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Effects Of Trans-Polyoctenamer (TOR) On Properties Of Rubberized





L I T E R A T U R E R E V I E W .

In Malaysia. the term of bitumen refers to the binder material. Petroleum bitumen – bitumen in colloidal form obtained from refinery process of crude oil and has been widely used in the road construction. The mixture of bitumen and aggregate is called asphaltic concrete.2. nitrogen and traces of various metals. the remainder being oxygen. (Benzene International. which produces from refinery of crude oil.1 LITERATURE REVIEW Bitumen grade 80/100 Bitumen is a non-crystalline viscous material. black or dark brown. possessing adhesive and water-proofing qualities. which is substantially soluble in carbon disulphide (CS2). The chemical composition of bitumen are listed as shown in Table 1: Minerals Percentage content (%) Carbon 80-85 Hydrogen 10 Sulfur 1-5 Nitrogen 1 Oxygen <1 Table 1: chemical composition of bitumen Bitumen can be obtained from two main sources which are:  Natural sources – bitumen which is located in geological stratum and can be obtained in  the hard and soft form. 2008). sulphur. PROPERTY GRADES BITUMEN 80/100 STANDARD ASTM / AASHTO . It consists essentially of hydrocarbons and would typically comprise at least 80% carbon and 15% hydrogen.

06 D70 Gravity @25/25 Penetration After Heating Temperature Max 90-100 above the soft (°C) Table 2: Properties of bitumen 80/100 Crumb Rubber Crumb rubber is produced by reducing scrap tires down to sizes ranging from 3/8” to 40 mesh particles and removing 99 percent or more of the steel and fabric from the scrap tires. Crumb rubber is manufactured from two tire buffings and scrap tire rubber. These processes from where that can be obtained. .5 MAX D-4 CS@ (wt)% Spot Test NEGATIVE - Density @25° C 1.5 MAX D-6 (wt)% Drop in 20 MAX D-6 & D-5 % Flash Point °C 225 MIN D-92 Solubility in 99.01/1. Two of the most common are ambient grinding and cryogenic processing. There are several processes for manufacturing crumb rubber.06 D-70 °C Penetration @ 80/100 D-5 25 ° C Softening Point 45/52 D-36 °C Ductility @ 25 ° 100 MIN D-113 C CMS Loss on Heating 0.01/1.Specification 1.

the rubber particles will tend to form a cut shape and rough particles. immersed in a "bath" of liquid nitrogen. or sprayed with liquid nitrogen to reduce the temperature of the rubber or tire chip. Typically. Meanwhile by using cracker mills. 2006) Cryogenic process is obtained through a process where the scrap tire rubber is frozen using liquid nitrogen or other frozen method to a temperature below the glass transition temperature of the rubber to make it brittle like glass.Ambient scrap tire is obtained by the grinding of the ground tire rubber at or above ambient temperature without the use of any cooling system to make the rubber brittle. The material can be cooled in a tunnel style chamber. Figure 1 : Ambient scrap tire procces (Reshner. the particles will be long and narrow in shape with a high surface. . By using granulator. the size of the feed material is a nominal 2 inch chip or smaller. 2006). and then the rubber is put in a hammermill and reduced to the desired particle size (Reschner. through either cracker mills or a granulator.

.2006) Transpolyoctenamer Transpolyoctenamer (TOR) is also known as Vestenamer is a mixture from butadiene by dimerization to 1.2012).5-cyclooctadiene.It consists of linear and cyclic macromolecules and is a low molecular weight polymer with a broad molecular weight distribution (Kyung Eui Min and Han Mo Jeong. followed by selective hydrogenation to cyclooctene and finally by a metathesis polymerization of this cyclic monomer. It contains one double bond for every eight carbon atoms with prevalent trans conformations.Figure 2: cryogenic scrap tire process (Reshner .

increased viscosity after polymerization to prevent drain down . high proportion of macrocycles ( around 25%) and unsaturation. TOR is a mixture of linear and macrocyclic polymers that exhibit special structural features when added crumb rubber modified bitumen: low initial viscosity during the initial mixing operation increased viscosity after polymerization to prevent drain down chemical bonding of the final rubberized bitumen to the aggreagte to reduce stripping chemical bonding of the crum rubber to bitumen conversion of the thermoplastic bitumen to a thermoset polymer which reduces cracking and rutting Crumb Rubber Modified Bitumen With Polyoctenamer(Crmb-Tor) Advantages:   Roads are less brittle at lower temperatures Roads have better rutting resistance . chemical bonding of the ground tire rubber (GTR) to the asphalt . 2007) It is believed that the addition of a binder additive like TOR will help decrease the viscosity of asphalt rubber binder without negatively affecting its rheological properties. chemical bonding of the final rubberized to the aggregate to reduce stripping and conversion of the thermoset polymer which is can reduces cracking and rutting are four special features of TOR as additives.(Evonik Industries. Low initial viscosity during the initial mixing operation .Figure 3: Synthesis of trans-polyoctenamer Characteristics of TOR can conduct unique characteristics such as crystallinity. low viscocity above the melting point.

Hence the softer the bitumen.2013) The effect of rubber content and TOR addition on the conventional physical properties of s presented in figure 4. the extent of decreased penetrations of CRMB is different from it increasing from the 15% to 20% increment. It was found that the penetrations of bitumen with increasing crumb rubber powder content present a downward trend.  Roads have higher stiffness Roads live longer Penetration Test Penetration Test determines the hardness of Bitumen by measuring the depth ( in tenths of a mm) to which a standard. Figure 4 : penetration test result (Hongying Liu. especially the increase from 15% to 20%. A previous study (Hongying Liu. and loaded needle will vertically penetrate in 5 seconds. In addition. When the content increases from 20% to 25%. the penetrations of CRMB with TOR show an obvious dropping trend. a sample of Bitumen maintained at a temperature of 25 °C. the greater will be its number of penetration units. which shows a significant decrease. which implies that the penetrations of CRMB would be improved further by TOR.2013) Softening Point Test .

figure 5 shown clearly when CR concentration increase. Bitumen with higher softening point may be preferred in warmer places.As an example if two samples have softening points of 40 °C and 80 °C respectively. It can concluded that TOR is very useful to high temperature performance of CRMB. both will have the same consistency at their softening point. Softening point is the temperature at which the bituminous binders have an equal viscosity which is the consistency of all the grades will be same at the softening point. Based on previous study (Hongying Liu. which is anticipated in that area otherwise bitumen may sufficiently soften and result in bleeding and development of ruts.2013) . Figure 5: softening point test graph (Hongyin Liu. softening point also increase especially for CRMB-TOR graph. Softening point should be higher than the hottest day temperature. thoroughly coating aggregates in the bitumen concrete mixing facility. 2013) Brookfield Viscosity Test The objective of this test is to study the viscosities of crumb rubber bitumen modified with and without TOR. Based on latest study (Hongying Liu and Zhijun . and be placed and compacted to form a new pavement surface. The viscosity of bitumen binders at high temperature is considered to be an important property because it represents the binder’s ability to be pumped through an bitumen plant.This method is useful in determining the consistency of bitumen as one element in establishing the uniformity of shipments or sources of supply. The test gives an idea of the temperature at which the bituminous materials attain a certain viscosity.

As it is known that. TOR was added to the mixture to increase the workability and compatibility of the mixture. should the crumb rubber mixed bitumen be applied again after a long storage time. the crumb rubber mixed bitumen needs to be tested as to whether the properties of crumb rubber mixed bitumen can still meet the technical requirement or not of the specification in use. The complex shear modulus (G*) and the phase angle (δ) of the samples are . The increase in the viscosity of crumb rubber mixed bitumen is thought to be caused by the addition of crumb rubber to the binder.Chen. In reality. which makes the binder more stickier. A general trend was found from the results that the viscosity values of crumb rubber mixed bitumen increase with increased crumb rubber concentration. the addition of TOR resulted in reducing the viscosity. However. and this finding is equally true for crumb rubber mixed bitumen at both testing temperatures. Figure 6: Brookfield viscosity result Dynamic Shear Rheometer Dynamic Shear Rheometer (DSR) test is conducted to determine rheological properties of bitumen binder. the crumb rubber mixed bitumen should be used within 24 hour inpractical engineering applications.2013) Figure 5 shown the viscosity values at 177 °C and 190°C for crumb rubber mixed bitumen with and without TOR.

After the one second load is removed. Black diagram is a complex modulus (G*) versus phase angle (d) plot and has the advantage that the rheological characteristics measured at various temperatures are illustrated by means of a single curve. likewise the lower the phase angle the more elastic-like the material will behave. Based on MSCR test “black diagram” will produced.independent of the temperature and frequencies.1 kpa) for 10 creep recovery cycles then the stress is increased to 3.2 kpa and repeated for additional 10 cycles. Procedure conducted by applying a one second creep load to the bitumen binder sample. the second modulus relates to the viscous properties of the material.E Zorro .measured in the DSR. 2012). The 70 °C MSCR results did not reveal any dramatic differences in the failure stress levels between the unmodified bitumen and the modified bitumen. whereas.2012) Two components make the complex shear modulus. the higher the phase angle the more viscous-like the material will behave. Based on previous study (S. The phase angle is then the angle between the storage modulus (G’) and the resultant complex shear modulus (G*). The performance-graded asphalt binder specification uses the values of G* and δ to determine the performance grade of the binders. the first modulus is related to the elastic properties of the material. the sample is allowed to recover for 9 seconds then the test started with the application of a low stress (0. (Airey GD. 2009). Multiple Stress Creep Recovery(MSCR) Multiple stress creep recovery (MSCR) is a test that conducted to evaluate the binders potential for permanent deformation by using DSR as the laboratory equipment. G* is considered the total resistance of the binder to deformation when sheared at a certain frequency and temperature and it is highly sensitive to the morphological state of a heterogeneous system( Kyung Eui Min and Han Mo Jeong.E Zorro . 2012) low shear viscosity was shown to adequately characterize of different type of bitumen but was deficient for a proprietary styrene-butadiene-styrene(SBS) modified bitumen as no viscosity plateau could be observed at low shear rates.70°C was used in this test as pre-determined temperature. The MSCR mode of loading at a pre-determine test temperature is subsequently adopted as the preferred test method( S. these are the storage modulus (G’) and the loss modulus (G”). The minor discontinuities/mismatches in the Black space diagrams of the .

2002).straight run bitumen curves has been attributed in earlier research to the differing test plate geometries used (8 mm versus 20 mm diameter) resulting in strain variations from one test to another (experimental errors) (GD. Black diagrams are often used as a ‘‘fingerprint’’ of the bitumen for quality control purposes. 2000) M E T H O D O L O G Y . As example when monitoring the consistency of delivered bitumen (T..

Brookfield viscosity test will be conducted to investigate physical properties of crumb rubber modified bitumen(CRMB) reinforced with trans-polyoctenamer (TOR).multiple stress creep recovery test and dynamic shear rheometer will be tested. To study the optimum content of TOR and crumb rubber. . while the second section will explain all the test that will be conducted. The first section will explain the preparation process of CRMB. softening test . penetration test. To determine the physical properties of crumb rubber modified bitumen(CRMB) reinforced with transpolyoctenamer(TOR) . Objectives for this project are 1. The third section will explained about viscosity test and lastly the forth section will discuss about the method and process. 2. To determine the rheological properties of crumb rubber modified bitumen(CRMB) reinforced with transpolyoctenamer(TOR) (CRMB-TOR).1 INTRODUCTION This project is conducted as a research and experiment base project.3. 3. For the laboratory test.TOR sample. To determine the relationship of CRMB-TOR with the rutting resistance. 4. Meanwhile to determine the rhelogical properties of crumb rubber modified bitumen(CRMB) reinforced with transpolyoctenamer(TOR) (CRMB-TOR). The research is including effects on transpolyoctenamer (TOR) on properties of rubberized bitumen to improvised road for better future.

softening point test and Brookfield viscosity test will be conducted to test physical properties .compare and justify • journals and articles related to crumb rubberized modified and transpolyoctenamer will be recorded and used literature studies objectives.• meeting with supervisor hhad been schedule once a week to inform the project progress and to make sure the project is always meeting the objectives of the project meeting with project supervisor preparation of sample and testing equipment • crumb rubberrized modified and transpolyoctenamer(TOR) will be mixed with temperature 180°C .speed 500 RPM with one hour duration for the test laboratory testing • penetration test . • multiple stress creep recovery test and dynamic shear rheometer will be tested to determine rheological properties analysis and data interpretation • result that will be obtained from the test will then in graph. The following approaches need to be conducted during the project to meet the project .

TOR And Testing Equipment Preparation Laboratory Testing Specification Of Laboratory Test Analysis And Interpretation Conclusion And Reccomendation Thesis Preparation .Process of Final Year Project Project Title Selection Literature Studies Crumb Rubber Modified.

15% and 20% by weight bitumen. 5%. in which the CRMB and TOR mixing with the base asphalt before introducing the bitumen into the aggregate. 2%. The mixing process will be used Propeller mixer with duration one hour. 500 rpm of speed and temperature with 180°C. Bitumen poured into the container is heated to melt the bitumen ago bitumen viscosity so that it is easily transferred into the container. The percentage of the CRMB will be added are 0%. the percentage of TOR is 0%. Other than that.3. It should be taken of bitumen from the same source to be used for each test. Stir constantly  until it became fluid state and absent of air bubbles. Materials Bitumen grade 80/100 Crum rubber Transpolyoctenamer Conducted test  Penetration Test  Apparatus  Penetrometer  Thermometer  Water bath  Container with 55mm diameter and 35mm depth  Bitumen speciemen  Procedure  Bitumen specimen is soften in a container to a temperature 75-100°C. 4% and 6% by weight of crumb rubber. From the top rim of distance 3mm . After the move crumb rubber and transpolyoctenamer will be added to the tin.2 PREPARATION OF CRUMB RUBBER MODIFIED BITUMEN (CRMB) AND TRANSPOLYOCTENAMER (TOR) Bitumen grade 80/100 will be collected in the laboratory of civil engineering UNITEN. .Method of mixing binder used in this project will be a wet process. The specimen will be cooled for 1 hour in a temperature less than 13°C and will be moved the sample to a constant water bath at temperature 25°C for another 1 hour. the bitumen will be poured sample into the  container.

The needle together will be released with 100g weight for a 5 seconds. The temperature when the softened bitumen sinks and the ball touches the base plate  will be recorded. . five readings on the surface of the sample will be recorded. The procedure will be repeated if the difference between the two temperatures exceeds 1°C. When the bitumen softens. The ring is will be placed on the ring holder and will be suspended in a bath that will   be filled with distilled water at 5°C.  Softening point test (ring and ball test)  Apparatus  Ring and ball testing equipment  Thermometer  Brass ring  Steel ball  Base plate  Procedure  Hot bitumen will be poured into the ring and will be cooled at room temperature for  about 30 minutes and the sample will be leveled.  Brookfield viscosity test  Apparatus  Rotational viscometer  Environmental Chamber  Temperature Controller  Procedure  Preheat spindle . The bath will be heated and stirred at control rate of 5°C/minute. The distance of each penetration did not less than 10mm apart and not less than 10mm from the side of the   container. Used the clean needle before next penetration proceed. the depth of  penetration will be recorded. the ball will be placed in each ball-centering guide.sample chamber and viscometer chamber to 135°C. Repeated for other bitumen specimen. The penetration needle will be adjusted until its tip touched the surface of sample and  will be moved the dial reading penetrometer at zero. the ball and bitumen sink toward the bottom of the beaker. The temperature  will be recorded at every minute and make sure it increase uniformly. Maintain such temperature for 15 minutes. By using forceps.

The sample size varies according to  the selected spindle and equipment manufacturer. The specimen around the edge of the test plates will be trimmed using a heated  trimming tool. Move the test plates together until the gap between them equals the test gap plus  0. The sample will be stirred  and not to entrap air bubbles The bitumen will be poured into sample chamber. The testing temperature will be selected according to the CRMB-TOR binder grade or testing schedule. The CRMB-TOR will be heated until fluid enough to pour. The spindle will be rotated at 20 RPM. . Heat the Dynamic Shear Rheometer will be heated to test temperature. and will be made sure the percent torque as indicate by the RV readout remains between 2 and 98 percent. This preheats the upper and lower plates which allows the specimen to   adhere to them. The specimen will be brought to the test temperature.  Dynamic Shear Rheometer  Apparatus  Dynamic Shear Rheometer  Computer  Plates  Trimming tool  Basic Procedure  The CRMB-TOR which the test specimens are will be selected until the sample is  sufficiently fluid to pour the test specimens. the sample will be brought to the desire test temperature which is typically 135°C within approximately 30 minutes and allow it to equilibrate at test temperature for 10  minutes. The bitumen binder sample will be placed between the test plates. The sample chamber will be inserted into Rotational Viscometer temperature  controller unit and carefully lower spindle into sample.002 inches (0. This will be created  a slight bulge in the bitumen binder specimen’s perimeter. The test will be started only after the specimen had been at the desired temperature for at least 10 minutes. therefore careful trim will insure more reliable  measurements The test plates together will be moved to the desired testing gap.05 mm) will be moved. The calculate complex modulus (G*) is proportional to the fourth power of the bitumen binder specimen radius.

 The Dynamic Shear Rheometer software will be determined a target torque at which to rotate the upper plate based on the material that will be tested. Movement of the test plates at 10rad/sec is so small that impossible to easily see it. If movement is obvious.59 Hz). the cycles will be repeated for 10 cycles  The 3200Pa Stress will be applied for a 1 second Creep period  The Stress will be removed for a 9 second Recovery period  10 cycles will be repeated .  Multiple Stress Creep Recovery ( To produce Black Diagram)  Apparatus  Dynamic Shear Rheometer  Computer  Plates  Trimming tool  Procedure  100 Pa Stress will be applied for a 1 second Creep period  Stress will be removed for a 9 second Recovery period  Then. the bond between the asphalt binder sample and the test plates  will be broken. This torque will be chosen to ensure that measurements are within the specimen’s region of linear  behavior. The Dynamic Shear Rheometer conditions the specimen for 10 cycles at a frequency  of 10 rad/sec (1. The Dynamic Shear Rheometer will be takes test measurements over the next 10 cycles and then the software reduces the data to produce a value for complex modulus (G*) and phase angle (δ) .