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Production of Precipitated Calcium Carbonate From Steel Converter Slag and Other Calcium-Containing Industrial Wastes and Residues
Production of Precipitated Calcium Carbonate From Steel Converter Slag and Other Calcium-Containing Industrial Wastes and Residues
Production of Precipitated
Calcium Carbonate from Steel
Converter Slag and Other
Calcium-Containing Industrial
Wastes and Residues
Hannu-Petteri Mattila, and Ron Zevenhoven
Thermal and Flow Engineering Laboratory, Åbo Akademi University, Turku, Finland
Contents
1. Introduction 348
2. Existing PCC Manufacturing Technologies 350
2.1 Carbonation process 350
2.2 Solvay process 353
2.3 Lime-soda process 354
2.4 Calcitech process 354
2.5 Filler recycling processes 355
3. Mineral Carbonation Processes 355
4. PCC Manufacturing Technologies Based on Industrial Waste Materials 356
4.1 Oil shale ash indirect aqueous carbonation 356
4.2 Salty water carbonation 359
4.3 Ash, dust, and concrete-based processes 360
4.4 Carbonation of gypsum waste 362
5. PCC Manufacturing Based on Steel Slag Carbonation 363
5.1 Waste streams from steelmaking processes 363
5.2 Direct versus indirect aqueous carbonation of steel converter slag 365
5.3 Leaching studies on steel slags 366
5.4 Selective extraction of calcium from steel converter slag 366
5.5 Vanadium extraction from the residual slag 370
5.6 Calcium carbonate precipitation 371
5.7 Current status of the development of the Finnish steel converter slag
carbonation process 375
6. Remarks on Applicability of Various Processes in Global Scale 378
7. Conclusions 380
Acknowledgments 380
References 381
Abstract
Precipitated calcium carbonate, a widely used filler material, is nowadays mainly pro-
duced by the so-called carbonation process. Natural limestone is first calcined and then
contacted with carbon dioxide to precipitate particles of a controlled purity, size, and
morphology. In the production process, an amount of carbon dioxide equal to or larger
than what is later bound to the actual product is released.
For climate change mitigation, it would be possible to reduce carbon dioxide
emissions by capturing CO2 from flue gases, if the required calcium could be obtained
from another source than the natural rocks. Industrial alkaline by-product and waste
streams such as slags and ashes contain calcium often in a readily soluble form. Recently,
several processes have been developed to apply these materials for carbon dioxide cap-
ture, utilization, and storage, while simultaneously producing materials with market value.
Since the chemistry of calcium carbonate precipitation is relatively complex, the levels
of impurities should be maintained low in the carbonation process. In case of utilizing a
solid waste stream, this requires efficient separation of the residual waste material from
the calcium-rich solution after extracting the soluble calcium from the solids.
Aspects related to a two-step aqueous process for steel converter slag carbonation are
discussed in more detail, since a continuous laboratory-scale setup has been constructed
and is currently under further development at Finnish universities. Even though the current
issues related to product quality can be resolved, the process is still in such a small scale that
it mainly serves the demonstration purposes for mineral carbonation technologies.
Keywords: Calcium carbonate, Carbon dioxide capture and utilization, Mineral
carbonation, Steel converter slag, Waste stream utilization
1. INTRODUCTION
Calcium carbonate (CaCO3) is a substance widely used for various
purposes, for example, as a filler and pigment material not only in paper,
plastics, rubbers, paints, and inks but also in pharmaceutics, cosmetics, con-
struction materials, and asphalts and as a nutritional supplement in animal
foods (1). Besides the so-called ground calcium carbonate (GCC), which
is milled from natural limestone, precipitated calcium carbonate (PCC) is
used in applications where, for example, higher brightness or a narrow par-
ticle size distribution is required. In PCC, manufacturing these properties
can be controlled, since unlike GCC, the product is fully synthetic (2).
Figure 10.1 shows the demand distribution between the different applica-
tions in North America, paper filler being the major use of PCC. In
2011, 14 Mt of PCC was consumed worldwide, Asia being the largest
regional market. GCC consumption reached 60 Mt in 2011, since as a
cheaper, less processed product, it has a wider area of applications. The
Production of Precipitated Calcium Carbonate from Industrial Wastes and Residues 349
144; 7 %
48; 2 %
96; 4 %
144; 7 %
Paper
Plastics
144; 7 % Rubber
Paint
Adhesives/Sealants
Others
1600; 73 %
Figure 10.1 2011 PCC consumption by end use in North America in kilotons. Data from
Ref. (2).
industrial waste streams and CO2 emissions, also bring direct economic ben-
efits for applying new PCC manufacturing routes like Slag2PCC—see
Section 5.7 (31).
Limestone
Waste gas Clean waste gas
1 3 4
Calcium hydroxide
2
7 8
Calcium oxide 5 6
Water
10
11 9
DryPCC 13 12
1. Limestone bin 2. Lime kiln 3. Gas filter 4. Gas scrubber 5. Calcium oxide bin and slaker with cooling
6. Slaked lime tank 7. and 8. Precipitation reactors 9. Prescreen tank 10. Screening for unreacted
calcium hydroxide 11. Postscreen tank 12. Filter press and dryer 13. Gas filter.
Figure 10.2 Main production stages in carbonation process for PCC making.
Reproduced from Ref. (33).
purity, however, the results indicate a need for further studies. The sulfate
content of the ash leachate resulted in calcium sulfate coprecipitation, and in
some experiments, levels as high as 5.9% CaSO4 levels were obtained (14).
The authors do not mention other impurities. Thus, the developed process
seems to have potential for production of PCC, product purification still
requiring additional process steps. Also, calcium content of the ashes is rel-
atively low (Table 10.1), which implies large mass flows of solid material in
carbonation processes.
Soong et al. (20) combined carbonation of brine solution and fly ash
(Table 10.1) in their studies. With a two-step process, they were able to
produce 90% pure PCC, with 9% sodium chloride coprecipitation. How-
ever, this result required addition of sodium hydroxide to increase the solu-
tion pH, which is recognized as a drawback by the authors. In the same
study, also the direct carbonation methods of fly ash in brine were
discussed, but even though the carbonation was performed successfully,
the highest calcium carbonate content obtained in the solid product was
only 53%.
Zevenhoven et al. (25) reported experimental results with paper bottom
ash (Table 10.1). Several elements were extracted from the material, but the
produced carbonate was 90–98.5 wt% pure calcium carbonate. The material
seems to be suitable for indirect aqueous carbonation, even though the pro-
cess requires large volumes of aqueous solutions due to a low solid-to-
liquid ratio.
Jo et al. (54) extracted calcium from lime, waste Portland cement, and
waste concrete by using water, hydrochloric acid, acetic acid, and ammo-
nium chloride solutions. They discovered that the ammonium chloride
solution was most effective in calcium extraction for all the tested materials,
although for the waste concrete the extraction efficiency was low compared
to other materials. For carbonation, only ammonium chloride solutions pre-
cipitated noticeable amounts of calcium carbonate, while almost no precip-
itates were found from the more acidic solutions. The product was found to
contain more than 95% of carbonates by TGA analysis, but the impurities
were not further discussed. Also, Iizuka et al. (28) performed experiments
with indirect carbonation of concrete sludge (Table 10.1) in water and con-
cluded that a maximum extraction of 45% was obtained after an experi-
ment of 100 min. The addition of seed crystals was also found to enhance
carbonate precipitation from the solution.
Katsuyama et al. (16) specifically aimed at production of high-purity cal-
cium carbonate precipitate by using waste cement with pressurized carbon
dioxide. A 98% pure PCC was generated, while the authors also proposed
further purification by reprecipitation in another step. In the indirect car-
bonation process concept, extraction occurs under high (up to 3.0 MPa)
CO2 pressure, which maintains an acidic pH and thus keeps the extracted
calcium dissolved. Precipitation occurs when the CO2 pressure is lowered
362 Hannu-Petteri Mattila and Ron Zevenhoven
Recycled
Pellets Oil (100 kg) steel
(350 kg) O2 (240 kg)
Air
Coking
plant Desulphur Basic
Coal oxygen Ladle
Blast ization Casting
(440 kg) furnace furnace
furnace
Sinter
plant
Iron ore
(740 kg)
Lime Steel slab
Desulphurization Ladle
kilns Steel (1000 kg)
slag (20 kg) slag (20 kg)
Limestone converter
Blast furnace slag (70 kg)
(210 kg)
slag (230 kg)
Primary phases often present in steel converter slag have been reported to
be larnite (dicalcium silicate, Ca2SiO4) and srebrodolskite (dicalcium ferrite,
Ca2Fe2O5). These compounds never exist as pure substances; instead, they
contain various amounts of, for example, phosphorus, manganese, and mag-
nesium bound to the main matrix (31,69).
Regenerated solvent
CO2
containing gas
Calcium-
rich
Slag solution Non reacted
Extraction Carbonation
gases
Residue CaCO3
Sun et al. (53) but with reaction conditions utilizing higher pressures and
temperatures compared to Teir and Eloneva.
1.0
HCO3–
0.8
H2CO3 CO32–
Fraction
0.6
0.4
0.2
0.0
4 5 6 7 8 9 10 11 12
pH
Figure 10.5 Coexistence of various forms of dissolved carbon dioxide as a function of
solution pH (76).
5.0
4.5
Ca dissolution efficiency decreases, dissolution of impurities increases
4.0
3.5
NH4Cl (mol/l)
3.0
NH4Cl in PCC product,
2.5 wash stage(s) needed
2.0
1.5
R
pH
TR
R
pH
PI PI
TR
Residue
Pi
PI PI
PCC fines
PCC
Slag
pHR pHR
TR TR
Residue
CO2
Figure 10.10 A reactor setup for production of PCC from steel converter slag according
to an indirect carbonation principle.
Figure 10.11 Photograph of the laboratory reactor setup for a continuous “slag2PCC”
process.
Production of Precipitated Calcium Carbonate from Industrial Wastes and Residues 377
inside the reactor are recorded during the experiments. The reacted, residual
slag is removed from the aqueous solution with a combination of filters, a
settler tank and a so-called inclined settler, the principle of which is more
closely described by Davis and Gecol (105). Based on earlier small-scale
experiments (31,76), a base case for the process conditions has been chosen,
from which variations are then possible based on new observations. In this
base case, 1.0 mol/L ammonium chloride solution and a 100 g/L slag-to-
liquid ratio are used, and the reactor system is operated under atmospheric
pressure and temperature.
The carbonation unit is shown on the right in Figure 10.10. The
calcium-rich and solid-free aqueous phase is divided into two reactor vessels.
In the actual carbonation reactor, gaseous carbon dioxide is introduced
through a porous sheet and thus bubbled through the calcium-containing
solution (total volume 30 L). The pH and temperature of this reactor
are also measured and recorded continuously and can be adjusted by chang-
ing both the CO2 flow rate and the aqueous stream flow rate. Precipitation is
mainly expected to occur in this vessel.
The second part of the calcium-rich stream from the extractor is fed to a
second settler tube, where it is combined with calcium-poor and carbonate-
rich stream from the carbonator while removing PCC by settling. The rea-
son for this setup is to adjust the pH and calcium content of the recycled
ammonium chloride solution in such a way that an amount of carbonate/
bicarbonate ions and dissolved CO2 that is as small as possible enters the
extraction reactor. In earlier work, the carbonation has been observed to
continue in the extraction reactor, which has led to reduction of the pure
carbonate yield, with valuable product partly mixed with unreacted and
spent slag material.
The main challenges of the technology are currently in ensuring the
desired particle size, particle size distribution, crystal shape, and purity
of the produced precipitates so that the commercial applicability of the
product will not be compromised. Factors related to particle and crystal
properties are strongly affected by residence times under different pH
conditions and at different concentration levels of calcium and carbon
species and require further experimental work to obtain the most valuable
product.
If elements other than calcium are extracted from the slag, there is a pos-
sibility for accumulation of these elements in the process solution, which,
however, has not been observed to be a problem (76). This is principally
due to the different solubilities of the various minerals, as discussed in
378 Hannu-Petteri Mattila and Ron Zevenhoven
Section 5.5 earlier, which leads to a selective extraction of calcium and sil-
icon, of which silicon is predominantly reprecipitated with the slag.
On the contrary, both the residual slag and the PCC product have been
found to contain some chlorine, originating from the ammonium chloride
solvent and thus indicating losses of the valuable solvent components. This
involves the need of additional washing steps for the solid streams compared
to the process equipment shown in Figure 10.10.
7. CONCLUSIONS
Climate change has given rise to several technologies aiming at reduction
of the anthropogenic carbon dioxide emissions. One interesting option seems
to be the CCUS (carbon capture, utilization, and storage), an option referred to
as mineral carbonation, where CO2 would be bound together preferably with
alkaline earth metals such as calcium or magnesium. The solid product, calcium
or magnesium carbonate, would provide stable storage under natural condi-
tions, thus removing the carbon dioxide from the atmosphere.
Besides natural minerals, also industrial waste materials could be utilized
as sources of the required metals. A selective separation of calcium followed
by carbonation would enable production of commercial-grade carbonate
products such as PCC. The financial benefit gained from marketing this
product could help to overcome the economical barrier connected to
implementing novel technologies on industrial scale.
Currently, research is ongoing with materials such as steel slag, oil shale
ash, brine, and gypsum. With the need of additional developments related to
product purity and other quality requirements, promising processes have
been designed, even though on a global scale, the significance of CO2 emis-
sion reduction would be quite small, requiring also implementation of other
types of measures.
ACKNOWLEDGMENTS
The Academy of Finland Graduate School in Chemical Engineering is acknowledged for
financial support for H.-P. Mattila. Sebastian Teir, Sanni Eloneva, Arshe Said, and Inga
Grigaliūnaitė as well as other (earlier) coworkers are acknowledged for their valuable
research work in development of the Finnish steel converter slag carbonation process.
Production of Precipitated Calcium Carbonate from Industrial Wastes and Residues 381
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