Construction and Building Materials 38 (2013) 8–13

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Utilization of phosphate fertilizer industry waste for belite–ferroaluminate

cement production
Lin Yang, Yun Yan ⇑, Zhihua Hu, Xiaoli Xie
State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, PR China

h i g h l i g h t s

" Phosphate fertilizer industry waste products were utilized in this work.
" Belite–ferroaluminate cement was prepared by utilizing the waste products.
" Belite–ferroaluminate cement is energy-saving cement.
" Effect of gypsum content on performances of cement were investigated.

a r t i c l e i n f o a b s t r a c t

Article history: Phosphogypsum (PG) and pyrite cinder (PC) are phosphate fertilizer industry wastes. At present, the uti-
Received 27 February 2012 lization of PG and PC is limited, their stockpiling brings about serious environmental problems. We stud-
Received in revised form 28 July 2012 ied the manufacturing technique for producing belite–ferroaluminate cement utilizing of PG and PC as
Accepted 6 August 2012
raw materials instead of natural materials. The mechanical properties, mineral composition and micro-
Available online 13 September 2012
structure of the resulting cement clinker were investigated using X-ray powder diffraction (XRD) with
Rietveld quantitative phase analysis, scanning electron microscope (SEM), etc. We found that burning
Keywords:
at 1250 °C for 60 min was suitable for clinker production. The effect of natural gypsum (NG) content
Belite–ferroaluminate cement
Hydration
on setting time, heat evolution, compressive strength, hydration products of cements were also investi-
Phosphogypsum gated. The results show that setting time of cement depends much on NG content. The early hydration
Industry waste accelerates with NG content increasing. The effect of NG content on compressive strength at different
curing age is variable. NG content in cement is also an important factor in the hydration products.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction such as H3PO4, Ca(H2PO4)2H2O, CaHPO42H2O, Ca3(PO4)2, residual

China consumes large quantity of chemical fertilizer every year,
in especial, phosphate fertilizer. Production of phosphate fertilizer
cannot be accomplished without phosphoric acid. PG is a main
byproduct of the manufacture of phosphate fertilizer using phos-
phoric acid through the wet process technique, which features dis-
solving phosphorus ore with sulfuric acid. The technology of
calcining low or medium grade pyrite for manufacturing sulfuric
acid is new in China but results in more PC than traditional tech-
nique. The recycling of PC is a challenge.
About 5 tons of PG is generated per ton of phosphoric acid pro-
duction, the average annual production of PG is exceeds 22 million
tons (MT) in China, and worldwide PG generation is estimated to
be around 100–280 MT per year [1–5]. The main composition of
PG is CaSO42H2O, at the same time, PG contains some impurities,
⇑ Corresponding author. Tel.: +86 816 2419216.
E-mail addresses: yanglin06142@163.com (L. Yang), yanyun@swust.edu.cn (Y.
Yan).
acids, fluorides (NaF, Na2SiF6, Na3AlF6, Na3FeF6 and CaF2), sulfate
ions, trace metals (e.g. Cr, Cu, Zn and Cd), and organic matter as
aliphatic compounds of carbonic acids, amines and ketones,
adhered to the surface of the gypsum crystals [6]. Globally, 15%
PG production is recycled as building materials, agricultural fertil-
izers or soil stabilization amendments and as setting controller in
the manufacture of Portland cement [4]. The rest is stored near
factories, which not only occupies large land areas but also causes
serious environmental contamination.
PC often contains Fe2O3, Fe3O4, metallic sulfate, metallic silicate,
hazardous heavy metals, etc. In China, more than 30% sulfuric acids
(18 MT) are produced from pyrites each year. Generally, to obtain
1 ton sulfuric acid, 0.7–1.0 ton PC will be generated, and produc-
tion depends on the purity of the sulfate ore and the scale of sulfu-
ric acid production plants. Therefore, the total generation of PC is
more than 10 MT per year in China, which accounts for approxi-
mately 30% by weight of chemical wastes [7]. Therefore, its com-
prehensive utilization has been a challenge for many years.
Although several new techniques for potential recycle of PC have

0950-0618/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.08.049
 L. Yang et al. / Construction and Building Materials 38 (2013) 8–13 9

been explored and reported, such as recycling of heavy metals, pro- Table 1
ducing of building materials directly and using as soil modifier, the Chemical composition of raw materials (wt.%).

recycling rate is still low [8–10]. Compositions Limestone PC PG Bauxite NG

Ordinary Portland cement (OPC) is used worldwide. The manu- CaO 53.92 2.50 26.79 0.59 36.50
facture process emits large amounts of CO2 principally due to the SiO2 0.22 31.84 14.50 25.47 2.30
high calcite (CaCO3) content of the raw mix. Moreover, vast Al2O3 0.30 27.86 0.74 55.32 0.30
amounts of energy are consumed for grinding of the raw mixtures Fe2O3 0.06 29.80 0.12 0.95 0.18
SO3 0.69 1.73 37.25 – 51.24
and clinker calcination. The combined decarbonation, thermal, and MgO 0.89 0.02 0.09 0.54 3.73
electrical-power CO2 emissions may total as much as 0.97 tons of TiO2 0.02 1.62 0.08 1.58 0.06
CO2 per average ton of Portland cement produced. Thus, the ce- P2O5 – 0.17 5.06 – –
ment industry contributes around 6% of all CO2 anthropogenic R2O – 0.10 0.34 0.24 0.41
F – – 0.21 – –
emissions [11]. Belite–ferroaluminate cement (BFAC) is a special
cement, the main mineral phases are C2S, C4 A3s, and C4AF (stand Loss on ignition 42.67 4.26 18.73 14.86 4.80
Total amount 98.77 99.9 103.91 99.55 99.52
for ferrite phase). Among which, C2S content of BFAC is much high-
er than OPC, so BFAC is regarded as belite-rich cement, which has
several advantages over OPC [12–14]:
Table 2
 Calcium demand of BFAC is less than OPC, therefore, the volume Estimated mineral and chemical compositions (wt.%).
of limestone in raw materials mix can be reduced that reduces
Mineral compositions Chemical compositions
the total CO2 emissions from manufacturing.
C2S C4 A3 s C4AF CaO SiO2 Al2O3 Fe2O3 SO3
 The burning temperature of BFAC is about 1250–1350 °C and
lower 100–150°C than OPC. In addition, BFAC clinker is porous, 45 35 20 51.40 15.70 21.74 6.57 4.59
which can be ground more easily than OPC clinker. Thus, the
energy consumption of BFAC is less than its competitor. Cements were obtained by grinding the clinker and NG at definite proportions.
 Early strength and rapid hardening are the outstanding features The mix proportions and ground fineness (specific surface area) are shown in Table
3.
of BFAC. Utilization of BFAC in engineering can shorten con-
struction schedule, accelerate the turnover of building tem-
2.3. Performance test
plates and reduce the number of templates, besides, it can be
used for emergency repairing. 2.3.1. Preparation of test specimens
 BFAC has excellent frost-resistance, anti-permeability, wear- Cement paste specimens were prepared with W/C = 0.3, and the size was
resistance, and adjustability of expansibleness. Concrete mixed 20 mm  20 mm  20 mm. Mortar specimens with the size 40 mm  40 mm 
160 mm were made with W/C = 0.42, cement/sand = 1/3. All the specimens above
with BFAC will not turn up sand on the surface and corrode steel
were cured at (20 ± 1) °C, relative humidity exceeding 90% for four hours before
but also owns outstanding anti-seawater intrusion ability. immersing them in water (20 ± 1 °C). The specimens used for XRD and SEM were
collected from the middle sections of the paste specimens.
However, natural raw materials used for belite–ferroaluminate
cement manufacture, e.g., laterite and NG, are costly. Therefore, the 2.3.2. Test methods
price of belite–ferroaluminate cement is high, which limits its Specific surface area of cements was measured by the Blaine method in accor-
widespread use. In this paper, phosphate fertilizer industry waste dance with Chinese standard (GB/T8074-2008) [15]. Water requirement of normal
consistency and setting time were tested in line with Chinese standard (GB/T1346-
products, PG and PC, were used as raw materials for preparation 2001) [16]. Compressive strength were tested by Method of testing cements—deter-
of belite–ferroaluminate cement. PC, as substitute for natural later- mination of strength (ISO)(GB/T17671-1999)[17]. Mineral phases were studied by
ite, not only offers iron source but also supplies silicon and alumi- powder XRD technique (X’Pert PRO, copper target), and microstructures were stud-
num. PG is used for supplying sulfur source and reducing burning ied by SEM (Leica Stereoscan 440). The quantitative analysis of minerals was ana-
lyzed with XRD on a Bruker Theta–Theta D8 Advance X-ray diffractometer
temperature. In this way, it not only consumes a great deal of
(voltage 40 KV, electric current 40 mA, copper target), Rietveld refinement per-
waste products but also offers a special cementitious material. formed with TOPAS software. The heat evolution was tested by TAM Air Isothermal
Calorimeter. Mixed cement with water at the ratio of 0.6 outside the apparatus.
2. Materials and methods After putting the mixture into the apparatus immediately, a test of the heat evolu-
tion occurred. The radioactivity of clinker was tested by the Low Background Multi-
2.1. Raw materials channel Gamma-Ray Spectrometry (voltage 82 V).

PC and PG were obtained from phosphate fertilizer plant in Yun Nan, China.
Natural limestone, bauxite, and NG were gained from the market in Sichuan, China.
3. Results and discussions
Chemical compositions of raw materials, which were analyzed by the chemical
method, are shown in Table 1. All the raw materials were dried first and then 3.1. Confirmation of burning conditions
ground to less than 80 lm separately.
XRD patterns of clinkers burned at different temperature for
2.2. Preparations of clinker and cement
40 min are shown in Fig. 1. The main minerals are C4 A3s, C2S,
In this study, backward pass computation was adopted for the proportion of
and C2AxF1x when burning temperature range from 1200 °C to
raw materials. Chemical compositions of BFAC clinker were gained from mineral 1330 °C, among which, C2AxF1x represent ferrite phase solid
compositions, and mixture calculation made based on the chemical compositions.
Depending on raw materials, the estimated mineral and chemical compositions Table 3
are shown in Table 2, the mix proportion of limestone, PC, PG, bauxite are 59.2%, Mix proportions and fineness of cements.
14.7%, 7.6% and 18.4%, respectively. Mix proportion (wt.%) Specific surface area (m2/kg)
Used were the following procedures to obtain cement clinkers. Weighed all raw
materials and mixed in a blender without water for 1 min. Next, added water in No. Clinker NG
accordance with water/solid = 0.18 and mixed again for 2 min. A pug ball of about 1 100 0 520 ± 10
15 mm in diameter was made and dried in a oven. Finally, burned the dry balls in 2 95 5
muffle furnace at predetermined temperature for a suitable duration of time, and 3 90 10
immediately cooled the calcined product to room temperature with a fan. So, ce- 4 85 15
ment clinkers were gained.
10 L. Yang et al. / Construction and Building Materials 38 (2013) 8–13

solution. As shown in Fig. 1, which reflects that 1200 °C is insuffi- 45

cient for burning the clinkers because of the weak intensity of the
diffraction peaks of C4 A3s and C2S and the existence of interim
product (2C2SCaSO4). Effect of burning temperature on compres-

Compressive strength (MPa)

sive strength is shown in Fig. 2, the paste specimens were cured 40

in water (20 ± 1 °C) for 3 days. The compressive strength goes up

with burning temperature increasing (for same duration of time:
40 min). However, there is no significant increase when the burn-
35
ing temperature is P1250 °C. When burning temperature is
1250 °C, effect of burning time on compressive strength is shown
in Fig. 3, the compressive strength of paste specimens that were
cured in water (20 ± 1 °C) for 3 days increases with burning time 30
prolonging.
Based on the above, 1250 °C/60 min were selected typically as
calcining regimen for making belite–ferroaluminate cement clink-
ers, even though this is not the best condition. Microstructures of 25
1200 1220 1240 1260 1280 1300 1320 1340
the clinker burned at 1250 °C for 60 min are shown in Fig. 4. The
o
clinker is loosened and porous; well crystallized cobblestone-like Burning temperature ( C)
C2S and polylateral C4 A3s are interweaved together by ferro phase.
Fig. 2. Effect of burning temperature on compressive strength.
As a mass of waste materials were used for manufacturing of clin-
ker, the radioactivity of clinker was tested. Table 4 shows the test
result of radioactivity, which meets the requirement of limits of 60
radionuclides in building materials (GB6566-2010) [18].
To contrast the effect of PG on burnability of clinker with NG, PG 55
was replaced unequally by NG, but it ensures the mineral compo-
sitions and chemical compositions invariant. Compressive strength
Compressive strength (MPa)

50
comparison of P–C and N–C is shown in Fig. 5, P–C represents the
clinker made of PG, and N–C represents the clinker made of NG. All 45
the paste specimens were cured in water (20 ± 1 °C) for 3 days. Un-
til the burning temperature comes up to 1300 °C, the compressive 40
strength of N–C cannot match the P–C burned at 1250 °C for the
same burning time. PG can reduce the burning temperature of clin- 35
ker in contrast with NG, because of PG contains a small amount of
fluorides that forms compound mineralizer with sulfate. Mineral 30
compositions of clinker made of PG or NG are shown in Table 5.
As shown in the table, there exist a small amount of C3S that was 25

not estimated in raw materials mixing. The silicate minerals (C3S

and C2S) amount of P–C is more than N–C. This may explain the 20
40 60 80 100 120
compressive strength of P–C burned at 1250 °C is higher than
Burning time (min)
N–C burned below 1300 °C.
Fig. 3. Effect of burning time on compressive strength.

3.2. Effect of NG content on setting time

depends much on NG content variation from 0% to 15%. Initial set-
The effect of NG content on setting time of BFAC is shown in ting time and final setting time of BFAC without NG are 150 min
Fig. 6. The setting time of BFAC, either initial setting or final setting, and 185 min, respectively. The initial and final setting time are
shortened when the cement contains 5% NG. However, the initial
Ca4Al6O12SO4 C2S and final setting time increase slightly with NG content increasing
● ● C2AxF1-x 2C2S ●
CaSO4 from 5% to 15%. The reason may be that 5% NG promotes the for-
●
mation of AFt, shortening the setting time. Nevertheless, a mass
of AFt cover the cement particle surface resulting to delay their fur-
ther hydration when NG content increases from 5% to 15%. The fi-
nal setting time of cements with NG content 5%, 10% and 15% are
all less than 25 min, which is much shorter than OPC and rapid set-
ting feature has been provided.

3.3. Effect of NG content on heat evolution in early hydration process

of BFAC

The heat evolutions of BFAC with different NG content are

shown in Figs. 7 and 8. As shown in Fig. 7A, the rate of heat evolu-
tion and the maximum rate of heat evolution of cement during the
5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 first hour depend on the NG content in cement. The cement with-
2-Theta (degree)
out NG reaches its maximum rate of heat evolution about 30 min
after the start of cement hydration. The peak of hydration heat evo-
Fig. 1. XRD patterns of clinkers burned at different temperature for 40 min. lution rate of cement with 5% NG appears much earlier than others.
 L. Yang et al. / Construction and Building Materials 38 (2013) 8–13 11

Fig. 4. Microstructures of the clinker burned at 1250 °C for 60 min. (a) 500, (b) 15,000.

Table 4
The radioactivity of clinker.

No. Nuclide Total counts Specific activity (Bq/kg) Rate (%) Uncertainty (%)
1 Th232 9379c 90.26 7.53 9.94
2 Ra226 6107c 67.26 5.61 13.72
3 K40 3956c 1040.51 86.85 15.18

Internal exposure index IRa = 0.336(±14.05%). External exposure index Ir = 0.777(±7.53%).

50
P-C 190
45 N-C
180
Initial setting
40
Compressive strength (MPa)

Final setting
170
35
Setting time (min)

160
30
150
25

20
30
15
20
10

5 10

0 0
1250 1250 1280 1300 0 5 10 15

Gypsum content (wt%)

Fig. 5. Compressive strength comparison of P–C and N–C.
Fig. 6. Effect of NG content on setting time.

Table 5
Mineral compositions of clinker (wt.%).
The cement with 10% NG has another normalized heat flow peak
Burning condition (°C/60 min) Mineral composition that is more exceptional than others. There are two shoulders in
C3S C2S C4 A3s C2AxF1x normalized heat flow curve when cement contains 5% NG, as the
P–C 1250 2.55 42.34 37.31 17.15
NG content is insufficient for C4 A3s hydration to form AFt and it
1250 1.13 39.63 37.72 16.24 transforms to AFm phase.
N–C 1280 1.27 40.58 35.42 19.51 Hydration heat evolution of cements with different NG content
1300 1.69 39.11 35.83 20.67 is shown in Fig. 8. The normalized hydration heat decreases with
NG content increasing from 0% to 15% due to the reduction of rel-
ative mineral content of cement.

The normalized heat flow curves of cements with 10%, 15% NG are
nearly the same from 20 min to 28 min with heat flows
decreasing gradually. Both of the cements with 10%, 15% NG have
similar hydration process in the first 1 hour. With NG content
increasing, the first normalized heat flow peak increases. The more
NG cement contains, the faster it hydrates in the early hydration
stage. Normalized hydration heat flow peak appears earlier with
NG content increasing and the heat evolution curves coincide after
48 h, which are shown in Fig. 7B. Only the cement without NG has
an induction period in the hydration process, as shown in Fig. 7B.
3.4. Effect of NG content on compressive strength
Effect of NG content on compressive strength of BFAC is shown
in Fig. 9. The compressive strength of cement with 5% NG is lowest
when the specimens were cured in water for 1 day and 3 days, yet
it increases with the NG content changes from 5% to 15%. The com-
pressive strength of cements with NG from 0% to 15% has the same
tendency at 28 days, 56 days. The peaks are achieved for cement
containing 5% NG, which are opposite to the strength of 1 day
12 L. Yang et al. / Construction and Building Materials 38 (2013) 8–13

60
1d
3d
55 28d

Compressive strength (MPa)

56d
50

45

40

35

30

25
0 5 10 15
Gypsum content (wt%)

Fig. 9. Effect of NG content on compressive strength.

1 2
1 1 AFt 3 Yeelimite
1
13 12 2 C2S 4 AFm-14
1 1 1 12
1 1 2 1 2 2 2 3 212 2
2 15%

10%

Fig. 7. Hydration heat evolution rate of cements with different NG content.

5%

4
4 0%

10 20 30 40 50 60 70 80
2-Theta (degree)
(a) 1day

1 2
1 1 AFt 2 C2S 3 Yeelimite
1 4 Stratlingite 5 AFm-14
13 1
1 2 12
1 11 1
2 2 2 3 212
15%

Fig. 8. Hydration heat evolution of cements with different NG content.

10%
and 3 days. Increasing NG content increases compressive strength
in early curing periods (i.e. 1 day and 3 days), but the compressive
strength of cement with 5% NG is lower than cement without NG.
The 5% NG may make the cement set too quickly and hinder early 5%
hydration. The compressive strength increasing rate from 1 day to
56 days with increases in NG is also shown in Fig. 9. The strength 5
4 2 2
increases with 10% NG is small, but the cement comprising 5% 4 0%
NG is noticeable.
10 20 30 40 50 60 70 80
2-Theta (degree)
3.5. Hydration of cements with different NG content
(b) 28days
XRD patterns of cements with different NG content hydrated for Fig. 10. XRD patterns of cements with different NG content hydrated for 1 day,
1 day, 28 days are shown in Fig. 10. The mineral phases of cements 28 days.
hydrated for 1 day, 28 days are mainly unhydrated C2S, C4 A3s, and
new formed AFt (ettringite, C3 A  3Cs  32H) (Eq. (1) and (6)). C–S–H peaks of AFt increases for cements hydrated at 1 day or 28 days.
cannot be found in the XRD patterns existing in a non-crystalline or Illustrating the volume of AFt is increasing as the tests were done
amorphous state. With the increase of NG content, the diffraction at same conditions. AFm-14 ðC3 A  Cs  14HÞ can be found in the
 L. Yang et al. / Construction and Building Materials 38 (2013) 8–13
hydration products of cements containing 0%, 5% NG hydrated for
1 day, the reactions are Eqs. (2), (3), (5), and (7). When the cement
without NG hydrated for 28 days, stratlingite (C2AS8H) appeared
due to the reaction of Eq. (5). The main hydration reactions are
summarized as follows [11,19–21]:
In the presence of NG,
C4 A3s þ 2CsH2 þ 36H ! C3 A  3Cs  32H þ 2AH3 ðgelÞ
In the absence of NG or NG is lacking,
C4 A3s þ 20H ! C3 A  Cs  14H þ 2AH3
2C4 A3s þ C3 A  3Cs  32H þ 22H ! 3ðC3 A  Cs  14HÞ þ 4AH3
The hydration of C2S,
C2 S þ xH ! C—S—H þ CH
C4 A3s þ 2C2 S þ 23H ! C3 A  Cs  14H þ C2 AS  8H þ AH3
In the presence of CH,
AH3 þ 3CH þ 3CsH2 þ 20H ! C3 A  3Cs  32H
or
AH3 þ 3CH þ CsH2 þ 20H ! C3 A  Cs  14H
AFm does not only exist as AFm-14, yet had been detected by
XRD at 28 days, then AFm-14 was used as representative for
AFm. The hydration of ferro phase is same as C4 A3s.
4. Conclusions
1. For this investigation of phosphate fertilizer industry waste
products, PG and PC were used as raw materials for manufac-
ture of belite–ferroaluminate cement clinker. Using XRD, SEM
and mechanical strength, 1250 °C/60 min is suitable for burning
the clinker.
2. NG content influences setting time. The final setting time of
cement without NG is over 3 h comparing to less than 25 min
with 5%–15% NG content. The effect of NG content on compres-
sive strength differs with curing age. The compressive strength
increasing rate of cement with 10% NG is small, but the cement
comprising 5% NG is notable.
3. The hydration products are also affected by NG content.
Unhydrated C2S, C4 A3s, and new formed AFt are the main
mineral phases of cements with different NG content
hydrated for 1 day, 28 days, C–S–H cannot be found in XRD
patterns. AFm-14 can be found in the hydration products of
cements containing 0%, 5% NG hydrated for 1 day and stra-
tlingite appears when the cement without NG hydrated for
28 days.
4. However, more work for researching on belite–ferroaluminate
cement must be done in the future, such as the relationship
between the mineral phase and heat release, effect of NG con-
tent on the expansibleness, and so on.
13
Acknowledgments
The authors want to acknowledge the financial support of the
National High-tech. R&D Program (863program) (2011AA06A106)
of China and Postgraduate Innovation Fund sponsored by South-
west University of Science and Technology, China, and thank the
administrators of the fund for their support in our research. The
ð1Þ
authors also thank English Editor Michael D. Wiltfong, MBA, CPA.
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