Abstract: The present invention provides a cured elastomeric nanocomposite comprised of polymer-coated carbon nanotube in bead form having improved mechanical properties, thermal stability, low water vapor transmissibility and high gas impermeability. The invention consists of a single elastomer or blend of two or more elastomers and polymer coated single wall or multi-walled carbon nanotubes having diameter 1-30 nanometer and length 50 nanometer to 500 micrometers. carbon nanotubes and the mixing of the same thereof. The nano composite composition comprises of one or more elastomers - 100 parts, reinforcing filler - 0-75 phr, a nano filler -0.5-10 phr, cure chemicals, and processing aid. The invention also provides method of manufacture of the elastomeric nanocomposite and bladder with such developed elastomeric nanocomposites having superior durability, thermal stability and barrier characteristics.
DESC:FIELD OF THE INVENTION:
The present invention relates to the field of tyres and elastomeric compositions. More particularly, it relates to bladder application in tyre curing process. More specifically, it relates to a cured elastomeric nanocomposite comprising of polymer coated carbon nanotubes in bead form having improved mechanical properties, thermal stability, low water vapor transmissibility and high gas impermeability. Bladder with such developed elastomeric nanocomposites has superior durability, thermal stability and barrier characteristics.
BACKGROUND OF THE INVENTION:
The existence of rubber nanocomposites and its potential applications are well known. Conventionally carbon black is the only filler used in bladders which lacks in thermal conductivity, low water vapor transmissibility and gas impermeability properties. However, very less works has been carried out in extracting the functional properties of nano fillers for bladder applications. Earlier many inventions are made by adding carbon nano tubes into the elastomeric composite as it is but they all resulted in poor dispersion of carbon nano tubes in the elastomeric composite and also huge amount of carbon nano tubes escaped into the atmosphere due to their low particle size which created severe threat to the living organisms. Reference may be made to the following: -
US2013261246A1 relates to a vulcanizable composition containing a specific hydrogenated nitrile rubber, at least one cross-linking agent and carbon nano tubes, a process for preparing such composition and the use thereof for preparing vulcanizates.
US 9212273B2 relates to carbon nano tubes as fillers in composites with materials such as elastomers, thermosets and thermoplastics. The invention relates to the development of a concentrate of carbon nano tubes with an elastomer wherein the concentrate can be further diluted with an elastomer and other polymers and fillers using conventional melt mixing.
US20150322232A1 relates to a rubber composite composition comprising aligned carbon nano tube bundles and to a production method for same.
US8961834 relates to an electrically conductive thermoplastic composition prepared by melt blending a polymer and a master batch of carbon nanotubes in wax having a melting point of about 45 to about 150.degree. C.
WO2011031437A1 relates to a copolymer formed from an isoolefm having from 4 to 7 carbon atoms and an alkylstyrene. The copolymer has a substantially homogeneous compositional distribution. The copolymer has from about 8 to about 12 wt% of alkylstyrene and at least 85 wt% of isoolefin. The copolymer is preferably halogenated with about 1.1 to about 1.5 wt% of a halogen. The copolymer may be elastomeric nanocomposites.
WO2014143140A1 relates to a fabricated elastomeric product including at least one curable, elastomer material, at least one vulcanizing agent, at least one vulcanization accelerator, and a processing aid, wherein the processing aid includes an effective amount of a non-aggregated nano material containing an effective amount of an organic solvent.
JP2015020939A relates to a carbon nano tube assembly; a method for synthesizing the carbon nano tube assembly having excellent electric conductivity; a resin composition containing the carbon nano tube assembly, which has excellent electric conductivity; an electro-conductive elastomer and a dispersion.
JP2014062179A relates to an antistatic thermoplastic resin composition comprising a resin composition made by blending 5-15 pts.wt. of carbon nano tube (III) with 100 pts.wt. of resin component (A) comprising 35-60 wt.% of styrene resin (I) and 40-65 wt.% of polyamide elastomer (II).
JP2003342480A relates to a recyclable electro conductive thermoplastic elastomer composition formed by dispersing a carbon nano tube to a thermoplastic elastomer material where a rubber is blended to a thermoplastic elastomer, and (a) a rubber portion of the thermoplastic elastomer material is crosslinked by a resin crosslinking agent to have compression set of 30% or less, (b) a blended amount of the rubber is in a ratio of 225 to 400 parts by weight based on the 100 parts by weight of the thermoplastic elastomer and (c) the carbon nano tube has a diameter of 70 nm or less.
Mensah et al, “Carbon nano tube - reinforced elastomeric nanocomposites: a review” Journal International Journal of Smart and Nano Materials Volume 6, Issue 4, 2015. Disclosed CNT type, surface modification, dispersion of CNT, and processing techniques that affect the physical properties of CNT-elastomeric polymer nanocomposites, and several key physical properties, including tensile, electrical, and thermal properties, were also included in this review. Some of the key challenges that undermine the effectiveness of CNTs and their composites with elastomeric polymers, and the potential applications of CNT-elastomeric composites are also captured.
Nakaramontri,et al. (2014), titled “The effect of surface functionalization of carbon nanotubes on properties of natural rubber/carbon nanotube composites”, Polymer Composites, 36, 10.1002/pc.23122. article entitled “The effect of surface functionalization of carbon nanotubes on properties of natural rubber/carbon nano tube composites” prepared natural rubber composites filled with carbon nano tubes (CNTs) that show an electrical percolation threshold at very low CNT concentrations.
Sanjib Bhattacharyya et al, Carbon Volume 46, Issue 7, June 2008, Pages 1037-1045, 31 January 2008, Titled “Improving reinforcement of natural rubber by networking of activated carbon nanotubes” achieved reinforcement of natural rubber using carboxylated multiwalled carbon nanotubes (c-MWCNT) dispersed with sodium dodecyl sulfate. The structure of the reinforced latex films was investigated by TEM and AFM.
Sui, G. & Zhong, W. & Yang, X.P. & Yu, Y. (2008)., Curing kinetics and mechanical behavior of natural rubber reinforced with pretreated carbon nanotubes. A-structural Materials Properties Microstructure and Processing - MATER SCI ENG A-STRUCT MATER,485, 524-531. Materials Science and Engineering. 10.1016/j.msea.2007.09.007 discloses curing kinetics and vulcanizate properties of carbon nanotubes (CNTs)/natural rubber (NR) nanocomposites. The pretreatment of CNTs was carried out by acid bath followed by ball milling with HRH bonding systems in experiments.
G.Sui, W.H.Zhong, X.P.Yang, Y.H.Yu ., Materials Science and Engineering: A Volume 485, Issues 1–2, Pages 524-53120. The CNT/NR nanocomposites were prepared through solvent mixing on the basis of pretreatment of CNTs. The surface characteristic of CNTs and physical interaction between CNTs and NR macromolecules were analyzed by Fourier transform infrared spectroscopy (FT-IR).
Bokobza et al., Vol.6, No.3, 213–223, 2012., titled “Multiwall carbon nanotube-filled natural rubber: Electrical and mechanical properties” talks about the influence of multiwall carbon nanotube (MWNTs) contents on electrical and mechanical properties of MWNTs-reinforced natural rubber (NR) composites.
Y-L. Lu, J. Ma, T-Y. Xu, W-C. Wang, Y. Jiang, L-Q. Zhang, Express Polymer Letters Vol.11, No.1, 21–34, 11 June 2016., titled “Preparation and properties of natural rubber reinforced with polydopamine-coating modified carbon nanotubes” talks about the multi-walled carbon nanotubes (MWCNTs) functionalized by polydopamine (PDA)-coating and mixed with natural rubber (NR) via latex compounding. Mechanical and electrical properties of the nanocomposites were studied.
The function of an elastomeric bladder is very critical as it combines thermal stability with low water vapor transmissibility. It also must possess durability along with good mechanical property. The development of high performance multi-functional rubber nanocomposite as a bladder caters to the stringent industrial needs.
The present invention attempts to overcome these drawbacks by the introduction of polymer-coated carbon nanotubes in bead form as filler.
Hence, the present invention aims to provide a cured elastomeric nanocomposite comprising of polymer - coated carbon nanotubes in bead form having improved mechanical properties, thermal stability, low water vapor transmissibility and high oxygen impermeability.
OBJECTS OF THE INVENTION
It is primary object of the present invention to provide an elastomeric composition for bladder application in tyre curing process.
It is another object of the present invention wherein the elastomeric composite comprises of a nanofiller along with reinforcing filler.
It is another object of the present invention to provide an elastomeric nanocomposite wherein a nanofiller comprises of polymer coated carbon nano tubules or CNT nanotubes in bead form to the properties of the bladder application.
It is another object of the present invention to provide an elastomeric nanocomposite for bladder application having improved mechanical properties, thermal stability, low water vapor transmissibility and high gas impermeability.
It is another object of the present invention to provide an elastomeric nanocomposite for bladder application having superior durability, thermal stability and barrier characteristics.
SUMMARY OF THE INVENTION:
It is the primary aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, comprising of:
one or more elastomeric blends – 100 parts;
a reinforcing filler – 0 – 75 parts;
a nano filler – 0.5 – 10 phr;
cure chemicals – 0 - 10 phr; and
a processing aid – 0 – 20 phr,
wherein the nano reinforcing filler is polymer coated carbon nanotubes in bead form comprising of diameter 1 to 30 nanometers and length range between 50nanometers and 500 micrometers.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the nano filler comprising of polymer coated carbon nanotube selected from one of single walled and multi-walled.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the elastomeric blend comprises of a combination of butyl rubber and chloroprene rubber.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the polymer comprises of butyl rubber, or halobutyl rubber or combinations of butyl rubber and chloroprene rubber, or combination of halobutyl rubber and Natural rubber
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the elastomeric blend comprises of butyl rubber and chloroprene rubber in a weight ratio of 90: 10.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the reinforcing filler is carbon black.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the cure chemicals are selected from one or more of phenolic resin, zinc oxides or sulphur or combinations thereof.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the cure chemicals comprise of zinc oxide and phenolic resin.
It is another aspect of the present invention to provide an elastomeric bladder rubber nanocomposite, wherein the processing aid is castor oil.
It is another aspect of the present invention to provide a process of preparation of an elastomeric bladder rubber nanocomposite, comprising of the steps:
conditioning of nano reinforcing filler by
subjecting the nano reinforcing filler to an initial conditioning comprising pre-drying at a temperature of 60°C - 80°C for 24 hours;
preparation of master batch by
processing using a mixer with rotor speed maintained constantly at
50 – 70 rpm, temperature maintained around 60°C – 80°C and ram pressure maintained at 3.5 – 5 kp / sq. cm;
fill factor of the chamber is maintained between 0.70 and 0.80;
masticating the elastomers for 20 – 40 seconds;
adding pre-conditioned nano reinforcing filler, 50% of total carbon black composition, to the masticated rubber and mixing for a time period of 100 – 140 seconds;
adding remaining 50% of carbon black along with castor oil and mixing for a time period of 130 – 180 seconds;
sweeping off the chemicals from the chamber side walls and further mixing for a time period of 40 – 80 seconds;
dumping of the rubber nanocomposite at temperature range of 145°C - 165°C,
preparation of final batch by
warming of master batch for 0 – 60 seconds;
adding of one or more of phenolic resin, metal oxides and sulfur and mixing for 60 – 100 seconds at 40 – 60 rpm at temperature range between 50°C - 75°C; and
dumping at a temperature range between 100°C and 110°C,
wherein the nano filler is polymer coated carbon nanotubes in bead form comprising of diameter 1 to 30 nanometers and length between 50 and 500 nanometers.
The curatives are preferably selected from zinc oxide and phenolic resin.
It is another aspect of the present invention to provide a process of preparation of elastomeric bladder rubber nanocomposite, wherein nano filler comprising polymer coated carbon nanotube selected from one of single walled and multi-walled.
It is another aspect of the present invention to provide a process of preparation of elastomeric bladder rubber nanocomposite, wherein the process is carried out in a mixer comprising banbury mixer or the like.
DETAILED DESCRIPTION OF THE INVENTION:
The present invention relates to the field of tyres and elastomeric compositions capable of providing products with superior durability, thermal stability and
barrier characteristics.
In accordance with the present invention, there is provided a cured elastomeric nanocomposite comprising of polymer coated carbon nanotubes in bead form comprising of diameter 1 to 30 nanometers and length range between 50 nanometers and 500 micrometers. The developed nanocomposite is capable of yielding products with improved mechanical properties, thermal stability, low water vapor transmissibility and high gas impermeability.
In accordance with the present invention, there is provided an elastomeric bladder rubber nanocomposite comprising of polymer coated carbon nanotubes having diameter 1 – 30 nanometer and length in the range of 50 nanometers and 500 micrometers in any one form of single walled and multi-walled.
In accordance with the present invention, there is provided an elastomeric nanocomposite comprising of elastomeric compounds selected from one or more of butyl rubber, halo butyl rubber, chloroprene rubber, natural rubber and combinations thereof, nano filler carbon black; cure chemical selected from one of phenolic resin, metal oxides, sulphur and combinations thereof; and castor oil as processing aid.
In accordance with the present invention, there is provided an elastomeric nanocomposite composition which consists of one or more elastomers or an elastomeric blend comprising of 100 parts by weight, 0.5 to 10 phr polymer coated carbon nanotubes in bead form having diameter 1 to 30 nanometers and length range between 50 nanometers and 500 micrometers as nano filler.
The bead shape of the polymer coated carbon nanotube used in the current invention helps in good dispersion of the nanomaterial in to the rubber matrix. Carbon nanotubes have been selected for its good thermal properties, barrier properties and compatibility with rubber matrix as compared to other inorganic nanofillers.
An elastomeric bladder rubber nanocomposite composition, according to an embodiment of the present invention, which can be used to produce bladder for tyres of improved durability, consists of elastomeric blend, with 100 parts by weight of elastomers selected from one or more of polymers comprising butyl rubber, halobutyl rubber, chloroprene rubber, natural rubber., preferably comprises 90 parts by weight of butyl rubber and 10 parts by weight of chloroprene rubber; 0.5 to 10 phr of SBR coated carbon nanotubes in bead form having diameter 1 to 30 nanometers and length range between 50 nanometers and 500 micrometers as nano filler.
An elastomeric bladder rubber nanocomposite composition, according to an embodiment of the present invention, also consists of reinforcing filler is carbon black 0 – 75 phr, preferably 45 phr; cure chemicals selected from one of phenolic resin, metal oxides, sulphur and combinations thereof at 0 – 10 phr, preferably combination of zinc oxide and phenolic resin in a weight ratio of 5: 10; and processing aid as castor oil 0 – 20 phr.
Method of preparation of an elastomeric nanocomposite reinforced with polymer coated nanotubes:
An embodiment of the present invention discloses a method of preparation of an elastomeric nanocomposite comprising of polymer coated carbon nanotubes in bead form having diameter of 1 to 30 nanometers and length range between 50 nanometers and 500 micrometers as nano filler. The polymer coated carbon nanotube is selected from one of single walled and multiwalled CNT or carbon nanotubes, with SBR as polymer coating.
The step comprises of:
The process is carried out in a banbury mixer for the purpose of demonstration.
A) Method of preparation of master batch comprising of the steps:
The ingredients are initially mixed in banbury mixer. The rotor speed is maintained constantly at 50 – 70 rpm, preferably at 60 rpm. The mix temperature is maintained around 60 – 80 °C, preferably at 70°C. The ram pressure is maintained at 3.5-5 kp / sq.cm, preferably at 4 kp / sq.cm. The batch weight is decided based on the chamber volume of the mixer. The fill factor of the chamber is maintained at 0.70 – 0.80. The total mixing time of the master batch compound is around 6 minutes. Rubbers (Butyl and chloroprene) are initially masticated for 20-40 seconds, preferably 30 seconds. This also ensures effective blending of rubber i.e., chloroprene with butyl rubber. The nanofiller and processing oil are added to the masticated rubber. The nanofiller (carbon nanotube) and half the loading of carbon black (50%) is loaded to the masticated rubber. Mixing time of 100 – 140 seconds, preferably 120 seconds is given for the chemical mixing. The initial addition of carbon nanotube (CNT) helps in fine dispersion of the nanomaterial into the rubber matrix. The remaining carbon black is added along with processing oil. The mixing time is 130 – 180 seconds, preferably 150 seconds. This is followed by sweeping off the chemicals from the chamber walls and the mixing is further continued for 40 – 80 seconds, preferably 60 seconds. After the completion of the mixing process, the mixed rubber nanocomposite is dumped. The dump temperature of the rubber nanocomposite is
145 °C – 165 °C, preferably 155°C.
B) Final batch mixing comprising of the steps:
Rotor speed is maintained at 40 – 60 rpm, preferably 50 rpm and the mix start temperature are 50 - 75°C, preferably 65°C. The master batch is warmed for 0 – 60 seconds, preferably 30 seconds. The cure chemicals (Zinc oxide and phenolic resin) is
further added and mixed for 60 – 100 seconds, preferably 78 seconds. The dump temperature varies between 100 ° to 110°C.
The present invention will be explained further by examples, but the scope of the present invention, is not limited to these examples.
Table 1
S. No Ingredients Control Trial 1 Trial 2
1 Butyl Rubbera 90.00 90.00 90.00
2 Carbon Black ISAF N220d 45.00 45.00 45.00
3 Castor Oil 5.00 5.00 5.00
4 Chloropreneb 10.00 10.00 10.00
5 CNTc 0.00 1.00 2.00
6 ZnO-White Seale 5.00 5.00 5.00
7 Phenolic Resinf 10.00 10.00 10.00
Total 165.00 166.00 167.00
a. Butyl rubber BK1675N, used as base polymer a co-polymer of isobutylene and isoprene rubber in methyl chloride medium from Neftekhim. ML (1+8) @125°C is 46-56.
b. Bayprene 210,2-chloro-1,3-butadiene emulsion Polymer, from ARLANXEO with ML (1+4) @100°C 48±4.
c. DRF 4110 Durobeads CNT, SBR polymer coated Carbon Nano Tubes which is multi-walled nanofiller having diameter 1-30 nanometer and length 50 nanometer to 500 micrometers from MITSUBISHI CORPORATION.
d. N220 black as a reinforcing filler from BIRLA CARBON
e. Zinc Oxide as a curative from PONDY OXIDES & CHEMICALS Ltd
f. Phenolic Resin as a curative from MANGALAM ORGANICS
TABLE 2
RESULTS
S. No Properties Control Trial 1 Trial 2
1 Tensile Strength 13.27 15.00 15.03
2 Modulus 100% 1.46 2.09 2.35
3 Modulus 300% 4.50 5.46 5.93
4 Tear Strength 0.116 0.125 0.126
5 WVTR 0.399 0.386 0.367
6 OTR 30.65 30.10 29.14
7 Thermal conductivity 0.114 0.180 0.164
INDEX
S. No Properties Control Trial 1 Trial 2
1 Tensile Strength 100 113 113
2 WVTR 100 97 92
3 OTR 100 98 95
4 Thermal conductivity 100 158 144
NOTE:
The results are compared with each other by index value.
In case of tensile strength and thermal conductivity higher the index value the better the property.
In case of WVTR and OTR the lower the value the better the property.
Table 2 shows the comparison results of Control Compound and CNT-filled compound with dosages 1 phr (Trial 1) and 2 phr (Trial 2) on various properties.
1. The tensile strength of the unfilled compound is 13.27 MPa and increases on adding CNT. Tensile strength increases to 15.00 MPa with the addition of 1 phr of CNT and 15.03 MPa with 2 phr of CNT addition, thus, showing an improvement of 13% in both the cases.
2. 100% modulus for the CNT-less bladder compound is 1.46 MPa and increases to 2.09 MPa with 1 phr CNT and 2.35 MPa with 2 phr CNT in the composite. Thus, the improvement seen is 30% and 37% respectively.
3. 300% modulus for the CNT-less bladder compound is 4.5 MPa and increases to 5.46 MPa with 1 phr CNT and 5.93 MPa with 2 phr CNT in the composite and hence, showing an improvement of 21% and 32% respectively.
4. The tear strength for CNT-less composite is 0.116 KN/mm and increases to 0.125 KN/mm with 1 phr and 0.126 KN/mm with 2 phr. Hence there is an improvement of 8% and 9% respectively.
5. The transmissibility rate should be low in bladder application. The transmissibility rate for CNT-less compound is 0.399g/m2.day. With 1 phr of CNT addition the WVTR reduces to 0.386 g/m2.day and 2 phr CNT the WVTR reduces to 0.367 g/m2.day and hence, shows an improvement of 3% and 8% respectively.
6. The permeability rate should be low in bladder application. The CNT-less compound has an OTR of 30.65 cc/m3.day. It reduces to 30.10 cc/ m3.day with 1 phr CNT and 29.14 cc/ m3.day with 2 phr of CNT addition and provides an improvement of 2% and 5% respectively.
7. The current invention relates to a thermally stable elastomeric bladder. The thermal conductivity in the bladder is achieved by the addition of nanofiller - resin coated carbon nanotubes. The thermal conductivity for a regular bladder compound is 0.114 W/mK. On addition of 1 phr of CNT, thermal conductivity increase to 0.180 W/mK and on addition of 2 phr thermal conductivity increases to 0.164 W/mK. Thus, the improvement found is 58% and 44% respectively
STANDARD TESTS AND PROCEDURES
1. Thermal conductivity of the nanocomposites is checked as per ASTM E 1530 which states the measure of heat flow through a material. This test method mainly states the technique for determination of resistance to thermal transition of materials having thickness of 25 mm or less.
2. The tensile strength of a nanocomposite is the measure of maximum tensile stress applied on a material to rupture. The tensile strength is measured as per ASTM D 412 with the help of universal testing machine (model: 5966, Instron, MA, USA).
3. Modulus of an elastomeric material is the stress needed to strain a material. The modulus is measured as per ASTM D 412 in universal testing machine (model: 5966, Instron, MA, USA).
4. The tear strength of an elastomeric material is the maximum force required to cause a nick to grow by tearing them. The standard used for finding tear strength is ASTM D 624 with universal testing machine (model: 5966, Instron, MA, USA).
5. The oxygen permeability in a sample is measured as per standard ASTM F 1927-14. Oxygen transmissibility rate (OTR) is defined as the quantity of oxygen gas that passes through a unit area of a surface per unit time at a given temperature and relative humidity. The permeability rate should be low in case of bladder application.
6. The water vapor transmissibility rate (WVTR) is the rate of water vapor flow normal to the surface under steady state condition. It is tested as per ASTM F 1249-13. The transmissibility rate should be low in bladder application.
Advantages:
1. The invention is to provides an elastomeric nanocomposite comprising multi-walled, SBR coated carbon nano tubes in bead form as a nano-filler
2. The cured elastomeric nanocomposite comprising of CNT provides improved thermal conductivity.
3. The cured elastomeric nanocomposite comprising of CNT provides improved tensile strength as compared to the control compound.
4. The cured elastomeric nanocomposite comprising of CNT provides improved tear strength as compared to the control compound.
5. The cured elastomeric nanocomposite comprising of CNT shows improvement in 100% modulus as compared to the control compound.
6. The cured elastomeric nanocomposite comprising of CNT shows improvement in 300% modulus as compared to the control compound.
7. The cured elastomeric nanocomposite comprising of CNT provides higher air impermeability as compared to the control compound.
8. The cured elastomeric nanocomposite comprising CNT allows lower water vapor transmissibility as compared to the control compound. ,CLAIMS:WE CLAIM:
1. An elastomeric bladder rubber nanocomposite, comprising of:
one or more elastomers – 100 parts;
a reinforcing filler – 0-75 phr;
a nano filler –0.5-10 phr;
cure chemicals – 0-10 phr; and
a processing aid – 0-20 phr,
wherein the nano filler is polymer coated carbon nanotubes in bead form comprising of diameter 1 to 30 nanometers and length range between 50 and 500 nanometers.
2. The elastomeric bladder rubber nanocomposite as claimed in claim 1, wherein the said nano filler is either single walled or multi-walled SBR coated carbon nanotube.
3. The elastomeric bladder rubber nanocomposite as claimed in claim 1, wherein said elastomer blend comprises of butyl rubber and chloroprene rubber in the ratio of 90:10 parts by weight.
4. The elastomeric bladder rubber nanocomposite as claimed in claim 2, wherein the polymer comprises of butyl rubber, or halobutyl rubber or combinations of butyl rubber and chloroprene rubber, or combination of halobutyl rubber and Natural rubber.
5. The elastomeric bladder rubber nanocomposite as claimed in claim 1, wherein said reinforcing filler is carbon black.
6. The elastomeric bladder rubber nanocomposite as claimed in claim 1, wherein said cure chemicals are selected from phenolic resin or metal oxides or sulphur or combinations thereof.
7. The elastomeric bladder rubber nanocomposite as claimed in claim 1, wherein said processing aid is castor oil.
8. A process of preparation of an elastomeric bladder rubber nanocomposite comprising of the steps:
conditioning of a nano filler by subjecting it to an initial pre-drying at a temperature of 60°C – 80°C for 24 hours;
Preparation of master batch by
processing using a mixer with rotor speed maintained constantly at 50 - 70 rpm, temperature maintained around 60°C – 80°C and ram pressure maintained at 3.5 - 5 kp/sq.cm;
fill factor of the chamber is maintained between 0.70 and 0.80;
masticating elastomers for 20 - 40 seconds;
adding pre-conditioned nano reinforcing filler, 50 % of total carbon black composition, to the masticated rubber and mixing for a time period of 100 – 140 seconds; adding remaining 50 % of carbon black along with castor oil and mixing for a time period of 130 - 180 seconds;
sweeping off the chemicals from the chamber side walls and further mixing for a time period of 40 - 80 seconds;
dumping of the rubber nanocomposite at temperature range of 145°C – 165°C,
Preparation of final batch by
warming of master batch for 0 - 60 seconds;
adding zinc oxide and phenolic resin as curatives and mixing for 60 - 100 seconds at 40 - 60 rpm at temperature range of 50°C – 75°C; and
dumping at a temperature range between 100°C and 110 °C,
wherein the nano reinforcing filler is polymer coated single walled or multi-walled carbon nano tubes in bead form comprising of diameter 1 to 30 nanometers and length between 50 and 500 nanometers.
9. A process of preparation of an elastomeric bladder rubber nanocomposite as claimed in claim 8, wherein the process is carried out in a mixer comprising banbury mixer or the like.
10. The process of preparation of an elastomeric bladder rubber nanocomposite as claimed in claim 8, wherein the polymer elastomer comprises of butyl rubber, or halobutyl rubber or combinations blends of butyl rubber and chloroprene rubber, or blends of halobutyl rubber and Natural rubber.
11. The elastomeric bladder rubber nanocomposite as claimed in claim 6, wherein said cure chemicals comprises of zinc oxide ZnO: phenolic resin of 5:10.
| Section | Controller | Decision Date |
|---|---|---|
| # | Name | Date |
|---|---|---|
| 1 | 201941009087-IntimationOfGrant03-09-2024.pdf | 2024-09-03 |
| 1 | 201941009087-STATEMENT OF UNDERTAKING (FORM 3) [08-03-2019(online)].pdf | 2019-03-08 |
| 2 | 201941009087-PatentCertificate03-09-2024.pdf | 2024-09-03 |
| 2 | 201941009087-PROVISIONAL SPECIFICATION [08-03-2019(online)].pdf | 2019-03-08 |
| 3 | 201941009087-Response to office action [02-09-2024(online)].pdf | 2024-09-02 |
| 3 | 201941009087-POWER OF AUTHORITY [08-03-2019(online)].pdf | 2019-03-08 |
| 4 | 201941009087-Written submissions and relevant documents [30-07-2024(online)].pdf | 2024-07-30 |
| 4 | 201941009087-FORM 1 [08-03-2019(online)].pdf | 2019-03-08 |
| 5 | 201941009087-DECLARATION OF INVENTORSHIP (FORM 5) [08-03-2019(online)].pdf | 2019-03-08 |
| 5 | 201941009087-Correspondence to notify the Controller [16-07-2024(online)].pdf | 2024-07-16 |
| 6 | Correspondence by Agent_Form1 And POA_11-03-2019.pdf | 2019-03-11 |
| 6 | 201941009087-Correspondence to notify the Controller [15-07-2024(online)].pdf | 2024-07-15 |
| 7 | 201941009087-PostDating-(04-03-2020)-(E-6-48-2020-CHE).pdf | 2020-03-04 |
| 7 | 201941009087-FORM-26 [15-07-2024(online)].pdf | 2024-07-15 |
| 8 | 201941009087-US(14)-HearingNotice-(HearingDate-16-07-2024).pdf | 2024-06-12 |
| 8 | 201941009087-APPLICATIONFORPOSTDATING [04-03-2020(online)].pdf | 2020-03-04 |
| 9 | 201941009087-CLAIMS [02-09-2023(online)].pdf | 2023-09-02 |
| 9 | 201941009087-Information under section 8(2) [15-04-2020(online)].pdf | 2020-04-15 |
| 10 | 201941009087-ENDORSEMENT BY INVENTORS [15-04-2020(online)].pdf | 2020-04-15 |
| 10 | 201941009087-FER_SER_REPLY [02-09-2023(online)].pdf | 2023-09-02 |
| 11 | 201941009087-CORRESPONDENCE-OTHERS [15-04-2020(online)].pdf | 2020-04-15 |
| 11 | 201941009087-FER.pdf | 2023-03-03 |
| 12 | 201941009087-COMPLETE SPECIFICATION [15-04-2020(online)].pdf | 2020-04-15 |
| 12 | 201941009087-Proof of Right [20-04-2022(online)].pdf | 2022-04-20 |
| 13 | 201941009087-FORM 18 [01-06-2021(online)].pdf | 2021-06-01 |
| 14 | 201941009087-COMPLETE SPECIFICATION [15-04-2020(online)].pdf | 2020-04-15 |
| 14 | 201941009087-Proof of Right [20-04-2022(online)].pdf | 2022-04-20 |
| 15 | 201941009087-CORRESPONDENCE-OTHERS [15-04-2020(online)].pdf | 2020-04-15 |
| 15 | 201941009087-FER.pdf | 2023-03-03 |
| 16 | 201941009087-ENDORSEMENT BY INVENTORS [15-04-2020(online)].pdf | 2020-04-15 |
| 16 | 201941009087-FER_SER_REPLY [02-09-2023(online)].pdf | 2023-09-02 |
| 17 | 201941009087-Information under section 8(2) [15-04-2020(online)].pdf | 2020-04-15 |
| 17 | 201941009087-CLAIMS [02-09-2023(online)].pdf | 2023-09-02 |
| 18 | 201941009087-APPLICATIONFORPOSTDATING [04-03-2020(online)].pdf | 2020-03-04 |
| 18 | 201941009087-US(14)-HearingNotice-(HearingDate-16-07-2024).pdf | 2024-06-12 |
| 19 | 201941009087-PostDating-(04-03-2020)-(E-6-48-2020-CHE).pdf | 2020-03-04 |
| 19 | 201941009087-FORM-26 [15-07-2024(online)].pdf | 2024-07-15 |
| 20 | Correspondence by Agent_Form1 And POA_11-03-2019.pdf | 2019-03-11 |
| 20 | 201941009087-Correspondence to notify the Controller [15-07-2024(online)].pdf | 2024-07-15 |
| 21 | 201941009087-DECLARATION OF INVENTORSHIP (FORM 5) [08-03-2019(online)].pdf | 2019-03-08 |
| 21 | 201941009087-Correspondence to notify the Controller [16-07-2024(online)].pdf | 2024-07-16 |
| 22 | 201941009087-Written submissions and relevant documents [30-07-2024(online)].pdf | 2024-07-30 |
| 22 | 201941009087-FORM 1 [08-03-2019(online)].pdf | 2019-03-08 |
| 23 | 201941009087-Response to office action [02-09-2024(online)].pdf | 2024-09-02 |
| 23 | 201941009087-POWER OF AUTHORITY [08-03-2019(online)].pdf | 2019-03-08 |
| 24 | 201941009087-PROVISIONAL SPECIFICATION [08-03-2019(online)].pdf | 2019-03-08 |
| 24 | 201941009087-PatentCertificate03-09-2024.pdf | 2024-09-03 |
| 25 | 201941009087-IntimationOfGrant03-09-2024.pdf | 2024-09-03 |
| 25 | 201941009087-STATEMENT OF UNDERTAKING (FORM 3) [08-03-2019(online)].pdf | 2019-03-08 |
| 1 | 201941009087_searchstrategyE_02-03-2023.pdf |