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US3922255A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of producing uniform polymer beads

Assignee: Rohm and Haas Co
•
Filing: 1974-06-03
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Granted: 1975-11-25
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Expires: 1994-06-03
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Abstract

Abstract This invention relates to methods of carrying out the polymerization of polymerizable liquids in suspension in an immiscible aqueous medium and concurrently forming solid polymer beads of controllable uniform size.

Inventors

  • 👤 Donald J Koestler
  • 👤 Melvin Barry Robin

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 02:36
CPC Classifications
C; C08; C08F; C08F2/00; C08F2/12; C08F2/16; C08F2/18

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 406 words
A METHOD OF SUSPENSION POLYMERIZATION FOR PROVIDING SUBSTANTIALLY UNIFORM PARTICLES OF POLYMER BEADS COMPRISING A POLYMER OR COPOLYMER DERIVED FROM THE MONOMERS SUITABLE FOR SUSPENSION POLYMERIZATION AND SELECTED FROM ONE OR MOR OF A MONOVINYL MONOMER AND A POLYVINYL MONOMER, WHICH COMPRISES: A. FORMING A FIRST FEED VESSEL A LIQUID MIXTURE OF THE POLYMERIZABLE MONOMER OR MONOMERS, AND A SUITABLE POLYMERIZATION INITIATOR, AT A TEMPERATURE LEVEL WHICH ESSENTIALLY INHIBITS THE INITIATION OF POLYMERIZATION; B. SEPARATELY PREPARING IN A SECOND FEED VESSEL AN AQUEOUS LIQUID THAT IS SUITABLE FOR MAINTAIN A DISPERSION OF LIQUID DROPLETS OF SAID MONOMER MIXTURE; C. PASSING THE MONOMER CONTAINING LIQUID FROM SAID FIRST VESSEL THROUGH A FIRST CONDUIT INTO ONE END OF A FIRST COLUMN TO FLOW THERETHROUGH; D. PASSING SAID MONOMER LIQUID INTO SAID COLUMN THROUGH A MECHANICAL MEANS HAVING A PLURALITY OF ORIFICES EACH HAVING A DIAMETER SIZE RANGING FROM 0.004 TO 0.015 INCHES WITH A JET VELOCITY RANGING FROM 0.25 TO 10.00 CC/MINUTE/ORIFICE; E. CONCURRENTLY PASSING THE AQUEOUS LIQUID, WHICH IS SUBSTANTIALLY IMMISCIBLE WITH SAID MONOMER, FROM SAID SECOND VESSEL THROUGH A SECOND CONDUIT TO SAID FIRST COLUMN AT A RATE SUFFICIENT TO STABILIZED THE MONOMER DROPLETS, WHERE THE EFFLUENT OF SAID SECOND CONDUIT IS IN CLOSE PROXIMITY TO SAID EFLUENT OF THE FIRST CONDUIT; F. PASSING THE DROPLET-CONTAINING THIRD LIQUID FROM THE OTHER END OF SAID FIRST COLUMN THROUGH A THIRD CONDUIT INTO THE UPPER SECTION OF A SECOND COLUMN TO FLOW THERETHROUGH AT A TEMPERATURE TO INITIATE POLYMERIZATION OF MONOMER WITHIN THE DROPLETS; G. PASSING THE DROPLET-CONTAINING THIRD LIQUID FROM THE OTHER SECOND COLUMN VIA A FOURTH CONDUIT A DOWNFLOWING AQEOUS STREAM AT A FLOW RATE WHICH WILL ALLOW THE MORE BUOYANT MONOMER DROPLETS RESIDENCE TIME SUFFICIENT TO REACH A POINT OF POLYMERIZATION WHEREBY THE DEOPLETS WILL NO LONGER LOSE THEIR PARTICULATE IDENTITY AS BEADS; H. ALLOWING THE PARTIALLY POLYMERIZED DROPLETS WHILE DISPERSED IN THE AQUEOUS LIQUID TO FLOW FROM THE LOWER SECTION OF SAID SECOND COMUMN THROUGH A FIFTH CONDIUT TO A SYSTEM FOR GRAVITY SEPARATION AND FOR CONCENTRATING SAID BEADS IN SAID AQUEOUS LIQUID; I. ALLOWING A COMPARATIVELY CONCENTRATED SLURRY OF SAID BEADS TO FLOW FROM SAID SEPARATION SYSTEM THROUGH A SIXTH CONDUIT TO A POLYMERIZATION ZONE WHEREIN SAID BEADS ARE FURTHER POLYMERIZED TO THE EXTENT DESIRED UNDER TEMPERATURE CONDITIONS SUITABLE TO THAT PURPOSE; AND J. TRANSFERRING THE POLLYMERIZED BEADS FROM THE LOWER PORTION OF SAID POLYMERIZATION ZONE THROUGH A SEVENTH CONDUIT FOR FURTHER PROCESSING.
Claim 2
Independent Claim 406 words
A METHOD OF SUSPENSION POLYMERIZATION FOR PROVIDING SUBSTANTIALLY UNIFORM PARTICLES OF POLYMER BEADS COMPRISING A POLYMER OR COPOLYMER DERIVED FROM THE MONOMERS SUITABLE FOR SUSPENSION POLYMERIZATION AND SELECTED FROM ONE OR MOR OF A MONOVINYL MONOMER AND A POLYVINYL MONOMER, WHICH COMPRISES: A. FORMING A FIRST FEED VESSEL A LIQUID MIXTURE OF THE POLYMERIZABLE MONOMER OR MONOMERS, AND A SUITABLE POLYMERIZATION INITIATOR, AT A TEMPERATURE LEVEL WHICH ESSENTIALLY INHIBITS THE INITIATION OF POLYMERIZATION; B. SEPARATELY PREPARING IN A SECOND FEED VESSEL AN AQUEOUS LIQUID THAT IS SUITABLE FOR MAINTAIN A DISPERSION OF LIQUID DROPLETS OF SAID MONOMER MIXTURE; C. PASSING THE MONOMER CONTAINING LIQUID FROM SAID FIRST VESSEL THROUGH A FIRST CONDUIT INTO ONE END OF A FIRST COLUMN TO FLOW THERETHROUGH; D. PASSING SAID MONOMER LIQUID INTO SAID COLUMN THROUGH A MECHANICAL MEANS HAVING A PLURALITY OF ORIFICES EACH HAVING A DIAMETER SIZE RANGING FROM 0.004 TO 0.015 INCHES WITH A JET VELOCITY RANGING FROM 0.25 TO 10.00 CC/MINUTE/ORIFICE; E. CONCURRENTLY PASSING THE AQUEOUS LIQUID, WHICH IS SUBSTANTIALLY IMMISCIBLE WITH SAID MONOMER, FROM SAID SECOND VESSEL THROUGH A SECOND CONDUIT TO SAID FIRST COLUMN AT A RATE SUFFICIENT TO STABILIZED THE MONOMER DROPLETS, WHERE THE EFFLUENT OF SAID SECOND CONDUIT IS IN CLOSE PROXIMITY TO SAID EFLUENT OF THE FIRST CONDUIT; F. PASSING THE DROPLET-CONTAINING THIRD LIQUID FROM THE OTHER END OF SAID FIRST COLUMN THROUGH A THIRD CONDUIT INTO THE UPPER SECTION OF A SECOND COLUMN TO FLOW THERETHROUGH AT A TEMPERATURE TO INITIATE POLYMERIZATION OF MONOMER WITHIN THE DROPLETS; G. PASSING THE DROPLET-CONTAINING THIRD LIQUID FROM THE OTHER SECOND COLUMN VIA A FOURTH CONDUIT A DOWNFLOWING AQEOUS STREAM AT A FLOW RATE WHICH WILL ALLOW THE MORE BUOYANT MONOMER DROPLETS RESIDENCE TIME SUFFICIENT TO REACH A POINT OF POLYMERIZATION WHEREBY THE DEOPLETS WILL NO LONGER LOSE THEIR PARTICULATE IDENTITY AS BEADS; H. ALLOWING THE PARTIALLY POLYMERIZED DROPLETS WHILE DISPERSED IN THE AQUEOUS LIQUID TO FLOW FROM THE LOWER SECTION OF SAID SECOND COMUMN THROUGH A FIFTH CONDIUT TO A SYSTEM FOR GRAVITY SEPARATION AND FOR CONCENTRATING SAID BEADS IN SAID AQUEOUS LIQUID; I. ALLOWING A COMPARATIVELY CONCENTRATED SLURRY OF SAID BEADS TO FLOW FROM SAID SEPARATION SYSTEM THROUGH A SIXTH CONDUIT TO A POLYMERIZATION ZONE WHEREIN SAID BEADS ARE FURTHER POLYMERIZED TO THE EXTENT DESIRED UNDER TEMPERATURE CONDITIONS SUITABLE TO THAT PURPOSE; AND J. TRANSFERRING THE POLLYMERIZED BEADS FROM THE LOWER PORTION OF SAID POLYMERIZATION ZONE THROUGH A SEVENTH CONDUIT FOR FURTHER PROCESSING.
Claim 3
Dependent Claim 38 words
The process of claim 1 wherein the excess aqueous phase formed in said gravity separation system is recycled to and through said second column via an eighth conduit, thereby providing the stream that drives the droplets downwardly therethrough.
Claim 4
Dependent Claim 30 words
The method of claim 2 wherein said excess aqueous stream is passed through a surge and settling means before entering said second column, whereby extraneous polymeric particles are substantially removed.
Claim 5
Dependent Claim 37 words
The method of claim 1 wherein said plurality of droplets are formed from filaments issuing at a jet velocity ranging from 0.8 to 5.0 cc/min/orifice whereby breakup of the filaments results in the formation of said droplets.
Claim 6
Dependent Claim 27 words
The method of claim 1 wherein the polymer leaving said polymerization zone is subjected to chemical treatment to enhance its properties as a selective ion exchange resin.
Claim 7
Dependent Claim 20 words
The method of claim 1 wherein four monomers are incorporated into said liquid mixture formed in said first feed vessel.
Claim 8
Dependent Claim 16 words
The method of claim 1 wherein said monomer mixture comprises styrene, divinylbenzene, acrylonitrile, and Methyl acrylate.
Claim 9
Dependent Claim 27 words
The method of claim 1 in which said monovinyl monomer component is selected from one of styrene, Alpha -methylstyrene, ethylstyrene, chlorostyrene, methyl acrylate, acrylonitrile, and vinylbenzyl chloride.
Claim 10
Dependent Claim 30 words
The method of claim 1 in which said polyvinyl monomer component is selected from one of divinylbenzene, trimethylolpropane, trimethacrylate, trimethylolpropane dimethacrylate, pentaerythritrol trimethacrylate, pentaerythritol tetramethacrylate, pentaerythritol dimethacrylate, and neopentyl dimethacrylate.
Claim 11
Dependent Claim 18 words
The method of claim 1 in which the mechanical means to extrude said monomers is a perforated disc.
Claim 12
Dependent Claim 29 words
The method of claim 1 wherein said aqueous liquid of step (b) contains poly(sodium acrylate) and hydrolyzed animal protein buffered with sodium borate within the pH range of 6-12.

References Cited (Backward Citations)

US2618626A Cited
US2694700A Cited
US2813850A Cited
US2715118A Cited
US3042970A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-11-24 1979-05-26 1979-11-25 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-11-24 1983-05-26 1983-11-25 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-11-24 1987-05-26 1987-11-25 $7700.00 Window Closed / Lapsed

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