Sugar – starch – and carbohydrates – Processes – Carbohydrate manufacture and refining
Reexamination Certificate
1999-03-10
2001-05-29
Brunsman, David (Department: 1755)
Sugar, starch, and carbohydrates
Processes
Carbohydrate manufacture and refining
C127S053000, C435S007900, C435S007920, C436S548000, C526S207000, C526S209000, C526S210000, C526S215000, C526S220000, C526S287000, C526S292200, C526S307000
Reexamination Certificate
active
06238486
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to compositions and methods for separating the solid component from a liquid-solid mixture of an industrial food process. More specifically, the present invention relates to compositions and methods for separating the solid component from a liquid-solid mixture present in an industrial food process, wherein it is desired to recover the liquid component of the industrial food process. More specifically, the present invention relates to a traceable high molecular weight cationic flocculant for use in flocculating a component of a stream in the manufacture of sugar, involving passing liquid through a filter medium, wherein the liquid present in said sugar process is further processed to recover additional sugar(s).
BACKGROUND OF THE INVENTION
In industrial food processes it is common that a solid-liquid mixture needs to be separated into its liquid component and its solid component. There are polymer flocculants available currently to perform this separation. However, useful materials in the liquid component of such separations are typically not harvested because of concern that the liquid component is contaminated with polymer flocculants. This concern about contamination has led to much valuable material being discarded.
For example, in the recovery of sugar, cationic flocculants are used to effect solid-liquid separation. The liquid portion still contains recoverable sugar, but this sugar is not recovered, because the liquid may have been contaminated with flocculant. In order not to waste this recoverable sugar, there is a recognized need to develop either an environmentally safe (for food use) polymer or a detectable polymer. Of these two routes, it was decided to pursue a detectable polymer as a solution.
In pursuing a solution it was noted that immunoassay detection technology was already in existence for the coagulant polymers epichlorohydrin dimethylamine (hereinafter “epi-DMA”) and polydiallyldiammonium chloride (hereinafter “polyDADMAC”). Epi-DMA is available as Nalco®8105 from Nalco Chemical Company, One Nalco Center, Naperville, Ill. 60563 ((630) 305-1000). PolyDADMAC is available as Nalco®8103 from Nalco Chemical Company. Although these polymers are detectable, it was found that these polymers did not have a sufficient molecular weight to act as flocculants.
Building on the use of immunoassay as the detection method of choice, a 30/70 mole percent acrylamide/DADMAC copolymer (which is available from Nalco Chemical Company as Nalco®7527) was tested in the sugar application. This polymer has molecular weights greater than the coagulants, but not as high as a flocculant. Because of the high concentration of DADMAC, this polymer was detectable using the Nalco®8103 (polyDADMAC) immunoassay test kit. A field trial was run, which was a failure. Although detectable in the liquid component, the polymer did not form strong robust flocs and the solids were not effectively dewatered. This failure can be related to both charge and molecular weight. It was known that DADMAC monomer does not polymerize to high molecular weights, so copolymers containing DADMAC are more like coagulants than flocculants.
Based on the above results, the criteria for a polymer flocculant to be successful in this application were determined to be as follows:
1) polymer flocculant must form effective flocs that will effect solid-liquid separation (i.e. getting the correct charge),
2) the floc strength must be sufficient to withstand the shear of the dewatering process (i.e. having sufficient molecular weight), and
3) the polymer must be detectable (by immunoassay) to quantify the level of polymer in the liquid.
SUMMARY OF THE INVENTION
The first aspect of this invention is a cationic flocculant dispersion polymer comprising:
a first monomer component, which is nonionic;
a second monomer component, which is cationic; and
a third monomer component which is diallyl dimethylammonium chloride;
wherein the first monomer component, which is nonionic, is selected from the group consisting of:
acrylamide, vinylacetate, vinylcaprolactam, protonated acrylamidopropylsulfonic acid, protonated 2-sulfoethylacrylate, substituted or non-substituted amides or esters of acrylic acid, including, but not limited to: N,N-dimethylacrylamide, N-t-butylacrylamide, N-isopropyl acrylamide, hydroxymethylacrylate, hydroxyethylacrylate, hydroxypropylacrylate, and hydroxybutylacrylate, substituted or non-substituted amides or esters of methacrylic acid, including, but not limited to: N,N-dimethylmethacrylamide, N-methylmethacrylamide, N-isopropyl methacrylamide, hydroxymethylmethacrylate, hydroxyethylmethacrylate, hydroxypropylmethacrylate, and hydroxybutylmethacirylate;
wherein the second monomer component, which is cationic, is selected from the group consisting of: dimethylaminoethylacrylate methyl chloride salt (DMAEA.MCQ); dimethylaminoethylmethacrylate methyl chloride salt (DMAEM.MCQ); dimethylaminoethylmethacrylate methyl sulfate salt (DMAEM.MSQ); dimethylaminoethylmethacrylate benzyl chloride salt (DMAEM.BCQ); dimethylaminoethylacrylate methyl sulfate salt (DMAEA.MSQ); dimethylaminoethylacrylate benzyl chloride salt (DMAEA.BCQ), methacrylamidopropyl trimethylammonium chloride (MAPTAC); acrylamidopropyl trimethylammonium chloride (APTAC); 2-vinylpyridine; and 4-vinylpyridine.
The second aspect of this invention is a method of flocculating solids from the liquid component of an industrial food process, the method comprising the steps of:
a) adding a cationic flocculant polymer to a liquid component of an industrial food process which causes the formation of flocculated particles, wherein said cationic flocculant polymer comprises a first monomer component, which is nonionic;
a second monomer component, which is cationic; and
a third monomer component which is diallyl dimethylammonium chloride;
wherein the first monomer component, which is nonionic, is selected from the group consisting of:
acrylamide, vinylacetate, vinylcaprolactam, protonated acrylamidopropylsulfonic acid, protonated 2-sulfoethylacrylate, substituted or non-substituted amides or esters of acrylic acid, including, but not limited to: N,N-dimethylacrylamide, N-t-butylacrylamide, N-isopropyl acrylamide, hydroxymethylacrylate, hydroxyethylacrylate, hydroxypropylacrylate, and hydroxybutylacrylate, substituted or non-substituted amides or esters of methacrylic acid, including, but not limited to: N,N-dimethylmethacrylamide, N-methylmethacrylamide, N-isopropyl methacrylamide, hydroxymethylmethacrylate, hydroxyethylmethacirylate, hydroxypropyhnethacrylate, and hydroxybutylmethacrylate;
wherein the second monomer component, which is cationic, is selected from the group consisting of: dimethylaminoethylacrylate methyl chloride salt (DMAEA.MCQ); dimethylaminoethylmethacrylate methyl chloride salt (DMAEM.MCQ); dimethylaminoethylmethacrylate methyl sulfate salt (DMAEM.MSQ); dimethylaminoethylmethacrylate benzyl chloride salt (DMAEM.BCQ); dimethylaminoethylacrylate methyl sulfate salt (DMAEA.MSQ); dimethylaminoethylacrylate benzyl chloride salt (DMAEA.BCQ), methacrylamidopropyl trimethylammonium chloride (MAPTAC); acrylamidopropyl trimethylammonium chloride (APTAC); 2-vinylpyridine; and 4-vinylpyridine;
b) separating said flocculated particles from said liquid component; and
c) determining the concentration of said cationic flocculant polymer in the liquid; wherein the step of determining the concentration of the cationic flocculant polymer further comprises:
i) incubating the sample of liquid with a monoclonal antibody having an affinity for the cationic flocculant polymer, the affinity being strong enough to recognize a monomer antigen in the cationic flocculant polymer and to differentiate the cationic flocculant polymer from other polymers in the sample;
ii) detecting and measuring the degree of binding of the monoclonal antibody with the monomer antigen; and
iii) determining the concentration of the cationic flocculant polymer based on the degree of binding of the monoclonal antibody.
DETAILED DESCRIPTION OF THE INV
Dunham Andrew J.
Johnson Cathy C.
Salmen Kristine S.
Sommese Anthony G.
Sparapany John W.
Breininger Thomas M.
Brumm Margaret M.
Brunsman David
Nalco Chemical Company
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