# US 5,705,564 A · In-situ stabilized compositions > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,705,564 A - Document ID: US5705564A - Status: Granted - Kind: A - Application number: 08/563,600 - Filed: 1995-11-28 - Granted: 1998-01-06 - Earliest claimed: 1991-09-30 - Assignees: The University of Toronto Innovations Foundation - Inventors: Zhi-Zhong Liang; Raymond T. Woodhams - Web page: https://patentgrep.com/patent/US5705564A ## CPC - C08L 95/00: Compositions of bituminous materials, e.g. asphalt, tar, pitch - C08L 95/005: {Aqueous compositions, e.g. emulsions} - C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06) ## Abstract Insoluble particulate materials, which may be in solid or liquid form, are dispersed in a continuous non-aqueous phase and the dispersion rendered stable and resistant to phase separation by an in-situ stabilization procedure involving the formation of chemical bonds among the stabilizer components and to dispersed phases to form a network surrounding the particles which is compatible with the continuous phase. The invention has particular application for the formation of stabilized polyolefin-modified bitumen compositions for paving and other applications. ## Claims ### Claim 1 A stable composition, comprising: a continuous bitumen phase, a dispersed particulate phase of a polyolefin insoluble in said liquid phase, and a steric stabilizer comprising: (i) a first individual component comprising a functionalized olefin polymer anchored to said particulate phase, (ii) a second individual component different from said first component which is a functionalized diene bonded to said first component by interaction of the functional groups and soluble in said liquid phase, and (iii) an unfunctionalized polydiene which is partially cross-linked with said functionalized diene and itself and which is soluble in or compatible with the bitumen and has a molecular weight of at least about 300 prior to incorporation into said composition, said steric stabilizer maintaining dispersed particles of said particulate phase spaced from each other in said liquid phase, so as to inhibit separation of said particulate phase from said liquid phase by progressive coalescence of dispersed particles. ### Claim 2 (depends on 1) The composition of claim 1, wherein said bitumen comprises an asphalt and said polyolefin comprises a homopolymer and/or copolymer of ethylene. ### Claim 3 (depends on 1) The composition of claim 1, wherein said functionalized diene is an amine terminated polybutadiene, said functionalized olefinic polymer is a carboxylated olefinic polymer and said unfunctionalized polydiene is an unfunctionalized polybutadiene. ### Claim 4 (depends on 3) The composition of claim 3, wherein said olefinic polymer is a polyethylene having a fusion temperature of about 115.degree. to about 130.degree. C. ### Claim 5 (depends on 4) The composition of claim 4, wherein said unfunctionalized polybutadiene has a molecular weight up to about 60,000. ### Claim 6 A composition for forming a stable dispersion of particulate polyolefin in a continuous bitumen phase, which comprises: a pro-steric stabilizer dissolved in bitumen and comprising a bitumen-compatible stabilizer segment which is a functionalized diene bonded to an olefinic polymer-compatible stabilizer segment which is a functionalized olefinic polymer, and an unfunctionalized polydiene which is soluble in or compatible with the bitumen and which has a molecular weight of at least about 300 prior to dissolution in bitumen. ### Claim 7 (depends on 6) The composition claimed in claim 6, wherein said olefinic polymeric material is a homopolymer and/or copolymer of ethylene. ### Claim 8 (depends on 7) The composition of claim 7 wherein said functionalized diene is an amine terminated polybutadiene, said functionalized olefinic polymer is a carboxylated olefinic polymer and said unfunctionalized polydiene is an unfunctionalized polybutadiene. ### Claim 9 (depends on 8) The composition of claim 8, wherein said unfunctionalized polybutadiene has a molecular weight up to about 60,000. ### Claim 10 A method of forming a stable composition, which comprises: dispersing an olefinic polymer in a continuous bitumen phase in which said olefinic polymeric material is insoluble to form a dispersion containing small particles of said olefinic polymer by contacting the olefinic polymer with the bitumen at a temperature above the fusion temperature of the olefinic polymer in the presence of steric stabilization forming components comprising a first individual component comprising a functionalized olefinic polymer for anchoring to the particulate phase, a second individual component different from said first component soluble in said liquid phase which is a functionalized diene, and an unfunctionalized polydiene which is soluble in or compatible with the bitumen and which has a molecular weight of at least about 300, and effecting chemical bonding between said steric stabilizer forming components and bonding to said particulate olefinic polymer to form a steric stabilizer in the form of an envelope surrounding and anchored to each particle in the particulate phase and comprising a cross-linked structure compatible with the liquid phase to maintain said particulate phase spaced apart from each other in said liquid phase. ### Claim 11 (depends on 10) The method of claim 10, wherein said olefinic polymer is a polyethylene having a fusion temperature of about 115.degree. to about 130.degree. C. which permits dispersion of said olefinic polymer as molten droplets in bitumen at a temperature of about 120.degree. to about 190.degree. C. ### Claim 12 (depends on 11) The method of claim 11, wherein said functionalized diene comprises a functionalized polymer of butadiene, said functionalized olefinic polymer comprises a functionalized ethylene polymer, said unfunctionalized polydiene is an unfunctionalized polybutadiene, and said bonding of said components is effected by interaction between amine termination on said butadiene polymer and carboxyl termination on said ethylene polymer. ### Claim 13 (depends on 12) The method of claim 12, wherein said unfunctionalized polybutadiene has a molecular weight of up to about 60,000. ### Claim 14 (depends on 13) The method claimed in claim 13, wherein additional bitumen is added to the bituminous composition. ### Claim 15 A method of forming a bituminous composition, which comprises: (a) dissolving a functionalized diene in bitumen, (b) dispersing a functionalized olefinic polymer in said bitumen, (c) dissolving an unfunctionalized polydiene having a molecular weight of at least about 300 in the bitumen, (d) reacting said functionalized olefinic polymer and said functionalized diene so as to bind one end of said olefinic polymer to said diene; and (e) partially cross-linking said unfunctionalized polydiene with the functionalized diene and itself. ### Claim 16 (depends on 15) The method of claim 15, wherein said functionalized diene is an amine-terminated polybutadiene and said functionalized olefinic polymer is a carboxylated olefinic polymer. ### Claim 17 (depends on 16) The method of claim 16, wherein carboxylated polyethylene, unfunctionalized polybutadiene, amine-terminated polybutadiene and elemental sulfur are dispersed in bitumen at a temperature of about 100.degree. to about 250.degree. C. by mixing until a homogenous composition is formed in about 0.25 to about 2.5 hours. ### Claim 18 (depends on 17) The method claimed in claim 17, wherein said polybutadiene has a molecular weight of up to about 60,000 and is soluble in or compatible with bitumen at a mixing temperature of about 150.degree. to about 200.degree. C. ### Claim 19 (depends on 18) A method of forming a stable dispersion, which comprises dispersing a polyethylene having a melting point of about 115.degree. to about 130.degree. C. in a bituminous composition as claimed in claim 18 at a temperature of about 120.degree. to about 190.degree. C. and above the melting point of the polyethylene to form liquid droplets of the polyethylene in the bitumen.