CN109824077A - Spherical calcium carbonate and preparation method thereof - Google Patents
Spherical calcium carbonate and preparation method thereof Download PDFInfo
- Publication number
- CN109824077A CN109824077A CN201910181025.9A CN201910181025A CN109824077A CN 109824077 A CN109824077 A CN 109824077A CN 201910181025 A CN201910181025 A CN 201910181025A CN 109824077 A CN109824077 A CN 109824077A
- Authority
- CN
- China
- Prior art keywords
- calcium carbonate
- preparation
- spherical
- spherical calcium
- calcium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of spherical calcium carbonate and preparation method thereof, preparation steps are as follows: is digested and is aged in proportion with water with quick lime, then sieving cleans, and adds alcohol solvent into raw pulp, purification adjusts and obtains calcium hydroxide slurry；Configured slurry is transferred in supergravity reactor, while chemical additives are added, controls carburizing temperature, CO2Throughput, hypergravity are horizontal, so that calcium hydroxide slurry and carbon dioxide gas counter current contacting, carry out carburizing reagent；Up to spherical calcium carbonate after the precipitating obtained after slurries centrifugation after carbonization is dried, is crushed.The present invention is using calcium hydroxide as raw material, using alcohol-water as solvent, cost is relatively low, and spherical calcium carbonate is prepared using carbonizatin method in super gravity field, it is greatly strengthened microcosmic mixing and mass transport process, carbonization time is short, high production efficiency, Granularity Distribution is narrow, partial size is small, pattern is uniform and favorable dispersibility, is conducive to industrialized application.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, and in particular to a kind of spherical calcium carbonate and preparation method thereof.
Background technique
Calcium carbonate is one of the most abundant biogenic mineral in nature, its chemical property is stablized, and good biocompatibility is easy
Surface modification possesses various forms, and has nontoxic advantageous property, is a kind of very promising inorganic material.It is extensive
Applied to numerous industries such as papermaking, coating, rubber, plastics, ink, cosmetics and medicine.The calcium carbonate of different-shape has not
Same application field, the shape and appearance of calcium carbonate developed at present have spindle, cube, threadiness, spherical shape, chain shape, petal
Shape, sheet, mushroom cloud-like, needle-shaped etc..Spherical calcium carbonate has preferable dispersibility, flatness due to its isotropism
And the excellent properties such as wearability, it can be applied to the raw materials of industry such as plastics, ink, toothpaste and its led in pharmaceuticals, cosmetics etc.
Domain.Therefore, regular appearance is developed, the spherical calcium carbonate of favorable dispersibility has a very important significance.
The preparation method majority of the spherical calcium carbonate of open report is in Ca2+-H2O-CO3 2-Subdivision is carried out in reaction system
Solution reaction generates, and industrially using milk of lime and carbon dioxide gas as raw material, chemical additives are added and carry out carburizing reagent system
Standby spherical calcium carbonate product out is also more rare.It is brilliant that Chinese patent (patent CN105060330A) discloses a kind of spherical calcium carbonate
The preparation method of body is using soluble starch as chemical additives, and ammonium hydroxide is regulator, utilizes calcium chloride water and two
Carbonoxide is raw material, and the spherical calcium carbonate that average grain diameter is 12-17 μm is prepared in carburizing reagent in supergravity reactor.The party
The raw material of method is calcium chloride, and higher cost is unfavorable for industrializing, and product cut size is larger.Chinese patent (the patent No.
CN107445191A a kind of preparation method of spherical calcium carbonate) is disclosed, is to be configured to hydrogen with calcium oxide using calcium oxide as calcium source
Calcium oxide solution adds freeze-dried powder made of fibroin albumen enzymolysis liquid as chemical additives, is then equably passed through dioxy
Change carbon and nitrogen mixed gas, reaction generates spherical calcium carbonate.This method prepares the complex process of chemical additives, and generate
Calcium carbonate spherical shape content is not high, is unfavorable for industrialized production.
Using calcium hydroxide as calcium source, using high-gravity reactive precipitation preparation is small with partial size, pattern is uniform and dispersed
There is not been reported for good pure spherical calcium carbonate.Since high-gravity reactive precipitation carbonization time is short, high production efficiency, granularity point
Cloth uniformly, the favorable reproducibility of different batches of product, be conducive to industrialized application.Therefore, research and utilization hypergravity reactive crystallization
Carbonizatin method, which is stablized, prepares spherical calcium carbonate with more realistic meaning.
The disclosure of background above technology contents is only used for auxiliary and understands design and technical solution of the invention, not necessarily
The prior art for belonging to present patent application, no tangible proof show above content present patent application the applying date
In disclosed situation, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The present invention provides a kind of spherical calcium carbonate and preparation method thereof, to solve the spherical carbonic acid that prior art preparation obtains
Calcium content is not high, higher cost, partial size is larger, is unfavorable for the technical issues of industrialized production.
To achieve the above object, the present invention adopts the following technical scheme:
The preparation method of spherical calcium carbonate, comprising the following steps:
S1. quick lime is digested in proportion with water, sieving cleans, and solvent is added, and adjusting is refining to obtain hydrogen-oxygen
Change calcium slurry；
S2., the step S1 calcium hydroxide slurry configured is put into following for the process unit of high-gravity carbonation reaction process
In ring feed liquid kettle, chemical additives are added, control carburizing temperature, carbon dioxide gas flow, hypergravity are horizontal, allow calcium hydroxide slurry
Material and carbon dioxide gas counter current contacting, carry out carburizing reagent, stop logical carbon dioxide after carburizing reagent；
S3. the slurries after step S2 carbonization are centrifuged, obtained precipitating is dried, crushes to get spherical shape
Calcium carbonate product.
Further, in the step S1 quick lime and water in ratio be mass ratio, specially 1:5-10；It is described molten
Agent is the ethanol solution of volume fraction 30%-80%.
Further, the concentration of the calcium hydroxide in the step S1 is 70-115g/L.
Further, 1-5wt% of the chemical additives additive amount by the step S1 calcium hydroxide slurry configured.
Further, the chemical additives in the step S2 are amino acid, and the amino acid is aspartic acid and paddy ammonia
The one or two of acid.
Further, the carburizing temperature in the step S2 is 10-40 DEG C.
Further, the carbon dioxide gas flow in the step S2 is 0.2-0.6m3/h；Rotor in supergravity reactor
Revolving speed be 1000-1800rpm.
Further, the condition being centrifuged in the step S3: 3min is centrifuged under the revolving speed of 3000rpm.
Further, the process unit of the high-gravity carbonation reaction process in the step S2 includes CO2Gas bomb, rotation
Turn packed bed, circulation feed liquid kettle, acidometer, thermostatical water bath；The CO2Gas bomb gas outlet is disposed with valve, gas
Flowmeter body；The CO2Gas bomb gas outlet is connect with the gas feed of the rotary packed bed；The rotary packed bed
Material liquid outlet is connect with the liquor inlet of circulation feed liquid kettle；The circulating water outlet and thermostatical water bath of the rotary packed bed are intake
Mouth connection；The thermostatical water bath water outlet is connect with circulation feed liquid kettle water inlet；The water outlet of the circulation feed liquid kettle and institute
State the circulating water intake connection of rotary packed bed；It is described circulation feed liquid kettle liquid outlet and the rotary packed bed liquid into
Mouth is connected by pipeline, is provided with air blower and acidometer in the connecting pipe；The intracavitary center of rotary packed bed is liquid
Body distributor, the liquid distribution trough outer rim set are embedded with filler rotor；The filler rotor is connect with external motor；The rotation
Gas vent is additionally provided on packed bed.
The present invention compared with prior art the utility model has the advantages that
The present invention is using calcium hydroxide as raw material, is 400- using carbonizatin method preparation average grain diameter using alcohol-water as solvent
The spherical calcium carbonate of 700nm.Carbonisation carries out in super gravity field, hypergravity equipment by its high speed rotation generate it is huge from
Mental and physical efforts simulate the environment of super gravity field, and alternate mass transfer rate is made to be higher by the 1-3 order of magnitude than traditional tower equipment, micro-
See mixing and mass transport process be greatly strengthened, carbonization time is short, high production efficiency, prepare with relatively narrow size distribution,
Partial size is small, pattern is uniform and the spherical calcium carbonate product of favorable dispersibility, and the favorable reproducibility of different batches of product, is conducive to work
The application of industry.
Detailed description of the invention
Fig. 1: the process device figure of the used high-gravity carbonation reaction process of the present invention；
Fig. 2: rotating packed-bed reactor schematic diagram；
Fig. 3；10.0k times of stereoscan photograph of spherical calcium carbonate made from the embodiment of the present invention 4；
Fig. 4: 30.0k times of stereoscan photograph of spherical calcium carbonate made from the embodiment of the present invention 3；
Fig. 5: 100k times of stereoscan photograph of spherical calcium carbonate made from the embodiment of the present invention 2.
In appended drawing reference: 1.CO2Gas bomb；2. valve；3. gas flowmeter；4. rotary packed bed；5. recycling feed liquid
Kettle；6. acidometer；7. liquor inlet；8. thermostatical water bath；41. gas feed；42. material liquid outlet；43. liquid-inlet；44. gas
Body outlet；45. filler rotor；46. liquid distribution trough；47. circulating water intake；48. circulating water outlet；49. motor.
As shown in Figure 1 and Figure 2: in Fig. 1, the preparation facilities of the spherical calcium carbonate mainly includes CO2Gas bomb 1,
Rotary packed bed 4, circulation feed liquid kettle 5, acidometer 6, thermostatical water bath 8；The CO2The gas outlet of gas bomb 1 is set gradually
There are valve 2, gas flowmeter 3；The CO2The gas outlet of gas bomb 1 is connected to the gas feed of the rotary packed bed 4
41；The material liquid outlet 42 of the rotary packed bed 4 is connect with the liquor inlet 7 of circulation feed liquid kettle 5；The rotary packed bed 4
Circulating water outlet 48 is connected to the water inlet of thermostatical water bath 8；8 water outlet of thermostatical water bath be connected to circulation feed liquid kettle into
The mouth of a river controls the temperature of water；The water outlet of the circulation feed liquid kettle 5 is connected to the circulating water intake 47 of rotary packed bed 4；It is described
The liquid outlet of circulation feed liquid kettle 5 is connect with the liquid-inlet 43 of the rotary packed bed 4 by pipeline, in the connecting pipe
It is provided with air blower and acidometer 6, measures the pH value of reacting slurry.In Fig. 2, the intracavitary center of the rotary packed bed 4 is liquid
Body distributor 46,46 outer rim of the liquid distribution trough set are embedded with filler rotor 45；The filler rotor 45 connects with external motor 49
It connects；Gas vent 44 is additionally provided in the rotary packed bed 4.Hypergravity rotation is realized in the setting of rotary packed bed 4, allows hydrogen-oxygen
Change calcium slurry and carbon dioxide gas counter current contacting, carries out carburizing reagent.
Specific embodiment
To facilitate a better understanding of the present invention, it is illustrated by the following examples, these examples belong to protection of the invention
Range, but do not limit the scope of the invention.
Embodiment 1
A kind of preparation method of spherical calcium carbonate, comprising the following steps:
S1. it is that 1:10 digests with hot water example in mass ratio by quick lime, crosses 200 meshes and clean, volume is added
The ethanol solution that score is 30% adjusts the slurry for being refining to obtain that the concentration of calcium hydroxide is 70g/L as solvent；
S2., the step S1 calcium hydroxide slurry configured is put into following for the process unit of high-gravity carbonation reaction process
In ring feed liquid kettle, the glutamic acid of the 5wt% for the calcium hydroxide slurry that addition step S1 is configured will be carbonized as chemical additives
Temperature be set as 10 DEG C, carbon dioxide gas flow be set as 0.6m3/ h, supergravity reactor rotor speed are set as 1000rpm,
It allows calcium hydroxide slurry and carbon dioxide gas counter current contacting, carries out carburizing reagent；It is complete using the tracking carburizing reagent of digital display pH meter
Process stops ventilation as the pH=6.9 of reacting slurry, and carburizing reagent terminates；
S3. the slurries after being carbonized in step S2 are centrifuged 3min with the revolving speed of 3000rpm, what is be centrifuged is deposited in
Drying for 24 hours, obtains spherical calcium carbonate product at 70 DEG C after crushing.
Embodiment 2
A kind of preparation method of spherical calcium carbonate, comprising the following steps:
S1. it is that 1:5 digests with hot water example in mass ratio by quick lime, crosses 200 meshes and clean, volume point is added
The ethanol solution that number is 80% adjusts the slurry for being refining to obtain that the concentration of calcium hydroxide is 115g/L as solvent；
S2., the step S1 calcium hydroxide slurry configured is put into following for the process unit of high-gravity carbonation reaction process
In ring feed liquid kettle, the aspartic acid of the 1wt% for the calcium hydroxide slurry that addition step S1 is configured is as chemical additives, by carbon
Change temperature be set as 40 DEG C, carbon dioxide gas flow be set as 0.2m3/ h, supergravity reactor rotor speed are set as
1800rpm, allows calcium hydroxide slurry and carbon dioxide gas counter current contacting, carries out carburizing reagent；Carbon is tracked using digital display pH meter
Change reaction overall process, as the pH=7 of reacting slurry, stops ventilation, carburizing reagent terminates；
S3. the slurries after being carbonized in step S2 are centrifuged 3min with the revolving speed of 3000rpm, what is be centrifuged is deposited in
Drying for 24 hours, obtains spherical calcium carbonate product at 90 DEG C after crushing.
Embodiment 3
A kind of preparation method of spherical calcium carbonate, comprising the following steps:
S1. it is that 1:8 digests with hot water example in mass ratio by quick lime, crosses 200 meshes and clean, volume point is added
The ethanol solution that number is 60% adjusts the slurry for being refining to obtain that the concentration of calcium hydroxide is 105g/L as solvent；
S2., the step S1 calcium hydroxide slurry configured is put into following for the process unit of high-gravity carbonation reaction process
In ring feed liquid kettle, the glutamic acid of the 3wt% for the calcium hydroxide slurry that addition step S1 is configured will be carbonized as chemical additives
Temperature be set as 30 DEG C, carbon dioxide gas flow be set as 0.5m3/ h, supergravity reactor rotor speed are set as 1600rpm,
It allows calcium hydroxide slurry and carbon dioxide gas counter current contacting, carries out carburizing reagent；It is complete using the tracking carburizing reagent of digital display pH meter
Process stops ventilation as the pH=6.6 of reacting slurry, and carburizing reagent terminates；
S3. the slurries after being carbonized in step S2 are centrifuged 3min with the revolving speed of 3000rpm, what is be centrifuged is deposited in
Drying for 24 hours, obtains spherical calcium carbonate product at 80 DEG C after crushing.
Embodiment 4
A kind of preparation method of spherical calcium carbonate, comprising the following steps:
S1. it is that 1:7 digests with hot water example in mass ratio by quick lime, crosses 200 meshes and clean, volume point is added
The ethanol solution that number is 50% adjusts the slurry for being refining to obtain that the concentration of calcium hydroxide is 95g/L as solvent；
S2., the step S1 calcium hydroxide slurry configured is put into following for the process unit of high-gravity carbonation reaction process
In ring feed liquid kettle, the aspartic acid of the 2wt% for the calcium hydroxide slurry that addition step S1 is configured is as chemical additives, by carbon
Change temperature be set as 20 DEG C, carbon dioxide gas flow be set as 0.4m3/ h, supergravity reactor rotor speed are set as
1400rpm, allows calcium hydroxide slurry and carbon dioxide gas counter current contacting, carries out carburizing reagent；Carbon is tracked using digital display pH meter
Change reaction overall process, as the pH=6.5 of reacting slurry, stops ventilation, carburizing reagent terminates；
S3. the slurries after being carbonized in step S2 are centrifuged 3min with the revolving speed of 3000rpm, what is be centrifuged is deposited in
Drying for 24 hours, obtains spherical calcium carbonate product at 80 DEG C after crushing.
Embodiment 5
A kind of preparation method of spherical calcium carbonate, comprising the following steps:
S1. it is that 1:7 digests with hot water example in mass ratio by quick lime, crosses 200 meshes and clean, volume point is added
The ethanol solution that number is 50% adjusts the slurry for being refining to obtain that the concentration of calcium hydroxide is 95g/L as solvent；
S2., the step S1 calcium hydroxide slurry configured is put into following for the process unit of high-gravity carbonation reaction process
In ring feed liquid kettle, the aspartic acid of the 4wt% for the calcium hydroxide slurry that addition step S1 is configured is as chemical additives, by carbon
Change temperature be set as 20 DEG C, carbon dioxide gas flow be set as 0.3m3/ h, supergravity reactor rotor speed are set as
1200rpm, allows calcium hydroxide slurry and carbon dioxide gas counter current contacting, carries out carburizing reagent；Carbon is tracked using digital display pH meter
Change reaction overall process, as the pH=6.8 of reacting slurry, stops ventilation, carburizing reagent terminates；
S3. the slurries after being carbonized in step S2 are centrifuged 3min with the revolving speed of 3000rpm, what is be centrifuged is deposited in
Drying for 24 hours, obtains spherical calcium carbonate product at 80 DEG C after crushing.
Comparative example 1
Using in patent document " a kind of preparation method of spherical calcium carbonate crystal (Authorization Notice No.: CN105060330B) "
The method of embodiment 1 prepares this spherical calcium carbonate, specifically includes the following steps:
Compound concentration is the CaCl of 0.20mol/L2Solution, wherein CaCl2Overall solution volume is 2.5L, and it is dense that 30ml is added
Degree adjusts pH for 25% ammonium hydroxide, and the 0.25wt% soluble starch of addition is transferred in supergravity reactor after sealing stirring.
Carburizing temperature is set as 15 DEG C, carbon dioxide gas flow set is 30L/h, and supergravity reactor rotor speed is set as
1400rpm.In the CaCl of supergravity reactor high speed rotation2Mixed liquor and CO2Counter current contacting carries out carburizing reagent.Using number
Aobvious pH meter tracks carburizing reagent overall process, as reacting slurry pH=6.8, stops ventilation, carburizing reagent terminates.Carbonization is completed
Slurries afterwards are centrifuged, and dry 5h, grinds to get spherical calcium carbonate product at 70 DEG C.
Comparative example 2
Implement using in patent document " a kind of preparation method of spherical calcium carbonate (Authorization Notice No.: CN107445191A) "
The method of example 1 prepares this spherical calcium carbonate, specifically includes the following steps:
S1. by useless silk removal of impurities, degumming, clean, be dried to obtain degumming fibroin, the calcium chloride for being 40% with mass fraction is molten
Simultaneously silk fibroin protein solution is obtained by filtration in liquid dissolution degumming fibroin, and silk fibroin protein solution is dialysed and removes calcium chloride, then husky with 2g
Thunder peptase digests 100g fibroin albumen 3h at 50 DEG C, obtains fibroin albumen enzymolysis liquid, collects molecule using 10000Da ultrafiltration membrane
The penetrating fluid in 360-11808Da is measured, penetrating fluid is 50 DEG C in temperature, and pressure is concentrated by rotary evaporation under conditions of 170Pa, is then existed
Temperature is -60 DEG C, and pressure is vacuum freeze drying 72h under conditions of 50Pa, obtains freeze-dried powder；
S2. according to parts by weight, 1 part of calcium oxide is added in 100 parts of deionized waters, constant temperature stirs 3h at 90 DEG C, so
Cross afterwards the sieve of 200 mesh and by filtrate sealing and standing for 24 hours, then by filtrate be diluted to mass fraction be 0.3% calcium hydroxide it is molten
Liquid；
S3. freeze-dried powder is added in calcium hydroxide solution, constant temperature is stirred to react 1h at 30 DEG C, then by CO2And N2It is mixed
Gas to be closed equably to be passed through in calcium hydroxide solution, reaction to pH value of solution is down to 7.0, then stirs 30min with the revolving speed of 150rpm,
Solid product is then demultiplex out and is washed with deionized water and dehydrated alcohol, is placed on after washing in 50 DEG C of vacuum oven dry
3h, finally spherical calcium carbonate, the mass ratio of the freeze-dried powder and calcium hydroxide are 0.5:1, CO in the mixed gas2And N2
The volume ratio pressed is 1:4, and the flow of mixed gas is 300mL/min.
Comparative example 3
Other than the process unit of the high-gravity carbonation reaction process in step S2 is changed to traditional carbonators, other preparations
The preparation process of technique and embodiment 5 is essentially identical.
This spherical calcium carbonate is prepared using the preparation method of embodiment 1-5 and comparative example 1-2, detects partial size, ball calcium respectively
Content and calculating cost of material, as a result as shown in the table.
This spherical calcium carbonate is prepared using the preparation method of embodiment 1-5 and comparative example 3, it is (raw to calculate carbonization time respectively
Produce efficiency), particle diameter distribution/size, as a result as shown in the table.
| Test group | Carbonization time | Particle diameter distribution/size |
| Embodiment 1 | 8min | Narrow (0.52-0.64 μm)/it is fine |
| Embodiment 2 | 15min | Narrow (0.45-0.53 μm)/it is fine |
| Embodiment 3 | 13min | Narrow (0.63-0.70 μm)/it is fine |
| Embodiment 4 | 10min | Narrow (0.56-0.65 μm)/it is fine |
| Embodiment 5 | 10min | Narrow (0.40-0.58 μm)/it is fine |
| Comparative example 3 | 78min | Wide (2.08-10.67 μm)/particle |
By the data of embodiment 1-5 and comparative example 1-2 it is found that relative to spherical calcium carbonate prepared by the present invention, comparative example 1
Used raw material is calcium chloride, rather than the common calcium oxide of industry digested made of calcium hydroxide as calcium source, cost
It is higher, and product cut size is larger；Comparative example 2 prepares the complex process of chemical additives, too low (its of raw material calcium hydroxide concentration
It is 0.3%, and is industrially 7%-12%), and the calcium carbonate spherical shape content generated is not high, is unfavorable for industrialized production.Using
Traditional carbonators of comparative example 3 carries out carburizing reagent, and carbonization time is long, and production efficiency is not high, and partial size is larger and wider distribution.This
Outside, in conjunction with the electromicroscopic photograph of Fig. 3-5 and upper table it is found that spherical calcium carbonate prepared by the present invention has relatively narrow size distribution, grain
Diameter is small, pattern is uniform and favorable dispersibility, illustrates ethyl alcohol, calcium hydroxide, amino acid chemical additives under hypergravity state
Synergistic effect is played when mixing, and the calcium chloride, ammonium hydroxide, soluble starch in comparative example 1 mix simultaneously under hypergravity state
Good synergistic effect cannot be played, so that the partial size of spherical calcium carbonate obtained is relatively large, and the present invention prepares work
The carbonization time of skill is short, high production efficiency, is conducive to industrialized application.
Protection scope of the present invention is not limited merely to above-described embodiment, and all technical solutions belonged under thinking of the present invention are equal
It belongs to the scope of protection of the present invention.It should be pointed out that for those skilled in the art, not departing from the present invention
Several improvements and modifications under the premise of principle, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (10)
1. the preparation method of spherical calcium carbonate, which comprises the following steps:
S1. quick lime is digested in proportion with water, sieving cleans, and solvent is added, and adjusting is refining to obtain calcium hydroxide
Slurry；
S2., the step S1 calcium hydroxide slurry configured is put into the cycle stock of the process unit of high-gravity carbonation reaction process
In liquid kettle, add chemical additives, control carburizing temperature, carbon dioxide gas flow, hypergravity are horizontal, allow calcium hydroxide slurry with
Carbon dioxide gas counter current contacting carries out carburizing reagent, stops logical carbon dioxide after carburizing reagent；
S3. the slurries after step S2 carbonization are centrifuged, obtained precipitating is dried, crushes to get spherical carbonic acid
Calcium product.
2. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that quick lime and water in the step S1
In ratio be mass ratio, specially 1:5-10；The solvent is the ethanol solution of volume fraction 30%-80%.
3. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that the calcium hydroxide in the step S1
Concentration be 70-115g/L.
4. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that the chemical additives additive amount is
The 1-5wt% for the calcium hydroxide slurry that step S1 is configured.
5. the preparation method of spherical calcium carbonate according to claim 4, which is characterized in that the crystal form control in the step S2
Agent is amino acid, and the amino acid is the one or two of aspartic acid and glutamic acid.
6. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that the carburizing temperature in the step S2
It is 10-40 DEG C.
7. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that the carbon dioxide in the step S2
Throughput is 0.2-0.6m3/h；The revolving speed of rotor is 1000-1800rpm in supergravity reactor.
8. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that the item being centrifuged in the step S3
Part: 3min is centrifuged under the revolving speed of 3000rpm.
9. a kind of spherical calcium carbonate of method preparation according to claim 1-8.
10. the preparation method of spherical calcium carbonate according to claim 1, which is characterized in that the hypergravity in the step S2
The process unit of carburizing reagent process includes CO2Gas bomb, rotary packed bed, circulation feed liquid kettle, acidometer, water bath with thermostatic control
Device；The CO2Gas bomb gas outlet is connect with the gas feed of the rotary packed bed；The feed liquid of the rotary packed bed goes out
Mouth is connect with the liquor inlet of circulation feed liquid kettle；The circulating water outlet and thermostatical water bath water inlet of the rotary packed bed connect
It connects；The thermostatical water bath water outlet is connect with circulation feed liquid kettle water inlet；The water outlet of the circulation feed liquid kettle and the rotation
Turn the circulating water intake connection of packed bed；The liquid outlet of the circulation feed liquid kettle and the liquid-inlet of the rotary packed bed are logical
Piping connects, and is provided with air blower and acidometer in the connecting pipe；The intracavitary center of rotary packed bed is liquid point
Cloth device, the liquid distribution trough outer rim set are embedded with filler rotor；The filler rotor is connect with external motor；The rotation filling
Gas vent is additionally provided on bed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910181025.9A CN109824077A (en) | 2019-03-11 | 2019-03-11 | Spherical calcium carbonate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910181025.9A CN109824077A (en) | 2019-03-11 | 2019-03-11 | Spherical calcium carbonate and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109824077A true CN109824077A (en) | 2019-05-31 |
Family
ID=66868878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910181025.9A Pending CN109824077A (en) | 2019-03-11 | 2019-03-11 | Spherical calcium carbonate and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109824077A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240188A (en) * | 2019-07-19 | 2019-09-17 | 良德纳米粉体创新科技(安徽)有限公司 | A kind of processing method of nanometer calcium carbonate |
| CN110451544A (en) * | 2019-08-14 | 2019-11-15 | 青海民族大学 | A kind of preparation method of ball shaped nano strontium carbonate |
| CN110484023A (en) * | 2019-09-30 | 2019-11-22 | 建德市华宇纳米科技有限公司 | A kind of high-dispersion nano calcium carbonate Preparation equipment and preparation method |
| 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 |
| CN111233051A (en) * | 2020-03-04 | 2020-06-05 | 陕西师范大学 | Method for preparing submicron spherical cobalt carbonate |
| CN111333096A (en) * | 2020-03-24 | 2020-06-26 | 立达超微工业（苏州）有限公司 | Production process of ultrafine calcium carbonate powder |
| CN113087004A (en) * | 2021-04-14 | 2021-07-09 | 上海抚翌科技有限公司 | Production method of calcium carbonate in cigarette paper |
| CN114408961A (en) * | 2022-01-26 | 2022-04-29 | 广西大学 | Submicron spindle-shaped calcium carbonate prepared by high-activity lime hypergravity reaction crystallization method and method thereof |
| CN114684838A (en) * | 2022-02-21 | 2022-07-01 | 内蒙古自治区人民医院（内蒙古自治区肿瘤研究所） | Preparation method and application of luminous calcium carbonate with different morphologies |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105060330A (en) * | 2015-09-14 | 2015-11-18 | 广西大学 | Preparation method of spherical calcium carbonate crystal |
| CN107986313A (en) * | 2017-12-25 | 2018-05-04 | 广西大学 | A kind of preparation method of spherical calcium carbonate |
-
2019
- 2019-03-11 CN CN201910181025.9A patent/CN109824077A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105060330A (en) * | 2015-09-14 | 2015-11-18 | 广西大学 | Preparation method of spherical calcium carbonate crystal |
| CN107986313A (en) * | 2017-12-25 | 2018-05-04 | 广西大学 | A kind of preparation method of spherical calcium carbonate |
Non-Patent Citations (2)
| Title |
|---|
| 李丽颖等: ""阴离子氨基酸表面活性剂调控碳酸钙的仿生合成"", 《高等学校化学学报》 * |
| 贺鑫等: ""超重力场中影响碳酸钙晶须断裂的影响因素分析"", 《高校化学工程学报》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240188A (en) * | 2019-07-19 | 2019-09-17 | 良德纳米粉体创新科技(安徽)有限公司 | A kind of processing method of nanometer calcium carbonate |
| CN110451544A (en) * | 2019-08-14 | 2019-11-15 | 青海民族大学 | A kind of preparation method of ball shaped nano strontium carbonate |
| CN110563015B (en) * | 2019-09-27 | 2022-03-29 | 河北立信化工有限公司 | Preparation method of light calcium carbonate for food |
| 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 |
| CN110484023B (en) * | 2019-09-30 | 2021-05-14 | 建德市华宇纳米科技有限公司 | Preparation equipment and preparation method of high-dispersion nano calcium carbonate |
| CN110484023A (en) * | 2019-09-30 | 2019-11-22 | 建德市华宇纳米科技有限公司 | A kind of high-dispersion nano calcium carbonate Preparation equipment and preparation method |
| CN111233051A (en) * | 2020-03-04 | 2020-06-05 | 陕西师范大学 | Method for preparing submicron spherical cobalt carbonate |
| CN111333096A (en) * | 2020-03-24 | 2020-06-26 | 立达超微工业（苏州）有限公司 | Production process of ultrafine calcium carbonate powder |
| CN113087004A (en) * | 2021-04-14 | 2021-07-09 | 上海抚翌科技有限公司 | Production method of calcium carbonate in cigarette paper |
| CN114408961A (en) * | 2022-01-26 | 2022-04-29 | 广西大学 | Submicron spindle-shaped calcium carbonate prepared by high-activity lime hypergravity reaction crystallization method and method thereof |
| CN114408961B (en) * | 2022-01-26 | 2023-09-22 | 广西大学 | Submicron spindle-shaped calcium carbonate prepared by high-activity lime hypergravity reaction crystallization method and method thereof |
| CN114684838A (en) * | 2022-02-21 | 2022-07-01 | 内蒙古自治区人民医院（内蒙古自治区肿瘤研究所） | Preparation method and application of luminous calcium carbonate with different morphologies |
| CN114684838B (en) * | 2022-02-21 | 2023-10-24 | 内蒙古自治区人民医院（内蒙古自治区肿瘤研究所） | Preparation method and application of luminous calcium carbonate with different appearances |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109824077A (en) | Spherical calcium carbonate and preparation method thereof | |
| CN108975372A (en) | A kind of preparation method of spindle winnofil | |
| CN105060330B (en) | A kind of preparation method of spherical calcium carbonate crystal | |
| CN106517285B (en) | A kind of preparation method of rod-like nano calcium carbonate | |
| CN105417566A (en) | Method for preparing nano calcium carbonate through full-automatic rotating pressure jet-carbonation technology | |
| CN107032382B (en) | Nano calcium carbonate and preparation method thereof | |
| CN104893361A (en) | Preparation method of nano calcium carbonate special for neutral silicone sealant | |
| CN106916515B (en) | A kind of Functional Powder Coating and preparation method thereof | |
| CN1962452A (en) | Nm-class calcium carbonate carbonization process | |
| CN102701255A (en) | Method for high-concentration carbonization production of spherical nano calcium carbonate | |
| CN102079525A (en) | Method for preparing white carbon black by taking rice hull ash as raw material | |
| CN110028702A (en) | A kind of nano silica dopen Nano cellulosic material and its preparation method and application | |
| CN109867986A (en) | A kind of macromolecule modified nanometer calcium carbonate new product family | |
| CN109437273A (en) | A kind of preparation method of monodisperse cube winnofil | |
| CN101665990B (en) | Fibroin blending regeneration cellulose fiber and preparation technique thereof | |
| CN108033476A (en) | A kind of preparation method of nano-calcium carbonate | |
| TWI636957B (en) | Method for preparing calcium carbonate particles | |
| CN102796401A (en) | Preparation method of nanometer calcium carbonate with silica-stearic acid composite coating and special for silicone sealant | |
| CN204737736U (en) | Carbonization reaction unit of nano calcium carbonate production | |
| CN106365191B (en) | A kind of method that high dispersion of nano-calcium carbonate is prepared using stalactite | |
| CN107746068B (en) | A kind of silica modified barium sulfate raw powder's production technology | |
| CN106830042B (en) | A kind of method that the ultra-fine carbonic acid fine particle calcium carbonate of rhombohedron shape is prepared using Weihe north Ordovician limestone | |
| CN1207209C (en) | Eddy flow process of preparing ultramicro calcium carbonate precipitate | |
| CN205575669U (en) | Preparation nano calcium carbonate's device | |
| CN101618307B (en) | Preparation method of microcapsule for novel environment-friendly insulating building coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190531 |