle surface and are dissolved into water, when meeting or exceeding solubility, and form new hydrogen
Calcium oxide nucleus, nucleus gradually long great achievement calcium hydroxide particle again;Another situation is the hydroxide that calcium oxide surface hydration is formed
Calcium causes calcium oxide surface capped without departing from calcium oxide surface, but hydrone can pass through product layer and enter inside particle
It is reacted with calcium oxide, but this process is slower.Therefore above-mentioned reaction condition is selected to obtain average grain diameter as 1.8-2.3 μm
Calcium hydroxide.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the SEM photograph for the calcium carbonate that test example 1 of the present invention provides;
Fig. 2 is the XRD photo for the calcium carbonate that test example 1 of the present invention provides;
Fig. 3 is the SEM photograph for the calcium carbonate that test example 2 of the present invention provides;
Fig. 4 is the SEM photograph for the calcium carbonate that test example 3 of the present invention provides;
Wherein, label a- embodiment 1 in Fig. 1, label b- embodiment 2, label c- comparative example 1, label d- comparative example 2;
Label a- embodiment 3 in Fig. 3, label b- embodiment 4, label c- embodiment 5, label d- embodiment 6;
Label a- comparative example 7 in Fig. 4, label b- embodiment 7, label c- embodiment 1, label d- embodiment 8.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 25 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and by 16.5g polycarboxylic acid salt's dispersing agent in carbonisation
Add water to be configured to the solution that concentration is 10wt%, solution is entered into reaction kiln progress by reacting the venthole in kiln bottom portion with kiln gas
Primary cladding, stops carbonization when reaction system pH is 7, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 15wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, turbine agitator is taken to carry out two with the speed stirring 20min of 800rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Embodiment 2
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 65 DEG C of the water of 60Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged 26h at 75 DEG C, crosses 200 meshes and obtains the Ca (OH) that average grain diameter is 2.25 μm2Slurry, and adjust concentration and be
14wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 28 DEG C
Throughput is 18L/h, and CO in kiln gas2Volume content is 29%, and 16.5g polycarboxylic acid salt dispersion is added in carbonisation
Agent adds water to be configured to the solution that concentration is 15wt%, solution and kiln gas are passed through react kiln bottom portion venthole enter react kiln into
The primary cladding of row, stops carbonization when reaction system pH is 7, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 20wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, turbine agitator is taken to carry out two with the speed stirring 20min of 800rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Comparative example 1
This comparative example provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
It step a, is Ca (OH) that 2.42 μm of concentration are 12wt% by average grain diameter2Slurry is transported in reaction kiln, is passed through
Kiln gas carries out carburizing reagent under the conditions of 25 DEG C, and kiln gas flow is 16L/h, and CO in kiln gas2Volume content is 28%, and in carbon
Add water to be configured to the solution that concentration is 20wt% 16.5g polycarboxylic acid salt's dispersing agent during change, solution and kiln gas are passed through
The venthole in reaction kiln bottom portion enters reaction kiln and is once coated, and stops carbonization when reaction system pH is 7, obtains clinker
Slurry;
Step b, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 10wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, turbine agitator is taken to carry out two with the speed stirring 20min of 800rpm
Secondary cladding, obtains slurry;
Step c, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Comparative example 2
This comparative example provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
It step a, is Ca (OH) that 2.56 μm of concentration are 12wt% by average grain diameter2Slurry is transported in reaction kiln, is passed through
Kiln gas carries out carburizing reagent under the conditions of 25 DEG C, and kiln gas flow is 16L/h, and CO in kiln gas2Volume content is 28%, and in carbon
16.5g polycarboxylic acid salt dispersing agent is added during changing once to be coated, stops carbonization when reaction system pH is 7, obtains
Clinker slurry;
Step b, clinker slurry is concentrated into Baume degrees is 20.Polycarboxylate is added into the clinker slurry after concentration in Be again
Class dispersing agent 38.5g takes turbine agitator to carry out secondary cladding with the speed stirring 20min of 800rpm, obtains slurry;
Step c, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Test example 1
The characteristic with resistance to settling precipitated calcium carbonate that embodiment provides in order to better illustrate the present invention, below will be real
It applies the calcium carbonate that example 1,2 is prepared with comparative example 1,2 to be tested for the property, test result is as shown in table 1.
1 test result of table
, it is apparent that the calcium carbonate monodisperse rate of preparation of the embodiment of the present invention is high from table 1, and partial size is small, partial size
Reach 1.7 μm, sedimentation volumn ratio reaches 70% or more.
Calcium carbonate prepared by embodiment 1,2 and comparative example 1,2 is scanned electron microscope analysis, scanning electron microscope (SEM) simultaneously
Photo is as shown in Figure 1.From figure 1 it appears that the calcium carbonate granule of comparative example 1 and comparative example 2 is reunited seriously.
The calcium carbonate simultaneously prepared by embodiment 1 carries out XRD analysis, and XRD spectrum is as shown in Figure 2.It can from Fig. 2
Out, precipitated calcium carbonate crystal property prepared by the present invention is good, and no obvious miscellaneous peak occurs, and shows calcium carbonate product stability very
It is good, purity is high.
Embodiment 3
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 55 DEG C of the water of 40Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged 22h at 85 DEG C, crosses 300 meshes and obtains the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 25%, and disperses 15.75g polycarboxylic acid salt in carbonisation
Agent adds water to be configured to the solution that concentration is 10wt%, solution and kiln gas are passed through react kiln bottom portion venthole enter react kiln into
The primary cladding of row, stops carbonization when reaction system pH is 7.5, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 29.25g dense
The solution that degree is 15wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Embodiment 4
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 26.2%, and by 15.75g polycarboxylic acid salt point in carbonisation
Powder adds water to be configured to the solution that concentration is 20wt%, and solution is entered reaction kiln by reacting the venthole in kiln bottom portion with kiln gas
It is once coated, stops carbonization when reaction system pH is 7.5, obtain clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 29.25g dense
The solution that degree is 15wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Embodiment 5
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28.0%, and by 15.75g polycarboxylic acid salt point in carbonisation
Powder adds water to be configured to the solution that concentration is 10wt%, and solution is entered reaction kiln by reacting the venthole in kiln bottom portion with kiln gas
It is once coated, stops carbonization when reaction system pH is 7.5, obtain clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 29.25g dense
The solution that degree is 15wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Embodiment 6
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 30%, and disperses 15.75g polycarboxylic acid salt in carbonisation
Agent adds water to be configured to the solution that concentration is 15wt%, solution and kiln gas are passed through react kiln bottom portion venthole enter react kiln into
The primary cladding of row, stops carbonization when reaction system pH is 7.5, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 29.25g dense
The solution that degree is 20wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Comparative example 3
The embodiment of the present invention provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 31.3%, and by 15.75g polycarboxylic acid salt point in carbonisation
Powder adds water to be configured to the solution that concentration is 10wt%, and solution is entered reaction kiln by reacting the venthole in kiln bottom portion with kiln gas
It is once coated, stops carbonization when reaction system pH is 7.5, obtain clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 29.25g dense
The solution that degree is 15wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Test example 2
The characteristic with resistance to settling precipitated calcium carbonate that embodiment provides in order to better illustrate the present invention, below will be real
It applies the calcium carbonate that a 3-6 is prepared with comparative example 3 to be tested for the property, test result is as shown in table 2.
2 test result of table
, it is apparent that the calcium carbonate monodisperse rate of preparation of the embodiment of the present invention is high from table 2, and partial size is small, partial size
Reach 1.6 μm, sedimentation volumn ratio reaches 70% or more.CO in kiln gas in comparative example 32Volume content is high, although partial size is small,
Monodisperse rate is low, and sedimentation volumn is than low.
The embodiment 3-6 calcium carbonate prepared is scanned electron microscope analysis, scanning electron microscope (SEM) photo such as Fig. 3 institute simultaneously
Show.From figure 3, it can be seen that calcium carbonate dispersion prepared by the present invention is relatively uniform, and particle diameter distribution is uniform.
Comparative example 4
The embodiment of the present invention provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and by 7.84g polycarboxylic acid salt's dispersing agent in carbonisation
Add water to be configured to the solution that concentration is 10wt%, solution is entered into reaction kiln progress by reacting the venthole in kiln bottom portion with kiln gas
Primary cladding, stops carbonization when reaction system pH is 7.5, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 14.56g dense
The solution that degree is 15wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Comparative example 5
The embodiment of the present invention provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 30 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and disperses 11.76g polycarboxylic acid salt in carbonisation
Agent adds water to be configured to the solution that concentration is 10wt%, solution and kiln gas are passed through react kiln bottom portion venthole enter react kiln into
The primary cladding of row, stops carbonization when reaction system pH is 7.5, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 22 ' Be, adds water to be made into polycarboxylic acid salt's dispersing agent 21.84g dense
The solution that degree is 15wt% enters reaction kiln by reacting the venthole in kiln bottom portion with nitrogen, again into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added and carries out secondary cladding, turbine agitator is taken to carry out with the speed stirring 20min of 600rpm
Secondary cladding, obtains slurry;
Step d, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Test example 3
The characteristic with resistance to settling precipitated calcium carbonate that embodiment provides in order to better illustrate the present invention, below will be real
The calcium carbonate for applying example 1, embodiment 5 and comparative example 4-5 preparation is tested for the property, and test result is as shown in table 3.
3 test result of table
, it is apparent that the calcium carbonate monodisperse rate of the preparation of the embodiment of the present invention 1,5 is high from table 3, and partial size is small, grain
Diameter reaches 1.7 μm, and sedimentation volumn ratio reaches 70% or more.Dispersant additional amount is few in comparative example 4-5, calcium carbonate partial size
Greatly, monodisperse rate is low, and sedimentation volumn is than low.
Embodiment 7
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 25 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and by 16.5g polycarboxylic acid salt's dispersing agent in carbonisation
Add water to be configured to the solution that concentration is 10wt%, solution is entered into reaction kiln progress by reacting the venthole in kiln bottom portion with kiln gas
Primary cladding, stops carbonization when reaction system pH is 7, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 15wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, turbine agitator is taken to carry out two with the speed stirring 15min of 800rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Embodiment 8
The embodiment of the present invention provides a kind of preparation method with resistance to settling precipitated calcium carbonate, and the preparation method includes
Following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 25 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and by 16.5g polycarboxylic acid salt's dispersing agent in carbonisation
Add water to be configured to the solution that concentration is 20wt%, solution is entered into reaction kiln progress by reacting the venthole in kiln bottom portion with kiln gas
Primary cladding, stops carbonization when reaction system pH is 7, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 10wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, turbine agitator is taken to carry out two with the speed stirring 25min of 800rpm
Secondary cladding, obtains slurry;
Step d, the material is obtained dehydration, drying, crushing, screening with resistance to settling precipitated calcium carbonate.
Comparative example 6
The embodiment of the present invention provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 25 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and by 16.5g polycarboxylic acid salt's dispersing agent in carbonisation
Add water to be configured to the solution that concentration is 15wt%, solution is entered into reaction kiln progress by reacting the venthole in kiln bottom portion with kiln gas
Primary cladding, stops carbonization when reaction system pH is 7, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 20wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, takes turbine agitator to carry out with the speed stirring 5min of 800rpm secondary
Cladding, obtains slurry;
Step d, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Comparative example 7
The embodiment of the present invention provides a kind of preparation method of precipitated calcium carbonate, and the preparation method comprises the following steps:
Step a, 10Kg calcium oxide and 60 DEG C of the water of 50Kg are subjected to digestion reaction, are sealed after digestion reaction, and
It is aged at 80 DEG C for 24 hours, crosses 300 meshes and obtain the Ca (OH) that average grain diameter is 1.81 μm2Slurry, and adjust concentration and be
12wt%;
Step b, by Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carried out carburizing reagent, kiln under the conditions of 25 DEG C
Throughput is 16L/h, and CO in kiln gas2Volume content is 28%, and by 16.5g polycarboxylic acid salt's dispersing agent in carbonisation
Add water to be configured to the solution that concentration is 10wt%, solution is entered into reaction kiln progress by reacting the venthole in kiln bottom portion with kiln gas
Primary cladding, stops carbonization when reaction system pH is 7, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 20 ' Be, adds water to be made into concentration polycarboxylic acid salt's dispersing agent 38.5g
Enter reaction kiln by reacting the venthole in kiln bottom portion with nitrogen for the solution of 15wt%, adds again into the clinker slurry after concentration
Enter polycarboxylic acid salt's dispersing agent and carry out secondary cladding, turbine agitator is taken to carry out two with the speed stirring 30min of 800rpm
Secondary cladding, obtains slurry;
Step d, dehydration, drying, crushing, screening are obtained into precipitated calcium carbonate by the material.
Test example 4
The characteristic with resistance to settling precipitated calcium carbonate that embodiment provides in order to better illustrate the present invention, below will be real
The calcium carbonate for applying example 1, embodiment 7-8 and comparative example 6-7 preparation is tested for the property, and test result is as shown in table 4.
4 test result of table
, it is apparent that the calcium carbonate monodisperse rate of the embodiment of the present invention 1, embodiment 7-8 preparation is high from table 4, and
Partial size is small, and partial size reaches 1.7 μm, and sedimentation volumn ratio reaches 70% or more.Although calcium carbonate partial size is small in comparative example 7, monodisperse
Rate is low, and sedimentation volumn is than low.
Calcium carbonate prepared by same embodiment 1, embodiment 7-8 and comparative example 6 is scanned electron microscope analysis, scanning electron microscope
(SEM) photo is as shown in Figure 4.Figure 4, it is seen that calcium carbonate granule prepared by comparative example 6 is reunited seriously.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method with resistance to settling precipitated calcium carbonate, it is characterised in that: the preparation method include at least with
Lower step:
Step a, it is reacted by calcium oxide with water and Ca (OH) is made2Slurry;
Step b, by the Ca (OH)2Slurry is transported in reaction kiln, is passed through kiln gas and is carbonized, and is added in carbonisation
Polycarboxylic acid salt's dispersing agent is once coated, and stops carbonization when reaction system pH is 6.5-7.5, obtains clinker slurry;
Step c, clinker slurry is concentrated into Baume degrees is 18-22 ' Be, under agitation, into the clinker slurry after concentration
Polycarboxylic acid salt's dispersing agent is added again and carries out secondary cladding, obtains slurry;
Step d, the slurry dewatering, drying, crushing, screening are obtained with resistance to settling precipitated calcium carbonate.
2. as described in claim 1 with the preparation method of resistance to settling precipitated calcium carbonate, which is characterized in that step b and step
In rapid c, total covering amount of polycarboxylic acid salt's dispersing agent are as follows: the 0.4-0.8% of the quality of calcium oxide butt.
3. as claimed in claim 2 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: in step b, one
The 30-35% of polycarboxylic acid salt's dispersing agent total amount is added when secondary cladding;And/or
In step c, the 65-70% of polycarboxylic acid salt's dispersing agent total amount is added when secondary cladding.
4. the preparation method as described in any one of claims 1-3 with resistance to settling precipitated calcium carbonate, it is characterised in that: step
Polycarboxylic acid salt's dispersing agent is made into the solution that mass concentration is 10-20% by rapid b, and polycarboxylic acid salt's dispersing agent and kiln gas is same
When by react kiln bottom portion venthole enter reaction kiln;And/or
Step c, by polycarboxylic acid salt's dispersing agent be made into mass concentration be 10-20% solution, by polycarboxylic acid salt's dispersing agent in
The venthole that nitrogen passes through reaction kiln bottom portion simultaneously enters reaction kiln.
5. as described in claim 1 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: in step c, adopt
With turbine agitator, stirring rate 500-800rpm, mixing time 15-25min.
6. as described in claim 1 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: in step b, instead
Answering the temperature in kiln is 25-30 DEG C, and kiln gas flow is 14-18L/hLCa (OH)2Lotion.
7. as claimed in claim 6 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: in step b, kiln
CO in gas2Volume content is 25-31%.
8. as described in claim 1 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: in step b, stir
Mixing speed is 300-500rpm.
9. as described in claim 1 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: the Ca (OH)2
The average grain diameter of slurry is 1.8-2.3 μm;And/or
The Ca (OH)2The mass concentration of slurry is 10-14%.
10. as claimed in claim 9 with the preparation method of resistance to settling precipitated calcium carbonate, it is characterised in that: the step a
It is middle to react calcium oxide with 55-65 DEG C of water, and the mass ratio of calcium oxide and water is 1:4-6, it is close after digestion reaction
Envelope, and 22-26h is aged at 75-85 DEG C, it crosses 200-300 mesh and obtains Ca (OH)2Slurry.
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CN110563015A (en) * | 2019-09-27 | 2019-12-13 | 河北立信化工有限公司 | preparation method of light calcium carbonate for food |
CN112209417A (en) * | 2019-08-28 | 2021-01-12 | 浙江天石纳米科技股份有限公司 | Preparation method of light calcium carbonate powder for papermaking coating |
CN113800787A (en) * | 2021-09-30 | 2021-12-17 | 清华大学 | Preparation method of high-activity calcium hydroxide |
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CN105883882A (en) * | 2016-04-19 | 2016-08-24 | 广西大学 | Aqueous slurry of nano calcium carbonate as well as preparation method and application thereof |
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CN112209417B (en) * | 2019-08-28 | 2022-04-19 | 浙江天石纳米科技股份有限公司 | Preparation method of light calcium carbonate powder for papermaking coating |
CN110563015A (en) * | 2019-09-27 | 2019-12-13 | 河北立信化工有限公司 | preparation method of light calcium carbonate for food |
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CN113800787A (en) * | 2021-09-30 | 2021-12-17 | 清华大学 | Preparation method of high-activity calcium hydroxide |
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