Patent US4619979A successfully refreshed from Google Patents.
US4619979A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Continuous free radial polymerization in a wiped-surface reactor
Assignee: 3M Co
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Filing: 1984-03-28
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Granted: 1986-10-28
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Expires: 2004-03-28
Abstract
Abstract A bulk polymerization process for free radical polymerization of vinyl monomers in a wiped surface reactor is disclosed. Referring to FIG. 1; monomer streams 5 (after purification and silica gel column 2) and 7 are combined with free radical initiator 9 to form a premix 16. Pump 18 transfers the premix stream 22 through static mixer 24 into a wiped surface reactor 27. The reactor can be a counter rotating twin screw extruder which produces polymer stream 36 without the need of solvent and using residence times much shorter than prior art solution or emulsion processes. Some unique pressure sensitive adhesive acrylate polymers have been produced. They are believed to have a relatively high degree of branching. The bulk polymerization process permits the manufacture of pressure sensitive adhesive articles by extruding directly from the twin screw extruder onto a substrate.
Inventors
- 👤 Thomas A. Kotnour
- 👤 Ronald L. Barber
- 👤 Walter L. Krueger
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 10:59
CPC Classifications
C; C08; C08F; C08F2/00; C08F2/02; C09; C09J; C09J7/00; C09J7/30; C09J7/38; C09J7/381
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
193 words
A process of making a pressure sensitive adhesive composition by bulk polymerizing one or more free radical polymerizable vinyl compounds which comprises: (a) continuously feeding to a wiped surface reactor comprising a vessel and at least one rotor inside the vessel having a wiping portion located close to the inside surface of the vessel and a root portion spaced substantially further from the inside surface than the wiping portion wherein the root surface is wiped continuously during rotation of the rotor raw materials which comprise unpolymerized vinyl compounds without any substantial amount of polymerized vinyl compounds, and at least two initiators for free radical polymerization under the following conditions: (i) all raw materials being fed substantially free of oxygen, and (ii) at least one monomer being a liquid unpolymerized vinyl compound having a viscosity less than about 4,000 centipoise which is fed under a pressure at least as high as the vapor pressure of the combined raw materials at the temperature to which the exotherm of the free radical polymerization brings them in the reactor; (b) reacting the raw materials to desired conversion; and (c) continuously withdrawing a polymeric material from the reactor.
Claim 2
Dependent Claim
193 words
A process of making a pressure sensitive adhesive composition by bulk polymerizing one or more free radical polymerizable vinyl compounds which comprises: (a) continuously feeding to a wiped surface reactor comprising a vessel and at least one rotor inside the vessel having a wiping portion located close to the inside surface of the vessel and a root portion spaced substantially further from the inside surface than the wiping portion wherein the root surface is wiped continuously during rotation of the rotor raw materials which comprise unpolymerized vinyl compounds without any substantial amount of polymerized vinyl compounds, and at least two initiators for free radical polymerization under the following conditions: (i) all raw materials being fed substantially free of oxygen, and (ii) at least one monomer being a liquid unpolymerized vinyl compound having a viscosity less than about 4,000 centipoise which is fed under a pressure at least as high as the vapor pressure of the combined raw materials at the temperature to which the exotherm of the free radical polymerization brings them in the reactor; (b) reacting the raw materials to desired conversion; and (c) continuously withdrawing a polymeric material from the reactor.
Claim 3
Dependent Claim
19 words
The process of claim 1 wherein the feed pressure of part (ii) is at least about 240 kiloPascals absolute.
Claim 4
Dependent Claim
18 words
The process of claim 1 wherein the vinyl compounds are fed to the reactor without diluents or solvents.
Claim 5
Dependent Claim
34 words
The process of claim 1 in which the vinyl compounds and initiators are mixed together to form a premix prior to feeding them to the reactor, and in which said premix is a liquid.
Claim 6
Dependent Claim
47 words
The process of claim 1 wherein the vinyl compounds are selected from the group consisting of 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate, lauryl methacrylate, methylbutylacrylate, n-butylacrylate, butylmethacrylate, isooctylacrylate, n-octylmethacrylate, acrylic acid, methacrylic acid, acrylamide, acrylonitrile, methacrylonitrile, vinyl acetate, N-substituted acrylamides, hydroxyacrylates, N-vinylpyrrolidone, maleic anhydride, itaconic acid and mixtures thereof.
Claim 7
Dependent Claim
26 words
The process of claim 5 wherein the initiators comprise at least two of the following free radical initiators: azobisisobutyronitrile, 2,5-dimethyl-2,5-di(t-butylperoxy) hexane, t-butyl perbenzoate and methyltricaprylylammonium persulfate.
Claim 8
Dependent Claim
29 words
The process of claim 6 in which the initiator is a combination of free radical initiators selected from the group consisting of: methyltricaprylylammoniumpersulfate and 2,5-dimethyl-2,5-di(t-butylperoxy)hexane; and azobisisobutyronitrile and 2,5-dimethyl-2,5-di(t-butylperoxy)hexane.
Claim 9
Dependent Claim
24 words
The process of claim 1 wherein the residence time of the reactants in the wiped surface reactor is from about one to 20 minutes.
Claim 10
Dependent Claim
30 words
The process of claim 8 wherein the wiped surface reactor discharges into a non-wiped surface reactor, and the desired conversion is reached at the discharge of the non-wiped surface reactor.
Claim 11
Dependent Claim
16 words
The process of claim 1 wherein the wiped surface reactor is an intermeshing twin screw extruder.
Claim 12
Dependent Claim
17 words
The process of claim 10 wherein the wiped surface reactor is a counter rotating twin screw extruder.
Claim 13
Dependent Claim
29 words
The process of claim 10 which further comprises coating the polymeric material which is withdrawn from the reactor onto a substrate at the end of the twin screw extruder.
Claim 14
Dependent Claim
22 words
The process of claim 10 which further comprises extruding the polymeric material in sheet form and exposing it to post curing radiation.
Claim 15
Dependent Claim
195 words
A process of making a pressure sensitive adhesive composition by polymerizing one or more free radical polymerizable vinyl compounds which process comprises: (a) continuously feeding to a wiped surface reactor comprising a vessel and at least one rotor inside the vessel having a wiping portion located close to the inside surface of the vessel and a root portion spaced susbtantially further from the inside surface than the wiping portion wherein the root surface is wiped continuously during rotation of the rotor raw materials which comprise unpolymerized vinyl compounds without any substantial amount of polymerized vinyl compounds, and at least one initiator for free radical polymerization under the following conditions: (i) all raw materials being fed substantially free of oxygen, and (ii) at least one monomer being a liquid unpolymerized vinyl compound having a viscosity less than about 4000 centipoise which is fed under a pressure at least as high as the vapor pressure of the combined raw materials at the temperature to which the exotherm of the free radical polymerization brings them in the reactor; (b) reacting the raw materials to desired conversion; and (c) continuously withdrawing a polymeric material from the wiped surface reactor.
Claim 16
Dependent Claim
195 words
A process of making a pressure sensitive adhesive composition by polymerizing one or more free radical polymerizable vinyl compounds which process comprises: (a) continuously feeding to a wiped surface reactor comprising a vessel and at least one rotor inside the vessel having a wiping portion located close to the inside surface of the vessel and a root portion spaced susbtantially further from the inside surface than the wiping portion wherein the root surface is wiped continuously during rotation of the rotor raw materials which comprise unpolymerized vinyl compounds without any substantial amount of polymerized vinyl compounds, and at least one initiator for free radical polymerization under the following conditions: (i) all raw materials being fed substantially free of oxygen, and (ii) at least one monomer being a liquid unpolymerized vinyl compound having a viscosity less than about 4000 centipoise which is fed under a pressure at least as high as the vapor pressure of the combined raw materials at the temperature to which the exotherm of the free radical polymerization brings them in the reactor; (b) reacting the raw materials to desired conversion; and (c) continuously withdrawing a polymeric material from the wiped surface reactor.
Claim 17
Dependent Claim
153 words
A process of making a pressure sensitive adhesive composition by bulk polymerizing one or more free radical polymerizable vinyl compounds which comprises: (a) continuously feeding to a wiped surface reactor comprising a vessel and at least one rotor inside the vessel having a wiping portion located close to the inside surface of the vessel and a root portion spaced substantially further from the inside surface than the wiping portion wherein the root surface is wiped continuously during rotation of the rotor raw materials which comprise a polymer syrup comprising at least one partially reacted vinyl monomer having been stabilized at a conversion of about 5 to 10 percent and at least one initiator for free radical polymerization, said raw materials being substantially free of oxygen; (b) reacting the raw materials to the desired conversion; and (c) continuously withdrawing a polymeric material from the reactor, said polymeric material having a bimodal molecular weight distribution.
Claim 18
Dependent Claim
153 words
A process of making a pressure sensitive adhesive composition by bulk polymerizing one or more free radical polymerizable vinyl compounds which comprises: (a) continuously feeding to a wiped surface reactor comprising a vessel and at least one rotor inside the vessel having a wiping portion located close to the inside surface of the vessel and a root portion spaced substantially further from the inside surface than the wiping portion wherein the root surface is wiped continuously during rotation of the rotor raw materials which comprise a polymer syrup comprising at least one partially reacted vinyl monomer having been stabilized at a conversion of about 5 to 10 percent and at least one initiator for free radical polymerization, said raw materials being substantially free of oxygen; (b) reacting the raw materials to the desired conversion; and (c) continuously withdrawing a polymeric material from the reactor, said polymeric material having a bimodal molecular weight distribution.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-10-27 | 1990-04-28 | 1990-10-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-10-27 | 1994-04-28 | 1994-10-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-10-27 | 1998-04-28 | 1998-10-28 | $7700.00 | Window Closed / Lapsed |