CN109368680A - It is a kind of with lime stone prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained - Google Patents
It is a kind of with lime stone prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained Download PDFInfo
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- CN109368680A CN109368680A CN201811639480.0A CN201811639480A CN109368680A CN 109368680 A CN109368680 A CN 109368680A CN 201811639480 A CN201811639480 A CN 201811639480A CN 109368680 A CN109368680 A CN 109368680A
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- high activity
- calcium carbonate
- activity porous
- porous light
- light calcium
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention belongs to precipitated calcium carbonate preparation fields, it is related to a kind of method with lime stone preparation high activity porous light Paris white, it solves and continues to use the technical problem that conventional limestone firing CaO method hardly results in high activity porous light Paris white, by carrying out negative pressure of vacuum low temperature calcination after being crushed lime stone, high activity porous CaO powder is obtained；Then the high activity porous CaO powder ultra-fine grinding that will be obtained；It is being passed through CO2Enclosure space under the conditions of keep certain humidity to carry out high activity porous light calcium carbonate slow reaction, high activity porous light calcium carbonate is made.It is improved using the performances such as the whiteness of high activity porous light calcium carbonate and BET made from preparation method of the invention, oil absorption is greater than 100ml/100g, and whiteness is greater than 90, BET and is greater than 15m2/g.In addition, using negative pressure of vacuum low temperature calcination method during preparation method of the present invention, energy-efficient technical effect is had also achieved.
Description
Technical field
The invention belongs to precipitated calcium carbonate preparation fields, are related to a kind of method and institute that precipitated calcium carbonate is prepared with lime stone
Obtain precipitated calcium carbonate.
Background technique
Existing shell mainly prepares powdered whiting during preparing calcium carbonate, for being prepared into precipitated calcium carbonate
Research it is less.In addition, traditional lightweight Paris white is largely to fire CaO by limestone block, place it in water, leads to CO2
Gas reaction obtains lightweight carbonate chemical product.Method continues to use conventional limestone and fires CaO method, hardly results in active porous light
Matter Paris white；And whiteness, oil absorption, the vibration density of the precipitated calcium carbonate that CaO method obtains are fired using conventional limestone
Degree and BET performance are relatively poor；In addition, tradition fires the old-fashioned kiln during the precipitated calcium carbonate that CaO method obtains at present
Furnace is substituted, and using new-type burner hearth generally calcined by the way of electricity using burning, and forged using this kind of mode
It burns, temperature needs to reach 1000 DEG C or more just can be with cost is too high.Therefore, those skilled in the art are badly in need of to active porous light
The preparation method of matter calcium carbonate makes further linguistic term.
Summary of the invention
The present invention provides a kind of method for preparing precipitated calcium carbonate with lime stone, using low temperature calcination method to lime stone into
Row calcining solves and continues to use the technical problem that conventional limestone firing CaO method hardly results in high activity porous light calcium carbonate.
In order to achieve the above object, the present invention provides a kind of sides with lime stone preparation high activity porous light calcium carbonate
Method includes the following steps:
Lime stone is crushed as needed, then carries out negative pressure of vacuum low temperature calcination, stops heating after calcining 1-4h, together
When stop vacuumizing, and convey air or oxygen into burner hearth, obtain high activity porous CaO；
By obtained high activity porous CaO air-flow crushing to particle powder, micro mist powder, fine powder or superfine powder,
It is subsequently placed under the conditions of enclosure space, so that the humidity of enclosure space is reached 95% using the water after ultrasonic atomization, be passed through simultaneously
CO2Gas carries out the flexible slow reaction 6-48h of porous CaO powder under the enclosure space reaction system, obtains porous light carbon
Sour calcium.
Further, lime stone is crushed to 1-5mm as needed.
Further, by obtained high activity porous CaO air-flow crushing to particle powder size be 5 μm, micro mist powder it is big
It is small be 1-5 μm, the rank that fine powder size is 0.1-1 μm or superfine powder size is 0.02-0.1 μm.
Further, the calcination temperature during the negative pressure of vacuum low temperature calcination be 650-750 DEG C, vacuum degree be-
Between 80KPa to -50KPa.
The high activity porous light carbon that the above-mentioned method with lime stone preparation high activity porous light calcium carbonate is prepared
The oil absorption of sour calcium activity degree is greater than 100ml/100g, and whiteness is greater than 90, BET and is greater than 15m2/g。
Compared with prior art, the advantages and beneficial effects of the present invention are:
1. provided by the invention prepare porous light calcium carbonate method with lime stone, solves and continue to use conventional limestone firing
CaO method hardly results in the technical problem of high activity porous light Paris white；It is anti-using negative pressure of vacuum low temperature calcination method+at a slow speed
The method answered prepares porous light calcium carbonate；Negative pressure of vacuum low temperature calcination method calcined shell powder, can be quickly by the CO of decomposition2Point
From discharge, reduce CO2Partial pressure size is to shell CaCO3Resolve into CaO and CO2Decomposition temperature influence, reached section
The technical effect of energy needs to reach 1000 DEG C or more compared to calcination temperature in current firing CaO mode, and the present invention uses vacuum
Temperature when negative pressure low temperature calcination method is calcined significantly reduces, and reduces costs；During slow reaction, using the water after atomization
So that enclosure space humidity reaches 95%, reaction constantly stirs high activity porous CaO powder during carrying out, so that in reaction process
The high activity porous light calcium carbonate that will not destroy of reaction heat.
2. using oil absorption, whiteness and the BET etc. of high activity porous light calcium carbonate made from preparation method of the invention
The opposite performance for using conventional limestone to fire the precipitated calcium carbonate that CaO method obtains of performance is improved, and the present invention is made
High activity porous light calcium carbonate oil absorption be greater than 100ml/100g, whiteness be greater than 90, BET be greater than 15m2/g。
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
It is including as follows the embodiment of the invention provides a kind of method with lime stone preparation high activity porous light calcium carbonate
Step:
S1: lime stone is crushed as needed, then carries out negative pressure of vacuum low temperature calcination, stops adding after calcining 1-4h
Heat is simultaneously stopped and vacuumizes, and air or oxygen is conveyed into burner hearth, obtains high activity porous CaO powder；
In above-mentioned steps, due to CO2Partial pressure can seriously affect CaCO in agstone3Resolve into CaO and CO2, this hair
In the step for the preparation method that bright embodiment provides, carry out lime burning mountain flour using negative pressure of vacuum low temperature calcination method, utilizes
Negative pressure technique accelerates the CO of thermal decomposition2Separation discharge, be more advantageous to obtained high activity porous CaO powder, and to burner hearth
During interior conveying air or oxygen, the air or oxygen of conveying is appropriate, is preferred with that will not blow afloat powder, can use waste heat
By carbon exhaustive oxidation in shell, whiteness is increased；The present invention uses negative pressure of vacuum low temperature calcination method simultaneously, has also achieved energy-efficient
Technical effect.
S2: by obtained high activity porous CaO air-flow crushing to particle powder, micro mist powder, fine powder or superfine powder
Body is subsequently placed under the conditions of enclosure space, so that the humidity of enclosure space is reached 95% using the water after ultrasonic atomization, is led to simultaneously
Enter CO2Gas carries out the flexible slow reaction 6-48h of porous CaO powder under the enclosure space reaction system, obtains porous light
Calcium carbonate.
In above-mentioned steps, usual CaO and H2Reaction is very violent when O is reacted, and a large amount of heat can be generated, to influence
The generation of precipitated calcium carbonate, but reaction can be made to carry out less acute using the flexible slow reaction in the embodiment of the present invention
It is strong, porous CaO powder is constantly stirred during the reaction, so that the high activity that the reaction heat in reaction process will not destroy is more
The porosity of hole precipitated calcium carbonate；
In an alternative embodiment, by obtained high activity porous CaO air-flow crushing to particle powder size be 5 μm, it is micro-
Powder powder size is 1-5 μm, the rank that fine powder size is 0.1-1 μm or superfine powder size is 0.02-0.1 μm, more
Conducive to the progress of subsequent flexible slow reaction.
In an alternative embodiment, the calcination temperature during the negative pressure of vacuum low temperature calcination is 650-750 DEG C, vacuum
Degree is between -80KPa to -50KPa.In the present embodiment, the calcination temperature can also be 650 DEG C, 700 DEG C, 750 DEG C.It can be with
Understand, restriction those skilled in the art of calcination temperature and vacuum degree for above-mentioned reaction system can be according to the actual situation
Floating adjustment is carried out within the above range or according to above range, as long as ensuring to react sufficiently progress.
In an alternative embodiment of the present invention, high activity porous light has been made using preparation method provided in this embodiment
Calcium carbonate.100ml/ is greater than using the oil absorption of high activity porous light calcium carbonate made from preparation method provided in this embodiment
100g, whiteness are greater than 90, BET and are greater than 15m2/ g, performance are more excellent.
High activity porous light carbon is prepared with lime stone provided by the embodiment of the present invention in order to become apparent to introduce in detail
The method of sour calcium, is described below in conjunction with specific embodiment.
Embodiment 1
A method of high activity porous light calcium carbonate being prepared with lime stone, is included the following steps:
After lime stone is crushed to 1-5mm as needed, in 700 DEG C of calcination temperatures and the condition of the vacuum degree of -70KPa
Lower progress negative pressure of vacuum low temperature calcination stops heating after calcining 2h, is simultaneously stopped and vacuumizes,
And air or oxygen is conveyed into burner hearth, obtains high activity porous CaO powder；
Obtained high activity porous CaO is crushed to fine 0.1-1 μm, is placed under the conditions of enclosure space, using ultrasonic wave
Water after atomization makes the humidity of enclosure space reach 95%, while being passed through CO2Gas carries out under the enclosure space reaction system
The flexible slow reaction of porous CaO powder for 24 hours, obtains porous light calcium carbonate.
Embodiment 2
The difference from embodiment 1 is that: the vacuum degree in the preparation step is -60KPa, and calcination temperature is 650 DEG C.
Embodiment 3
The difference from embodiment 1 is that: the vacuum degree in the preparation step is -80KPa, and calcination temperature is 750 DEG C.
Comparative example 1
The difference from embodiment 1 is that: it is calcined during the preparation process using conventional calcination method.
Comparative example 2
The difference from embodiment 1 is that: the vacuum degree in the preparation step is -60KPa, and calcination temperature is 600 DEG C.
Comparative example 3
The difference from embodiment 1 is that: the vacuum degree in the preparation step is -30KPa, and calcination temperature is 800 DEG C.
Comparative example 4
The difference from embodiment 1 is that: the vacuum degree in the preparation step is -20KPa, and calcination temperature is 700 DEG C.
Performance test
High activity porous porous precipitated calcium carbonate obtained by above-described embodiment 1-3 and comparative example 1-4 is tested for the property, is surveyed
Method for testing is as follows, the results are shown in Table 1.
Oil suction quantity measuring method: high activity porous light calcium carbonate sample obtained by embodiment 1-3 and comparative example 1-4 is placed in
On glass plate or glaze paint porcelain plate, DOP is added dropwise with the drop bottle for filling o-phthalic acid dibutyl ester (DOP) of known quality, is being added dropwise
When constantly carried out stirring grinding with toolsetting, originally sample is in dispersed, after gradually agglomerating until all soaked by DOP, and shape
It is terminal at a whole group.Drop bottle quality is weighed, 0.01g is accurate to.Entire measurement requires to complete in 90min, calculates suction
Oil mass.
Whiteness: being measured using measuring brightness analyzer, which is used to measure the blue streak whiteness of body surface, technology
Performance meets JB/T9327-1999 leucometer standard, measurement result digital-scroll technique.
BET: it is measured using BET specific surface area tester.
The performance of high activity porous light calcium carbonate obtained by 1 embodiment 1-3 of table and comparative example 1-4 compares
From the data in table 1, it can be seen that using 1-3 of the embodiment of the present invention provide preparation method made from high activity porous light carbon
Oil absorption, whiteness and the BET of sour calcium are greater than comparative example 1-4, use negative pressure of vacuum low temperature calcination in preparation method of the present invention
Mode is calcined, and compared high activity porous light obtained when being calcined during the preparation process using conventional calcination method
The oil absorption of calcium carbonate, whiteness and BET value are bigger.
Claims (6)
1. a kind of method with lime stone preparation high activity porous light calcium carbonate, characterized by the following steps:
Lime stone is crushed as needed, then carries out negative pressure of vacuum low temperature calcination, stops heating after calcining 1-4h, stops simultaneously
It only vacuumizes, and conveys air or oxygen into burner hearth, obtain high activity porous CaO；
By obtained high activity porous CaO air-flow crushing to particle powder, micro mist powder, fine powder or superfine powder, then
It is placed under the conditions of enclosure space, so that the humidity of enclosure space is reached 95% using the water after ultrasonic atomization, while being passed through CO2Gas
Body carries out the flexible slow reaction 6-48h of porous CaO powder under the enclosure space reaction system, obtains porous light calcium carbonate.
2. the method according to claim 1 with lime stone preparation high activity porous light calcium carbonate, it is characterised in that: will
Lime stone is crushed to 1-5mm as needed.
3. the method according to claim 1 with lime stone preparation high activity porous light calcium carbonate, it is characterised in that: will
Obtained high activity porous CaO air-flow crushing to particle powder size is 5 μm, micro mist powder size is 1-5 μm, fine powder is big
The rank that small is 0.1-1 μm or superfine powder size is 0.02-0.1 μm.
4. the method according to claim 1 with shell preparation high activity porous light calcium carbonate, it is characterised in that: described
Calcination temperature during negative pressure of vacuum low temperature calcination is 650-750 DEG C, and vacuum degree is between -80KPa to -50KPa.
5. the method according to claim 1-4 with eggshell preparation high activity porous light calcium carbonate is prepared
High activity porous light calcium carbonate.
6. high activity porous light calcium carbonate according to claim 5, it is characterised in that: the high activity porous light carbon
The oil absorption of sour calcium is greater than 100ml/100g, and whiteness is greater than 90, BET and is greater than 15m2/g。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811639480.0A CN109368680A (en) | 2018-12-29 | 2018-12-29 | It is a kind of with lime stone prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811639480.0A CN109368680A (en) | 2018-12-29 | 2018-12-29 | It is a kind of with lime stone prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112340776A (en) * | 2020-11-06 | 2021-02-09 | 铜仁学院 | Bismuth oxycarbonate nano material and preparation method and application thereof |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
Citations (4)
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|---|---|---|---|---|
| JPS62171921A (en) * | 1986-01-24 | 1987-07-28 | Mitsubishi Heavy Ind Ltd | Production of fine light calcium carbonate |
| CN1278781A (en) * | 1997-09-08 | 2001-01-03 | Fp颜料有限公司 | Process and apparatus for preparing preoiptated calcium carbonate |
| CN1830863A (en) * | 2006-03-31 | 2006-09-13 | 河北理工大学 | Method and device of obtaining active lime by vacuum calcining limestone |
| CN101033075A (en) * | 2007-04-13 | 2007-09-12 | 安徽工业大学 | Method of preparing ultra-fine lightweight calcium carbonate |
-
2018
- 2018-12-29 CN CN201811639480.0A patent/CN109368680A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62171921A (en) * | 1986-01-24 | 1987-07-28 | Mitsubishi Heavy Ind Ltd | Production of fine light calcium carbonate |
| CN1278781A (en) * | 1997-09-08 | 2001-01-03 | Fp颜料有限公司 | Process and apparatus for preparing preoiptated calcium carbonate |
| CN1830863A (en) * | 2006-03-31 | 2006-09-13 | 河北理工大学 | Method and device of obtaining active lime by vacuum calcining limestone |
| CN101033075A (en) * | 2007-04-13 | 2007-09-12 | 安徽工业大学 | Method of preparing ultra-fine lightweight calcium carbonate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112340776A (en) * | 2020-11-06 | 2021-02-09 | 铜仁学院 | Bismuth oxycarbonate nano material and preparation method and application thereof |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
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Application publication date: 20190222 |