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Characteristics of Gypsum Recycling in Different Cycles

Article  in  International Journal of Engineering and Technology · June 2015

DOI: 10.7763/IJET.2015.V7.794

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 IACSIT International Journal of Engineering and Technology, Vol. 7, No. 3, June 2015

Characteristics of Gypsum Recycling in Different Cycles

Sayonara M. M. Pinheiro and Gladis Camarini

provide to the final product (commercial gypsum plaster)

Abstract—In Brazil, the gypsum plaster waste is 4% to different behavior, changing the kinetic of hydration
15% of construction and demolition waste. The reactions and, consequently, their mechanical properties [5].
environmental legislation advises that this waste should be Commercial gypsum plaster from Brazil is constituted
recycled to avoid the contamination of soil and groundwater.
The aim of this work is to show that the recycled gypsum
manly by hemihydrates whose contents ranges from 54.8% to
plaster maintains its characteristics when submitted to 96.2%; anhydrite contents ranges from 0.0% to 19.0% and
different recycling cycles. The recycled gypsum plasters were dihydrates contents ranges from 0.0% to 10.0% [3].
produced by grinding and burning the waste along three Gypsum plaster is used in building constructions such as
successive recycling cycles. The recycled materials were pastes, mortars, components (plasterboards, masonry blocks
evaluated by chemical and physical properties. The obtained and ceilings) and decorative elements [3].
results showed that both recycled and commercial gypsum
plaster are similar to using in the Construction Industry.
To be used, it is mixed with water. In contact with water,
gypsum hemihydrates particles reacts, rehydrating and
Index Terms—Gypsum plaster, physical properties, recycling, become a hard mass, by an exothermic reaction, showed in (2)
waste. [6].

CaSO 4 ⋅ 0.5H 2 O + 1.5H 2O ⎯⎯

→ CaSO 4 ⋅ 2H 2O (2)
I. INTRODUCTION
Gypsum plaster or “plaster of Paris” is an air-hardening The mechanism of hydration reaction is explained by Le
binding material. It is produced from calcination of gypsum Chatellier. When mixing the materials, hemihydrates
(CaSO4∙2H2O – calcium sulfate dihydrate), that partially (CaSO4·0.5H2O) are dissolved in water, forming a saturated
dehydrates producing gypsum plaster (CaSO4∙0.5H2O – solution of Ca2+ and SO42- ions, followed by precipitation of
calcium sulfate hemihydrate) [1], [2]. acicular dihydrate crystals (CaSO4·2H2O). So, the
In Brazil, the gypsum plaster used as construction material crystallization nuclei are formed and around it the crystals
is obtained by drying calcination of natural gypsum rock at grow, forming an interlocking net of long crystals providing
temperatures ranging from 140 ºC to 200 ºC as in (1). It is the strength of the material [1]-[7]. The resulting material is
called β-hemihydrate, which is constituted of calcium sulfate calcium sulfate dihydrate (CaSO4·2H2O) having the same
hemihydrate (CaSO4∙0.5H2O), anhydrite III - unstable chemical nature of the natural gypsum rock [8].
(CaSO4∙εH2O – 0.06 < ε < 0.11), anhydrite II - insoluble During the hydration process the microstructure of the
(CaSO4), calcium sulfate dihydrate (CaSO4∙2H2O) and hardened paste is defined. It depends on the water/gypsum
smaller amounts of impurities [3]-[4]. rate, responsible to lead the hydration reactions and to keep
the workability of gypsum slurry. In general, when the water
140 to 200 0 C amount increase the voids fractions increase and the bond
CaSO4 ⋅ 2H 2O ⎯⎯⎯⎯⎯→ CaSO4 ⋅ 0.5H 2O + 1.5H 2O (1) between the gypsum crystals decrease, leading to lower the
strength of the material [9], [10].
The presence of these calcium sulfate phases is the result According to Kojima and Yasue [11], the water required to
of different interaction such as temperature; water pressure of keep the workability of gypsum slurry is a function of the
calcination environment inside the kiln; particle size particle size distribution, as well as, it varies to the particle
distribution and residence time [5]. diameter (fineness) and the uniformity coefficient (size).
The presence and amount of each calcium sulfate phase In general, the amount of water increases with the
decreasing of the particle diameter and with the increasing of
the coefficient of uniformity. However, small changes in the
particle size distribution can reduce the workability of the
Manuscript received April 5, 2014; revised July 1, 2014. This work was pastes, even when the materials have the same specific
supported in part by the Civil Engineering Graduate Program of the School
of Civil Engineering, Architecture and Urban Design, University of surface area [11].
Campinas, Brazil. The authors thank the National Counsel of Technological In Brazil, during the construction process a significant
and Scientific Development – CNPq and the Brazilian Federal Agency for amount of gypsum plaster waste is generated, being in the
Support and Evaluation of Postgraduate Education – CAPES for the
scholarships. range of 4% to 15% of construction and demolition waste
Sayonara M. M. Pinheiro is with the Department of Civil Engineering at [12]. The forming waste depends on the constructive process
Federal University of Espírito Santo, UFES, Brazil (e-mail: used, as well as, the culture of the region. In 2012, the amount
sayonara.pinheiro@gmail.com).
Gladis Camarini is with the Civil Engineering and Urban Design at of gypsum plaster waste in Brazil was about 5.400.000 t.
University of Campinas, UNICAMP. Campinas, São Paulo, Brazil, Av. However, this number could be greatly increased due to the
Albert Einstein, 951, POBox 6021, CEP: 13083-852, Campinas, SP, Brazil lack of data control related to gypsum plaster waste [13].
(e-mail: gcamarini@gmail.com, camarini@fec.unicamp.br).
This waste material is mainly composed of calcium sulfate

DOI: 10.7763/IJET.2015.V7.794 215

 IACSIT International Journal of Engineering and Technology, Vol. 7, No. 3, June 2015

dihydrate (CaSO4·2H2O) which is not inert and contaminates D. Homogenization

soil and groundwater. Brazilian Environmental Legislation The recycled gypsum plaster (RGP-1 and RGP-2) was
establishes that the gypsum waste should be recycled or homogenized by the method proposed by Cheverton [17].
placed on specific areas. However, the gypsum plaster waste The material is distributed along successive layers that are
is found in irregular areas due to the absence of specific piled in alternate directions, with continuous and uniform
landfills and mostly by the lack of inspection by the distribution (Fig. 2).
government, as well as by few recycling plants [12].
Recent researches of gypsum plaster waste recycling are
related to the use as dihydrate, mixing it with hemihydrates to
use as renderings, or as raw material in the production of
Portland cement and plasterboards [11]-[14].
Due to the chemical characteristics of gypsum plaster
waste, this material can be recycled as a binding material by a Fig. 2. Homogenization of the recycling gypsum plaster (RGP-1 and
simple recycling process, similar to the industrial process to RGP-3).
produce commercial plaster [15]. Recent studies showed
similar characteristics between recycled gypsum plaster E. Evaluated Properties
(RGP) and commercial gypsum plaster (CGP) assessed by CGP, RGP-1 and RGP-3 were evaluated by physical
thermal analyses (TG/DTG) [16] and crystal morphology proprieties and chemical characteristics such as particle
(SEM) [8]. However, there is little information about the size distribution, bulk unit weight; specific gravity; specific
properties of this recycled material when it is recycled surface area; free water, water crystallization, calcium oxide,
several times. sulfuric anhydride; thermal analysis by TGA/DTGA and
This study evaluates the chemical and physical properties X-ray diffraction (XRD).
of RGP along three successive recycling cycle processes to TGA/DTGA was made in a Shimadzu detector (TGA-50),
evaluate the characteristics and properties of the recycled with Nitrogen atmosphere at heating at a rate of 10 ºC/min
material. and XRD in a Shimadzu-XRD 7000.
Physical proprieties took place at the Laboratory of
Binders and Wastes (LARES) at the School of Civil
II. MATERIALS AND METHODS Engineering, Architecture and Urban Design - FEC –
A. Materials UNICAMP. Determination of the free water, water
The materials used in this experimental work were crystallization, calcium oxide, sulfuric anhydride, TG/DTA
commercial gypsum plaster (CGP) obtained in the Brazilian and XRD were made at Chemistry Institute – UNICAMP.
market; and recycled gypsum plaster, obtained by grinding
and burning the gypsum plaster waste (GPW) three times.
The properties were evaluated in the first cycle (RGP-1) and
the third one (RGP-3).
B. Recycling Process
The recycling process was made by grinding and burning
the waste (GPW). The GPW was crushed in a ball mill
reaching a fineness modulus of less than 1.10, homogenized
and burned in a stationary oven at 150 ºC for 1hour.
C. Recycling Cycles
Recycled gypsum plaster from the first (RGP-1) and the
third (RGP-3) cycles were obtained by successive recycling
Fig. 3. Particle size distribution of commercial (CGP) and recycled (RGP-1
of the GPW (Fig. 1). and RGP-3) gypsum plaster.

III. RESULTS AND DISCUSSION

A. Physical Properties
Table I show the results of the physical properties of
commercial gypsum plaster (CGP) and recycled gypsum
plaster at the first cycle (RGP-1) and third cycle (RGP-3).
The particle size distribution is shown in Fig. 3.
Data were treated statistically and the results were
analyzed as follows.
1) The RGP-1 and RGP-3 had the same specific gravity and
specific surface area of the CGP;
2) Fineness modulus and bulk unit weight were different
Fig. 1. Recycling cycles to obtain RGP-1 and RGP-3.
for RGP-1, RGP-3 and CGP;

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 IACSIT International Journal of Engineering and Technology, Vol. 7, No. 3, June 2015

3) The fineness modulus increases in the following order: explained by the grinding step used in the recycling process.
RGP-3 > RGP-1 > CGP; The grinding recycled process is different than the
4) The bulk unit weight decreases in the following order: commercial one. So, they generated materials with different
RGP-3 < RGP-1 < CGP. particle size distribution and fineness modulus. However,
The difference between recycled gypsum plaster (RGP-1 both of them showed fineness modulus < 1.10, according
and RGP-3) and commercial gypsum plaster (CGP) can be specification of Brazilian Standards [18].

Fig. 4. X-ray Diffraction of commercial (CGP) and recycled (RGP-1 and RGP-3) gypsum plaster.

The difference between the recycled gypsum plasters are

the bulk unit weight and the fineness modulus. The bulk unit TABLE II: CHEMICAL CHARACTERISTICS OF COMMERCIAL (CGP) AND
RECYCLED (RGP-1 AND RGP-3) GYPSUM PLASTER
weight decreases and the fineness modulus increases along
the recycled cycles. Mass (%)
Material Free Water
According to Pinheiro [15], during the recycling cycle CaO SO3
water crystallization
some alteration can occur on the microstructure of the
CGP 1.27 1.04 37.3 49.9
recycled material. The crystals become weaker, and during RGP-1 0.85 2.96 39.0 49.4
the grinding process, these observed physical alterations can RGP-3 1.03 1.91 39.0 47.0
occur.
These alterations are not desirable. The amount of water
TABLE III: CHEMICAL CHARACTERISTICS OF COMMERCIAL (CGP) AND
required to keep the workability of gypsum slurry, can RZCYCLED GYPSUM PLASTER (RGP-1 AND RGP-3)
increase, leading to the decrease of the strength of the Levels (%)
recycled material [9], [10].
Material Hemihydrate Dihydrate
B. Chemical (CaSO4∙0.5H2O) (CaSO4∙2H2O)
The Chemical results of the commercial gypsum plaster CGP 94.45 -
RGP-1 89.49 10.51
(CGP) and recycled gypsum plaster (RGP-1and RGP-3) are
RGP-3 98.24 -
presented in Tables II, III and in Fig. 4.
Table II shows the percentages of free water, water
crystallization, calcium oxide (CaO) and sulfuric anhydride The XRD patterns (Fig. 3) show the calcium sulfate
(SO3) by mass. hemihydrate crystal (H - CaSO4∙0.5H2O) and a small
presence of calcium sulfate dihydrate (D - CaSO4∙2H2O) and
TABLE I: RESULTS OF PHYSICAL PROPERTIES OF COMMERCIAL (CGP) AND anhydrite (A - CaSO4). The hemihydrate crystal is
RECYCLED GYPSUM PLASTER (RGP-1 AND RGP-3) predominant in these results.
Fineness
Bulk unit Specific Specific The contents of hemihydrate (CaSO4∙0.5H2O) and
Material weight gravity surface area
modulus dihydrate (CaSO4∙2H2O) were estimated based on TG/DTG
(kg/m3) (kg/m3) (m2/kg)
CGP 0.06 746 2600 6235 curves that are shown in Table III.
RGP-1 0.38 429 2550 6345 Data were analyzed as follows:
RGP-3 0.41 384 2550 6266 1) CGP, RGP-1 and RGP-2 had the same chemical
characteristics. All of them had a high content of
The values of free water, water crystallization, calcium hemihydrates. These results are also in accordance with
oxide and sulfuric anhydride are auxiliary data to determine Cincotto, Agopyan and Florindo [3], and
gypsum chemical composition. They are in accordance to the 2) RGP-1 presented a significant amount of dihydrate.
Brazilian Standards [18], as well as the results of Cincotto, Although the results are in agreement with Cincotto,
Agopyan and Florindo [3]. Agopyan and Florindo [3], it differs from RGP-3 and

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 IACSIT International Journal of Engineering and Technology, Vol. 7, No. 3, June 2015

CGP due the presence of dihydrate. [6] W. C. Hansen, “Hydration of calcined gypsum,” Industrial and
Engineering Chemistry, vol. 22, pp. 611-613, 1930.
The presence of dihydrate in the composition of recycled [7] A. J. Lewry and J. Williamson, “The setting of gypsum plaster: part I
gypsum plaster at the first cycle (RGP-1) can be explained by the hydration of calcium sulphate hemihydrate,” Journal of Materials
the burned step used in the recycling process. Science, vol. 29, pp. 5524-5528, 1994.
[8] G. Camarini, S. M. M. Pinheiro, “Microstructure of recycled gypsum
During calcination, the gypsum plaster compounds are plaster by SEM,” Advanced Materials Research, vol. 912-914, pp.
formed depending on the temperature, time of calcination, 243-246, 2014.
particle size distribution and water vapor pressure [5]. [9] J. Lewry and J. Williamson, “The setting of gypsum plaster: part II The
As observed in Fig. 2 the particle size from RGP-1 and development of microstructure and strength,” Journal of Materials
Science, vol. 29, pp.5 524-5528, 1994.
RGP-3 are different and this fact, as well as an eventual [10] Q. L. Yu and H. J. H. Brouwers, “Microstructure and mechanical
presence of water vapor pressure surrounding the particle, properties of b-hemihydrate produced gypsum: An insight from its
could lead to the presence of dihydrate in the composition of hydration process,” Construction and Building Materials, vol. 25, pp.
3149-3157, 2011.
RGP-1. [11] Y. Kojima and T. Yasue, “Synthesis of large plate-like gypsum
dehydrate from waste gypsum board,” Journal of the European
Ceramic Society, vol. 26, pp. 777–783, 2006.
[12] G. Camarini, L. L. Pimentel, N. H. R. Sa, “Assessment of the material
IV. CONCLUSION loss in wall renderings with B-hemihydrate paste,” Applied mechanics
This study observed the physical properties and chemical and Materials, vol. 71-78, pp. 1242-1245, 2011
[13] ABRELPE: Brazilian Association of Public Cleaning and Special
characteristics of two types of recycled gypsum plaster, Waste. [Online]. Available: http://www.
obtained at first (RGP-1) and third (RGP-3) successive a3p.jbrj.gov.br/pdf/ABRELPE%20%20Panorama2012.pdf.
recycling cycles. [14] C. Chandara, K. A. Azizli, Z. A. Ahmad, and E. Sakai, “Use of waste
gypsum to replace natural gypsum as set retarders in Portland cement,”
The recycled gypsum plasters presented chemical Waste Management, vol. 29, pp. 1675-1679, 1999.
characteristics similar to the commercial gypsum plaster, [15] S. M. M. Pinheiro, “Recycled gypsum plaster: properties evaluation for
even with different fineness, particle size distribution and using in components,” M.S. thesis, Graduate Program in Civil
Engineering, Architecture and Urban Design – FEC, University of
bulk unit weight. Campinas – UNICAMP, Campinas, Brazil, 2011.
RGP-1 and RGP-3 showed a high level of calcium sulfate [16] G. Camarini, S. M. M. Pinheiro, and K. Tannous, “Thermal analysis of
hemihydrate (CaSO4·0.5H2O). This characteristic gives the recycled gypsum from construction and demolition waste,” Applied
binding properties of the recycled material, maintaining the Mechanics and Materials, vol. 260-261, pp. 977-980, 2012.
[17] I. F. Petersen, “Blending in circular and longitudinal mixing piles”,
main characteristic to be considered similar to the Chemometrics and Intelligent Laboratory Systems, vol. 74, pp.
commercial gypsum plaster. 135-141, 2004
In this way, this study show that the gypsum plaster waste [18] Gypsum for Construction, ABNT Standard NBR 13207 – 1994.
can be recycled and re-recycled several times for the same Sayonara M. M. Pinheiro was born in Brazil, 1961.
purpose than the original binder. She was graduated in civil engineering from the
However, more studies must be developed to improve the Federal University of Espírito Santo - UFES in 1986,
She received her M.Sc. in civil engineering from the
recycling process. Crushing and burning steps should be Federal University of Espírito Santo - UFES in 2003
controlled to maintain the recycled material quality. and She received her PHD in civil engineering from the
University of Campinas – UNICAMP in 2011.
She is currently an adjunct professor of civil
ACKNOWLEDGMENT engineering in Federal University of Espírito Santo – UFES - Brazil. She is
The authors are grateful to the Brazilian Federal Agency teaching courses of buildings such as materials, technology, budget and
planning. She conducts researches in the field of building materials such as
for Support and Evaluation of Postgraduate Education – recycling of construction waste (emphasis on gypsum plaster), concrete
CAPES, and the National Counsel of Technological and biodeterioration and durability/performance – concrete, mortar and plaster.
Scientific Development – CNPq for the scholarships, and
LARES-FEC-UNICAMP where the tests took place.
Gladis Camarini is a civil engineer and a professor at
School of Civil Engineering, Architecture and Urban
REFERENCES Design, University of Campinas. She had her master
degree in 1988 and PhD. degree in 1995 at University
[1] J. Karni and E. Karni, “Gypsum in construction: origin and properties”,
of São Paulo. She did postdoctoral studies at the
Materials and Structures, vol. 28, pp. 92-100, 1995.
Laboratoire des Materiaux et Durabilité des
[2] M. Singh, “Making of gypsum plaster in Bhutan – an experience”,
Constructions (LMDC) at Institut National des
Journal of Scientific and Industrial Research, vol. 65, pp. 826-829,
Sciences Apliquées (INSA, Toulouse, France, 1998).
October 2006.
She also did postdoctoral studies at the National
[3] M. A. Cincotto, V. Agopyan, and M. C. Florindo, “Gypsum plaster as a
Institute for Space Research (INPE, São José dos Campos, Brazil, 2008).
construction material: chemical compound,” in Technology of Building,
Then she also did postdoctoral studies at the Institute of Science and
Ed. Technological Research Institute, pp. 53-56, 1998.
Technology del Hormigón (ICITECH), the Polytechnic School of Valencia
[4] J. A. D. Milito and G. Camarini, “Gypsum hemihydrate–cement blends
(UPV) (Valencia, Spain, 2012). She is a peer-reviewed of scientific journals
to improve renderings durability,” Constr. Build. Mat. vol. 25, pp.
indexed on the Journal Citation Reports, national and international journals,
4121-4125, 2011.
Congress and Seminars, and Brazilian Research Foundations. She is an
[5] J. Moisset, Review of the Main Process Used for Plaster Products.
IACSIT senior member. Her research interests include: building materials,
Gypsum Fair 97, ed. Technological Institute of Pernambuco - ITEP,
mineral binders, mortars, industrial and construction wastes, reusing and
Brazil. 1997
recycling of materials, mortar, concrete, and steam curing.

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