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Continuous process for solution polymerization of acrylamide

Assignee: Milchem Inc
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Filing: 1979-07-16
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Granted: 1981-08-11
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Expires: 1999-07-16
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Abstract

Abstract A continuous process is provided for producing substantially homogeneous, non-tacky solid terpolymers of acrylamide, an alkali metal salt of acrylic acid and a hydroxyalkyl acrylate, and copolymers, optionally cross-linked, of a (meth)acrylamidoalkylsulfonic acid or alkali metal salt thereof and (meth)acrylamide or N-alkyl(meth)acrylamide, by rapidly heating a single phase high solids aqueous solution of the monomers to polymerization initiation temperature immediately prior to depositing a uniform layer of the solution and, at the same time, a solution of a polymerization initiator, onto a moving surface, the surface and the reaction mixture only being heated if necessary to keep the temperature of the polymerizing mixing from dropping substantially below the polymerization initiation temperature.

Inventors

  • 👤 Alphonse C. Perricone
  • 👤 James M. Lucas

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 19:34
CPC Classifications
C; C08; C08F; C08F220/00; C08F220/02; C08F220/52; C08F220/54; C08F220/56; Y; Y10; Y10S; Y10S526/00; Y10S526/92

Claims Analysis

Total Claims: 22
Claim 1
Independent Claim 350 words
A continuous polymerization process for producing a continuous, substantially homogeneous stream of a solid, non-tacky polymer which comprises the steps of: (a) forming a concentrated aqueous monomer solution at a temperature of from 23° to 40° C. to form a single phase solution said monomers being: (i) a mixture consisting essentially of an alkali metal salt of acrylic acid, a hydroxyalkyl acrylate and acrylamide, in proportions of from 5 to 62 mole%, from 2.1 to 40 mole% and from 31 to 91 mole%, respectively; or (ii) a mixture consisting essentially of (a) a (meth)acrylamidoalkylsulfonic acid or alkali metal salt thereof and (b) (meth)acrylamide or N-alkyl(meth)acrylamide, in proportions of from 8 to 70 mole% and from 30 to 92 mole %, respectively; or (iii) mixture (ii), further containing from 0.2 to 4.4 moles of a quaternary ammonium salt cross-linking agent; (b) heating a continuous stream of the monomer solution of step (a) to a polymerization initiation temperature of from 60° to 80° C. for mixture (i) or from 55° to 65° C. for mixture (ii) or (iii), by passage through an indirect heat exchanger at a rate such that the residence time of the solution in the heat exchanger is not longer than 0.5 minute; (c) immediately and continuously thereafter depositing the heated stream of monomer solution as a continuous, substantially uniform layer on a moving surface; (d) substantially simultaneously with step (c), continuously and substantially uniformly applying to the moving surface of catalytically effective amount of an aqueous solution of a polymerization initiator for the monomers, thereby continuously forming a substantially uniform reaction mixture of the heated monomer solution and the initiator on the moving surface said moving surface and said reaction mixture being unheated or heated only sufficiently to keep the temperature of the polymerizing mixture on the moving surface from falling substantially below said polymerization initiation temperature until polymerization is substantially complete; whereby the monomers exothermically and substantially homogeneously polymerize and a portion of the water therein evaporates to form a continuous stream of a substantially homogeneous solid, non-tacky polymer; and (e) recovering the resultant solid, non-tacky polymer.
Claim 2
Dependent Claim 350 words
A continuous polymerization process for producing a continuous, substantially homogeneous stream of a solid, non-tacky polymer which comprises the steps of: (a) forming a concentrated aqueous monomer solution at a temperature of from 23° to 40° C. to form a single phase solution said monomers being: (i) a mixture consisting essentially of an alkali metal salt of acrylic acid, a hydroxyalkyl acrylate and acrylamide, in proportions of from 5 to 62 mole%, from 2.1 to 40 mole% and from 31 to 91 mole%, respectively; or (ii) a mixture consisting essentially of (a) a (meth)acrylamidoalkylsulfonic acid or alkali metal salt thereof and (b) (meth)acrylamide or N-alkyl(meth)acrylamide, in proportions of from 8 to 70 mole% and from 30 to 92 mole %, respectively; or (iii) mixture (ii), further containing from 0.2 to 4.4 moles of a quaternary ammonium salt cross-linking agent; (b) heating a continuous stream of the monomer solution of step (a) to a polymerization initiation temperature of from 60° to 80° C. for mixture (i) or from 55° to 65° C. for mixture (ii) or (iii), by passage through an indirect heat exchanger at a rate such that the residence time of the solution in the heat exchanger is not longer than 0.5 minute; (c) immediately and continuously thereafter depositing the heated stream of monomer solution as a continuous, substantially uniform layer on a moving surface; (d) substantially simultaneously with step (c), continuously and substantially uniformly applying to the moving surface of catalytically effective amount of an aqueous solution of a polymerization initiator for the monomers, thereby continuously forming a substantially uniform reaction mixture of the heated monomer solution and the initiator on the moving surface said moving surface and said reaction mixture being unheated or heated only sufficiently to keep the temperature of the polymerizing mixture on the moving surface from falling substantially below said polymerization initiation temperature until polymerization is substantially complete; whereby the monomers exothermically and substantially homogeneously polymerize and a portion of the water therein evaporates to form a continuous stream of a substantially homogeneous solid, non-tacky polymer; and (e) recovering the resultant solid, non-tacky polymer.
Claim 3
Dependent Claim 20 words
The process of claim 1, wherein the moisture content of the resultant polymer is less than about 12% by weight.
Claim 4
Dependent Claim 15 words
The process of claim 1, wherein the temperature in step (a) is about 30° C.
Claim 5
Dependent Claim 18 words
The process of claim 1, wherein in step (b) said residence time is not longer than 0.3 minute.
Claim 6
Dependent Claim 13 words
The process of claim 1, wherein the aqueous monomer solution is solution (i).
Claim 7
Dependent Claim 26 words
The process of claim 5, wherein the monomers are sodium acrylate, 2-hydroxypropyl acrylate and acrylamide, in proportions of 16-27 mole%, 3-5 mole% and 70-80 mole%, respectively.
Claim 8
Dependent Claim 18 words
The process of claim 6, wherein the monomer solution is heated in step (b) to about 70° C.
Claim 9
Dependent Claim 12 words
The process of claim 7, wherein the polymerization initiator is potassium persulfate.
Claim 10
Dependent Claim 32 words
The process of claim 8, which further comprises the step of drying the solid polymer produced in step (e) for about 1 hour at about 150° C., and milling the dried polymer.
Claim 11
Dependent Claim 46 words
The process of claim 8, wherein in step (b) the stream of monomer solution is heated to 70° C. within 0.3 minute by passage through an indirect heat exchanger maintained at 78° C.; and in step (d) the polymerizing mixture is heated to maintain the temperature.
Claim 12
Dependent Claim 13 words
The process of claim 1, wherein the aqueous monomer solution is solution (ii).
Claim 13
Dependent Claim 29 words
The process of claim 11, wherein the monomers are 2-acrylamido-2-methylpropanesulfonic acid or the sodium salt thereof, and acrylamide, in proportions of about 20-10 mole% and about 80-90 mole%, respectively.
Claim 14
Dependent Claim 32 words
The process of claim 12, wherein the monomer solution is heated in step (b) to about 60° C. and wherein no heat is applied to the polymerizing mixture on the moving belt.
Claim 15
Dependent Claim 12 words
The process of claim 13, wherein the polymerization initiator is potassium persulfate.
Claim 16
Dependent Claim 34 words
The process of claim 14, wherein in step (b) the stream of monomer solution is heated to 60° C. within about 0.3 minute by passage through an indirect heat exchanger maintained at 60° C.
Claim 17
Dependent Claim 13 words
The process of claim 1, wherein the aqueous monomer solution is solution (iii).
Claim 18
Dependent Claim 39 words
The process of claim 16, wherein the monomers are 2-acrylamido-2-methylpropanesulfonic acid or the sodium salt thereof, and acrylamide, and the cross-linking agent is methacryloyloxyethyltrimethylamnmonium methanesulfonate, in proportions of about 20-9 mole%, about 80-90 mole% and about 4-2 mole%, respectively.
Claim 19
Dependent Claim 32 words
The process of claim 17, wherein the monomer solution is heated in step (b) to about 60° C., and wherein no heat is applied to the polymerizing mixture on the moving surface.
Claim 20
Dependent Claim 12 words
The process of claim 18, wherein the polymerization initiator is potassium persulfate.
Claim 21
Dependent Claim 34 words
The process of claim 19, wherein in step (b) the stream of monomer solution is heated to 60° C. within about 0.3 minute by passage through an indirect heat exchanger maintained at 60° C.
Claim 22
Dependent Claim 31 words
The process of claim 1, wherein in step (b), the heated monomer solution is deposited on the surface as a layer having an average thickness of about one to two cm.

References Cited (Backward Citations)

US3058958A Cited
US3732193A Cited
US3923756A Cited
US4138539A Cited
US4032701A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-08-10 1985-02-09 1985-08-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-08-10 1989-02-09 1989-08-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-08-10 1993-02-09 1993-08-11 $7700.00 Window Closed / Lapsed

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