Materials Science Forum Vols 775-776 (2014) pp 653-658 Online: 2014-01-03

© (2014) Trans Tech Publications, Switzerland

doi:10.4028/www.scientific.net/MSF.775-776.653

KAOLIN RESIDUE AS AN ALTERNATIVE BINDER FOR GROUT SEAT

AND REVETMENT
Beltrão, S.L.D1; Severo, C.G.S2; Bezerra, I.M.T2; Lira, B.S2; Ferreira, H.C2;
Neves,G. A2;
1,2
Federal University of Campina Grande - Paraiba, Brazil
1
e-mail: slisboabeltao@gmail.com

Keywords: recycling, kaolin residue, grout

Abstract: The kaolin residue presents in its composition significant levels of sílica and alumina,
making it a material with chemical and physical properties appropriate to use as an alternative
material with pozzolanic characteristics in substitution to the cement for grout utilization. Thus, this
work aimed evaluate the influence from the addition of different amounts of kaolin residual
calcined in partial substitution of Portland cement on grout in dash 1:2:6
(cement+%residue:lime:sand). It was evaluated grouts with and without residue substitution in the
strengths of 0%, 5% and 30%, through resistor the simple compression at 30, 60 and 90 healing
days. The results of resistor from the grouts were over the one required by NBR 13281 [1],
classifying them as type I e II.

Introduction
Due to the kaolin benefication the exaggerated production of residue becomes an worrying
action since this residues are discarded in an indiscriminate way near their generator pole, that
doesn’t have condition to absorb such a high volume of residue. The consequences of the disposal
of these residues for the local population near the residues are sundry, ranging from respisratory
problems due to the small silica particles in suspension up to the aggression of animals and
vegetation.
According to Massena [2] in a time when is desired to adopt sustainable practices and that
be “eco-friendly” the solution can pass through the materials production from residues , with high
level of recycling , more durable, that incorporate less energy or are chosen by an analysis of their
lifecycle. The search for solutions that minimize damage to the environment we have in the civil
construction sector, a specialty of technological activity that, by the amount of natural resources
consumed, can be widely indicated absorbing solid residues according to Lucas and Benatti [3].
According Jhon [4], the civil construction is the sector responsible for the largest volume of
consumption of natural resources, on estimations that vary between 15 e 50% of the extracted
resources, beyond their products are major energy consumers, and for these reason, it is of
fundamental importance to develop alternative materials that meet this activity.
Binders materials with low carbon emissions, more durable materials, which allow the
reutilization of residues, recyclable materials or obtained from renewable sources, materials with
low energy incorporated or non-toxic and does not pollute the air inside the housing, are examples
of what maybe several variants that fit the eco-efficiency of construction materials (Torgal, et al.,)
[5].
In a reality where we can say that during the production of 1 ton of cement clinker are
produced almost 1 ton of CO2 and existent projections point to an increase of duplicated world
consumption of Portland cement in the next 40 years, such fact will aggravate these negative
emissions according to Torgal, et al., [5] and accelerate the urgent need for implementations of
sustainable practices.
The residues of kaolin may represent a promising alternative acting as pozzolanic material
when treated adequately. Basically consist of mica, quartz and part of kaolinite according to Varela
[6] that when thermally treated provided changes in the stages which favors its use as pozzolan that

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654 20th Brazilian Conference on Materials Science and Engineering

could have expanded its application in civil construction in the substitution of cement in mortar
among other products for the insdustry.
Therefore, this study aimed to evaluate the influence of mechanical incorporation of
calcined kaolin`s residue as pozzolan, at different levels of replacement for the cement in laying
mortar and coating, healed for 30, 60 e 90 days.

Materials and Methods

This research was done in the Laboratory of Recycling Material of UFCG-PB.

Beneficiation of kaolin`s residues

Were used two types of residues from the process of kaolin processing, being this, the
residue of thick kaolin (RCG) and the residue of thin kaolin (RCF) both mixed in a proportion of
50% each. The residues were ground in the mill type MultiNo® opposing jets of air with 98% of the
particles passers in ABNT n° 325 (0,044mm). Then they were calcined in na electric furnace at
800°C for 2 hours with a heating rate of 5°C/min, after cooled have been stored in plastic bags and
taken samples for characterization of natural and calcined residue through the analysis by
fluorescence ray-X(Shimadzu EDX 700), ray-X diffraction (Shimadzu, XRD 6000) and thermal
analysis (Shimadzu, DTG-60) and for embedding in mortar.
Preparing the mortars
Were prepared three mortars with dash 1:2:6, varying the amount of cement contained in
that, being 0% (mortars reference),5% and 30% of residue, similar percentages were also evaluated
by Souza [7]. Were molded cylindrical specimens following the methods presented by NBR 13279
[8], PINI [9] and by NBR 7215 [10]. The specimens were healed for 30 days submerged in a tank
filled with water saturated with lime, after this period were submitted in a natural environment
healing by 60 and 90 Souza [7]. Frame 1- Shows the proportions by mass of the mortars used in the
composition.

Frame 1 – Demonstrative of the amount of cement replacement by RCC

*RCC- residue calcined kaolin
Content of replacement 1:2:6 (kg)
0% 1cim.: 0.838 cal : 7.9 sand
5% 1cim.: 0.020 RCC*: 0.882 lime: 8.33 sand
30% 1cim.: 0.165 RCC: 1.19 lime: 11.31 sand

Mechanical resistance
Were submitted to this test four specimens. The mechanical resistance was determined in a
universal presses (Shimadzu AG-IS 100KN) after the healing period of 30, 60 and 90 days.

Test results
Chemical charactarization
Table 1 presents the results of chemical compositions. It is verified in a general way a higher
content of SiO2 , these levels, higher than those found by Varela [6], when summed over only the
contents of SiO2 and also Al2O3 those already satisfy the chemical conditions to be considered
pozzolanic materials according to ASTM [11] and ABNT 12653 [12]. As for oxides fluxing,
normally low on kaolin it is noted to K2O (oxide present in kaolins depending on the natural
occurrence of mica in the same) that the presence of such oxide is minimal compared to the levels
evaluated by Santos et al [13].
 Materials Science Forum Vols. 775-776 655

Table 1- Chemical analysis of the residue of calcined kaolin

SiO2 58,80 %
Al2O3 36,025 %
MgO 2,280 %
K2O 1,630 %
Fe2O3 0,247 %
Others oxides <5
PF 0,85%

Mineralogical characterization
The mineralogical analyzes (Figure 1) indicate that the sample of natural kaolin (A) shows
peaks associated with lamellar mineral kaolinite, (7.18, 3.58 and 1.66 Å) to quartz (4.20, 3.35 and
2.56 Å) and mica (9.99 and 5.04 Å). Figure 1 (B) refers to the residue of kaolin calcined at 800ºC,
this one can observe the absence of the peak of the kaolinite, resulting from breakage of its
crystalline structure, which makes amorphous.

Fig. 1 - Diffractogram of natural kaolin waste (A) and calcined (B)

Thermal analysis
Figure 2 presents the differential thermal analysis (DTA) of the residue natural kaolin and
calcined at 800°C.

6
RC 2% 325 800°C
RC Natural 6
4
A B
Diferença de Temperatura (°C)
Diferença de Temperatura (ºC)

2
4

-2 2

-4
0
-6

-8 -2

-10
0 200 400 600 800 1000
0 200 400 600 800 1000 Tem peratura (°C)
Temperatura (°C)

Fig. 2 - DTA the residue of natural kaolin (A) and calcined (B)
In (A) the RC is natural without calcination this, it on the peak of adsorbed water loss at
110°C, intense endothermic peak at 600°C characteristic of the hydroxyls present in the kaolinite.
In Figure 2 (B) are observed peaks characteristic of loss of adsorbed moisture and water at
approximately 111°C. From 540°C begins the reaction completed by dehydroxylation endothermic
656 20th Brazilian Conference on Materials Science and Engineering

peak at 600°C, conditions in which form metakaolin. At about 980°C to metakaolinite is

transformed into mulite Souza Santos [14].

Evaluation of mortars
After ages curing the mortars were evaluated mechanically by axial compression of the
specimens produced.
In Figure 3 are shown the values of mechanical resistance of the mortar after each curing
period and their contents for cement replacement by RCC.
In accordance with the resistance values presented in Figure 3 it can be seen an increase of
the resistance with respect to the reference mortar when the cement replacement content was 5% at
the ages above 30 days of curing.
It is also observed for concentrations of 5% a marked decrease in mechanical strength at 30
days of curing which may be explained by curing up to 30 days submerged not providing the
hardening reaction of lime in the presence of CO2. This can be confirmed when evaluated increased
mechanical strength to the level of substitution of 30% at the same age of curing.
At 30% substitution is observed a decay resistance compared to the reference mortar at the
ages of 60 and 90 days of curing. This fact might be related to the amount of RCC may have been
overly. However, as the research of Lima [15] showed that for contents above 20% replacement of
cement with metakaolin is able to detect the presence of free calcium hydroxide in the cement paste
favoring the pozzolanic reaction. A fact that can not be observed at 30% substitution for this mortar
due to the reduced resistance values.
8

90 D
RCS (MPa)

60 D
2 30 D

0% 5% 30%

Teor de substituição do cimento (%)

Fig. 3 - Compressive strength of mortar simple (RCS)

Mineralogical analysis of mortars
Figure 4 shows the diffractogram of mortars containing 0%, 5% and 30% of the cement
replacement by RCC after the mechanical strength test of cure at ages of 30 and 60 days.

P CSH
800 1600
700 0%30D 1400 0%60D
600 CSH 1200
500 1000
400 CSH 800
300 C C 600 P
200 PCSH C P C CSH CC
100
400
200 CQ
0 0
-100 -200
1000 0 10 20 30 40 50 60
1000 0 10 20 30 40 50 60
800 5%30D 800 5%60D
600 600
400 400
200 200
0 0
0 10 20 30 40 50 60
600 1000 0 10 20 30 40 50 60
500 30%30D 800
400 600 30%60D
300
200 400
100 200
0 0
0 10 20 30 40 50 60
0 10 20 30 40 50 60
2θ
2θ

Fig. 4 - Diffractogram of mortars at 30 and 60 days of curing

 Materials Science Forum Vols. 775-776 657

It can be seen in the diffractograms relative to 30 days cure the presence of peaks
characteristic of portlandite (P) characterized by interplanar spacings of 2.62Å, 5.60Å and 3.23Å,
calcium silicate hydrate (CSH) characterized the interplanar distances 3.36 and 3.19Å, calcite (C)
characterized by interplanar distances 3.03Å and 2.13Å, and quartz (Q) for all samples, peak
relative the peak appears very intense portlandite this age due to healing of these mortars
submerged, no curing reactions in the presence of CO2; it can be seen also for all samples peaks
characteristic of CSH, for the hydration reaction of cement and pozzolan with these products. See
also for all peaks characteristic samples of CSH, relative for the hydration reaction of cement with
pozzolan with these products. It can be seen in the samples with addition of kaolin waste in the
form of metakaolinite, intense peaks relative to the for composition 5% and 30%, being more
pronounced in the composition with 5% replacement, which may have been provided by the
pozzolanic reactions have been observed resistance values higher than the reference mortar
throughout the curing time.
Figure 5 shows the XRD patterns of the mortars at 90 days of curing after the mechanical
resistance tests.

1600 SCH
1400 0%90D
1200
1000
800
600 P SCH
400 QC Q P SCH C
200
0
-200
0 10 20 30 40 50 60
1400
1200
1000 5%90D
800
600
400
200
0
-200
1400 0 10 20 30 40 50 60
1200 30%90D
1000
800
600 A
400
200
0
0 10 20 30 40 50 60
2θ

Fig. 5 - Diffractogram of mortar at 90 days of curing

In the XRD patterns of mortars with 90 days of healing can be observed in the specimes
mortar alternatives based on the content of substitution part of the binder residue calcined kaolin
(RC) the presence of mineralogical phases corresponding to: portlandite (P ) the calcium silicate
hydrate (CSH) and calcite (C), quartz (Q) and albite (A), this second Palhares et al [16] belonging
to slicatos series of feldspars, which was possible only be identified presenting only the most
intense peaks at this age and composition.
Conclusions

According to the obtained results it can be concluded that chemical analysis of the residues
is above the regulatory requirements of ASTM and NBR; mineralogical phases found determines
the temperature of 800ºC was sufficient for complete dehydroxylation of the kaolinite present in the
residue; however insufficient for the phase transformation of quartz and mica; mortar with addition
of kaolin waste replacing part of the cement present values of compressive strength higher than the
reference (0% substitution) and the values of 5% at 60 and 90 days of curing most significant.
658 20th Brazilian Conference on Materials Science and Engineering

References
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and wall cladding and ceilings – Specification
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varying amounts of metakaolin in natural exposure. Master (Dissertation). Lisboa, 2011.
Universidade Nova de Lisboa (UNL). (Portugal)
[3] D. Lucas and C.T. Benatti: Journal of Agribusiness and Environment.
[4] John, V. M. - The construction, the environment and recycling. Available at:
<http://www.reciclagem.pcc.usp.br/a_construcao_e.htm> Accessed on: 14 December. 2008.
[5] F.P. Torgal and S. Jalali: Engineering and Life Vol. 42 January 2008.
[6] M.L Varela et al: Ceramics Magazine (2009), p. 209.
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[11] ASTM - American Society for Testing and Materials. Flay ash and raw or calcined natural
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Annual book of ASTM Standards. Philadelphia, 1991.
[12] [12] ABNT - Brazilian Association of Technical Standards. Pozzolanic materials-Specification.
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[13] R.F, Santos, F.G. Melchiades, E. Biscaro, A. Ferrari and A.O. Boschi: Industrial Ceramics Vol.
15(5-6) (2010)
[14] P. Souza Santos: Science and Technology Clays. (São Paulo: Edgard Blücher 1992).
[15] P.R.L. Lima and R.D. Toledo Filho: Built Environment Vol. 8 (4) (2008), p. 7.
[16] L.B Palhares, B.H.M, Moreira and P.C.D. Perini: Reuse of slate in the manufacture of ceramic
parts using the technique of collage slips. Rev. in Post Magazine Ed. 6 2012.
20th Brazilian Conference on Materials Science and Engineering
10.4028/www.scientific.net/MSF.775-776

Kaolin Residue as an Alternative Binder for Grout Seat and Revetment

10.4028/www.scientific.net/MSF.775-776.653