# US 10,370,479 B2 · Process for making a polymer polyol > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,370,479 B2 - Document ID: US10370479B2 - Status: Granted - Kind: B2 - Application number: 15/306,338 - Filed: 2015-04-20 - Published: 2017-02-16 - Granted: 2019-08-06 - Earliest claimed: 2014-04-30 - Assignees: BASF SE - Applicants: BASF SE - Inventors: Christian Koenig; Dejan Petrovic; Achim Loeffler; Andreas Bauder; Daniel Freidank; Dirk Opfermann; Isa Alexandra Queiroz Da Fonseca; Caroline Mages-Sauter; Chuan Long Fu; Shu Kui Wang - Web page: https://patentgrep.com/patent/US10370479B2 ## CPC - C08G 18/0876: {the dispersing or dispersed phase being a polyol} - C08F 257/00: Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 - C08G 18/633: {onto polymers of compounds having carbon-to-carbon double bonds} - C08G 18/636: {characterised by the presence of a dispersion-stabiliser} - C08G 18/72: Polyisocyanates or polyisothiocyanates - C08J 3/005: {Processes for mixing polymers} - C08J 3/09: in organic liquids - C08J 9/00: Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof (mechanical aspects of shaping of plastics or substances in a plastic state for the production of porous or cellular articles B29C) - C08L 71/02: Polyalkylene oxides - C08L 75/04: Polyurethanes - C08J 2205/06: Flexible foams - C08J 2371/02: Polyalkylene oxides - C08J 2425/12: with unsaturated nitriles - C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS - C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) - C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06) ## Abstract This invention relates to a continuous process for making a polymer polyol, the polymer polyol produced according to the said process and its applications. ## Claims ### Claim 1 A continuous process for making a polymer polyol, the polymer polyol comprising: particles of a thermoplastic styrene-acrylonitrile-copolymer (TP); at least one polyol (P); and a stabilizer (S); wherein the stabilizer (S) comprises: from 10 to 70% by weight, based on the sum of all components, of at least one polyol P2, and at least one polyol CSP which is a reaction product of at least one macromere M, styrene and acrylonitrile in P2, optionally with an initiator and/or a chain transfer agent, wherein the macromere comprises one or more polymerizable double bonds and one or more hydroxyl-terminated polyether tails, a content of the macromere M in the stabilizer (S) is between 30-70 wt %, based on the sum of all components of the stabilizer, wherein the polyol CSP comprises two or more —OH groups, the process comprising: continuously feeding the TP, the P and the S to an extruder (E) having a plurality of process zones, preparing an initial dispersion of the TP, the P and the S in the extruder (E); continuously passing the initial dispersion obtained in the extruder into at least one rotor-stator device (RS) decoupled from the extruder comprising at least one rotor-stator combination; and cooling the rotor-stator treated dispersion below the glass transition temperature (Tg) of the thermoplastic styrene-acrylonitrile-copolymer (TP) after passing all of the rotor-stators (RS) to obtain the polymer polyol, wherein in the preparation of the initial dispersion, TP is continuously fed into a first process zone Z1 of the extruder E, S is continuously fed into a second process zone Z2 or a later process zone, and P is continuously fed into a process zone following the process zone of addition of S, wherein the terms “first” and “second” refer to a direction of flow of the reaction mixture through the extruder E. ### Claim 2 (depends on 1) The process according to claim 1, wherein there is at least one process zone of the extruder E wherein no components are added between the zone of addition of the stabilizer S and the zone of addition of the polyol P. ### Claim 3 (depends on 1) The process according to claim 1, wherein P is fed into at least two different process zones after the zone of addition of the stabilizer S of the extruder E. ### Claim 4 (depends on 1) The process according to claim 1, wherein the extruder (E) is operated at a barrel temperature in the range of between 160° to 250° C. in at least one of the plurality of process zones. ### Claim 5 (depends on 1) The process according to claim 1, wherein a rotation speed of the extruder (E) is from 400 to 1200 rpm. ### Claim 6 (depends on 1) The process according to claim 1, further comprising removing volatile material in a stripping column or stripping-vessel after the rotor-stator device. ### Claim 7 (depends on 1) The process according to claim 1, wherein at least one of the at least one-level rotor-stator devices (RS) are operated at a set temperature of 160° to 250° C. ### Claim 8 (depends on 1) The process according to claim 1, wherein at least one of the rotor-stator devices (RS) has a circumferential speed in the range of 10 to 60 s−1. ### Claim 9 (depends on 1) The process according to claim 1, wherein at least one of the rotor-stator devices comprises at least two rotor-stator combinations. ### Claim 10 (depends on 9) The process according to claim 9, wherein each single rotor-stator combination of the at least two rotor-stator combinations have differing teeth. ### Claim 11 (depends on 1) The process according to claim 1, wherein the polyol (P) is added to the extruder (E) at a temperature of above 100° C. ### Claim 12 (depends on 1) The process according to claim 1, wherein the stabilizer (S) is added to the extruder (E) at a temperature of above 100° C. ### Claim 13 (depends on 1) The process according to claim 1, wherein the polyol (P) is liquid at room temperature. ### Claim 14 (depends on 1) The process according to claim 1, wherein the polyol (P) is selected from the group of polyols consisting of polyols employed for slabstock foam applications and polyols employed for molded foam applications. ### Claim 15 (depends on 1) The process according to claim 1, wherein an average OH value of the polyol (P) is between 20 and 300 mg KOH/g. ### Claim 16 (depends on 1) The process according to claim 1, wherein an average functionality of the polyol (P) is from 2 to 6. ### Claim 17 (depends on 1) The process according to claim 1, wherein an average particle size of the product according to D50 is below 25 μm, as determined by static laser diffraction. ### Claim 18 (depends on 1) The process according to claim 1, wherein the polyol P2 contained in the stabilizer S is a polyether polyol (PEOL). ### Claim 19 (depends on 1) The process according to claim 1, wherein an average molecular weight of the macromere M is from 1000 to 50000 g/mol. ### Claim 20 (depends on 1) The process according to claim 1, wherein the macromere M is obtained by reaction of 1,1-dimethyl meta isopropenyl benzyl isocyanat (TMI) with a polyether polyol PM, selected from the group consisting of three- and sixfunctional polyether polyols, the reaction optionally conducted in the presence of a Lewis acid catalyst. ### Claim 21 (depends on 1) The process according to claim 1, wherein a ratio of styrene to acrylonitrile in the polyol CSP is greater than 1:1. ### Claim 22 (depends on 1) The process according to claim 1, comprising a chain transfer agent and an initiator in production of the stabilized S wherein the chain transfer agent is selected from the group consisting of dodecane thiol, isopropanol and 2-butanol, and the initiator is selected from the group consisting of azoisobutyro nitrite (AIBN) and Dimethyl 2,2′-azobis(2-methylpropionate). ### Claim 23 (depends on 1) The process according to claim 1, wherein a ratio of styrene to acrylonitrile in the styrene-acrylonitrile-copolymer (TP) is greater than 1:1. ### Claim 24 (depends on 1) The process according to claim 1, wherein the dispersion is cooled below the Tg of the thermoplastic styrene-acrylonitrile-copolymer (TP) within a maximum time range of four hours after passing all of the rotor-stator devices (RS). ### Claim 25 (depends on 1) The process according to claim 1, wherein the dispersion is cooled to a temperature of equal to or less than 60° C., within a maximum time range of four hours after passing all of the rotor-stator devices (RS). ### Claim 26 (depends on 1) The process according to claim 1, wherein a particle size distribution of the polymer polyol is monomodal, bimodal or multimodal. ### Claim 27 (depends on 9) The process according to claim 9, wherein the first rotor-stator combination has coarse teeth, the next rotor-stator combination in the flow direction has medium fine teeth, and the third rotor-stator combination in the flow direction has fine teeth.