# US 6,296,696 B1 · One-pass method for preparing paper size emulsions

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- Number: US 6,296,696 B1
- Document ID: US6296696B1
- Status: Granted
- Kind: B1
- Application number: 09/212,068
- Filed: 1998-12-15
- Granted: 2001-10-02
- Earliest claimed: 1998-12-15
- Assignees: National Starch and Chemical Investment Holding Corporation
- Inventors: Michel D. Létourneau; Walter Maliczyszyn
- Web page: https://patentgrep.com/patent/US6296696B1

## CPC

- D21H 21/16: Sizing or water-repelling agents
- B01F 23/41: Emulsifying
- B01F 23/43: using driven stirrers
- B01F 27/86: co-operating with deflectors or baffles fixed to the receptacle
- B01F 27/87: the receptacle being divided into superimposed compartments
- B01F 23/4143: {Microemulsions}
- B01F 27/0721: {parallel with respect to the rotating axis}
- B01F 27/0724: {directly mounted on the rotating axis}
- B01F 27/1125: with vanes or blades extending parallel or oblique to the stirrer axis
- B01F 27/191: with similar elements
- D21H 17/16: Addition products thereof with hydrocarbons
- D21H: PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06)

## Abstract

A one-pass, non-tolerance dependent method for preparing paper size emulsions comprising an aqueous emulsion of a substituted cyclic dicarboxylic anhydride, a colloidal stabilizer, and a surfactant wherein the emulsion after one-pass through a dispersion system has an average particle size of less than 2 microns.

## Claims

### Claim 1

A one-pass method through a non-tolerance dependent dispersion system for preparing a paper size emulsion wherein the emulsion after one-pass through a dispersion system has an average particle size of less than 2 microns, said method comprising:
(I) preparing raw materials which comprise at least one substituted cyclic dicarboxylic anhydride, at least one colloidal stabilizer, and water;
(II) adding the raw materials prepared in Step (I) to a dispersion system comprising:
a housing having a bottom chamber and an upper chamber wherein said housing has a means for cooling in contact therewith;
a motor mounted to said housing for turning a shaft extending into said housing;
a baffle plate mounted to said housing to separate said upper chamber from said lower chamber, said baffle plate having an aperture for receiving said shaft therethrough and forming an annular passage therebetween;
at least two kinetic baffles mounted within said lower chamber to form pressure zones;
an inlet cap mounted to said housing and having a primary inlet and a secondary inlet for delivering said plurality of materials into said lower chamber; and,
at least two blades mounted to said shaft, at least one of said blades disposed in said lower chamber and at least one of said blades disposed in said upper chamber; and
(III) emulsifying the raw materials in the dispersion system at a temperature of from about 40° F. to about 160° F. to form a paper size emulsion.

### Claim 2 (depends on 1)

The method according to claim 1 wherein the substituted cyclic dicarboxylic acid anhydride is selected from the group consisting of
and combinations thereof, wherein R is a dimethylene or trimethylene radical; R1 is a alkyl, alkenyl, aralkyl, or aralkenyl group having 6 to 23 carbon atoms; R2 and R3 are independently an alkyl radical having 4 to 23 carbon atoms; and R4 and R5 are independently an alkyl radical having 5 to 23 carbon atoms.

### Claim 3 (depends on 2)

The method according to claim 2 wherein the substituted cyclic dicarboxylic acid anhydride is selected from the group consisting of iso-octadecenyl succinic acid anhydride, n- or iso-hexadecenyl succinic acid anhydride, dodecenyl succinic acid anhydride, dodecyl succinic acid anhydride, decenyl succinic acid anhydride, octenyl succinic acid anhydride, triisobutenyl succinic acid anhydride, (1-octyl-2-decenyl)-succinic acid anhydride, (1-hexyl-2-octenyl)-succinic acid anhydride, and cyclic dicarboxylic acid anhydrides prepared by the reaction of maleic acid anyhydride with vinylidene olefins selected from the group consisting of 2-n-hexyl-1-octene, 2-n-octyl-1-dodecene, 2-n-octyl-1-decene, 2-n-dodecyl-1-octene, 2-n-octyl-1-octene, 2-n-octyl-1-nonene, 2-n-hexyl-decene and 2-n-heptyl-1-octene.

### Claim 4 (depends on 1)

The method according to claim 1 wherein the colloidal stabilizer is selected from the group consisting of gelatinized or cold water soluble starches or modified starches, carboxymethyl cellulose, natural gums, gelatin, cationic polymers, polyvinyl alcohol, and combinations thereof.

### Claim 5 (depends on 4)

The method according to claim 4 wherein the colloidal stabilizer is a starch selected from the group consisting of corn, waxy maize, potato, tapioca and amylose starch.

### Claim 6 (depends on 4)

The method according to claim 4 wherein the starch is modified by a substituent group which is selected from the group consisting of cationic, anionic, nonionic, amphoteric, zwitterionic groups, and combinations thereof.

### Claim 7 (depends on 6)

The method according to claim 6 wherein the modified starch is waxy maize.

### Claim 8 (depends on 1)

The one-pass method according to claim 1 further comprising a surfant in step (I).

### Claim 9 (depends on 8)

The method according to claim 8 wherein the surfactant is selected from the group consisting of polyoxyethylene or polyoxypropylene alkyl and alkyl-aryl ethers or esters containing 5 to 20 polyoxyethylene or polyoxypropylene units wherein the alkyl radical contains from 8 to 20 carbon atoms and the aryl radical contains 6 to 12 carbon atoms.

### Claim 10 (depends on 9)

The method according to claim 9 wherein the surfactant is selected from the group consisting of HO—[(CH2)[i]—CH2—CH2O][m]—R6—C[n]H2n+1 and HO—[(CH2)[i]—CH2—CH2—O][m]—C[n]H2n+1 wherein x and n are from 8 to 20; R6 is an aryl radical having 6 to 12 carbon atoms; m is from 5 to 20; and i is 0 or 1.

### Claim 11 (depends on 1)

The method according to claim 1 wherein the dispersion system further comprises a cylindrical screen disposed in said upper chamber to be spaced apart and to encircle said turbine blade.

### Claim 12 (depends on 1)

The method according to claim 1 wherein the dispersion system further comprises a dispersion ring mounted to an end of said shaft, said dispersion ring having a skirt having a plurality of apertures.

### Claim 13 (depends on 1)

The method according to claim 1 wherein said primary inlet of said inlet plate is disposed in axial alignment with said shaft.

### Claim 14 (depends on 1)

The method according to claim 1 wherein the kinetic baffles of the dispersion apparatus comprise L-shaped members disposed between said housing and said blade to form pressure zones.

### Claim 15 (depends on 1)

The method according to claim 1 wherein said inlet cap of the dispersion apparatus is mounted for removal from said housing.

### Claim 16

A one-pass method through a non-tolerance dependent dispersion system for preparing a paper size emulsion wherein 95% of the emulsion particles after one-pass through a dispersion system have a particle size of less than 2 microns, said method comprising:
(I) preparing raw materials which comprise at least one substituted cyclic dicarboxylic anhydride, at least one colloidal stabilizer, and water;
(II) adding the raw materials prepared in Step (I) to a dispersion system comprising:
a housing having a bottom chamber and an upper chamber wherein said housing has a means for cooling in contact therewith;
a motor mounted to said housing for turning a shaft extending into said housing;
a baffle plate mounted to said housing to separate said upper chamber from said lower chamber, said baffle plate having an aperture for receiving said shaft therethrough and forming an annular passage therebetween;
at least two kinetic baffles mounted within said lower chamber to form pressure zones;
an inlet cap mounted to said housing and having a primary inlet and a secondary inlet for delivering said plurality of materials into said lower chamber; and,
at least two blades mounted to said shaft, at least one of said blades disposed in said lower chamber and at least one of said blades disposed in said upper chamber; and
(III) emulsifying the raw materials in the dispersion system at a temperature of from about 40° F. to about 160° F. to form a paper size emulsion.
