CN109516488A - It is a kind of to prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained with shell - Google Patents
It is a kind of to prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained with shell Download PDFInfo
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- CN109516488A CN109516488A CN201811638695.0A CN201811638695A CN109516488A CN 109516488 A CN109516488 A CN 109516488A CN 201811638695 A CN201811638695 A CN 201811638695A CN 109516488 A CN109516488 A CN 109516488A
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- shell
- calcium carbonate
- light calcium
- porous light
- porous
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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
- 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
- C01F11/02—Oxides or hydroxides
- C01F11/04—Oxides or hydroxides by thermal decomposition
- C01F11/06—Oxides or hydroxides by thermal decomposition of carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to shell recycling fields, it is related to a kind of method for preparing porous light calcium carbonate with shell, it solves and continues to use the technical problem that conventional limestone firing CaO method hardly results in active porous precipitated calcium carbonate powder, negative pressure of vacuum low temperature calcination is carried out by the conch meal for being crushed the shell after progress overpickling, alkali cleaning, obtains high activity porous CaO powder；Then obtained high activity porous CaO powder is kept under the conditions of enclosure space to humidity while being passed through CO2Gas carries out high activity porous light calcium carbonate slow reaction, and high activity porous light calcium carbonate is made.It is improved using the performances such as activity degree, whiteness, tap density and BET of high activity porous light calcium carbonate made from preparation method of the invention, whiteness is greater than 80, and tap density is less than 4.5g/cm3, BET is greater than 20m2/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 shell recycling fields, are related to a kind of method and institute that porous light calcium carbonate is prepared with shell
Obtain porous precipitated calcium carbonate.
Background technique
Precipitated calcium carbonate is a kind of inorganic filler that purposes is extremely wide, and the output of current whole nation precipitated calcium carbonate is
Reach 400,000 tons/year.With the rapid development of the national economy, its demand still locates ascendant trend.In terms of national market, lightweight carbon
Still in the state that supply falls short of demand, the demand of precipitated calcium carbonate required for especially some special quality materials is even more sour calcium
It is growing.95% main component of shell is calcium carbonate, and there are also a small amount of amino acid and polysaccharide materials.Shell prepares lightweight carbon
Sour calcium is new one of the application of conch meal, and natural environmental protection is its most important advantage.
But in the prior art, existing shell mainly prepares powdered whiting during preparing calcium carbonate, for
The research for being prepared into precipitated calcium carbonate is less.In addition, traditional lightweight Paris white is largely to fire CaO by lime stone, by it
It is placed in water, adds CO2Gas reaction obtains lightweight carbonate chemical product.Also useful shell fires calcium oxide, and method continues to use tradition
Lime stone fires CaO method, hardly results in active porous precipitated calcium carbonate powder；And CaO method is fired using conventional limestone
The whiteness of obtained precipitated calcium carbonate, tap density and BET performance are relatively poor；In addition, tradition firing CaO method obtains at present
Old-fashioned kiln during the precipitated calcium carbonate arrived is substituted, and using new-type burner hearth generally using burn electricity by the way of into
Row calcining, and calcined using this kind of mode, temperature needs to reach 1000 DEG C or more just can be with cost is too high.Therefore, ability
Field technique personnel are badly in need of making further linguistic term to the preparation method of active porous precipitated calcium carbonate.
Summary of the invention
Precipitated calcium carbonate method is prepared with shell the present invention provides a kind of, solves and continues to use conventional limestone firing CaO
Method hardly results in the technical problem of active porous precipitated calcium carbonate powder.
In order to achieve the above object, the present invention provides a kind of methods for preparing porous light calcium carbonate with shell, including
Following steps:
It after shell is carried out alkali cleaning and pickling, is crushed as needed, obtained conch meal is subjected to negative pressure of vacuum low temperature
Calcining, under the conditions of certain temperature calcine 2-8h after stop heating, be simultaneously stopped and vacuumize, and into burner hearth convey air or
Oxygen obtains porous CaO powder；
Under the conditions of obtained porous CaO powder is placed in enclosure space, enclosure space is made using the water after ultrasonic atomization
Humidity reaches 95%, while being passed through CO2Gas, the flexibility that porous CaO powder is carried out under the enclosure space reaction system are anti-at a slow speed
6-48h is answered, porous light calcium carbonate is obtained.
Further, the alkaline cleaning procedure is as follows: weight ratio is weighed as the shell and alkali of 100:(1-3), is dissolved in water, shellfish
The weight ratio of shell and water be 1:(2-4), heating boiling destroyed to the phosphorous film of shell inner wall after, shell is cleaned, carry out from
Heart dehydration, drying.
Further, the alkali in the alkaline cleaning procedure is KOH or NaOH；Preferably KOH.
Further, the acid cleaning process is as follows: the shell of alkali cleaning being put into acid solution, the weight of shell and acid solution
Amount is than being 1:(1.5-2), after stirring is got rid of to shell outer wall impurity, shell is cleaned, carries out centrifugal dehydration, drying.
Further, the acid in the acid cleaning process be mass concentration be 1%-5% HCl solution, mass concentration be
The H of 1%-5%2SO4Or mass concentration is the HNO of 1%-5%3Solution；Preferably mass concentration be 1%-5% HCl solution.
Further, the shell after progress overpickling and alkali cleaning is crushed to 0.1-0.5 μm as needed.
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 whiteness for the porous light calcium carbonate that the above-mentioned method for preparing porous light calcium carbonate with shell is prepared is greater than
80, tap density is less than 4.5g/cm3, BET is greater than 20m2/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 shell, 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 the activity degree of high activity porous light calcium carbonate made from preparation method of the invention, whiteness, vibration density
The opposite performance for using conventional limestone to fire the precipitated calcium carbonate that CaO method obtains of the performances such as degree and BET is improved, this
The whiteness of invention more empty precipitated calcium carbonates obtained is greater than 80, and tap density is less than 4.5g/cm3, BET is greater than 20m2/g。
Detailed description of the invention
Fig. 1 is high activity porous light calcium carbonate powder XRD diagram produced by the present invention.
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.
The embodiment of the invention provides a kind of methods for preparing porous light calcium carbonate with shell, include the following steps:
S1: after shell is carried out alkali cleaning and pickling, being crushed as needed, and it is low that obtained conch meal is carried out negative pressure of vacuum
Temperature calcining stops heating after calcining 2-8h under the conditions of certain temperature, is simultaneously stopped and vacuumizes, and convey air into burner hearth
Or oxygen, obtain porous CaO powder；
In above-mentioned steps, due to CO2Partial pressure can seriously affect CaCO in conch meal3Resolve into CaO and CO2, the present invention
In the step for the preparation method that embodiment provides, carrys out calcined shell powder using negative pressure of vacuum low temperature calcination method, utilize negative pressure
Technology accelerates the CO of thermal decomposition2Separation discharge, be more advantageous to obtained high activity porous CaO powder, and defeated into burner hearth
During sending air or oxygen, the air or oxygen of conveying is appropriate, is preferred with that will not blow afloat powder, can use waste heat for shellfish
Carbon exhaustive oxidation in shell, increases whiteness；The present invention uses negative pressure of vacuum low temperature calcination method simultaneously, has also achieved energy-efficient technology
Effect.
S2: under the conditions of obtained porous CaO powder is placed in enclosure space, enclosure space is made using the water after ultrasonic atomization
Humidity reach 95%, while being passed through CO2Gas carries out the flexibility of porous CaO powder at a slow speed under the enclosure space reaction system
6-48h is reacted, porous light calcium carbonate is obtained.
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 light
The porosity of matter calcium carbonate powder；
In an alternative embodiment, the alkaline cleaning procedure is as follows: weighing weight ratio as the shell and alkali of 100:(1-3), adds
The weight ratio of water dissolution, shell and water is 1:(2-4), after heating boiling is destroyed to the phosphorous film of shell inner wall, shell is washed
Only, centrifugal dehydration, drying are carried out；Alkali in the alkaline cleaning procedure is KOH or NaOH, preferably KOH.The present embodiment uses KOH
Equal alkali destroy the phosphorous high film of shell inner wall, have achieved the effect that dephosphorization.
In an alternative embodiment, the acid cleaning process is as follows: the shell of alkali cleaning being put into acid solution, shell and acid
The weight ratio of solution is 1:(1.5-2), after stirring is got rid of to shell outer wall impurity, shell is cleaned, centrifugal dehydration is carried out, does
It is dry；Acid in the acid cleaning process be mass concentration be 1%-5% HCl solution, mass concentration be 1%-5% H2SO4Or matter
Measure the HNO that concentration is 1%-5%3Solution, preferably mass concentration are the HCl of 1%-5%.The present embodiment will using HCl solution
The impurity such as shell outer wall iron content destroy, and have achieved the effect that removing impurities.
In an alternative embodiment, the shell after progress overpickling and alkali cleaning is crushed to 0.1-0.5 μm as needed.This reality
It applies when shell being crushed to 0.1-0.5 μm in example, it is easier to the abundant progress of subsequent reactions, in negative pressure of vacuum low temperature calcination process
In, conch meal can contact more abundant with air or oxygen.
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 670 DEG C, 700 DEG C, 740 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.
As seen from Figure 1, it in an alternative embodiment of the present invention, is made using preparation method provided in this embodiment
Porous light calcium carbonate product.It is greater than 80 using the whiteness of precipitated calcium carbonate made from preparation method provided in this embodiment, vibration
Real density is less than 4.5g/cm3, BET is greater than 20m2/ g, performance are more excellent.
The side for preparing porous light calcium carbonate provided by the embodiment of the present invention with shell is introduced in detail in order to become apparent from
Method is described below in conjunction with specific embodiment.
Embodiment 1
A method of porous light calcium carbonate being prepared with shell, is included the following steps:
The shell and KOH that weight ratio is 50:1 are weighed, is dissolved in water, the weight ratio of shell and water is 1:3, and heating boiling is extremely
After the phosphorous film of shell inner wall destroys, shell is cleaned, carries out centrifugal dehydration, it is dry；
Then the shell of alkali cleaning is put into the HCl solution that mass concentration is 1%-5%, shell is with mass concentration
The weight ratio of the HCl solution of 1%-5% be 1:1.8, stirring got rid of to shell outer wall impurity after, shell is cleaned, carry out from
Heart dehydration, is then dried；
Shell after alkali cleaning and pickling is carried out as needed after being crushed to 0.3 μm, 700 DEG C of calcination temperatures and-
Negative pressure of vacuum low temperature calcination is carried out under conditions of the vacuum degree of 70KPa, is stopped heating after calcining 6h, is simultaneously stopped and vacuumizes, and
And air or oxygen is conveyed into burner hearth, obtain high activity porous CaO powder；
Under the conditions of obtained porous CaO powder is placed in enclosure space, enclosure space is made using the water after ultrasonic atomization
Humidity reaches 95%, while being passed through CO2Gas, the flexibility that porous CaO powder is carried out under the enclosure space reaction system are anti-at a slow speed
6-48h is answered, porous light calcium carbonate is obtained.
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 -55KPa, 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 -60KPa, and calcination temperature is 800 DEG C.
Performance test
Precipitated calcium carbonate obtained by above-described embodiment 1-3 and comparative example 1-3 is tested for the property, test method is as follows, knot
Fruit is shown in Table 1.
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.
Tap density: it is tested using HY-100 type powder tapping density tester.
BET: it is measured using the BET specific surface area tester of model JW-BK122W.
The performance of precipitated calcium carbonate obtained by 1 embodiment 1-3 of table and comparative example 1-3 compares
From the data in table 1, it can be seen that the performance of precipitated calcium carbonate made from embodiment 1-3 is better than comparative example 1-3, illustrate only to exist
The whiteness, tap density and BET performance of precipitated calcium carbonate obtained are more excellent under the conditions of method provided by the invention.
Claims (9)
1. a kind of method for preparing porous light calcium carbonate using shell, characterized by the following steps:
It after shell is carried out alkali cleaning and pickling, is crushed as needed, obtained conch meal is subjected to negative pressure of vacuum low temperature calcination,
Stop heating after calcining 2-8h at a certain temperature, is simultaneously stopped and vacuumizes, and convey air or oxygen into burner hearth, obtain
Porous CaO powder；
Under the conditions of obtained porous CaO powder is placed in enclosure space, the humidity of enclosure space is made using the water after ultrasonic atomization
Reach 95%, while being passed through CO2Gas carries out the flexible slow reaction 6- of porous CaO powder under the enclosure space reaction system
48h obtains porous light calcium carbonate.
2. the method according to claim 1 for preparing porous light calcium carbonate with shell, it is characterised in that: alkaline cleaning procedure is such as
Under: weigh weight ratio as the shell and alkali of 100:(1-3), be dissolved in water, the weight ratio of shell and water is 1:(2-4), heating is steamed
It boils to the phosphorous film of shell inner wall after destroying, shell is cleaned, carry out centrifugal dehydration, drying.
3. the method according to claim 2 for preparing porous light calcium carbonate with shell, it is characterised in that: the alkali cleaning
Alkali in journey is KOH or NaOH.
4. the method according to claim 1 for preparing porous light calcium carbonate with shell, it is characterised in that: acid cleaning process is such as
Under: the shell of alkali cleaning is put into acid solution, the weight ratio of shell and acid solution is 1:(1.5-2), stirring to shell outer wall
After impurity is got rid of, shell is cleaned, carries out centrifugal dehydration, drying.
5. the method according to claim 4 for preparing porous light calcium carbonate with shell, it is characterised in that: the pickling
Acid in journey be mass concentration be 1%-5% HCl solution, mass concentration be 1%-5% H2SO4Or mass concentration is 1%-
5% HNO3Solution.
6. the method according to claim 1 for preparing porous light calcium carbonate with shell, it is characterised in that: peracid will be carried out
It washes and is crushed to 0.1-0.5 μm as needed with the shell after alkali cleaning.
7. the method according to claim 1 for preparing porous light calcium carbonate with shell, it is characterised in that: the vacuum is negative
Forcing down the calcination temperature in warm calcination process is 650-750 DEG C, and vacuum degree is between -80KPa to -50KPa.
8. the method according to claim 1-7 for preparing porous light calcium carbonate with shell is prepared porous
Precipitated calcium carbonate.
9. porous light calcium carbonate according to claim 8, it is characterised in that: the whiteness of the porous light calcium carbonate is big
In 80, tap density is less than 4.5g/cm3, BET is greater than 20m2/g。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811638695.0A CN109516488A (en) | 2018-12-29 | 2018-12-29 | It is a kind of to prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained with shell |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811638695.0A CN109516488A (en) | 2018-12-29 | 2018-12-29 | It is a kind of to prepare precipitated calcium carbonate method and its precipitated calcium carbonate obtained with shell |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229560A (en) * | 2019-06-14 | 2019-09-13 | 岭南师范学院 | A kind of preparation method that nontoxic dustless shell chalk being made using waste shell |
| CN112480715A (en) * | 2020-12-08 | 2021-03-12 | 深圳市锦昊辉实业发展有限公司 | Modified heavy calcium carbonate and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN203173991U (en) * | 2013-04-02 | 2013-09-04 | 周战利 | Sealed-tank quicklime slaker |
| CN206244653U (en) * | 2016-10-28 | 2017-06-13 | 广东贝尤安新材料科技有限公司 | A kind of white lime production equipment for preparing shell powder paint |
-
2018
- 2018-12-29 CN CN201811638695.0A patent/CN109516488A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN203173991U (en) * | 2013-04-02 | 2013-09-04 | 周战利 | Sealed-tank quicklime slaker |
| CN206244653U (en) * | 2016-10-28 | 2017-06-13 | 广东贝尤安新材料科技有限公司 | A kind of white lime production equipment for preparing shell powder paint |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229560A (en) * | 2019-06-14 | 2019-09-13 | 岭南师范学院 | A kind of preparation method that nontoxic dustless shell chalk being made using waste shell |
| CN112480715A (en) * | 2020-12-08 | 2021-03-12 | 深圳市锦昊辉实业发展有限公司 | Modified heavy calcium carbonate and preparation method and application thereof |
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