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US5268437A Expired / Lapsed US ⏱️ 0.0 years remaining

High temperature aqueous polymerization process

Assignee: Rohm and Haas Co
•
Filing: 1992-01-22
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Granted: 1993-12-07
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Expires: 2012-01-22
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Abstract

Abstract This invention relates to high temperature aqueous processes for the polymerization of one or more carboxylic monomer to produce low molecular weight, water-soluble polymer products useful as detergent additives, scale inhibitors, dispersants and crystal growth modifiers.

Inventors

  • 👤 Norman L. Holy
  • 👤 Newman M. Bortnick
  • 👤 Graham Swift
  • 👤 Kathleen A. Hughes

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 05:40
CPC Classifications
C; C11; C11D; C11D3/00; C11D3/16; C11D3/37; C11D3/3746; C11D3/3769; C08; C08F; C08F20/00; C08F20/02; C08F20/04; C09; C09D; C09D7/00; C09D7/40; C09D7/45; C11D3/3757

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 218 words
An aqueous process for polymerizing carboxylic acid monomers comprising: (a) forming a reaction mixture by feeding into a reactor containing water at a temperature in the range of from about 130° to about 240° C. under elevated pressure (i) one or more carboxylic acid monomers or aqueous solutions thereof selected from the group consisting of C 3 -C 6 monoethylenically unsaturated monocarboxylic acids, C 4 -C 6 monoethylenically unsaturated dicarboxylic acids, anhydrides of C 4 -C 6 monoethylenically unsaturated cis-dicarboxylic acids and the and ammonium salts thereof, (ii) initiator, or an aqueous solution thereof, in an effective amount for initiating free-radical polymerization of said monomers, and (iii) one or more monoethylenically unsaturated carboxyl-free monomers, or aqueous solutions thereof, at a level of from 0 to 20 percent by weight based on the total carboxylic acid monomers, such that water always makes up at least 35 percent by weight of the reaction mixture and wherein the reaction mixture is substantially free of metal ions and substantially free of organic solvent; and wherein substantially all carboxylic acid monomers used are fed into the reactor containing water at a temperature in the range of from about 130° to about 240° C., and (b) maintaining the reaction mixture in said temperature range to form a polymer product having M n below 10,000.
Claim 2
Dependent Claim 218 words
An aqueous process for polymerizing carboxylic acid monomers comprising: (a) forming a reaction mixture by feeding into a reactor containing water at a temperature in the range of from about 130° to about 240° C. under elevated pressure (i) one or more carboxylic acid monomers or aqueous solutions thereof selected from the group consisting of C 3 -C 6 monoethylenically unsaturated monocarboxylic acids, C 4 -C 6 monoethylenically unsaturated dicarboxylic acids, anhydrides of C 4 -C 6 monoethylenically unsaturated cis-dicarboxylic acids and the and ammonium salts thereof, (ii) initiator, or an aqueous solution thereof, in an effective amount for initiating free-radical polymerization of said monomers, and (iii) one or more monoethylenically unsaturated carboxyl-free monomers, or aqueous solutions thereof, at a level of from 0 to 20 percent by weight based on the total carboxylic acid monomers, such that water always makes up at least 35 percent by weight of the reaction mixture and wherein the reaction mixture is substantially free of metal ions and substantially free of organic solvent; and wherein substantially all carboxylic acid monomers used are fed into the reactor containing water at a temperature in the range of from about 130° to about 240° C., and (b) maintaining the reaction mixture in said temperature range to form a polymer product having M n below 10,000.
Claim 3
Dependent Claim 35 words
The process of claim 1 wherein the one or more carboxylic acid monomers are selected from the group consisting of acrylic acid, methacrylic acid, maleic acid, maleic anhydride, itaconic acid, crotonic acid, and fumaric acid.
Claim 4
Dependent Claim 29 words
The process of claim 2 wherein the one or more carboxylic acid monomers are selected from the group consisting of acrylic acid, methacrylic acid, maleic acid and maleic anhydride.
Claim 5
Dependent Claim 25 words
The process of claim 3 wherein the one or more carboxylic acid monomers are selected from the group consisting of acrylic acid and methacrylic acid.
Claim 6
Dependent Claim 18 words
The process of claim 1 wherein the one or more carboxylic acid monomers are at least partially neutralized.
Claim 7
Dependent Claim 23 words
The process of claim 1 wherein the initiator is selected from the group consisting of hydrogen peroxide, t-butyl hydroperoxide, and di-tertiary butyl peroxide.
Claim 8
Dependent Claim 17 words
The process of claim 1 wherein the temperature range is from about 140° to about 230° C.
Claim 9
Dependent Claim 17 words
The process of claim 1 wherein the temperature range is from about 150° to about 220° C.
Claim 10
Dependent Claim 19 words
The process of claim 1 wherein the polymer product has M n below 10,000 and a polydispersity below 2.5.
Claim 11
Dependent Claim 21 words
The process of claim 1 wherein the polymer product has M n from 500 to 8,000 and a polydispersity below 2.5.
Claim 12
Dependent Claim 21 words
The process of claim 1 wherein the polymer product has M n from 600 to 5,000 and a polydispersity below 2.5.
Claim 13
Dependent Claim 80 words
The process of claim 1 wherein the monoethylenically unsaturated carboxyl-free monomers are selected from the group consisting of C 1 -C 4 alkyl esters of acrylic acid, C 1 -C 4 alkyl esters of methacrylic acid, hydroxyalkyl esters of acrylic acid, hydroxyalkyl esters of methacrylic acid, acrylamide, methacrylamide, N-tertiarybutylacrylamide, N-methylacrylamide, N,N-dimethylacrylamide, acrylonitrile, methacrylonitrile, allyl alcohol, allylsulfonic acid, allylphosphonic acid, vinylphosphonic acid, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, phosphoethyl methacrylate, N-vinylpyrrolidone, N-vinylformamide, N-vinylimidazole, vinyl acetate, styrene, styrenesulfonic acid, vinylsulfonic acid, and 2-acrylamido-2-methylpropanesulfonic acid.
Claim 14
Dependent Claim 12 words
The process of claim 1 wherein the process is a continuous process.
Claim 15
Dependent Claim 19 words
The process of claim 13 wherein a residence time of from about 2 to about 45 minutes is provided.
Claim 16
Dependent Claim 188 words
An aqueous process for polymerizing carboxylic acid monomers comprising: (a) forming a reaction mixture by feeding into a reactor containing water at a temperature in the range of from about 130° to about 240° C. under elevated pressure (i) one or more carboxylic acid monomers or aqueous solutions thereof selected from the group consisting of C 3 -C 6 monoethylenically unsaturated monocarboxylic acids, C 4 -C 6 monoethylenically unsaturated dicarboxylic acids, anhydrides of C 4 -C 6 monoethylenically unsaturated cis-dicarboxylic acids and the ammonium salts thereof, and (ii) initiator, or an aqueous solution thereof, in an effective amount for initiating free-radical polymerization of said monomers, such that water always makes up at least 35 percent by weight of the reaction mixture and wherein the reaction mixture is substantially free of metal ions and substantially free of chain transfer agent; and wherein substantially all carboxylic acid monomers used are fed into the reactor containing water at a temperature in the range of from about 130° to about 240° C., and (b) maintaining the reaction mixture in said temperature range to form a polymer product having M n below 10,000.
Claim 17
Dependent Claim 188 words
An aqueous process for polymerizing carboxylic acid monomers comprising: (a) forming a reaction mixture by feeding into a reactor containing water at a temperature in the range of from about 130° to about 240° C. under elevated pressure (i) one or more carboxylic acid monomers or aqueous solutions thereof selected from the group consisting of C 3 -C 6 monoethylenically unsaturated monocarboxylic acids, C 4 -C 6 monoethylenically unsaturated dicarboxylic acids, anhydrides of C 4 -C 6 monoethylenically unsaturated cis-dicarboxylic acids and the ammonium salts thereof, and (ii) initiator, or an aqueous solution thereof, in an effective amount for initiating free-radical polymerization of said monomers, such that water always makes up at least 35 percent by weight of the reaction mixture and wherein the reaction mixture is substantially free of metal ions and substantially free of chain transfer agent; and wherein substantially all carboxylic acid monomers used are fed into the reactor containing water at a temperature in the range of from about 130° to about 240° C., and (b) maintaining the reaction mixture in said temperature range to form a polymer product having M n below 10,000.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1996-12-06 1997-06-07 1997-12-07 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2000-12-06 2001-06-07 2001-12-07 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2004-12-06 2005-06-07 2005-12-07 $7700.00 Window Closed / Lapsed

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