Making Composites from Mixing Limestone with Addition of Latex

Amir Hamzah Siregar

, Saharman Gea, Nora Indriani

Departement of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Sumatera Utara, Medan, Indonesia

Keywords: Latex, Limestone Powder, SEM, TGA, XRD.

Abstract: Research on mixing of limestone with the addition of latex in making composites have been done. This

study uses limestone originating from Sidikalang where crushed limestone using ball mill then calcined at

900

C for 2 hours then tested using XRD Pan Analytical X’pert Powder PW 30/40 to determine the

presence of CaO compounds with the greatest intensity of 3036 at θ=37.3556 and particle size tested using

PSA Shimadzu SALD-2300 is obtained an average of 731.7 nm. Then limestone powder (LSP) is used as a

filler with various variations on latex composites. Analyzing of the morphology using SEM FEI Inspect-S50

can be seen from the photo that limestone powder can be evenly distributed on compsites 800 g of latex +

200 g of limestone powder while in the next variation the limestone powder is not evenly distributed

because the addition of the filler increases but the addition of the matrix decreases. The mechanical

properties of latex composites with limestone powder were tested using ASTM D-412 where optimum

tensile strength was found in 800 g of latex + 200 g of limestone powder is 1.279 MPa and optimum

elongation of 1000 g latex is 4.328 mm/mm. Thermal properties were tested using TGA ASTM E1131

obtained by decomposition thermal at 300-400

C because in the sample 1000 g of latex has thermal stability

at 377.39

C and in the sample 800 g of latex + 200 g of limestone powder has thermal stability at 378.21

1 INTRODUCTION

Natural latex is a substance obtained from rubber

latex (Havea Brasiliensis). Natural latex is composed

of hydrocarbons and contains small amounts of non-

rubber parts, such as fat, glycolipid, phosphorus,

proteins, and other organic materials (Kohjiya et al.,

2014).

Natural rubber is one of the important

agricultural products because it holds a role in

improving human living standards and increasing

foreign exchange. The consumption of natural

rubber and world synthetic rubber in 2004 only

reached 20.03 million tons, among them 11.5

million tons were natural rubber. However, as the

largest landowner in fact processing latex into

finished or processed goods, Indonesia is only able

to control the market 10% which is still far below

Thailand with land that is narrower than Indonesia.

Where Thailand was able to dominate the market by

29% and Malaysia by 59%. One of the factors that

caused this weakness was the high production costs

in processing rubber finished goods (Sinaga, 2015).

This is what encourages researchers to conduct

research in suppressing production costs in

processing latex by carrying out special treatment

for latex raw materials namely by adding fillers.

Indonesia as a country that is rich in natural

products has abundance in various sectors. One of

the natural resources produced is limestone with a

large CaCO

content (Lukman et al., 2012).

Most forms of calcium in limestone are found as

calcium carbonate (CaCO

). Limestone has a density

of 2.6-2.8 g/cm

and is pure in the form of calcite

crystals consisting of CaCO

. CaCO

content in

limestone reaches more than 90% and the rest are

other substances (Oates, 1998).

The potential for limestone production in

Indonesia is very large and almost evenly distributed

throughout Indonesia, mainly used as industrial

excavation (Shubri et al., 2014). In general, the

amount of limestone in Indonesia reached 28.678

billion tons. Statistics show that the industrial sector

for the use of limestone tends to increase at 10.45%

every year (Rumengan et al., 2017). The distribution

of limestone deposits are almost evenly distributed

throughout Indonesia, but the largest deposits are in

West Sumatra (Mukarrom, 2017).

(Keliat, 2015) Has investigated the role of

limestone addition to the mechanical properties and

Siregar, A., Gea, S. and Indriani, N.

Making Composites from Mixing Limestone with Addition of Latex.

DOI: 10.5220/0008864001650173

In Proceedings of the 1st International Conference on Chemical Science and Technology Innovation (ICOCSTI 2019), pages 165-173

ISBN: 978-989-758-415-2

165

thermal resistance of HDPE-g-MA composites

where the results of the mechanical properties of

HDPE-g-MA composites showed that the optimum

tensile strength was 15.51 MPa and optimum

elongation was 62% while the thermal properties

using TGA on HDPE-g-MA + limestone composites

have a decomposition point by 498,42

Saputra (2016) has investigated the research on

making composites using fillers namely black

carbon and matrix namely natural rubber which aims

to determine the tensile test properties of composites

where the addition of black carbon at 20, 25 and

30% results in an average of the highest tensile

strength occurred in the natural black carbon

composites of 20% at 1.18 MPa, at 25% at 0.91

MPa, at 30% at 0.56 MPa while at the addition of

black carbon 20, 25 and 30% yielded the average

value of natural rubber composite strain 20% black

carbon for 42.53%, at 25% at 25.19%, at 30% at

6.69%, while the addition of black carbon 20%, 25%

and 30% yielded the highest average modulus of

elasticity occurs in natural rubber composites-black

carbon at 20% at 2.21 x 10

-2

MPa, at 25% at 2.16 x

-2

MPa, at 30% at 1.91 x 10

-2

MPa.

Sinaga (2015) has investigated research on the

making and characterization of composite matrix

polymers where filler namely silica rice husk and

matrix, which is concentrated latex where aims to

determine the nature of mechanical tests where the

optimal composition for modulus of elasticity for

making latex-silica based composites is 0.221 MPa.

In this study we will develop composites by mixing

limestone as filler and latex as a matrix. Where in

limestone generally there is calcium carbonate

(CaCO

). The choice of limestone as a filler in the

manufacture of composites is based on the properties

of limestone which can improve the mechanical

properties of rubber and the amount is very abundant

in Indonesia so can reduce the emphasis on

processing rubber goods. Where the character of

limestone is plastic, it can harden quickly so that it

gives the strength of the binder, easy to do, produces

a good bond for plastering. Therefore, the

researchers hope that this research will be able to

reduce production costs in processing latex and add

value to limestone. In addition, composites can be

produced with better durability.

2 MATERIALS AND METHODS

2.1 Materials

The tools used in this study include: ball mill, 170

mesh sieve, analytical balance, mechanical mixer, x-

ray diffraction, particle size analyzer, oven, furnace

stove, thermogravimetric analysis, scanning electron

microscopy, tensile test tools, glass tools, two roll

mill, limestone, latex, aquadest.

2.2 Procedure

2.2.1 Sample Preparation

2000 g of limestone is taken from the mountains of

Sidikalang, Dairi, North Sumatra and then cleaned

using aquadest and then dried in the oven for 6 hours

at 110.

2.2.2 Making Limestone Powder using Ball

Mill

Limestone and seven metal balls (balls change) are

inserted into the grinding jar. Then put into grinding

station. Close the engine cover, then set the rotation

speed to 250 rpm and set the playback time to 60

minutes and press the start button. Next, limestone

powder was obtained and then filtered using a 170

mesh sieve. Then the limestone powder that has

escaped from the sieve is weighed as much as 100

grams, then calcined 100 grams of limestone powder

from the sieve at 900 for 2 hours. Furthermore, it

was characterized using x-ray diffraction or X-Ray

Diffraction (XRD).

2.2.3 XRD Characterization of Limestone

Powder

Determine the structure of limestone powder

material was carried out using x-ray diffraction

brand Pan Analytical X’Pert Powder PW 30/40. 2 g

of ball mill limestone powder is put into a 2x2 cm2

holder. Then the holder containing the sample is

connected to the diffractometer. Set the sample

name, initial angle, final angle and speed of analysis

on the computer and press the start button. From the

XRD data it can be seen the composition of

compounds from limestone powder.

ICOCSTI 2019 - International Conference on Chemical Science and Technology Innovation

166

2.2.4 Particle Size Analyzer

Determine the particle size of limestone powder was

carried out using particle size analyzer brand

Shimadzu SALD-2300. ± 1 ml of limestone powder

solution is inserted into the PSA to test the particle

size characteristics of the solution. The working

principle of this PSA is to use a laser beam

diffraction method that is fired on the liquid sample

being tested, the particles in the sample solution

undergo a movement called Brownian motion. The

light source (laser) used in the PSA in this study

uses the principle of Dynamic Light Scattering

(DLS). Measuring with this PSA is done at room

temperature. This temperature affects the movement

of particles in a solution (Brownian motion) during

measurement by a device. The higher the

temperature, the more active the motion of the

particles, this affects the accuracy of the

measurement results. Furthermore, the results of the

average particle size of limestone powder can be

determined based on the graph obtained.

2.3 Preparation of Composites

200 g of calcined limestone powder at 900 for 2

hours mixed with 800 g of latex using a mechanical

mixer with a speed of 1000 rpm for 15 minutes.

Then the same procedure was carried out for mixing

750 g of latex and 250 g of limestone powder; 700 g

of latex and 300 g of limestone powder; 650 g of

latex and 350 g of limestone powder; 600 g of latex

and 400 g of limestone powder; 1000 g of latex, then

milled using two roll mill and dried for 1 week.

Composites obtained were ground back using a two

roll mill. Furthermore, it was characterized by

tensile test, TGA analysis, SEM analysis.

2.3.1 Test of Tensile and Extensibility

Tensile strength and elongation testing were carried

out by tensile testing instruments brand Cometech

Qc 502M1 on each specimen by means of dumbbell

and specimen sizes based on ASTM D-412. Turn on

the Torsee's Electronic System tool. Left for 1 hour.

Clamped the sample using giff. Set voltage, strain,

and unit. Turn on recorder (ON). Installed note ink.

Set the x axis (strain) and y axis (voltage) and set the

unit. Installed sample. Press the start button. Rated

load and stroke values. Judging by the numbers in

load (stress) and stroke (strain), if the sample has

broken up. Note the load and stroke values of the

sample.

2.3.2 Analysis of Thermal Properties with

Thermogravimetric Analysis

Analysis of thermal properties was carried out using

the thermogravimetric analysis brand ASTM E1131.

Weighed a sample 10 mg and then put it into an

aluminum cell, then press it. The cell that has been

pressed is placed in a position adjacent to the

reference cell, where after the device is in

equilibrium, then the analysis device is operated

with a temperature of 30

C to 600

C with a speed of

heating increase of 10

C / minute and the gas used is

nitrogen. The results obtained in the form of a graph

of flow of heat flow to temperature and mass graphs

that are lost to temperature.

2.3.3 Analysis of Morphological Properties

by SEM

Analysis of morphological properties was carried

out using the scanning electron microscopy brand

FEI Inspect-S50. The microscopic observation

process using SEM begins with glueing the sample

with a stick made of older metal specimens. Then

after the sample is cleaned with a blower, the sample

is coated with gold and palladium with a dionspater

machine pressurized 1492x10

-2

atm. The sample is

then put into a special room and then irradiated with

10 Kvolt electron beam so that the sample emits

secondary electrons and bounced electrons which

can be detected by scientor detectors which are then

amplified by an electrical circuit which causes

Chatode Ray Tube images. Shooting is done after

selecting a particular part of the object (sample) and

the desired magnification so that a good and clear

photo is obtained.

3 RESULTS AND DISCUSSION

3.1 Characterization of Limestone

Powder

The results of the characterization of limestone

powder produce a diffractogram as shown in Figure

4.1 by matching the results of the limestone

diffractogram with the diffractogram that contained

JCPDS (Join Committee On Difraction) so that

limestone constituents can be identified.

Making Composites from Mixing Limestone with Addition of Latex

167

Figure 1: Diffractogram of limestone powder from the

Sidikalang mountains, Dairi, North Sumatra

Identification results showed that limestone from

the Sidikalang mountain range, Dairi, North Sumatra

contained CaO minerals which were characterized

by the presence of peaks at 2θ = 32.20280

37.35560

and 53.86320

(Table 4.1). Similar results

were also reported by Husin (2013), CaO constituent

minerals with peak characteristics at 2θ = 32.290

37.40

and 53.870

Table 1: Angle Value 2θ of CaO

Standard (JCPDS) Sidikalang Mountain

32.29 32.20

37.40 37.35

53.87 53.86

The results of the characterization of limestone

that has become limestone powder showed that the

particles of limestone powder had an average

particle size of 731.7 nm.

3.2 Composite Characterization

Composite characterization was carried out to

determine the quality produced by mixing a

polymeric material, where characterization was

carried out, namely characterization of mechanical

properties by tensile strength test, elongation and

elastic modulus, characterization of thermal

properties using TGA (Thermogravimetric Analysis)

and characterization of morphological properties by

using SEM (Scanning Electron Microscopy).

3.2.1 Tensile Test

Tensile strength testing is carried out to determine

the tensile strength of the test object against the pull

and the extent to which the material increases in

length. This test uses the ASTM D-412 standard.

From the results of the tensile strength

measurements of latex composite specimens with

the use of limestone powder as fillers showed a

better value than without using fillers. The highest

tensile strength measurements were 1.279 MPa (800

g latex + 200 g limestone powder) and the lowest

tensile strength was 0.272 MPa (1000 g latex). For

full results can be seen in Table 2 below.

For the measurement of tensile strength obtained

that the value of tensile strength increases lower

when the addition of filler increases. This is because

if the number of fillers increases and the number of

matrices decreases, the spread of fillers will be

uneven in the latex compound, resulting in

agglomeration of fillers which decreases the

effectiveness of the tensile force between the filler

particles and the matrix which decreases the tensile

strength 2012; Fang et al., 2014).

Table 2: Testing Results of Mechanical Properties of

Tensile Test of Latex Composite Specimens

Sample

(Ltx : LSP)

Wide

(mm)

Thick

(mm)

Stress

(MPa)

10:0 14 4.9 0.272

8:2 10.5 3 1.279

7:3 10.2 3.2 1.109

6:4 10.7 3.4 0.910

6.5:3.5 10.4 3.1 0.814

6:4 10.6 3.3 0.718

Figure 2: Graph of Stress vs Amount of Limestone

Powder

3.2.2 Extensibility

For the measurement of strain (strain or elongation)

the highest was 4.328 mm / mm (1000 g latex) and

the lowest elongation was 2.915 mm / mm (600 g

latex + 400 limestone powder). For full results, see

Table 3 below.

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168

Table 3: Testing Results of Mechanical Properties of

Strain of Latex Composite Specimens

Sample

(Ltx : LSP)

Gauge

(mm)

∆

l(mm)

Strain

(mm/mm)

10:0 69 298.64 4.32

8:2 64 242.30 3.78

7:3 71 253.21 3.56

6:4 63 215.76 3.42

6.5:3.5 54 169.22 3.13

6:4 47 137.02 2.92

For the measurement of elongation, it is obtained

that the value of elongation increases when the

addition of filler increases. This is because rubber

has elastic properties but because of the increasing

number of fillers and the addition of fewer matrices,

the elastic properties of the rubber (as a matrix)

decrease. In addition, increasing increments of fillers

tend to form agglomerations which cause composite

mixtures to become brittle so that they break more

easily which causes the value of elongation to

decrease (Veronika et al., 2013).

Figure 3: Graph of Strain vs Amount of Limestone

Powder

3.2.3 Modulus of Elasticity

The highest young modulus measurement is 0.337

MPa (800 g latex + 200 g limestone powder) while

the lowest modulus is 0.063 MPa (1000 g latex). For

full results can be seen in Table 4 below.

Table 4: Testing Results of Young Modulus of Latex

Composite Specimens

Sample

(Ltx : LSP)

Stress

(MPa)

Strain

(mm/mm)

MoE

(MPa)

10:0 0.272 4.328 0.063

8:2 1.279 3.785 0.337

7:3 1.109 3.566 0.311

6:4 0.910 3.424 0.265

6.5:3.5 0.814 3.133 0.259

6:4 0.718 2.915 0.246

For the measurement of young modulus it was

found that the value of young modulus decreases

when the addition of filler increases. If more and

more fillers were added there will be an uneven

distribution of latex compounds, thereby reducing

the value of young modulus (Veronika et al.,2013).

Tensile strength indicates the maximum force

required to decide on the lime powder latex

composite. Observation results of tensile strength are

expressed in the form of stress curves, namely the

ratio of loads to cross-sectional area = F / A, to the

extension of the material (strain / strain), namely the

length increase divided by the initial length of

material, expressed in stress-strain curves.

Figure 4: Graph of Modulus of Elasticity vs Amount of

Limestone Powder

Making Composites from Mixing Limestone with Addition of Latex

169

Figure 5: Curve of stress vs strain

From the graph above, it can be seen that the

highest stress is shown in 800 g of latex + 200 g of

limestone powder which is 1.279 MPa because in

subsequent variations the addition of filler increases

and the number of matrices decreases, spread of

filler will be uneven in the latex compound resulting

in agglomeration of fillers which decreases the

effectiveness of tensile forces between particles of

fillers and matrices which then decreases tensile

strength (Nuraya et al., 2012; Fang et al., 2014)

while the highest strain is shown in 1000 g of latex

which is 4.328 mm / mm because rubber has

properties the elastic but in the next variation the

increase in filler increases but the addition of the

matrix decreases, causing the elastic properties of

rubber (as a matrix) to decrease and the increase in

filler tends to form agglomeration which causes the

composite mixture to become brittle so that it breaks

easily causing a value elongation s decreases

(Veronika et al., 2013).

3.2.4 Morphological Analysis of SEM

Characterization using SEM was carried out to look

at the morphology of latex composites with fillers of

limestone powder, where the morphological results

that appeared could show which combination of

fillers and matrices in this case to see the dispersion

(distribution) of filler particles into the polymer

matrix. The results of particle board morphology

analysis can be shown in Figure 6 and Figure 7 as

below.

Figure 6: SEM photos of latex

Figure 7: SEM photo of Latex/LSP (8:2)

In Figure 6, there are blank spaces in the latex

matrix while in Figure 7 it appears that the empty

ICOCSTI 2019 - International Conference on Chemical Science and Technology Innovation

170

spaces have been filled with CaO aggregates and

distributed almost evenly to the latex matrix. This is

due to the small size of the particles from the filler

which allows limestone to be able to combine with

latex. The more amount of CaO added in the latex

compound, the rubber matrix will be increasingly

filled by the dispersion of the filler material so that it

will cause agglomeration of latex and decrease

mechanical properties (Dewi et al., 2014).

3.2.5 Characterization of Thermal

Properties

The characterization of thermal properties in latex

composites with limestone powder fillers using

Thermogravimetry Analysis (TGA) is a technique to

measure changes in thermal transition or material

heat to the function of temperature or time in a

controlled atmosphere.

Thermogravimetry Analysis (TGA) is a test

performed on a sample to determine changes in

weight (loss) due to changes in temperature.

Analysis provides information on the point at which

the lost mass is seen most clearly with respect to

temperature changes so that the resulting data can be

used to predict thermal stability.

Figure 8:TGA curve (a) Latex and (b) Latex/LSP (8:2)

On the curve shown in Figure 4.8 it can be seen

that the sample of 1000 g of latex has thermal

stability at 377.39

C while a sample of 800 g of

latex + 200 g of limestone powder has thermal

stability at 378.210

C. This shows that the

composite experienced thermal decomposition at a

temperature of 300-400

C. Because after passing the

400

C temperature both curves are not at the same

point (not coincide again) and separated into 2

curves.

In Figure 4.8 it can be seen that in a sample of

800 g of latex + 200 g of limestone powder which is

at a temperature of 100

C mass is obtained 10.4727

mg; at a temperature of 200

C a mass of 10.2941 mg

is obtained; at a temperature of 300

C mass is

obtained 10.1138 mg; at a temperature of 4000 0C a

mass of 4.30106 mg was obtained; at a temperature

of 500

C a mass of 2.60660 mg is obtained; at 600

a mass of 2.56472 mg was obtained. Whereas the

sample of 1000 g of latex at a temperature of 100

obtained a mass of 10.4583 mg; at a temperature of

200

C a mass of 10.3953 mg is obtained; at a

temperature of 300

C a mass of 10.2337 mg was

obtained; at a temperature of 400

C a mass of

2.26365 mg is obtained; at a temperature of 500

the mass is 0.0882131 mg; at 600

C the mass is

0.0300798 mg.

From the above data it can be concluded that in

the sample of 1000 g of latex at a temperature of

600

C the mass of 0.0300798 mg was obtained

while in the sample 800 g of latex + 200 g of lime

powder at a temperature of 600

C a mass of 2,56472

mg was obtained. The mass in the sample of 800 g

of latex + 200 g of limestone powder was greater

than in the sample of 1000 g of latex. This is

because limestone generally has a melting

temperature of 900-1000

C so it cannot decompose

thoroughly and produce a greater amount of mass

(Keliat, 2015).

4 CONCLUSIONS

The morphological results of SEM on a mixture of

1000 g latex show that there are empty spaces in the

latex matrix whereas in a mixture of 800 g latex +

200 g limestone powder it appears that the empty

spaces have been filled with CaO aggregates and are

evenly distributed on the latex matrix.

The results of the characterization of the

mechanical properties of latex composites found that

the optimum tensile strength was found in a

composite of 800 g of latex + 200 g of limestone

powder of 1.279 MPa, optimum elongation was in

1000 g of latex of 4.328 mm / mm and optimum

young modulus was in composite 800 g latex + 200

g limestone powder of 0.337 MPa.

The results of the characterization of thermal

properties with TGA on latex composites is that the

composite decomposes at 300-400

C because in the

sample 1000 g of latex has thermal stability at

377.390

C and in the sample 800 g of latex + 200 g

Making Composites from Mixing Limestone with Addition of Latex

171

of limestone powder has thermal stability at

temperature of 378,210

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