# US 11,299,565 B2 · Method of preparing conjugated diene-based polymer and apparatus for preparing conjugated diene-based polymer > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,299,565 B2 - Document ID: US11299565B2 - Status: Granted - Kind: B2 - Application number: 16/489,544 - Filed: 2019-01-11 - Published: 2019-12-26 - Granted: 2022-04-12 - Earliest claimed: 2018-02-09 - Assignees: LG Chem, Ltd. - Applicants: LG Chem, Ltd. - Inventors: Hoi In Jeong; Jun Seok Ko; Woo Sung Hwang; Dong Min Kim; Jeong Seok Lee - Web page: https://patentgrep.com/patent/US11299565B2 ## CPC - C08F 6/003: {from polymer solutions, suspensions, dispersions or emulsions without recovery of the polymer therefrom} - C08F 36/04: conjugated - C08F 2/01: characterised by special features of the polymerisation apparatus used - C08F 2/04: Polymerisation in solution (C08F2/32 takes precedence) - C08F 4/52: selected from boron, aluminium, gallium, indium, thallium or rare earths (C08F4/14 takes precedence) - C08F 4/619: Component covered by group C08F4/60 containing a transition metal-carbon bond {(C08F4/60003 - C08F4/60196 take precedence)} - C08F 236/06: Butadiene - C08F 236/10: with vinyl-aromatic monomers - B01D 3/14: Fractional distillation {or use of a fractionation or rectification column} - C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) ## Abstract A method of preparing a conjugated diene-based polymer is provided including: a step of polymerizing a first conjugated diene-based monomer in solution in a first polymerization reactor to prepare a first polymer solution including a first conjugated diene-based polymer; a step of polymerizing a second conjugated diene-based monomer in solution in a second polymerization reactor to prepare a second polymer solution including a second conjugated diene-based polymer; a step of supplying a first fluid separated from the first polymer solution to a first purification unit and purifying the first fluid; and a step of supplying a second fluid separated from the second polymer solution to a second purification unit and purifying the second fluid. An apparatus for preparing a conjugated diene-based polymer is also provided. ## Claims ### Claim 1 A method of preparing a conjugated diene-based polymer, comprising: polymerizing a first conjugated diene-based monomer in solution in a first polymerization reactor to prepare a first polymer solution including a first conjugated diene-based polymer (S10); polymerizing a second conjugated diene-based monomer in solution in a second polymerization reactor to prepare a second polymer solution including a second conjugated diene-based polymer (S20); supplying a first fluid separated from the first polymer solution to a first purification unit and purifying the first fluid (S30); and supplying a second fluid separated from the second polymer solution to a second purification unit and purifying the second fluid (S40), wherein the first purification unit comprises a first feed tank, a first column connected to the first feed tank, and a first′ column connected to the first column, the second purification unit comprises a second feed tank, a second column connected to the second feed tank, and a second′ column connected to the second column, a fluid discharged from an upper portion of the first column is supplied to the second feed tank, and the first feed tank is supplied with a third fluid from the second feed tank. ### Claim 2 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein the first conjugated diene-based polymer is prepared in a solvent having a purity of 99.5% or more, and the second conjugated diene-based polymer is prepared in a solvent having a purity of 95.0% or more. ### Claim 3 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein the first conjugated diene-based polymer is a lanthanide rare earth element compound catalyzed conjugated diene-based polymer or an alkali metal compound catalyzed conjugated diene-based polymer, and the second conjugated diene-based polymer is a transition metal compound catalyzed conjugated diene-based polymer. ### Claim 4 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein the fluid discharged from the upper portion of the first column includes C4 compounds and a solvent, and the solvent is included at 10 wt % or more based on a total content of the fluid. ### Claim 5 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein a fluid discharged from a lower portion of the first column is supplied to the first′ column, and the fluid discharged from the lower portion of the first column includes less than 0.5 wt % of C4 compounds. ### Claim 6 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein a fluid discharged from the lower portion of the first column is supplied to the first′ column, and the fluid discharged from the lower portion of the first column includes 0.21 wt % or less of C4 compounds. ### Claim 7 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein a fluid discharged from the lower portion of the first column is supplied to the first′ column, and the fluid discharged from the lower portion of the first column includes less than 40 ppm of moisture. ### Claim 8 (depends on 7) The method of preparing a conjugated diene-based polymer of claim 7, wherein the fluid discharged from the lower portion of the first column is supplied to the first′ column, and the fluid discharged from the lower portion of the first column includes 25 ppm or less of moisture. ### Claim 9 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, comprising: supplying a fluid discharged from the lower portion of the first column to the first′ column (S50); supplying a fluid discharged from a lower portion of the second column to the second′ column (S60); supplying a solvent purified from the first′ column to the first polymerization reactor (S70); and supplying a solvent purified from the second′ column to the second polymerization reactor (S80). ### Claim 10 An apparatus for preparing a conjugated diene-based polymer, comprising: an apparatus for preparing a first conjugated diene-based polymer comprising a first polymerization reactor for polymerizing a first conjugated diene-based polymer in solution and a first purification unit for purifying a first fluid separated from a first polymer solution prepared in the first polymerization reactor; and an apparatus for preparing a second conjugated diene-based polymer comprising a second polymerization reactor for polymerizing a second conjugated diene-based polymer in solution and a second purification unit for purifying a second fluid separated from a second polymer solution prepared in the second polymerization reactor, wherein the first purification unit comprises a first feed tank, a first column connected to the first feed tank, and a first′ column connected to the first column, the second purification unit comprises a second feed tank, a second column connected to the second feed tank, and a second′ column connected to the second column, an upper portion of the first column is connected to the second feed tank by a connecting pipe for supplying a fluid discharged from the upper portion of the first column to the second feed tank, and the second feed tank is connected to the first feed tank by a connecting pipe for supplying a third fluid to the first feed tank. ### Claim 11 (depends on 10) The apparatus for preparing a conjugated diene-based polymer of claim 10, wherein the first column and the second column comprise a condenser in an upper portion of a tower, respectively. ### Claim 12 (depends on 10) The apparatus for preparing a conjugated diene-based polymer of claim 10, wherein the first column and the second column comprise a reboiler in a lower portion of a tower, respectively. ### Claim 13 (depends on 1) The method of preparing a conjugated diene-based polymer of claim 1, wherein the fluid discharged from the upper portion of the first column includes C4 compounds and a solvent, and the solvent is included at 10 wt % to 80 wt % based on a total content of the fluid.