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Page 1: Preparation of Portland cement with sugar filter mud as lime-based raw material

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Journal of Cleaner Production 66 (2014) 107e112

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Journal of Cleaner Production

journal homepage: www.elsevier .com/locate/ jc lepro

Preparation of Portland cement with sugar filter mud as lime-basedraw material

Haoxin Li a,*, Wei Xu b, Xiaojie Yang a,*, Jianguo Wu a

aKey Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, Shanghai 201804, PR Chinab State Key Laboratory of Pollution Control and Resource Reuse, Tongji University, Shanghai 200092, PR China

a r t i c l e i n f o

Article history:Received 22 April 2013Received in revised form30 October 2013Accepted 2 November 2013Available online 9 November 2013

Keywords:BurnabilityLiquid phaseMineral phasePhysical performanceHydration characteristic

* Corresponding authors. Fax: þ86 21 69584723.E-mail addresses: [email protected] (H. Li

(X. Yang).

0959-6526/$ e see front matter � 2013 Elsevier Ltd.http://dx.doi.org/10.1016/j.jclepro.2013.11.003

a b s t r a c t

The objective of this study was to assess the preparation of Portland cement with sugar filter mud (FM)as lime-based raw material. Burnability of raw mix, SEM characteristic and phase component of clinker,compressive strength, setting time and hydration characteristic of cement are investigated. The resultsshow that FM can improve the raw mix burnability, and increase liquid phase amount. Less than 20% FMis helpful to promote the C3S formation, and heighten the C3S content in clinker. More than 20% FM willresult in the new phase formation. Compressive strength, setting time and hydration characteristic ofcement all are related to the replacement ratio of limestone with FM. It is found that the proper FMamount can raise the compressive strength, cut down the setting time, and promote the cement hy-dration in the initial and acceleration period. Excessive FM will lead to the decrease of compressivestrength, the delay of setting time and prolongation of cement hydration.

� 2013 Elsevier Ltd. All rights reserved.

1. Introduction

Solid waste (SW) is generated in the industrial production ac-tivities such as manufacturing, energy production, water supply,chemical engineering and food processing et al., and it generally isassociated with hazardous constituents such as toxic heavy metal,bacteria and harmful organic substance et al., and has a high publichealth and environmental risk. But if it is disposed with thereasonable technology or approach, it may be changed valuablematerial or fuel. Public health and environment will be preventedfrom its potential threat. The appropriate disposal method for SWconsequently has been the expectance, which the enterprise,researcher and government have given their great efforts to makecome true.

Sugar filter mud (FM) is produced after sugar juice clarified, andis the main solid waste in sugar industry. Its safe disposal alwayshas been the hot topic for random stacking occupies land andpollutes the air, landfill pollutes the underground water. Althoughit is fairly rich in inorganic and organic nutrients (Yaduvanshi andYadav, 1990), it finds that little is used to produce agriculture fer-tilizer (Elsayed et al., 2008). The major reason for this is the

), [email protected]

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insoluble and imbalance nature of the nutrient in it. Besides, ittakes long time to decompose, and the intense heat and foul smellare generated (Sen and Chandra, 2006). It is reported that FM canbe reused to desulphurize the fuel gases (Dolignier and Martin,1997), and to prepare the octacosanol (Qu et al., 2012). Unfortu-nately, other kinds of SW are produced, and also have to bedisposed. Lime can be prepared with FM (Nikolaos, 2004). But, it isnecessary to avoid the presence of unsuitable substances. Sarkaet al. (2008) state FM can be used as raw material to produce thebreezeblock. The concern is that its high calorific value will not beexploited to the full in this process. There have been many ap-proaches for FM utilization, but all of them still have variousdrawbacks. In China, more than 16,000,000 t of sugar (in 2011) isproduced annually, and about 16,000,000 t of FM also is dischargedevery year. Serious environment problems have happened becauseit is stacked around the factory without safe disposal. It is pressingto find a new method to reuse FM reasonably. This method shouldbe the better one, and the sugar industry and environment all canbe developed sustainably.

In recent years, sustainable development and natural resourcesreservation have become global issues (Sabine, 2013). The cementindustry, which is known as one of the important consumptiveindustry for rawmaterial and energy, has integrated these issues toits development policy (Schneider et al., 2011). Many industrial SWare reused to replace the traditional materials or fuel in the pro-duction process (Li et al., 2012; Rodriguez et al., 2013). Alternative

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H. Li et al. / Journal of Cleaner Production 66 (2014) 107e112108

raw materials mainly provide the necessary chemical compounds,such as CaO, SiO2, Fe2O3 and Al2O3 for cement raw mill. The mainchemical component of FM is CaO (Neha et al., 2011), which is alsothe main chemical compound of lime-based cement raw materials.Thereby, at least in theory, it can be used as the alternatives of lime-based materials for clinker production. There are also several ad-vantages of utilizing FM in the cement clinker production. The hightemperature (above 1400 �C) in kiln can decompose the toxicorganic matters and the bacteria; fuel can be also saved due to highcalorific value of FM (Ribbing, 2007). But, FM also contains severalhigher contents of impurities except for the CaO, such as MgO, SO3and P2O5 as compared with the traditional lime-based raw mate-rials. Minor content of MgO, sulfur compounds and phosphatesnormally are used as mineralizers to decrease the viscosity of theinterstitial melt, stabilize different polymorphs of tricalcium silicate(C3S) and dicalcium silicate (C2S), and improve the Portland cementstrength, alone or together with other minor components (Stanekand Sulovsky, 2002; Kolovos et al., 2001). In practical production,the content of sulfate and magnesium added to the raw mix arelimited for the restrictions on the SO3 and MgO content in theclinker. Additionally, high content of P2O5 will decrease the C3S: C2Srate, and give rise to the formation of a-C2S (Lin et al., 2009).

Although there is lot of research efforts as reported in these litera-ture, it is difficult, through them, to evaluate the preparation of Port-land cement clinker with sugar filter mud as lime-based rawmaterialbecause of the varieties of materials used in the previous researches.There still remain some important points needed to systematicallyclarify. They are crucial tomake effective use of FM in Portland cementproduction. Therefore, the raw mix burnability is discussed, themorphology and composition characteristics of the clinker are pre-sented, and the physical performance and the hydration characteristicof cement prepared with FM are investigated in this paper.

2. Experimental

2.1. Materials

Limestone and gypsum were industrial materials. Powders ofaluminum sesquioxide, silicon dioxide and ferric oxide were usedto adjust the contents of Al2O3, SiO2 and Fe2O3 in the raw mixes,and all of them are chemical reagents. FM was obtained from asugar manufacture corporation. FM and limestone were dried toconstant weight at 105 �C, crushed by jaw crusher and ground toASTM 200 mesh size with a centrifugal ball mill. Chemical com-positions of FM and limestone are shown in Table 1.

Table 2Chemical composition and parameter of all raw mixes (wt %).

Oxides SiO2 Al2O3 Fe2O3 CaO Na2O K2O MgO SO3 P2O5

Control 24.08 4.91 2.96 70.04 0.07 0.04 1.23 e e

FM1 24.08 4.91 2.96 70.04 0.07 0.07 1.26 0.21 0.18

2.2. Clinker preparation

The compositional parameters in cement chemistry are listed asfollows (Eqs. (1)e(3)).

Lime saturation ratio ðKHÞ ¼ CaO� 1:65Al2O3 � 0:35Fe2O3

2:80SiO2

(1)

Silica ratio ðSMÞ ¼ SiO2

Al2O3 þ Fe2O3(2)

Table 1Chemical compositions of FM and limestone (wt %).

Oxides SiO2 Al2O3 Fe2O3 CaO Na2O K2O MgO SO3 P2O5

Limestone 3.62 0.65 0.35 50.37 0.05 0.03 0.88 e e

FM 2.30 0.39 0.37 48.40 0.08 0.49 1.32 2.85 2.5

Alumina ratio ðIMÞ ¼ Al2O3

Fe O(3)

2 3

All raw materials were blended with a similar set of parameters(KH ¼ 0.90, SM ¼ 3.0, IM ¼ 1.7). The difference was that thelimestone was replaced with different percentages of FM. FM1,FM2, FM3, FM4 and FM5 represent respectively the mixes in whichFM substitutes for 5, 10, 15, 20 and 40 wt % the limestone. Thechemical composition and parameter of all mixes are given inTable 2.

All mixes were prepared with appropriate water, put into thecylindrical mold, and pressed to a slice with a pressure of200 MPa. Then these slices were heated to 1450 �C with the rate of25 �C/min, kept the temperature for 2 h in the furnace, and cooledrapidly in the air to room temperature. With 3 wt % gypsum, theclinkers were ground to ASTM 200 mesh, and the cements wereobtained.

2.3. Testing methods

The contents of free lime (f-CaO) in clinkers were analyzed bythe glyceroleethanol method.

Scanning electron microscope (SEM) was carried out on aQuanta 200 FEG to observe the microcosmic characteristics of theobtained clinkers. The accelerating voltage was 20 kV, and themagnification was 2000.

Mineral phases of clinkers and pastes were identified by a D/max 2550 X-ray powder diffractometer (XRD), and the 2q rangewas20�w60�, in 0.02� steps, counting by 4 s per step. The radiationwasCuKa at wavelength of 0.1541 nm (40 kV).

Compressive strength tests were carried out according to theChinese National Standard GB/T 17671-1999. Mortars were pre-pared bymixing cements with drinking water at awater-to-cementweight ratio of 0.5 and cement-to-sand ratio of three, casted in40 mm � 40 mm � 160 mm molds and vibrated at the time ofcasting to remove air bubbles. The molded pastes were kept at20 � 20 �C and relative humidity exceeding 90% for 24 h, and thenremoved from the molds. The demoulded samples were cured in awater tank at 20 � 2 �C for the set ages and then their strengthswere measured.

Setting time of cement was examined according to the ChineseNational Standard GB/T 1346-2001.

An isothermal heat-conduction calorimetry (TAM air C80,Thermometric, Sweden) was used to measure the hydration heatevolution of cements. The water-cement ratio was 0.5 andexperimental temperature was 20 � 0.1 �C. Cement and waterwere tempered for several hours before mixing, then the waterwas injected into the reaction vessel and the samples were stirredin the calorimeter for several minutes. This procedure allowedmonitoring the heat evolution from the very beginning whenwater was added to cement. Data logging was continued for about3 days.

FM2 24.08 4.91 2.96 70.04 0.07 0.11 1.30 0.41 0.36FM3 24.08 4.91 2.96 70.04 0.08 0.15 1.33 0.62 0.55FM4 24.08 4.91 2.96 70.04 0.08 0.17 1.36 0.82 0.72FM5 24.08 4.91 2.96 70.04 0.09 0.30 1.50 1.65 1.45LSF 0.90IM 1.70SM 3.0

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H. Li et al. / Journal of Cleaner Production 66 (2014) 107e112 109

3. Result and discussion

3.1. Burnability

Raw mix burnability is related to the conversion rate at whichCaO combines with other chemical components in the sinteringprocess. It commonly is evaluated by the content of f-CaO in clinker.In this study, all mixes were respectively sintered at 1250 �C,1300 �C, 1350 �C, 1400 �C, 1450 �C and 1500 �C for 60 min, and theheating-up speed was 25 �C/min. Then all clinkers were cooled toroom temperature rapidly. After ground to ASTM 200 mesh, the f-CaO contents in themwere determined. The results of free lime aregiven in Fig 1.

Fig.1 shows that the free lime contents of clinkers prepared withFM are lower than that of control at all sintering temperatures.When more content of FM is substituted for limestone in thepreparation of cement, then it is observed that lesser is the freelime available in the clinkers. FM improves the burnability of rawmix. The improvement is related to the presence of impurity ele-ments in FM, such as P, S, Mg, K and Na. This conclusion implies thatthe CaO conversion rate can be raised, due to the replacement oflimestone with FM. The sintering temperature or time can bedecreased or reduced, and a part of the energy, which is required tomake the f-CaO content in the clinker below 1.5%, can be saved.

3.2. Clinker characteristic

3.2.1. SEM observationThe initial raw materials, mineral composition and particle size

determine the cement sintering behavior. In general, this behaviorimplies the formation of liquid phase (Anton et al., 2000). It iscrucial to the C3S formation because the reaction between CaO andC2S commonly takes place through the liquid phase. This reactionmay be accelerated as the amount of liquid phase increases and itsviscosity decreases. The liquid phases in the different clinkers wereobserved by SEM. The fracture surface micrographs of clinkers areshown in Fig. 2.

In the control, the approximate orthogonal structures areobserved, and one of them is labeled as A (shown in Fig. 2a). Largecrystal grains are stacked together closely, and their outlines andboundary lines are visible. Crystal grains change round and smallfor the clinker produced with 5% FM (shown in Fig. 2b). Theiroutlines almost are not found, and the boundary lines are blurred.In addition, drooping-shape microstructures appear, and some ofthem are marked as the B, C, D and E. The same cases are also found

0 10 20 30 400

2

4

6

8

10

12

14

Fre

e li

me

con

ten

t in

cli

nk

ers

(wt

%)

Sugar filter mud replacement ratios (wt %)

1250 13001350 14001450 1500

Fig. 1. The free lime content in clinkers sintered at different temperatures.

in the clinker added with 10% FM (shown in Fig. 2c). Obviously, theliquid phases in FM1 and FM2 clinkers increase, compared withthat in the control.

It is the obvious fact that the separate crystal grains almost can’tbe observed, the boundary lines disappear, and the orthogonaledges of crystal grains change to the aculeated convexes in the FM3.There are several annular zones marked as H, I and J except for thedrooping-shape structure signed as G (shown in Fig. 2d). Theaculeated convexes and the annular zones disappear, and allcement phases almostmelt together into awhole (shown in Figs. 2eand f). The liquid phase amount continues to increase in the FM3,FM4 and FM5. FM raises the amount of liquid phase notably.

3.2.2. XRD patternsAll clinker XRD patterns are shown in Fig. 3. It can be seen from

the Fig. 3 that the major phases of the ordinary Portland cement,C3S, C2S, C3A and C4AF are all identified in each clinker. But themostimportant characteristic peaks of C3S appeared at 2q about 32�, areprovided with different intensities (shown in Fig. 3b). The intensityto some extent determines the relative content of C3S in clinker.Among all clinkers, the intensity of FM2 is the strongest. The fol-lowings are FM1, FM3, control, FM4 and FM5. The C3S content inFM1, FM2 and FM3 are higher that in the control, but the situationsin FM4 and FM5 are reverse. The suitable content of P2O5 in Port-land cement can improve the C3S formation, and increase the C3Scontent. However, P2O5 contents in FM4 and FM5 reach to 0.72%and 1.45% respectively, and the presence of high content P2O5 leadsto the C3S decomposition. In turn, the C3S contents in FM4 and FM5decrease, and are lower than that in the control. Similar observationhas been reported by Yen et al. (2011)

The significant a-C2S (2q ¼ 31.6) peak is found in the clinker ofFM4 and FM5. None exists in FM1, FM2 and control. The resultsindicate that high content of P2O5 will result in the modulation ofC2S structure. The characteristic peak, which commonly appears at2q about 32.4�, also appears in the FM5 clinker. It is identified as theC2S$0.5 Ca3 (PO4)2 (C2S$0.5C3P2). It can be concluded that newphase will be produced during cement sintering, when the contentof P2O5 is too high in the raw mill.

The appropriate replacement content is effective to promote theC3S formation and heighten the C3S content in clinker. Excessive FMwill introduce high content of P2O5, which can lead to the forma-tion of new phases of a-C2S and C2S$0.5C3P2. Thus, FM replacementcontent should be considered in its utilization as lime-basedcement raw material.

3.3. Physical performance

3.3.1. Strength developmentThe compressive strengths of all mortars were measured after

being cured for 3, 7 and 28 days, and the results are given in Fig.4.The compressive strengths of control are compared with these ofothers. Comparison results show that the compressive strengths ofFM1, FM2 and FM3 are greater than these of the control, and thecompressive strengths of FM4 and FM5 are lower than these of thecontrol at all hydration ages.

Theminor contents of P2O5, SO3 andMgO are commonly used tolower the cement sintering temperature, and improve the burn-ability. However, the high content of P2O5 will contribute to the C3Sdecomposition into C2S, and lower the C3S content in clinker, evenproduce the a-C2S and the new phase of C2S$0.5C3P2. Therefore, thecompressive strengths of mortars are adversely affected.

3.3.2. Setting timeTable 3 lists the setting times for the cements prepared with

different contents of FM. The experimental results prove that FM

Page 4: Preparation of Portland cement with sugar filter mud as lime-based raw material

Fig. 2. SEM fracture surface micrographs of clinkers.

H. Li et al. / Journal of Cleaner Production 66 (2014) 107e112110

has the prominent impact on the cement setting. Initial and finalsetting retardation times for FM4 and FM5 are 16 and 50, 22 and68 min, accelerating times for FM1, FM2 and FM3 are 24, 43 and 11,37, 67 and 24 min respectively. The delay in setting time is likelyascribed to the rate of hydration reaction. Appearances of newphases, such as a-C2S and C2S$0.5C3P2, all are the reasons fordelaying the setting time. Moreover, the content decrement of earlyhydration phase (C3S) also is other reason of setting time retarda-tion for the FM4 and FM5. FM1, FM2 and FM3 have the highercontent of C3S, thus their setting times for initial and final areshortened as compared with the control.

3.4. Hydration characteristic

3.4.1. Hydration heatThe hydration heat liberation was also measured during 3 days

as shown in Fig. 5. Heat liberation is rather intense within a fewminutes for the initial rapid hydration of C3A and C3S in the pre-induction period. Soon thereafter, the overall rate of hydration isslowed down and almost zero in the induction period and then asecond main exothermic peak appears as a main result of furtherhydration for C3S (Fig. 5a). The end time of the induction periodhas an important effect on cement hydration property. It is found

Page 5: Preparation of Portland cement with sugar filter mud as lime-based raw material

Fig. 3. Detailed peak pattern of clinker.

H. Li et al. / Journal of Cleaner Production 66 (2014) 107e112 111

that FM2, FM1 and FM3 are provided with the earliest end timesof induction period than that of the control, but the cases areadverse for the FM4 and FM5. The increases of P2O5 and SO3contents prolong the induction period, especially FM more than40%. In addition, the heat release rates of all these cements alsorepresent remarkable difference within the hydration time from4 h to16 h. FM2, FM1 and FM3 have the higher heat release ratesthan that of the others. It is clear that heat release rates of FM4and FM5 are lower than that of the control in the further hydra-tion period of C3S.

In the initial hydration, the amounts of heat liberation slightlyrise for the cements prepared with 5%, 10% and 15% FM, but for thespecimens with 20% and 40% FM, the decrease is obvious ascompared with control. In the following hydration period, FM posessignificant impact on the hydration heat release. The heat libera-tions of specimens with less than 15% FMwill eventually be beyondthat of the control, and the reverse results are observed with thecements prepared with more than 15% FM. Appropriate content ofFM is found to promote the cement hydration in the initial andacceleration period. Thus their compressive strengths are higherthan that of the control. Instead, their compressive strengths will beaffected negatively by FM.

3.4.2. XRD patternThe phase compositions of hardened cement pastes cured at

3d and 28d were observed by XRD, and their XRD patterns are

0 5 10 15 20 25 30 35 40

25

30

35

40

45

50

55

60

(MP

a)st

ren

gth

Com

pre

ssiv

e

Replacement content (wt %)

3d 7d 28d

Fig. 4. Influence of filter mud replacement content on the compressive strength.

given in Fig. 6. The unhydrated C3S and C2S, the hydrationproduct Ca(OH)2 all are identified in these specimens. Althoughthe diffraction peak intensity was not directly proportional tothe content of crystalline phases, some important informationcan be obtained from comparisons of the relative intensity orchanges of the intensity with age. After 3 days, it is found fromthe variation in Ca(OH)2 peak at 18.007� that less than 20% FMpromotes the cement hydration, but more than 20% FM has anevident delayed effect. After 28 days, the similar trend appearsbut the variation becomes unobvious. The main hydrationproduct of Ca(OH)2 will be reduced as an excessive replacementresult of FM.

4. Conclusions

FM can be used to prepare the Portland cement clinker. More-over, FM can improve the burnabilities of raw mixes and increasethe liquid phase amount, which is important to the C3S formation.The major phase components of the ordinary Portland cement, C3S,C2S, C3A and C4AF all are identified in each cement clinker.Appropriate FM content is effective to promote the C3S formationand heighten the C3S content in clinker. High replacement contentof limestone with FM will result in the formation of a-C2S andC2S$0.5C3P2.

Compressive strengths of all mortars are related to thereplacement ratios of limestone with FM. When it is less than 20%,the compressive strengths of all mortars are greater than these ofthe control. The compressive strengths are affected negativelywhile it is more than 20%. Besides, the initial and final setting timesalso are prolonged for the specimens prepared with more than 20%content of FM.

Appropriate content of FM is found to promote the cement hy-dration in the initial and acceleration period. Thus the highercompressive strength than that of the control can be obtained.Instead, high content FM will lead to the decrease of compressivestrength.

Table 3Setting time of cement prepared with different replacement FM.

Specimens Initial setting time (min) Final setting time (min)

Control 148 342FM1 124 305FM2 105 275FM3 137 318FM4 164 364FM5 198 410

Page 6: Preparation of Portland cement with sugar filter mud as lime-based raw material

0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

FM3

)g

/w

m(

no

it

ar

eb

il

ta

eh

fo

et

aR

Hydration time (h)

FM2

FM1

control

FM4

FM5

Rate of heat liberation

a

0 4 8 12 16 20 24 28 32 36 40 44 48 52 56 60 64 68 72

0

20

40

60

80

100

120

140

160

180

200

Hy

dra

tio

n h

ea

t (m

w/g

)

Hydration time (h)

Hydration heat

FM2

FM1

FM5

FM4

control

FM3

b

Fig. 5. Rates of heat liberation for cements prepared with different FM.

10 20 30 40 50 60

cbbca a

Inte

nsi

ty

control

FM1

FM2

FM3

FM4

FM53d a a

abc a Ca(OH)2 b C3S c C2S

10 20 30 40 50 60

cc b

ba aa

In

ten

sity

control

FM1

FM2

FM3

FM4

FM5

28d a ab

c a Ca(OH)2

b C3S c C2S

Fig. 6. XRD patterns of hardened cement pastes at 3d and 28d.

H. Li et al. / Journal of Cleaner Production 66 (2014) 107e112112

Acknowledgments

Thanks to National Natural Science Foundation of China,Fundamental Research Funds for the Central Universities andMinistry of Housing and Urban-Rural Development of the People’sRepublic of China for their financial supports for the projectsNo.51302189, No.51308406 No.0500219143 and 2010ZX07319-001-02.

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