Preparation of polyvinylamide cellulose reactive adducts
View Patent ↗The present disclosure is directed to a continuous process for preparing cellulose reactive adducts of polyvinylamide.
1. A method for preparing a cellulose reactive functionalized polyvinylamide adduct using a continuous process comprising:
continuously reacting a substantially aqueous reaction mixture of a vinylamide polymer comprising at least about 70 wt. % acrylamide monomer or methacrylamide monomer and 0 to about 30 wt. % cationic monomer selected from the group consisting of diallyldialkyl ammonium salts, (dialkylamino)alkyl(meth)acrylates acid addition or quaternary salts, 2-vinylpyridines acid addition or quaternary salts, dialkylamino alkyl(meth)acrylamides acid addition or quaternary salts, (p-vinylphenyl)-trimethylammonium chloride, 1-methacryloyl-4-methyl piperazine, and acid addition or quaternary ammonium salts thereof; and a cellulose reactive agent selected from the group consisting of glyoxal, glutaraldehyde, furan dialdehyde, 2-hydroxyadipaldehyde, succinaldehyde, dialdehyde starch, diepoxy compounds, and combinations thereof, at a temperature of about 2° C. to about 50° C. and a reaction pH set point of about 8.5 to about 12, for a reaction time of about 2 minutes to about 150 minutes,
wherein:
i) the temperature of incoming water is continuously measured;
ii) the pH of the reaction mixture is adjusted to maintain an approximately constant reaction rate based on the following equation:
pH=−0.0404 T+ 10.961
where: pH=reaction pH set point
T=reaction temperature (° C.);
iii) between 12% and 85% of the cellulose reactive agent is consumed, and the molar ratio of the amide functionality on the vinylamide polymer to cellulose reactive agent is between 6 to 1 and 2.5 to 1; and
iv) the concentration of the vinylamide polymer prior to and during formation of the adduct is about 0.5-6% of the total reaction mixture, thereby forming the adduct.
2. The method of claim 1 , wherein the adduct is prepared at a temperature of about 4° C. to about 30° C. and a pH of about 8.5 to about 11.5, and a reaction time of about 2 to 90 minutes.
3. The method of claim 1 , wherein the concentration of the vinylamide polymer prior to and during formation of the adduct is about 1% to 4%.
4. The method according to claim 3 , wherein the vinylamide polymer concentration is less than about 4 weight % of the total reaction mixture, and has an average molecular weight of about 50,000 to about 1,000,000 Daltons.
5. The method of claim 1 , wherein about 40% to 60% of the cellulose reactive agent is consumed.
6. The method according to claim 1 , wherein the cellulose reactive agent comprises more than one aldehyde functionality.
7. The method according to claim 1 , wherein the cellulose reactive agent comprises glyoxal.
8. The method according to claim 1 , wherein the vinylamide polymer is a copolymer formed from acrylamide monomer.
9. The method according to claim 1 , wherein the vinylamide polymer is formed from acrylamide monomer and the cationic monomer is selected from the group consisting of diallyldialkyl ammonium salts.
10. The method according to claim 9 , wherein the cationic monomer is diallyldimethyl ammonium chloride.
11. The method according to claim 1 , wherein the vinylamide polymer or the polyvinylamide adduct is linear, crosslinked, chain-transferred, or crosslinked and chain-transferred.
12. The method according to claim 11 , wherein the vinylamide polymer or the polyvinylamide adduct is crosslinked using at least a difunctional monomer selected from the group consisting of methylene bis(meth)acrylamide, triallylammonium chloride, tetraallyl ammonium chloride, polyethyleneglycol diacrylate, polyethyleneglycol dimethacrylate, N-vinyl acrylamide, divinylbenzene, tetra(ethyleneglycol)diacrylate, dimethylallylaminoethylacrylate ammonium chloride, sodium salt of diallyloxyacetic acid, diallyloctylamide, trimethyllpropane ethoxylate triacryalte, N-allylacrylamide, N-methylallylacrylamide, pentaerythritol triacrylate, and combinations thereof.
13. The method according to claim 1 , wherein the vinylamide polymer is a copolymer of (meth)acrylamide and diallyldimethylammonium halide.
14. The method according to claim 1 , wherein the vinylamide polymer has an average molecular weight of about 5000 to about 5,000,000 Daltons.
15. The method according to claim 1 , wherein adduct formation is monitored by measuring a change in turbidity or viscosity of the aqueous reaction, wherein the change in turbidity results from the adduct formation and the turbidity change is in the range of 0.5 to 500 NTU (nephelometric units).
16. The method according to claim 1 , wherein the vinylamide polymer, the cellulose reactive agent, and the base are combined into one flow, and wherein said flow has a flow rate of approximately 2.6 milliliters per minute.
17. A method of preparing an aqueous cellulosic slurry comprising
continuously reacting a substantially aqueous reaction mixture of a vinylamide polymer comprising at least about 70 wt. % acrylamide monomer or methacrylamide monomer and 0 to about 30 wt. % cationic monomer selected from the group consisting of diallyldialkyl ammonium salts, (dialkylamino)alkyl(meth)acrylates acid addition or quaternary salts, 2-vinylpyridines acid addition or quaternary salts, dialkylamino alkyl(meth)acrylamides acid addition or quaternary salts, (p-vinylphenyl)-trimethylammonium chloride, 1-methacryloyl-4-methyl piperazine, and acid addition or quaternary ammonium salts thereof; and a cellulose reactive agent selected from the group consisting of glyoxal, glutaraldehyde, furan dialdehyde, 2-hydroxyadipaldehyde, succinaldehyde, dialdehyde starch, diepoxy compounds, and combinations thereof, at a temperature of about 2° C. to about 50° C. and a reaction pH set point of about 8.5 to about 12, for about 2 minutes to about 150 minutes;
wherein:
i) the temperature of incoming water is continuously measured;
ii) the pH of the reaction mixture is adjusted to maintain an approximately constant reaction rate based on the following equation:
pH=−0.0404 T+ 10.961
where: pH=reaction pH set point
T=reaction temperature (° C.);
iii) between 12% and 85% of the cellulose reactive agent is consumed, and the molar ratio of the amide functionality on the vinylamide polymer to cellulose reactive agent is between 6 to 1 and 2.5 to 1; and
iv) the concentration of the vinylamide polymer prior to and during formation of the adduct is about 0.5-6% of the total reaction mixture, thereby forming the adduct; and
adding the adduct to a slurry to form the aqueous cellulosic slurry.
18. The method according to claim 17 , wherein the vinylamide polymer, the cellulose reactive agent, and the base are combined into one flow, and wherein said flow has a flow rate of approximately 2.6 milliliters per minute.
19. A method of making a paper or board comprising
continuously reacting a substantially aqueous reaction mixture of a vinylamide polymer comprising at least about 70 wt. % acrylamide monomer or methacrylamide monomer and 0 to about 30 wt. % cationic monomer selected from the group consisting of diallyldialkyl ammonium salts, (dialkylamino)alkyl(meth)acrylates acid addition or quaternary salts, 2-vinylpyridines acid addition or quaternary salts, dialkylamino alkyl(meth)acrylamides acid addition or quaternary salts, (p-vinylphenyl)-trimethylammonium chloride, 1-methacryloyl-4-methyl piperazine, and acid addition or quaternary ammonium salts thereof; and a cellulose reactive agent selected from the group consisting of glyoxal, glutaraldehyde, furan dialdehyde, 2-hydroxyadipaldehyde, succinaldehyde, dialdehyde starch, diepoxy compounds, and combinations thereof, at a temperature of about 2° C. to about 50° C. and a reaction pH set point of about 8.5 to about 12, for about 2 minutes to about 150 minutes;
wherein:
i) the temperature of incoming water is continuously measured;
ii) the pH of the reaction mixture is adjusted to maintain an approximately constant reaction rate based on the following equation:
pH=−0.0404 T+ 10.961
where: pH=reaction pH set point
T=reaction temperature (° C.);
iii) between 12% and 85% of the cellulose reactive agent is consumed, and the molar ratio of the amide functionality on the vinylamide polymer to cellulose reactive agent is between 6 to 1 and 2.5 to 1; and
iv) the concentration of the vinylamide polymer prior to and during formation of the adduct is about 0.5-6% of the total reaction mixture, thereby forming the adduct; and
adding the adduct to paper or board.
20. The method according to claim 19 , wherein the vinylamide polymer, the cellulose reactive agent, and the base are combined into one flow, and wherein said flow has a flow rate of approximately 2.6 milliliters per minute.