CN109809457A - Regular spherical calcium carbonate and its preparation process - Google Patents
Regular spherical calcium carbonate and its preparation process Download PDFInfo
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Abstract
The invention discloses a kind of regular spherical calcium carbonate and its preparation processes, preparation method are as follows: refine and compound crystal control agent is added in the calcium hydroxide slurry that modulates and stir evenly, it adjusts to be passed through carbon dioxide gas after controlling initial carburizing temperature and be carbonized and stop to pH lower than 7, obtain regular spherical calcium carbonate through dehydration, drying, crushing, screening.The regular spherical calcium carbonate of gained of the invention does not need to be surface-treated, good dispersion, simple process, carbonization time is short, and production cost is low, is adjustably controlled in regular spherical calcium carbonate partial size 300-900 nanometer range obtained, there is good processing fluidity as downstream product filler, mould material as hollow-particle has compared with high added value, is not only suitable for food, medicine, cosmetics light industry, is also applied for plastics, rubber, coating, ink, papermaking, new material, chemical industry.
Description
Technical field
The invention belongs to inorganic non-metallic material calcium carbonate powder preparation technical fields, and in particular to calcium hydroxide prepares ball
Aragonite crystal form crystal morphology is the calcium carbonate and its technique of regular spherical shape.
Background technique
The calcium carbonate product of different shape, application field and function difference.Its function quality, depends primarily on calcium carbonate
The parameters such as chemical composition, morphological feature, the granule size of product, most important of which is that the crystalline form and granularity of calcium carbonate particle point
Cloth.Currently, special crystal form nano calcium carbonate product is made, so that it is higher to assign product by artificially controlling calcium carbonate crystal
Application performance and added value be still calcium carbonate industry exploitation hot spot.In the nano-calcium carbonate calcium product of various special crystalline forms
In, spherical calcium carbonate structure compared with it is simple, heap lower small volume, oil factor and good opacity (opacity) and
To the absorbent properties of ink, thus it is mainly used for the industries such as papermaking.In addition, spherical calcium carbonate has good flatness, flowing
Property the features such as, and be widely used in the industries such as rubber, coating and high-grade ink, spherical calcium carbonate can be added to lubricating oil
In, greatly improve its greasy property, it can also be used to the production of electronic ceramics, biological medicine carrier etc..
Recent study discovery, hollow-particle is a kind of new material with special cavity structure, since its is special
Geometry and high inner space, low-density, large specific surface area, stability is good and the physics such as surface penetration ability is strong
Chemical property is concerned in field of scientific study, is had a good application prospect in fields such as medicine, catalysis, materials,
Template is to prepare the most simple and effective method of hollow-particle, and common template has polymer, inorganic oxide, metal simple-substance etc.
The various soft templates such as various hard templates and emulsion droplets, bubble, micella.Different templates has different advantage and disadvantage, and calcium carbonate is former
Expect cheap and easy to get, preparation method is simple, easily removes, and therefore, spherical calcium carbonate is considered as a kind of template material of great potential
Material.
The preparation research of domestic spherical calcium carbonate has had made some progress, and prepares CaCO3The common method of particle is main
It is double decomposition and carbonizatin method.Double decomposition the advantage is that preparation method is simple and easily controllable CaCO3The crystal form of particle, shape
Looks, particle size, but the disadvantage is that production cost is higher, production efficiency is lower, is not able to achieve scale industrial production at present.Carbonization
Method is preparation specific morphology CaCO in current industrial production3The main method of product.According to the difference of the carbonisation way of contact
Be divided into intermittent bubbling carbonizing method and batch type carbonizatin method, the former it is easy to operate but consume energy higher and size uniformity compared with
Difference, although the latter's operation is relative complex, product cut size uniformity is higher with respect to the former, and high-gravity carbonation method has production cost
Low, the features such as particle diameter distribution is uniform, carbonization time is short, but equipment investment is larger.The product of spherical calcium carbonate is basically used at present
In the industries such as papermaking, rubber, coating and high-grade ink, price is at per ton thousand yuan or so, can not conduct and since partial size is larger
Prepare the mould material of hollow-particle.As the spherical carbonic acid of mould material submicron order (500-800nm) for preparing hollow-particle
Calcium particle, due to easily removing, price has reached 400 yuan/kg at present, and this kind of high added value refines the production of calcium carbonate product
Industry is nearly at the state of blank, and therefore, exploitation carbonizatin method prepares submicron order spherical calcium carbonate as template, by changing
Into carbonization technique, the spherical calcium carbonate product that performance is stable, meets different demands is prepared, to meet ever-increasing market need
It wants, there is positive meaning to the added value for improving calcium carbonate product.
Summary of the invention
The present invention provides a kind of regular spherical calcium carbonate and its preparation process, for the mould material sub-micro as hollow-particle
Meter level (500-800nm) spherical calcium carbonate particle certainly solves the technical issues of preparation process.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of regular spherical calcium carbonate belongs to calcium hydroxide carbonizatin method and prepares spherical calcium carbonate, it modulates hydrogen-oxygen first
Change calcium slurries, compound crystal control agent is then added in calcium hydride slurries and is thoroughly mixed, adjusts initial carburizing temperature
After be passed through carbon dioxide gas carbonization, obtain calcium carbonate serosity through dehydration, drying, crushing, sieve up to regular spherical calcium carbonate,
Preparation method includes the following steps:
1) lime slaking, refine and be modulated into calcium hydroxide slurry;
2) compound crystal control agent is added in the calcium hydroxide slurry modulated;
3) calcium hydroxide slurry is passed through carbon dioxide gas progress carburizing reagent after adjusting initial carburizing temperature, and pH is lower than 7
When determine reaction terminate, stopping be passed through carbon dioxide gas;
4) regular spherical calcium carbonate is obtained through dehydration, drying, crushing, screening after carburizing reagent terminates.
Further, regular spherical calcium carbonate crystal form is the mixing crystal form of vaterite crystal form and calcite crystal form, crystal shape
Looks are regular spherical shape, and mixing vaterite crystal form in crystal form is high-content main composition part, and calcite crystal form is that low content is secondary
Composition part, 300-900 nanometers of regular spherical calcium carbonate partial size, uniform particle sizes, particle size are controllable.
Further, regular spherical calcium carbonate can be the complete spherical calcium carbonate of uniformly rule and be also possible to because of reaction
Condition and process parameter control is not in place forms the uneven or regular spherical calcium carbonate containing partial crushing ball calcium.
Further, in step 1) lime digestion, can directly be digested with water, be also possible to water with methanol or ethyl alcohol
It is digested after mixing according to a certain percentage, is also possible to be digested after water, methanol, ethyl alcohol are mixed in a certain ratio, it can also
To be that the clear liquid that regular ball calcium carbonate preparation dehydration obtains is used to digest;Hydrogen in calcium hydroxide slurry is modulated after lime slaking purification
Calcium oxide content 4-16%, the mixture content of methanol or ethyl alcohol or the two is calcium hydroxide slurry in calcium hydroxide slurry
The 25-80% of quality;For reduce digestion heat release cause methanol, ethyl alcohol volatilization loss, after preferably being digested and refined with water by than
Methanol or ethyl alcohol is added in example or the mixed liquor of the two adjusts required concentration ratio.
Further, compound crystal control agent, compound crystalline form is added in step 2) in the calcium hydroxide slurry modulated
Controlling agent is divided into two components, and a component is calcium carbonate crystalline form directed agents, another component is shape and appearance of calcium carbonate controlling agent;It is brilliant
Shape directed agents are as by the flocculating agent of vaterite crystal condensation balling-up, and pattern controlling agent is as spherical calcium carbonate Morphological control agent tune
Section calcium carbonate granule pattern is intended to complete spherical;The crystalline form directed agents be by heat aging soluble starch slurries,
The compound of one or more of polyvinylpyrrolidone, polyvinylbenzenesulfonic acid sodium, polyethyleneimine;The crystalline form regulation
Agent is one of Sodium Polyacrylate, polysorbate, poly (sodium aspartate), sorbitan fatty acid ester or a variety of compounds;
The amount of the crystalline form directed agents of addition is the 0.5-8% of calcium hydroxide solid content, and the amount of the crystal control agent of addition is hydroxide
The 0.6-10% of calcium solid content.
Further, comprehensive preparation cost and preparation efficiency crystalline form directed agents additional amount 1-6% are proper, are surpassed
Preparation cost and efficiency can be influenced but still fall within patent claims range by crossing range above.
Further, in step 3) in band stirring carbonizing plant, compound crystal control agent stirring is added in calcium hydroxide slurry
Uniformly, 3-40 DEG C of initial carburizing temperature is adjusted, is passed through carbon dioxide containing gas concentration 20-100%'s in the case where opening stirring
Gas progress carburizing reagent, which is passed through gas lower than 7 stoppings to pH, to be terminated to be carbonized.
Further, the middle stopping of step 3), which is passed through gas, terminates stopping stirring waiting slurries formation gel after carbonization, is formed
Waiting gel to dissolve or suitably heat after gel accelerates gel to dissolve.Slurries pH belonged to carbonization lower than 7 and forms calcium carbonate
Calcium bicarbonate is had during sol-gel and is decomposed to form calcium carbonate after stopping being passed through gas with calcium bicarbonate mixed serum
It releases to form bubble with carbon dioxide gas.
Further, calcium carbonate filter cake, filter cake warp can be obtained after gel dissolves by filtering or centrifugal dehydration
Cross dry, crushing, screening obtains regular spherical calcium carbonate.
Further, the filtrate that calcium carbonate serosity is dehydrated in step 4) can return after precipitating, filtering, clarifying treatment
Receipts recycle.
The invention has the following advantages:
1. lime is reacted with water is effectively transformed into white lime calcium hydride slurries for quick lime, using water as solvent dissolved oxygen
Change the cost that calcium greatly reduces modulation calcium hydroxide slurry in lime slaking and calcium hydroxide slurry screening impurity removal and purification process.
2. refining the mixture that methanol or ethyl alcohol or the two are added in calcium hydroxide slurry, it can effectively accelerate dioxy
Change carbon dissolution in calcium hydroxide slurry, effectively facilitate the progress of carbonation reaction, promotes the formation of vaterite crystal form calcium carbonate.
3. vaterite crystal form calcium carbonate has relatively good stability in methanol, ethanol solution, vaterite is not convert to
In the case where calcite crystal form, it is more advantageous to form regular spherical calcium carbonate under the action of compound crystal control agent.
4. present invention process design is simple, it is easy to implement volume production, has that process costs are low, the carburizing reagent time is short, easy
The characteristics of operation control, using regular spherical calcium carbonate uniform particle sizes product with stable quality produced by the invention.
5. regular spherical calcium carbonate size tunable produced by the present invention has good processing stream as downstream product filler
Dynamic property, the mould material as hollow-particle have compared with high added value, are not only suitable for food, medicine, cosmetics light industry,
Suitable for plastics, rubber, coating, ink, papermaking, new material, chemical industry.
Detailed description of the invention
Fig. 1 is that regular spherical calcium carbonate product prepared by embodiment 1 tests and analyzes figure through scanning electron microscope;
Fig. 2 is that regular spherical calcium carbonate product prepared by embodiment 2 tests and analyzes figure through scanning electron microscope.
Specific embodiment
It to facilitate a better understanding of the present invention, is illustrated by following embodiment, these embodiments belong to of the invention
Protection scope, but do not limit the scope of the invention.
Embodiment 1
A kind of regular spherical calcium carbonate belongs to calcium hydroxide carbonizatin method and prepares spherical calcium carbonate, preparation method include with
Lower step:
(1) lime slaking and calcium hydroxide slurry modulation: the ratio of mass ratio 1:4 is sufficiently stirred and disappears at room temperature for lime and water
Change and suitably ageing cooling, will obtain that lime white is filtered to remove bulky grain insoluble substance and impurity obtains refining calcium hydroxide slurry,
Methanol is added after calcium hydroxide slurry is cooled to room temperature and modulates calcium hydroxide content 10%, methanol additional amount is the hydrogen modulated
The 50% of calcium oxide grind slurries quality;
(2) chemical additives are added: being squeezed into the calcium hydroxide slurry debugged with the intermittent of agitating device with pump
Bubbling carbonization tower, it is the heat aging soluble starch solution of calcium hydroxide quality 3.8% as crystalline form directed agents that quality, which is added,
It is 3.0% polyoxyethylene of calcium hydroxide quality (20) sorbitanmonolaureate as pattern controlling agent, stirring that quality, which is added,
Uniformly;
(3) be carbonized: adjusting the initial carburizing temperature of calcium hydroxide slurry is 10 DEG C, opens air valve, is passed through containing pure titanium dioxide
Carbon gas carries out carburizing reagent, and air valve is closed in carbonization to reaction solution pH when being 6.9, stop reaction, stops stirring;
(4) it dehydrates: to calcium carbonate serosity gel and after dissolving, after the processes such as dehydration, drying, crushing, screening
Obtain the regular spherical calcium carbonate that average grain diameter is 758 nanometers.
Embodiment 2
A kind of regular spherical calcium carbonate belongs to calcium hydroxide solution carbonizatin method and prepares spherical calcium carbonate, preparation method packet
Include following steps:
(1) lime slaking and calcium hydroxide slurry modulation: the ratio of mass ratio 1:3 is sufficiently stirred and disappears at room temperature for lime and water
Change and suitably ageing cooling, will obtain that lime white is filtered to remove bulky grain insoluble substance and impurity obtains refining calcium hydroxide slurry,
Methanol is added after calcium hydroxide slurry is cooled to room temperature and modulates calcium hydroxide content 12%, methanol additional amount is the hydrogen modulated
The 60% of calcium oxide grind slurries quality;
(2) chemical additives are added: being squeezed into the calcium hydroxide slurry debugged with the intermittent of agitating device with pump
Bubbling carbonization tower, it is 2.6% polyethyleneimine of calcium hydroxide quality as crystalline form directed agents that quality, which is added, and addition quality is hydrogen-oxygen
Change calcareous 3.8% poly (sodium aspartate) of amount as pattern controlling agent, stirs evenly;
(3) be carbonized: adjusting the initial carburizing temperature of calcium hydroxide slurry is 20 DEG C, opens air valve, is passed through containing CO2Volumetric concentration
Carburizing reagent is carried out for 33% gas, air valve is closed in carbonization to reaction solution pH when being 6.8, stop reaction, stops stirring;
(4) it dehydrates: to calcium carbonate serosity gel and after dissolving, after the processes such as dehydration, drying, crushing, screening
Obtain the regular spherical calcium carbonate that average grain diameter is 646 nanometers.
Embodiment 3
A kind of regular spherical calcium carbonate belongs to calcium hydroxide solution carbonizatin method and prepares spherical calcium carbonate, preparation method packet
Include following steps:
(1) lime slaking and calcium hydroxide slurry modulation: the ratio of mass ratio 1:3 is sufficiently stirred and disappears at room temperature for lime and water
Change and suitably ageing cooling, will obtain that lime white is filtered to remove bulky grain insoluble substance and impurity obtains refining calcium hydroxide slurry.
Second alcohol and water is added after calcium hydroxide slurry is cooled to room temperature and modulates calcium hydroxide content 10%, amount of alcohol added is to modulate
Calcium hydroxide slurry quality 60%;
(2) chemical additives are added: being squeezed into the calcium hydroxide slurry debugged with the intermittent of agitating device with pump
Bubbling carbonization tower, it is 2.8% polyvinylpyrrolidone of calcium hydroxide quality as crystal control agent that quality, which is added, and quality, which is added, is
2.8% sorbitan monostearate of calcium hydroxide quality is stirred evenly as pattern controlling agent;
(3) be carbonized: adjusting the initial carburizing temperature of calcium hydroxide slurry is 5 DEG C, opens air valve, is passed through containing CO2Volumetric concentration
Carburizing reagent is carried out for 36% gas, air valve is closed in carbonization to reaction solution pH when being 6.9, stop reaction, stops stirring;
(4) it dehydrates: to calcium carbonate serosity gel and after dissolving, after the processes such as dehydration, drying, crushing, screening
Obtain the regular spherical calcium carbonate that average grain diameter is 710 nanometers.
Embodiment 4
A kind of regular spherical calcium carbonate belongs to calcium hydroxide solution carbonizatin method and prepares spherical calcium carbonate, preparation method packet
Include following steps:
(1) lime slaking and calcium hydroxide slurry modulation: lime and prepare regular spherical calcium carbonate dehydration filtrate (methanol and
The mixing of water) digestion is sufficiently stirred in the ratio of mass ratio 1:8 at room temperature and suitably ageing cools down, and it will obtain lime white and be filtered to remove
Bulky grain insoluble substance and impurity obtain purification calcium hydroxide slurry;Methanol modulation is added after calcium hydroxide slurry is cooled to room temperature
Calcium hydroxide content 8%, methanol additional amount are the 60% of the calcium hydroxide slurry quality modulated;
(2) chemical additives are added: being squeezed into the calcium hydroxide slurry debugged with the intermittent of agitating device with pump
Bubbling carbonization tower, it is 3.8% polyvinylbenzenesulfonic acid sodium of calcium hydroxide quality as crystalline form directed agents that quality, which is added, and quality, which is added, is
3.2% poly (sodium aspartate) of calcium hydroxide quality is stirred evenly as pattern controlling agent;
(3) be carbonized: adjusting the initial carburizing temperature of calcium hydroxide slurry is 15 DEG C, opens air valve, is passed through containing CO2Volumetric concentration
Carburizing reagent is carried out for 40% gas, air valve is closed in carbonization to reaction solution pH when being 6.9, stop reaction, stops stirring;
(4) it dehydrates: to calcium carbonate serosity gel and after dissolving, after the processes such as dehydration, drying, crushing, screening
Obtain the regular spherical calcium carbonate that average grain diameter is 532 nanometers.
Embodiment 5
A kind of regular spherical calcium carbonate belongs to calcium hydroxide solution carbonizatin method and prepares spherical calcium carbonate, preparation method packet
Include following steps:
(1) lime slaking and calcium hydroxide slurry modulation: lime and prepare regular spherical calcium carbonate dehydration filtrate (ethyl alcohol and
The mixing of water) digestion is sufficiently stirred in the ratio of mass ratio 1:7 at room temperature and suitably ageing cools down, and it will obtain lime white and be filtered to remove
Bulky grain insoluble substance and impurity obtain purification calcium hydroxide slurry, and ethyl alcohol modulation is added after calcium hydroxide slurry is cooled to room temperature
Calcium hydroxide content 9%, amount of alcohol added are the 50% of the calcium hydroxide slurry quality modulated;
(2) chemical additives are added: being squeezed into the calcium hydroxide slurry debugged with the intermittent of agitating device with pump
Bubbling carbonization tower, it is the heat aging soluble starch solution of calcium hydroxide quality 4.2% as crystal control agent that quality, which is added,
It is 3.5% Sodium Polyacrylate of calcium hydroxide quality as pattern controlling agent that quality, which is added, is stirred evenly;
(3) be carbonized: adjusting the initial carburizing temperature of calcium hydroxide slurry is 16 DEG C, opens air valve, is passed through containing CO2Volumetric concentration
Carburizing reagent is carried out for 36% gas, air valve is closed in carbonization to reaction solution pH when being 6.9, stop reaction, stops stirring;
(4) it dehydrates: to calcium carbonate serosity gel and after dissolving, after the processes such as dehydration, drying, crushing, screening
Obtain the regular spherical calcium carbonate that average grain diameter is 682 nanometers.
Embodiment 6
A kind of regular spherical calcium carbonate belongs to calcium hydroxide solution carbonizatin method and prepares spherical calcium carbonate, preparation method packet
Include following steps:
(1) lime slaking and calcium hydroxide slurry modulation: the ratio of mass ratio 1:4 is sufficiently stirred and disappears at room temperature for lime and water
Change and suitably ageing cooling, will obtain that lime white is filtered to remove bulky grain insoluble substance and impurity obtains refining calcium hydroxide slurry,
Methanol and ethyl alcohol mass ratio are added after calcium hydroxide slurry is cooled to room temperature and modulates calcium hydroxide content for the solution of 1:1
10%, methanol and ethyl alcohol addition total amount are the 50% of the calcium hydroxide slurry quality modulated;
(2) chemical additives are added: being squeezed into the calcium hydroxide slurry debugged with the intermittent of agitating device with pump
Bubbling carbonization tower, it is 2.2% polyethyleneimine of calcium hydroxide quality as crystalline form directed agents that quality, which is added, and addition quality is hydrogen-oxygen
Change calcareous 3.1% Sodium Polyacrylate of amount as pattern controlling agent, stirs evenly;
(3) be carbonized: adjusting the initial carburizing temperature of calcium hydroxide slurry is 12 DEG C, opens air valve, is passed through containing CO2Volumetric concentration
Carburizing reagent is carried out for 28% gas, air valve is closed in carbonization to reaction solution pH when being 6.9, stop reaction, stops stirring;
(4) it dehydrates: to calcium carbonate serosity gel and after dissolving, after the processes such as dehydration, drying, crushing, screening
Obtain the regular spherical calcium carbonate that average grain diameter is 638 nanometers.
Claims (10)
1. a kind of regular spherical calcium carbonate, it is characterised in that: belong to calcium hydroxide carbonizatin method and prepare spherical calcium carbonate, it is adjusted first
Calcium hydroxide slurry is made, compound crystal control agent is then added in calcium hydride slurries and is thoroughly mixed, is adjusted initial
Carbon dioxide gas carbonization is passed through after carburizing temperature, obtain calcium carbonate serosity through dehydration, drying, crushing, sieve up to regular ball
Shape calcium carbonate, preparation method includes the following steps:
1) lime slaking, refine and be modulated into calcium hydroxide slurry;
2) compound crystal control agent is added in the calcium hydroxide slurry modulated;
3) calcium hydroxide slurry is passed through carbon dioxide gas progress carburizing reagent after adjusting initial carburizing temperature, and pH sentences when being lower than 7
Fixed reaction terminates, and stopping is passed through carbon dioxide gas;
4) regular spherical calcium carbonate is obtained through dehydration, drying, crushing, screening after carburizing reagent terminates.
2. regular spherical calcium carbonate according to claim 1, it is characterised in that: crystal form is that vaterite crystal form and calcite are brilliant
The mixing crystal form of type, crystal morphology are the calcium carbonate of regular spherical shape, and vaterite crystal form content accounts for 50% or more, and calcite crystal form contains
Amount accounts for 50% hereinafter, 300-900 nanometers of regular spherical calcium carbonate partial size.
3. regular spherical calcium carbonate according to claim 1, it is characterised in that: can be the complete spherical carbon of uniformly rule
Sour calcium is also possible to because reaction condition and process parameter control formation not in place are unevenly or containing partial crushing ball calcium
Regular spherical calcium carbonate.
4. regular spherical calcium carbonate according to claim 1, it is characterised in that: the digestion of lime, Ke Yizhi in step 1)
It connects and is digested with water, be also possible to water with being digested after methanol or ethyl alcohol mixing, after being also possible to water, methanol, ethyl alcohol mixing
It is digested, is also possible to the clear liquid that regular spherical calcium carbonate preparation dehydration obtains and is used to digest;It is modulated after lime slaking purification
Calcium hydroxide content 4-16% in calcium hydroxide slurry, methanol or ethyl alcohol or the mixture of the two contain in calcium hydroxide slurry
Amount is the 25-80% of calcium hydroxide slurry quality.
5. regular spherical calcium carbonate according to claim 1, it is characterised in that: in the calcium hydroxide modulated in step 2)
Compound crystal control agent is added in slurries, compound crystal control agent is divided into two components, and a component is calcium carbonate crystalline form guiding
Agent, the other is component is pattern controlling agent;Crystalline form directed agents are as the flocculating agent that vaterite crystal is condensed to balling-up, pattern control
Preparation adjusts calcium carbonate granule pattern as spherical calcium carbonate Morphological control agent and is intended to complete spherical;The crystalline form directed agents are
By one of heat aging soluble starch slurries, polyvinylpyrrolidone, polyvinylbenzenesulfonic acid sodium, polyethyleneimine
Or a variety of compound;The crystalline form adjusting control agent is Sodium Polyacrylate, polysorbate, poly (sodium aspartate), anhydrous sorbitol
One of aliphatic ester or a variety of compounds;The amount of the crystalline form directed agents of addition is the 0.5-8% of calcium hydroxide solid content;
The amount of the crystal control agent of addition is the 0.6-10% of calcium hydroxide solid content.
6. regular spherical calcium carbonate according to claim 5, it is characterised in that: the amount of the crystalline form directed agents of addition is hydrogen-oxygen
Change the 1-6% of calcium solid content.
7. regular spherical calcium carbonate according to claim 1, it is characterised in that: in step 3) in band stirring carbonizing plant,
Calcium hydroxide slurry is added compound crystal control agent and stirs evenly, and adjusts 3-40 DEG C of initial carburizing temperature, is opening stirring
Under be passed through the gas of carbon dioxide containing gas concentration 20-100% and carry out carburizing reagent and stop being passed through gas and terminating carbon lower than 7 to pH
Change.
8. regular spherical calcium carbonate according to claim 1, it is characterised in that: stop being passed through carbon dioxide gas in step 3)
Body stops stirring waiting slurries formation gel after terminating carbonization, and waiting gel dissolves or suitably heat acceleration after forming gel
Gel dissolves;Slurries pH belonged to carbonization lower than 7 and forms calcium carbonate and calcium bicarbonate mixed serum, after stopping being passed through gas,
Have that calcium bicarbonate is decomposed to form calcium carbonate and carbon dioxide gas releases to form bubble during sol-gel.
9. regular spherical calcium carbonate according to claim 1, it is characterised in that: gel dissolve after can by filtering or
Person's centrifugal dehydration obtains calcium carbonate filter cake, and filter cake obtains regular spherical calcium carbonate by dry, crushing, screening.
10. regular spherical calcium carbonate according to claim 1, it is characterised in that: calcium carbonate serosity is dehydrated in step 4)
To filtrate can be recycled after precipitating, filtering, clarifying treatment.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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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CN115448346A (en) * | 2022-08-11 | 2022-12-09 | 中南大学 | Preparation method of superfine light calcium carbonate |
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Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060165583A1 (en) * | 2003-02-27 | 2006-07-27 | Okutama Kogyo Co., Ltd. | Spherical calcium carbonate and method for producing thereof |
JP2009518280A (en) * | 2005-12-12 | 2009-05-07 | ソルヴェイ(ソシエテ アノニム) | Precipitated calcium carbonate particles, process for producing the particles and use of the particles as fillers |
CN101525147A (en) * | 2008-12-04 | 2009-09-09 | 兰州理工大学 | Preparation method of nano calcium carbonate |
CN102557099A (en) * | 2011-12-16 | 2012-07-11 | 杭州师范大学 | Method for preparing calcite phase and/or vaterite phase calcium carbonate |
CN102674425A (en) * | 2012-05-19 | 2012-09-19 | 祁阳建明化工有限责任公司 | A kind of normal temperature method nanoscale calcium carbonate production process |
CN102701255A (en) * | 2012-06-21 | 2012-10-03 | 石家庄市红日钙业有限公司 | Method for high-concentration carbonization production of spherical nano calcium carbonate |
CN105060330A (en) * | 2015-09-14 | 2015-11-18 | 广西大学 | Preparation method of spherical calcium carbonate crystal |
CN106335917A (en) * | 2015-07-13 | 2017-01-18 | 上海宥纳新材料科技有限公司 | Preparation method of nanometer calcium carbonate |
-
2019
- 2019-03-21 CN CN201910219330.2A patent/CN109809457B/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060165583A1 (en) * | 2003-02-27 | 2006-07-27 | Okutama Kogyo Co., Ltd. | Spherical calcium carbonate and method for producing thereof |
JP2009518280A (en) * | 2005-12-12 | 2009-05-07 | ソルヴェイ(ソシエテ アノニム) | Precipitated calcium carbonate particles, process for producing the particles and use of the particles as fillers |
CN101525147A (en) * | 2008-12-04 | 2009-09-09 | 兰州理工大学 | Preparation method of nano calcium carbonate |
CN102557099A (en) * | 2011-12-16 | 2012-07-11 | 杭州师范大学 | Method for preparing calcite phase and/or vaterite phase calcium carbonate |
CN102674425A (en) * | 2012-05-19 | 2012-09-19 | 祁阳建明化工有限责任公司 | A kind of normal temperature method nanoscale calcium carbonate production process |
CN102701255A (en) * | 2012-06-21 | 2012-10-03 | 石家庄市红日钙业有限公司 | Method for high-concentration carbonization production of spherical nano calcium carbonate |
CN106335917A (en) * | 2015-07-13 | 2017-01-18 | 上海宥纳新材料科技有限公司 | Preparation method of nanometer calcium carbonate |
CN105060330A (en) * | 2015-09-14 | 2015-11-18 | 广西大学 | Preparation method of spherical calcium carbonate crystal |
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