公开(公告)号：US10370461B2

公开(公告)日：2019-08-06

申请号：US14908872

申请日：2014-07-29

Applicant: BASF SE

Inventor： Pascal Hesse ,  Aleksandra Jelicic ,  Gabriela Eugenia Fonseca Zepeda ,  Robert Haschick ,  Shankara Narayanan Keelapandal Ramamoorthy ,  Gareth Ian Naylor ,  John Scott Barratt ,  Oliver Soetje ,  Marcel Lievre ,  Florian Rainau ,  Mark Lebkuecher

IPC: C08F2/32 ,  C08F220/56 ,  B01J19/10 ,  C08F2/01 ,  C08F220/06 ,  C08F220/20 ,  C08F226/10 ,  C08F220/38

Abstract: A reverse-phase suspension polymerization process for the manufacture of polymer beads comprising forming aqueous monomer beads comprising an aqueous solution of water-soluble ethylenically unsaturated monomer or monomer blend and polymerizing the monomer or monomer blend, to form polymer beads while suspended in a non-aqueous liquid, and recovering polymer beads, in which the process comprises providing in a vessel (1) a volume (2) of non-aqueous liquid wherein the volume of non-aqueous liquid extends between at least one polymer bead discharge point (3) and at least one monomer feed point (4), feeding the aqueous monomer or monomer blend through orifices (5) into, or onto, the non-aqueous liquid to form aqueous monomer beads, allowing the aqueous monomer beads to flow towards the polymer bead discharge point initiating polymerization of the aqueous monomer beads to form polymerizing beads, wherein the polymerizing beads form polymer beads when they reach the polymer bead discharge point, removing a suspension of the polymer beads in non-aqueous liquid from the vessel at the polymer bead discharge point and recovering, water soluble or water swellable polymer beads from the suspension, in which the aqueous monomer or monomer blend and/or the orifices is/are vibrated such that the frequency multiplied by the weight average droplet diameter is between 150 and 800 mm/s. The invention also relates to the apparatus suitable for carrying out a reverse-phase suspension polymerization and polymer beads obtainable by the process or employing the apparatus. Furthermore, the invention also relates to polymer beads having a weight mean particle size in the range of 0.05 to 5 mm which are held in a container in an amount of at least 300 kg having a standard deviation of particle size less than 20%. In addition, the invention also provides polymer beads having a weight mean particle size in the range 0.05 to 5 mm having a standard deviation of particle size less than 20% and having an amount of residual acrylamide of less than 500 ppm.

公开(公告)号：US10604611B2

公开(公告)日：2020-03-31

申请号：US14908823

申请日：2014-07-29

Applicant: BASF SE

Inventor： John Scott Barratt ,  Aleksandra Jelicic ,  Pascal Hesse ,  Oliver Soetje ,  Robert Haschick ,  Gabriela Eugenia Fonseca Zepeda ,  Shankara Narayanan Keelapandal Ramamoorthy ,  Sandra Jeck ,  Jelan Kuhn

IPC: C08F265/04 ,  C08J11/02 ,  C08F2/32 ,  B01J19/12 ,  B01D61/14 ,  B01J19/24 ,  B01J4/00 ,  B01D61/02 ,  C08J3/12 ,  C08F220/56 ,  C08F220/20 ,  C08F220/06 ,  C08F220/38 ,  C08F226/10

Abstract: A reverse-phase suspension polymerisation process for the manufacture of polymer beads comprising forming aqueous monomer beads of an aqueous solution comprising water-soluble ethylenically unsaturated monomer or monomer blend and polymerising the monomer or monomer blend to form polymer beads while suspended in a non-aqueous liquid, recovering polymer beads, and then cleaning the non-aqueous liquid in which the process comprises providing the non-aqueous liquid in a vessel (1), forming a suspension of monomer beads from the aqueous monomer or monomer blend in the non-aqueous liquid, initiating polymerisation to form polymerising beads, removing a suspension of the polymer beads in non-aqueous liquid from the vessel and recovering, water soluble or water swellable polymer beads from the suspension, in which the non-aqueous liquid contains impurities which comprise particles, and then transferring the non-aqueous liquid from the suspension to a cleaning stage, in which the cleaning stage provides a cleaned non-aqueous liquid suitable for use in a reverse-phase suspension polymerisation process, which cleaning stage comprises removing particles from the non-aqueous liquid in at least one filtration step. The invention also relates to the apparatus suitable for carrying out a reverse-phase suspension polymerisation and polymer beads obtainable by the process or employing the apparatus. The invention further relates to a cleaned non-aqueous liquid obtainable by the process.

公开(公告)号：US09963521B2

公开(公告)日：2018-05-08

申请号：US13765031

申请日：2013-02-12

Applicant: BASF SE

Inventor： Thomas Wettling ,  Stefan Hirsch ,  Markus Brym ,  Markus Weis ,  Rosa Corberan Roc ,  Klaus Muehlbach ,  Robert Haschick ,  Andreas Daiss ,  Marco-Christian Volland

IPC: C08F110/10 ,  C08F4/52 ,  C08F4/70

CPC classification number: C08F4/52 ,  C08F4/70 ,  C08F110/10 ,  C08F4/14 ,  C08F2/06 ,  C08F2/38 ,  C08F2500/01 ,  C08F2500/04

Abstract: Preparation of isobutene homopolymers having a weight-average molecular weight of 75 000 to 10 000 000 by polymerization of isobutene, by (a) performing the polymerization at −80° C. to −190° C., (b) using, as an inert solvent, optionally halogenated C1 to C5 hydrocarbons, (c) using, as a polymerization catalyst, a Lewis acid complex, (d) performing the polymerization in the presence of at least one reaction accelerator in the form of an ethylenically saturated hydrocarbon compound comprising one oxygen atom and no abstractable proton, and (e) performing the polymerization in the presence of at least one chain length regulator comprising one tertiary olefinic carbon atom.

公开(公告)号：US09765167B2

公开(公告)日：2017-09-19

申请号：US14908925

申请日：2014-07-29

Applicant: BASF SE

Inventor： Robert Haschick ,  Aleksandra Jelicic ,  John Scott Barratt ,  Pascal Hesse ,  Oliver Soetje ,  Gabriela Eugenia Fonseca Zepeda ,  Shankara Narayanan Keelapandal Ramamoorthy ,  Bjoern Langlotz

IPC: C08F2/46 ,  C08F2/50 ,  C08G61/04 ,  C08F220/56 ,  C08F2/32 ,  B01J19/12 ,  B01J19/24 ,  C08F220/06 ,  C08F220/20 ,  C08F226/10 ,  C08F220/38

CPC classification number: C08F220/56 ,  B01J19/123 ,  B01J19/24 ,  B01J2219/0869 ,  B01J2219/1203 ,  B01J2219/24 ,  C08F2/32 ,  C08F220/06 ,  C08F220/20 ,  C08F226/10 ,  C08F2220/382 ,  C08F2220/385 ,  C08F220/34

Abstract: A reverse-phase suspension polymerization process for the manufacture of polymer beads comprising forming aqueous monomer beads comprising an aqueous solution of water-soluble ethylenically unsaturated monomer or monomer blend and polymerizing the monomer or monomer blend to form polymer beads while suspended in a non-aqueous liquid, and recovering polymer beads, in which the process comprises, providing in a vessel (1) a volume (2) of non-aqueous liquid wherein the volume of non-aqueous liquid extends between at least one polymer bead discharge point (3) and at least one monomer feed point (4), feeding the aqueous monomer or monomer blend through orifices (5) into, or onto, the non-aqueous liquid to form aqueous monomer beads, allowing the aqueous monomer beads to flow towards the polymer bead discharge point subjecting the aqueous monomer beads to polymerization conditions to initiate polymerization to form polymerizing beads, wherein the polymerizing beads have formed polymer beads when they reach the polymer bead discharge point, removing a suspension of the polymer beads in non-aqueous liquid from the vessel at the polymer bead discharge point and recovering water soluble or water swellable polymer beads from the suspension. The invention also relates to the apparatus suitable for carrying out a reverse-phase suspension polymerization and polymer beads obtainable by the process or employing the apparatus.