Claims:We Claim:
1. Water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers that are agglomerated and/or infused with silica providing clump free easy/even dispersibility in aqueous systems and controlled uniform hydration favouring easy processibility.
2. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in claim 1 wherein said polymers are at least partially agglomerated and/or at least partially infused with silica.
3. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1 or 2 comprising rheology modifier polymers including viscosifiers and thickeners.
4. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1-3 wherein said polymer particulates at least partially agglomerated and/ or at least partially infused with silica are obtained of wetted polymer and said silica.
5. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in claim 4 wherein said wetted polymer comprise solvent wetted polymers including water wetted polymers free of binders and/ or additives.
6. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1-5 comprising said at least partially agglomerated and/or at least partially infused particulates with or without binders and/ or additives.
7. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1-6 with controlled wettability, clump free dispersibility, cold water solubility and higher polymer loading capability of up to 2 gms for 100 ml in aqueous systems as a uniform dispersion for controlled hydration.
8. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in claim 7 of size upto 3000 microns.
9. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1 to 8 which are crush resistant.
10. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1 to 9 wherein said silica includes treated silica and is selected from crystalline and amorphous silica including precipitated, and fumed silica.
11. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1 to 10 wherein said water soluble/water swell able natural polymers and their derivatives include starch derivatives, cellulose derivatives, alginate, agar, arrowroot, carageenan, collagen, gelatin, guar gum, pectin, diutan gum, welan gum, polysaccharide and xanthan gum. and said water soluble/water swell able colloidally dispersable synthetic polymers include AMPS (2-Acrylamido-2-methylpropane sulfonic acid)& NNDMA (n,n-dimethyl acrylamide), Polyacrylamide (PAM), Partially Hydrolysed Polyacrylamide (PHPA), acrylate copolymers, modified acrylamide polymers and graft polymers.
12. Water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1 to 11 wherein said natural and/or synthetic polymers: silica is in the ratio range of 80 to 99.90 : 0.10 to 20 respectively.
13. A process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 1-12 comprising
infusing wetted water soluble/ swellable, colloidally dispersible polymer particulates with silica to thereby provide said water swellable, soluble/colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers agglomerated and infused with silica for clump free easy/even dispersibility in aqueous systems and controlled uniform hydration favouring easy processibility.
14. A process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates as claimed in claim 13 comprising infusing at least partially wetted water swellable, soluble/colloidally dispersible polymer particulates with silica to thereby provide said polymers at least partially agglomerated and/or at least partially infused with silica.
15. A process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 13 or 14 wherein said infusion comprises solvent based wetting of the natural or synthetic polymer including water based wetting of polymer particles free of binders and/or additives.
16. A process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 13-15 wherein said partially infused and/or at least partially agglomerated particles are obtained with or without binders and/ or additives.
17. A process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates as claimed in anyone of claims 13 and 16 comprising the steps of
(a) providing water soluble/ swellable, colloidally dispersible polymer particulates and silica with or without binders and/or additives as loose at least partially agglomerated particles;
(b) using solvent including water and/or binders to impart wettability to said polymer particulates to thereby atleast partially infuse said water soluble/water swellable natural and/or synthetic polymers with silica to produce the clump free easy/evenly dispersible polymer particulates.
18. A process as claimed in claim 17 wherein said natural and/or synthetic polymers: silica: solvent including water are employed in ratio range of 80 to 99.90: 0.10 to 20: 10 to 50 respectively.
19. A process as claimed in anyone of claims 17 or 18 wherein said step (a) comprises
(a) providing water soluble/ swellable, colloidally dispersible polymer particulates in combined ratio range of 80 to 99.90 and said silica in ratio range of 0.10 to 20 whereby said silica enter into the crevices and gaps of the water soluble/ swellable, colloidally dispersible polymer agglomerates;
(b) spraying solvent including water and/or binders in ratio range of 10 to 50 preferably 20 to 30 whereby said silica atleast partially fuses with said wetted polymer particulates also on the particle surface facilitating formation of a partial coating of said silica and/or said polymer to produce said clump free easily/evenly dispersible polymer particulates in aqueous systems.
20. A process as claimed in claim 19 wherein said step (a) comprises
(i) providing water soluble/ swellable, colloidally dispersible polymer particulates in the form of fine powder in a granulator under rotation followed by addition of solvent including water and/or binders for a desired time to yield loose at least partially agglomerated particles;
(ii) drying the said granules at a desired temperature for a desired time in a suitable dryer followed by sieving to attain at least partially agglomerated particles of size of preferably <3000 micron, more preferably 100-1000 micron.
step (b) comprises
(i) providing said at least partially agglomerated particles in a tumbler type granulator followed by addition of said silica under rotation for a desired time;
(ii) spraying desired amounts of solvent including water and/or binders for a desired time on the rotating granules and further rotating for desired time;
(iii) drying the granules followed by sieving to yield said clump free easy/evenly dispersible polymer particulates in sizes of upto 3000 microns.
21. A process as claimed in claim 20 wherein said step (a) comprises
(i) providing water soluble/ swellable, colloidally dispersible polymer particulates in the form of fine powder in amounts of 8 to 10 kg in a granulator rotating at a 10 to 40 preferably about 20- 30 rpm followed by addition of about 1.0 to 5.0 kg preferably about 2 to 3 kg of water for 3 to 6 preferably about 4-5 hrs to yield loose at least partially agglomerated particles;
(ii) drying the said granules at 110-120oC for 2 to 4 hrs preferably about 2-3 hrs in a suitable dryer followed by sieving to attain at least partially agglomerated particles of size of preferably <3000 micron, more preferably 100-1000 micron.
step (b) comprises
(i) providing said at least partially agglomerated particles in amounts of 500 gms in a tumbler type granulator followed by addition of 10 to 125 preferably about 50-70 gms of said silica under rotation at 10 to 40 preferably about 20-30 rpm for 4 to 5 hrs preferably about 2-3 hrs;
(ii) spraying 50 to 250 preferably about 150-200 gm of solvent including water and/or binders for 1 to 5 preferably about 2-3 hrs on the rotating granules and was rotated for another 1 to 4 preferably about 2-3 hrs;
(iii) drying the granules followed by sieving to yield said clump free easy/evenly dispersible polymer particulates in sizes in sizes of upto 3000 microns preferably in range of 100-1000 microns.
22. Use of water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers that are agglomerated and/or infused with silica in various application including food, pharmaceuticals, cosmetics, personal care, agriculture, adhesives, textile, detergents, paints, coatings, explosives, mining, synthetic resins and water treatment.

23. Use as claimed in claim 22 wherein said polymers are at least partially agglomerated and/or at least partially infused with silica.
24. A formulation comprising water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers that are at least partially agglomerated and/or partially infused with silica with or without binders/carriers/builders favouring easy processing in aqueous and aqueous based systems of the same.
25. A formulation as claimed in claim 24 wherein said easy processing in aqueous and aqueous based systems of the same includes using energy efficient standard mixing, processing and transferring equipments including pumps facilitating clump free uniform dispersion leading to controlled hydration even at high polymer loading even in cold water to achieve improved degree of hydration thereby facilitating overall enhanced performance and ease of application of the same.
26. A method of application of agglomerated water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers in aqueous and aqueous based systems comprises providing said polymer particulates that form a dispersion for controlled and delayed hydration favouring complete hydration and viscosity build up after enabling facile mixing, formulating, blending, processing and pumping in said aqueous and aqueous based systems.
27. A method of application as claimed in claim 26 wherein said agglomerated water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers are provided in amounts of 0.01 to 5.00 % in aqueous and aqueous based systems.

Dated this the 18th day of April, 2016 Anjan Sen
Of Anjan Sen and Associates
(Applicants Agent)
, Description:FIELD OF THE INVENTION
The present invention particularly provides for water soluble/ sellable, colloidally dispersible polymer particulates having size <3000 microns comprising natural and/ or synthetic polymers that are agglomerated and/or infused with silica, optionally involving binders and/ or additives that advantageously acquires clump free ready and even dispersibility in aqueous systems while also having unique controlled uniform and superior hydration in aqueous systems to thereby favour easy processibility.

More particularly, the present invention also provides for a facile and economical process for manufacturing above said polymer particulates, including rheology modifiers which includes thickeners and viscosifiers to find end use and application including food, pharmaceuticals, cosmetics, personal care, health care, nutrition, animal feed, agriculture, adhesives, textile, ceramics, paper, detergents, paints, inks, coatings, explosives, mining, synthetic resins, water treatment, floatation agent, antistatic film and packaging, polymerization aid and PVC.
BACKGROUND ART
All the natural & synthetic polymers that are water soluble / colloidally dispersible or that swell in water particularly rheology modifiers (commonly referred to as thickeners, or viscosifiers.), are commercially available in the powder form or the particles of the size < 800 microns. The use of these additives cut across several process industries including, but not limited to food, pharmaceuticals, cosmetics, personal care, agriculture, adhesives, textile, detergents, paints, coatings, explosives, mining, synthetic resins and water treatment.

They serve the purpose of not just altering the viscosity of the formulation but also that of providing specific functionality to the product. This could range from improving mouth feel, body, texture, moisture retention and suspensibility of soluble ingredients to increasing stability and dry strength, inhibiting syneresis, resisting bacterial attack, preventing shrinkage and controlling crystal ice formation.

While some finely divided carriers such as kaolinites, bentonites, diatomaceous earth etc, are sometimes used as diluents to adjust the polymer content to the desired concentration and give strength and prevent agglomeration of the finished product, on the other hand some finely divided naturally derived polymers like lignin sulphonates, dextrose, and other water soluble salts like sodium sulphate, ammonium sulphate are also generally used as fillers to help in the disintegration of the granule in water.
Thickeners and viscosifiers come from both natural and synthetic sources. Naturally occurring polymers comprised of amino acid building blocks, and are generally water-soluble/ water swellable or form colloidal dispersions. Common examples are starch derivatives, cellulose derivatives, alginate, agar, arrowroot, carageenan, collagen, gelatin, guar gum, pectin, diutan gum, welan gum, polysaccharide and xanthan gum.

Various synthetic acrylic/acrylamide-based polymers are also widely available in the market and are used as thickeners.

The ease by which thickeners are effectively dispersed or dissolved in the solvent chemically depends on particle size, molecular weight and structure (average number and distribution of hydroxyl groups per compound) and also the presence of a surfactant.

The primary objectives of the mixing step to disperse and dissolve the thickeners in the solvent are to provide a homogenous mixture and to expose as much surface area of the additive particles. To achieve this goal mechanically, the system is subject to high shear mixing conditions. The above discussed relevant background in relation to mixing of thickeners in solvent systems can be also found in the publication “A guide to understanding and mixing thickeners” by Charles Ross and Son Company, 710 Old Willets Path, Hauppauge, New York 11788.

The problems encountered while dispersing and dissolving such available conventional rheology modifiers in the solvent commercially are the following:
While both the natural and synthetic polymers used for rheology modification which includes thickeners and viscosifiers are commercially available in powder form, simply adding powders on top of an agitated batch used to be the only way to introduce thickeners and since most thickeners have hydrophobic groups they tend to resist wet-out upon contact with water and could float on the surface for hours.
Mixing operators are then forced to carefully sift and add powders only as fast as the liquid will take them. Adding powders slowly into a small batch of vigorously agitated liquid may provide enough time for individual solid particles to hydrate. But in a full-scale production setting, this method of addition is very costly and time-consuming.

Moreover, if powders are added too slowly, an uncontrolled viscosity build-up can occur mid-processing thus preventing the rest of the solids to be fully dissolved.

In contrast, manually adding the powders too fast can cause particles to clump up. The clumps solvate to form a tough outer layer that prevents complete wetting of the interior particles in the clump. This can result in solution defects such as grainy texture, reduced viscosity, or the presence of insoluble particles resembling “fish eyes” and solid remained undissolved. The high shear conditions usually needed to break up these agglomerations can also over shear the already hydrated particles resulting in a permanent viscosity loss.

The relevant solutions attained in the prevailing state of the art on the above discussed problems associated with the rheology modifiers which includes thickeners and viscosifiers are as follows:

EP0009858 discloses the granulate of a gum which comprises agglomerating a powder of the said gum having an average particle size below 100 micron obtained by treating said powder under vigorous agitation with water wherein the water treatment is preferably accomplished by spraying the water in fine droplets into the agitated gum or by blowing water vapour through the agitated gum powder. This prior art thus provided new form of gums which could be dispersed in water to give moderate solutions of moderate viscosity that could be drunk easily.

US5869029 relates to compositions comprising particulate water-soluble or water-swellable polymer at least partially agglomerated without formation of polymer lumps by treatment with at least one polyol, wherein the polyol is at a level greater than about 10 wt. % based on the total weight of the composition. A toothpaste composition is also provided comprising said polyol treated polymer together with dental abrasives such as silicas and insoluble inorganic salts. The composition of this prior art is dispersible in solvents substantially faster due to the polyol than the corresponding untreated water-soluble or water-swellable polymer, without formation of polymer lumps.

US3396034 is directed to a process that inexpensively accomplished readily dispersible, granular free-flowing, and substantially dust-free materials or, respectively, reaction products from substantially solid, divided materials when the finely divided material is fluidized and conveyed on a vibrating inclined surface while being sprayed with a swelling agent or, respectively, liquid reactant, continuously new surfaces of the material particles being exposed to the spray by the vibration which also separates the treated particles from the untreated ones. This prior art is thus directed to convert difficultly dispersible particulates into readily dispersible form.

US3455714 relates to a composition of matter, a water-soluble gum of improved water dispersibility having a polymeric water-soluble and organo-soluble coating thereon of a material selected from the group consisting of hydroxyl propyl cellulose, hydroxyethyl hydroxypropyl cellulose, hydroxypropyl cellulose having ionic substituent, hydroxypropyl cellulose having additional nonionic substituent, cellulose esters, and mixed cellulose esters. This prior art is thus directed to improvement in dispersibility and the solution rate in water of the water soluble gums when coated with a organo-soluble coating.

US4557938 teaches increment in the rate and quality of dispersion of vegetable gum in water when dry blended with food grade particulate carrier on a fluidized bed.

US5496376 discloses a laundry detergent composition wherein the solid content comprises an active surfactant, a water-soluble alkaline carbonate, and a polymeric polycarboxylate, based on the total weight of solids in the composition, said composition containing delayed release agglomerated granules consisting essentially of said polymeric polycarboxylate together with a binder of polyethylene glycol such that the compete release of said polymeric polycarboxylate into wash water under normal washing conditions is delayed to at least about 60 seconds after the complete dissolution of said alkaline carbonate .

US 6084011 teaches cementitious pastes capable of setting after an interval of time comprise (1) a mixture of a fines component selected from cement and a blend of cement and pozzolanic material (e.g., fly ash) 0.8-80 wt.% and (2) water 1.6-20 wt.% with a water soluble polymer 0.004-0.134 wt.%, preferably 0.008 wt.% that is capable of taking up and releasing water when incorporated into the mixture. The polymer is selected from acrylamide homopolymers, acrylamide copolymers, and combination thereof.

JP 10120451 A 19980512 is directed to compositions containing water-soluble polymer with adsorption to cement <10% and that =10%, superplasticizer, hydraulic particles, and water. A concrete prepared from water 160, cement 350, sand 956, and crushed stone 850 kg/m3 with addition of a water-soluble polymer with adsorption to cement 2.0% prepared from a mixture of stearyl alcohol and cetanol with addition of ethylene oxide 0.8, and methylcellulose with adsorption to cement 20.3% 0.05 wt.% (vs. water), and superplasticizer 0.40 wt.% (vs. cement) showed slump flow and excellent segregation resistance.
Thus while polymers, particularly rheology modifiers which includes thickeners and viscosifiers of different varieties and origins offer numerous benefits and have been made available by the state of the art, their incorporation into any liquid formulation to reveal all the advantageous attributes simultaneously to overcome the above discussed disadvantages still remains a challenge requiring advancement and hence there is a need to explore improved polymers and their processing techniques for attainment of the same that reveals full functionality when applied in liquid and other formulations.

OBJECTS OF THE INVENTION
Thus the primary object of the present invention is to provide for water swellable, water soluble, colloidally dispersible polymer particulates of natural and/or synthetic polymers that are at least partially agglomerated and/or at least partially infused with silica and a process for preparing the same, which would display clump free ready and even dispersibility in aqueous systems while also having controlled uniform and superior hydration in aqueous systems to thereby favour easy processibility.
Another object of the present invention is to provide for said polymer particulates which when provided in sizes up to 3000 microns would display said desired characteristics in aqueous systems.
Another object of the present invention is to provide for said polymer particulates that would disperse evenly in aqueous systems without forming clumps/ gel coated lumps/gel particles/ and “fish eyes” even at smaller particle size that would thereby circumvent the problems of clumping experienced with small particle polymers presently encountered in the art.
Yet another object of the present invention is to provide for said polymer particulates that would facilitate cold water solubility in aqueous systems and the use of standard mixing, processing and transferring equipment for energy efficient improved processibility of said particulate seven at high polymer loading.
Another object of the present invention is to provide for said polymer particulates, which due to its even dispersion in aqueous system would achieve improved degree of hydration both at low as well as high polymer loading/dosage levels in aqueous systems to facilitate overall enhanced performance and ease of application of said polymers.
Another object of the present invention is to provide for said polymer particulates, which polymer particulates in providing for fine and uniform dispersion would delay hydration and yielding till after processibility is achieved.
Yet another object of the present invention is to provide for said polymer particulates that would avoid the need for over-shear of the hydrated particles thereby preventing permanent viscosity loss.
Another object of the present invention is to provide for said polymer particulates that would also be crush resistant and would remain intact in transportation and storage like conventional particles in use.
SUMMARY OF THE INVENTION
It is thus the basic aspect of the present invention to provide for water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers that are agglomerated and/or infused with silica providing clump free easy/even dispersibility in aqueous systems and controlled uniform and superior hydration favouring easy processibility.
According to a preferred aspect of the present invention said water soluble/ swellable, colloidally dispersible polymer are provided wherein said polymers are at least partially agglomerated and/or at least partially infused with silica.
Preferably said water soluble/ swellable, colloidally dispersible polymer particulates comprising rheology modifier polymers includes viscosifiers and thickeners.
According to another preferred aspect of the present invention there is provided said water soluble/ swellable, colloidally dispersible polymer particulates wherein said polymer particulates at least partially agglomerated and/ or at least partially infused with silica are obtained of wetted polymer and said silica.
According to yet another preferred aspect of the present invention there is provided said water soluble/ swellable, colloidally dispersible polymer particulates wherein said wetted polymer comprise solvent wetted polymers including water wetted polymers free of binders and/ or additives.
Advantageously said water soluble/ swellable, colloidally dispersible polymer particulates comprise said at least partially agglomerated and/or at least partially infused particulates with or without binders and/ or additives.
According to yet another preferred aspect of the present invention water soluble/ swellable, colloidally dispersible polymer particulates is provided with controlled wettability, clump free dispersibility, cold water solubility and higher polymer loading capability of up to 2 gms for 100 ml aqueous systems as a uniform dispersion for controlled hydration.
It is thus surprisingly found by way of the present invention that water soluble/ swellable, colloidally dispersible polymer particulates in varied particles sizes of up to 3000 microns comprising natural and/ or synthetic polymers when partially agglomerated and/or partially infused with silica provided clump free easy/even dispersibility in aqueous systems even at high polymer loading while also achieving unique improved, controlled, as well as uniform hydration in aqueous systems to thereby favour easy processibility. Furthermore said polymer particulates consistently achieve superior yielding of the polymers as apparent from the higher viscosity levels achieved even at low dosage levels. Such improvement in viscosity levels was found to vary from polymer to polymer and the dosage level used.
Significantly the clump free easy/even dispersibility in aqueous systems achieved by said polymer particulates even at high polymer loading and before hydration of the particulates for subsequent yielding enables uniform and fine dispersions by avoiding the formation of clumps, fish-eyes and gel coated lumps, which lead to unhydrated polymer gels getting stranded in the partially hydrated polymer aqueous systems.
Additionally, such ready dispersibility of said silica infused agglomerated polymer particulates of the present invention in aqueous systems even in cold water system sand even at high polymer loading/ dosage level prior to hydration of the particulates for subsequent yielding, favours improved processibility of said particulates by energy efficient standard mixing, processing and transferring equipment to facilitate ease of application of the said polymers.
Most advantageously, complete hydration of said particulates and its' viscosity build-up in aqueous systems is delayed untill achievement of processibility, such as efficient and facile mixing, formulating, blending, processing and pumping, through the formation of such fine and uniform dispersions of the silica infused agglomerated polymer particulates of the present invention in aqueous systems. Advantageously, said water soluble/ swellable, colloidally dispersible polymer particulates are of size up to 3000 microns.
According to another preferred aspect of the present invention said water soluble/water swellable polymer particulates are provided which are crush resistant. According to a yet another preferred aspect of the present invention said water soluble/ swellable, colloidally dispersible polymer particulates are provided wherein said silica includes treated silica and is selected from crystalline and amorphous silica including precipitated and fumed silica.
Preferably said polymer particulates are provided wherein said water soluble/ swellable, colloidally dispersible natural polymers and their derivatives include starch derivatives, cellulose derivatives, alginate, agar, arrowroot, carageenan, collagen, gelatin, guar gum, pectin, diutan gum, welan gum, polysaccharide and xanthan gum. and said water soluble/ swellable, colloidally dispersible synthetic polymers include AMPS (2-Acrylamido-2-methylpropane sulfonic acid) & NNDMA (n,n-dimethyl acrylamide), Polyacrylamide (PAM), partially Hydrolysed Polyacrylamide (PHPA), acrylate copolymers, modified acrylamide polymers and graft polymers.

According to yet another preferred aspect of the present invention said water soluble/ swellable, colloidally dispersible particulates are provided wherein said natural and/or synthetic polymers: silica is in the ratio range of 80 to 99.90: 0.10 to 20 respectively.
According to another aspect of the present invention a process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates are provided comprising infusing wetted water soluble/ swellable, colloidally dispersible polymer particulates with silica to thereby provide said water swellable, soluble/colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers agglomerated and infused with silica for clump free easy/even dispersibility in aqueous systems and controlled uniform and superior hydration favouring easy processibility.
Preferably said process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates comprise infusing at least partially wetted water swellable, soluble/colloidally dispersible polymer particulates with silica to thereby provide said polymers at least partially agglomerated and/or at least partially infused with silica.
According to another preferred aspect of the present invention a process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates are provided wherein said infusion comprises solvent based wetting of the natural or synthetic polymer including water based wetting of polymer particles free of binders and/or additives.
Preferably, in said process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates said partially infused and/or at least partially agglomerated particles are obtained with or without binders and/ or additives.
According to another preferred aspect of the present invention said process for manufacturing water soluble/ swellable, colloidally dispersible polymer particulates comprises the steps of
(a) providing water soluble/ swellable, colloidally dispersible polymer particulates and silica with or without binders and/or additives as loose at least partially agglomerated particles;
(b) using solvent including water and/or binders to impart wettability to said polymer particulates to thereby at least partially infuse said water soluble/water swellable natural and/or synthetic polymers with silica to produce the clump free easy/evenly dispersible polymer particulates.
Preferably, in said process said natural and/or synthetic polymers: silica: solvent including water are employed in ratio range of 80 to 99.90: 0.10 to 20: 10 to 50 respectively.
According to another preferred aspect of the present invention a process is provided wherein said step (a) comprises
(a) providing water soluble/ swellable, colloidally dispersible polymer particulates in combined ratio range of 80 to 99.90 and said silica in ratio range of 0.10 to 20 whereby said silica enter into the crevices and gaps of the water soluble/ swellable, colloidally dispersible polymer agglomerates;
(b) spraying solvent including water and/or binders in ratio range of 10 to 50 preferably 20 to 30 whereby said silica at least partially fuses with said wetted polymer particulates also on the particle surface facilitating formation of a partial coating of said silica and/or said polymer to produce said clump free easily/evenly dispersible polymer particulates in aqueous systems.
Preferably in said process said step (a) comprises
(i) providing water soluble/ swellable, colloidally dispersible polymer particulates in the form of fine powder in a granulator under rotation followed by addition of solvent including water and/or binders for a desired time to yield loose at least partially agglomerated particles;
(ii) drying the said granules at a desired temperature for a desired time in a suitable dryer followed by sieving to attain at least partially agglomerated particles of size of preferably <3000 micron, more preferably 100-1000 micron.
step (b) comprises
(i) providing said at least partially agglomerated particles in a tumbler type granulator followed by addition of said silica under rotation for a desired time;
(ii) spraying desired amounts of solvent including water and/or binders for a desired time on the rotating granules and further rotating for desired time;
(iii) drying the granules followed by sieving to yield said clump free easy/evenly dispersible polymer particulates in sizes of up to 3000 microns.
More preferably said step (a) comprises
(i) providing water soluble/ swellable, colloidally dispersible polymer particulates in the form of fine powder in amounts of 8 to 10 kg in a granulator rotating at a 10 to 40 preferably about 20- 30 rpm followed by addition of about 1.0 to 5.0 kg preferably about 2 to 3 kg of water for 3 to 6 preferably about 4-5 hrs to yield loose at least partially agglomerated particles;
(ii) drying the said granules at 110-120oC for 2 to 4 hrs preferably about 2-3 hrs in a suitable dryer followed by sieving to attain at least partially agglomerated particles of size of preferably <3000 micron, more preferably 100-1000 micron.
step (b) comprises
(i) providing said at least partially agglomerated particles in amounts of 500 gms in a tumbler type granulator followed by addition of 10 to 125 preferably about 50-70 gms of said silica under rotation at 10 to 40 preferably about 20-30 rpm for 4 to 5 hrs preferably about 2-3 hrs;
(ii) spraying 50 to 250 preferably about 150-200 gm of solvent including water and/or binders for 1 to 5 preferably about 2-3 hrs on the rotating granules and was rotated for another 1 to 4 preferably about 2-3 hrs;
(iii) drying the granules followed by sieving to yield said clump free easy/evenly dispersible polymer particulates in sizes of upto 3000 microns preferably in range of 100-1000 microns.
According to another aspect of the present invention use of a water soluble/ swellable, colloidally dispersible particulates comprising natural and/ or synthetic polymers that are agglomerated and/or infused with silica is provided in various applications including food, pharmaceuticals, cosmetics, personal care, agriculture, adhesives, textile, detergents, paints, coatings, explosives, mining, synthetic resins and water treatment. Preferably for said use said polymers are at least partially agglomerated and/or at least partially infused with silica.
According to another aspect of the present invention a formulation comprising water soluble/ swellable, colloidally dispersible polymer particulates is provided comprising natural and/ or synthetic polymers that are at least partially agglomerated and/or partially infused with silica with or without binders/carriers/builders favouring easy processing in aqueous and aqueous based systems of the same.
Preferably in said formulation said easy processing in aqueous and aqueous based systems of the same includes using energy efficient standard mixing, processing and transferring equipment facilitating clump free uniform dispersion leading to controlled hydration even at high polymer loading even in cold water to achieve improved degree of hydration thereby facilitating overall enhanced performance and ease of application of the same.
According to another aspect of the present invention a method of application of agglomerated water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers in aqueous and aqueous based systems is provided comprises providing said polymer particulates that form a dispersion for controlled and delayed hydration favouring complete hydration and viscosity build up after enabling facile mixing, formulating, blending, processing and pumping in said aqueous and aqueous based systems.
Preferably in said method of application said agglomerated water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers are provided in amounts of 0.01 to 5.00 % in aqueous and aqueous based systems.
The present invention is discussed hereunder in greater details in relation to the non-limiting exemplary illustrations and figures and in no way should be construed to limit the scope of the present invention.
BRIEF DESCRIPTION OF FIGURES
Fig. 1(a) (b) (c) illustrates polymer powder sample; agglomerated particles of size <500 microns; silica infused agglomerated polymer particulates in accordance with the present invention of particles of size <500 microns respectively.
Fig.C1 illustrates the viscosity chart for diutan gum at 0.3% polymer loading in aqueous systems.
Fig.C2 illustrates the viscosity chart for diutan gum at 0.5% polymer loading in aqueous systems.
Fig.C3 illustrates the viscosity chart for diutan gum at 1% polymer loading in aqueous systems.
Fig.C4 illustrates the viscosity chart for 2-Acrylamido-2-methylpropane sulfonic acid & n, n-dimethyl acrylamide copolymer at 1% polymer loading in aqueous systems.
Fig.C5 illustrates the viscosity chart for 2-Acrylamido-2-methylpropane sulfonic acid & n, n-dimethyl acrylamide copolymer at 2% polymer loading in aqueous systems.
Fig.C6 illustrates the viscosity chart for diutan gum with treated silica at 0.5% polymer loading in aqueous systems.
Fig.C7 illustrates the viscosity chart for diutan gum with treated silica at 1% polymer loading in aqueous systems.
Table A1 Illustrates the extent of clumping observed with polymer powders and agglomerated granules in aqueous system. It also shows that silica infused agglomerated polymer particulates of the present invention shows no clumping and a very even dispersion in aqueous systems. Further, it shows agglomerated and ad-mixed silica, ad-mixed silica and wet-blended silica as per respective Comparative Examples shows clumping in aqueous systems.
Table B1 shows that the silica infused agglomerated polymer particulates of the current invention are at least as crush resistant as are agglomerated granules.
Tables C1-C7 illustrates the viscosity results obtained at different dosages of the natural and synthetic polymers including data for treated silica infused agglomerated polymer particulates.

Tables D1-D3 summarizes the viscosity data of the polymer powders, agglomerated granules, silica infused agglomerated polymer particulates, and treated silica infused agglomerated polymer particulates of the present invention showing that the silica infused and treated silica infused agglomerated polymer particulates provides for superior hydration seen in higher viscosities. It also demonstrates the higher loading of silica infused agglomerated polymer particulates of the present invention in aqueous systems.

DETAILED DESCRIPTION OF THE INVENTION
As discussed herein before the present invention provides for water soluble/ swellable, colloidally dispersible polymer particulates comprising natural and/ or synthetic polymers that are at least partially agglomerated and/or at least partially infused with silica with or without binders and /or additives providing clump free easy/even dispersibility in aqueous systems and controlled uniform and superior hydration favouring easy processibility. Advantageously, the polymer particulates of the present invention are in size upto 3000 micron. Importantly, the infused polymer particulates of the present invention evenly/ readily disperse in aqueous systems prior to hydration and subsequent yielding by minimizing the formation of clumps, fish-eyes and gel coated lumps that eventually minimizes the formation of unhydrated polymer gels getting stranded in the partially hydrated polymer aqueous systems that thereby not only allows loading/dosing at higher levels in cold aqueous systems but also enables improved processibility of said particulates by energy efficient standard mixing, processing and transferring equipment to facilitate ease of application of said polymers.
The polymer particulates of the present invention not only thus display properties of clump free easy/even dispersibility in aqueous systems at high polymer loading but also achieves unique improved, controlled, as well as uniform and superior hydration in aqueous systems to thereby favour easy processibility. The silica infused agglomerated polymer particulatesof the present invention, due to the improved hydration, consistently achieves superior yielding of the polymers as apparent from the higher viscosity levels achieved even at low dosage levels. Such improvement in viscosity levels was found to vary from polymer to polymer and the dosage level used. Most advantageously, processibility such as efficient and facile mixing, formulating, blending, processing and pumping, could be achieved because of the formation of such fine and uniform dispersions of the silica infused agglomerated polymer particulates of the present invention in aqueous systems before the delayed and complete hydration of said particulates and viscosity build-up in aqueous systems.
Additional advantages achieved by the polymer particulates of the present invention are as follows:
(i) The polymer particulates of the present invention also immediately wets upon contact with water and does not float on the surface or clumps and thus aids in making solutions with ease in less time with simpler equipment at low processing costs and yet displays unique controlled, as well as uniform hydration and superior yielding of the polymers as apparent from the higher viscosity levels achieved even at low dosage levels.
(ii) The polymer particulates of the present invention also avoids uncontrollable viscosity build up while making solutions from it enabling making solutions of higher loading/ dosage levels and curtailing the disadvantages usually encountered with existing powders and also enabling processibility before yielding / viscosity build-up.
(iii) The polymer particulates of the present invention avoids the need for over-shear of the hydrated particles thereby preventing permanent viscosity loss;

(iv) The polymer particulates of the present invention are crush resistant and remain intact in transportation and storage which resistance is achieved even with or without using any binders that usually appears to interfere with polymer performance like conventional particles presently in use.
Examples: PROCESS STEPS INVOLVED IN MAKING THE POLYMERS IN THE FORM OF PARTIALLY AGGLOMERATED AND SILICA INFUSED PARTICLES OF THE PRESENT INVENTION
Step1:
Finely divided particles of water soluble/ swellable, colloidally dispersible natural and/or synthetic polymers are agglomerated in a conventional granulator and then dried by suitable drying method. Granulator could be of any type e.g. vertical or horizontal; tumbler; vibrator etc. It is important for the agglomerates to be such that infusion of said silica is facilitated
Step 2:
Finely divided particles of said silica are added to the above dried agglomerates in the granulator to enable the said silica to enter into the crevices and gaps in the loose agglomerates.
Step 3:
After an appropriate time solvent including water and/or binder is finely sprayed / added into the mix to enable the said silica to fuse with the water soluble/ swellable, colloidally dispersible polymer. The silica also fuses with the wetted polymer on the surface of the particles to form a skin.
Step 4:
The wet particles are dried to form at least partially agglomerated and silica infused crush resistant particles of mentioned attributes.
Step 5:
The dried at least partially agglomerated particles are sieved to yield particles of size upto 3000 microns preferably 100-1000 microns. The finer particles are recycled along with the coarser particles after crushing.
The above process was followed to obtain exemplary formulations of the polymer in the form of at least partially agglomerated and at least partially infused particles involving silica in accordance with the present advancement as per Examples 1 to 7 detailed hereunder:
Example 1
In a tumbler type granulator 1 kg fine powder of guar gum was taken. The tumbler was rotated at 20 rpm and 250 gms of water was sprayed in 4 hrs on the rotating powder. Agglomerated particles of different sizes are getting formed. These agglomerated particles were dried at 110-120oC for 2 hrs in a suitable dryer. The dried particles were sieved and separated the 100-1000 micron agglomerated particles were selected. Coarser particles were crushed and reused along with the finer particles in the next batch of agglomeration. These selected low density particles are loosely agglomerated. These finer particles are floating on the water and forming gel-coated lumps or clumps when added to water However, they do not allow polymer to be dispersed in the solvent systems including aqueous systems. The particles obtained were also not crush resistant.
Agglomerated 400 gms particles of size 100-1000 microns were again put in the tumbler type granulator. 100 gms of fine precipitated silica was added to it. The tumbler was rotated at 20 rpm for 30 mins after which 200 gm water was sprayed in 2 hrs on the rotating particles. The particles were rotated in the tumbler for further 2 hrs. The particles were dried and sieved to yield particles of size 100-1000 micron. These agglomerated and silica infused polymer particles are denser than the original particles. When they were added to the water it sinks in water without forming gel-coated lumps or clumps. They disperse in the solvent system including water without forming gel-coated particles even at smaller particle size. They display properties of the desired controlled hydration and subsequent complete yielding in aqueous systems and eventually go into solution. The particles are also crush resistant.
Example 2
The agglomerated and silica infused polymer particles were made of the diutan gum in place of guar gum as per the Example-1.
Example 3
The agglomerated and silica infused polymer particles were made of the hydroxyethyl cellulose in place of guar gum as per the Example-1.
Example 4
The agglomerated and silica infused polymer particles were made of the synthetic AMPS and NNDMA copolymer in place of guar gum as per the Example-1.
Example 5
The agglomerated and fumed silica infused particles were made of the diutan gum per the Example-1. Hydrophobic material used was a fine fumed silica powder in place of precipitated silica.
Example 6
The agglomerated and fumed silica infused particles were made of the hydroxy ethyl cellulose in place of guar gum as per the Example-1. Hydrophobic material used was a fine fumed silica powder in place of precipitated silica.
Example 7
The agglomerated and silica infused polymer particles were made of diutan gum in place of guar gum and organic silicone compound treated silica (4 gms) in place of precipitated silica (100 gms) as per Example-1.
Example 8
The agglomerated and silica infused polymer particles were made of diutan gum in place of guar gum and organic silicone compound treated silica (2 gms) in place of precipitated silica (100 gms) as per Example-1.
The comparative process was followed to obtain exemplary formulations of the polymer based rheology modifiers as loosely agglomerated particles free of silica as per Comparative Examples 1 to 4 detailed hereunder:
Comparative Example 1
In a tumbler type granulator 1 kg fine powder of guar gum was taken. The tumbler was rotated at 20 rpm and 250 gms of water was sprayed in 4 hrs on the rotating powder. Agglomerated particles of different sizes are getting formed. These agglomerated particles were dried at 110-120oC for 2 hrs in a suitable dryer. The dried particles were sieved and separated the 100-1000 micron agglomerated particles were selected. Coarser particles were crushed and reused along with the finer particles in the next batch of agglomeration. These selected low density granules are loosely agglomerated. These finer particles are floating on the water and forming gel-coated lumps or clumps when added to water However, they do not allow polymer to be dispersed in the aqueous system. The particles obtained were also not crush resistant.
Comparative Example 2
The loosely agglomerated particles of the size 100-1000 microns were made of the diutan gum in place of guar gum as per the comparative Example-1.
Comparative Example 3
The loosely agglomerated particles of the size 100-1000 microns were made of the Hydoxyethyl cellulose in place of guar gum as per the comparative Example-1.
Comparative Example 4
The loosely agglomerated particles of the size 100-1000 microns were made of the synthetic AMPS-NNDMA copolymer in place of guar gum as per the comparative Example-1.
Comparative Example 5
The loosely agglomerated 400 gms diutan gum particles of size 100-1000 microns of the comparative example-2 again put in the tumbler. 40 gms of fine precipited silica was added to it. The tumbler was rotated at 20 rpm for 30 mins.
Comparative Example 6
The 400 gms powder of diutan gum put in the tumbler. 40 gms of fine precipited silica was added to it. The tumbler was rotated at 20 rpm for 30 mins .
Comparative Example 7
The 400 gms powder of AMPS-NNDMA copolymer tumbled with 40 gms of precipited silica and 200 gms of water sprayed on it in 60 mins to make it wet uniformly. The wet material is dried using the suitable drier and sieved it to collect the particles of 100-1000 microns. Since the process of the present invention was not followed the desired silica infused agglomerated polymer particulates could not be attained even when the ingredients were taken in desired effective quantities.
Comparative Example 8
The loosely agglomerated 500 gms particles of the size 100-1000 microns were made of the diutan gum as per the comparative Example-2 were again put in the tumbler type granulator. 100 gms of fine precipitated silica was added to it. The tumbler was rotated at 20 rpm for 30 mins after which 50 gm water was sprayed in 2 hrs on the rotating particles. The particles were rotated in the tumbler for further 2 hrs. The particles were dried and sieved to yield particles of size 100-1000 micron. Silica particles found free and not infused and/or encapsulated with the polymer particles, which is not desirable, since the water quantity used is less than the required quantity.
Comparative Example 9
The loosely agglomerated 500 gms particles of the size 100-1000 microns were made of the diutan gum as per the comparative Example-2 were again put in the tumbler type granulator. 100 gms of fine precipitated silica was added to it. The tumbler was rotated at 20 rpm for 30 mins after which 400 gm water was sprayed in 2 hrs on the rotating particles. The particles were rotated in the tumbler for further 2 hrs. The particles were found more agglomerated and forming lumps which are not desirable. This is so since excess quantity of water used.
Comparative Example 10
The loosely agglomerated 500 gms particles of the size 100-1000 microns were made of the Diutan gum as per the comparative Example-2 were again put in the tumbler type granulator. 200 mgs of fine precipitated silica was added to it. The tumbler was rotated at 20 rpm for 30 mins after which 200 gm water was sprayed in 2 hrs on the rotating particles. The particles were rotated in the tumbler for further 2 hrs. The particles were found more agglomerated and forming lumps which is not desirable since less quantity of silica used.
Comparative Example 11
The loosely agglomerated 500 gms particles of the size 100-1000 microns were made of the diutan gum as per the comparative Example-2 were again put in the tumbler type granulator. 300 gms of fine precipitated silica was added to it. The tumbler was rotated at 200 rpm for 30 mins after which 200 gm water was sprayed in 2 hrs on the rotating particles. The particles were rotated in the tumbler for further 2 hrs and dried. The silica particles are found free and not infused and/or with the polymer particles, which is not desirable, since higher quantity of silica used.
Comparative properties:
Comparative properties of the loosely agglomerated particles (as per Comparative Examples 1 to 10 and the silica infused agglomerated polymer particulates of the present invention of synthetic and natural polymers (as per Examples 1 to 6) while making solutions as obtained during scale up trials are as Table 1 below.
Table A1: Dispersion tests
Dispersion test (Lumps/clumps formation while making aqueous solution/colloidal dispersion)
196 gms of water in beaker; stirred at 50 rpm; 4 gms of the water soluble/ swellable, colloidally dispersible natural and/or synthetic polymer particles of 250-420 microns added; stirring continued for additional 15 seconds; solution passed through ASTM 20 mesh; retained lumps/clumps on mesh collected, measured in gms and tabulated here under.

No. Polymer Examples Weight of dried polymer in collected lumps (gms) Polymer forming lumps/clumps (%)

1 Guar Gum (Natural polymer) Example -1 0.00 0.0
Comparative Example -1 2.87 71.8

2 Diutan Gum (Natural polymer) Example -2 0.00 0.0
Comparative Example -2 2.62 65.5

3 AMPS-NNDMA synthetic copolymer Example -3 0.47 11.7
Comparative Example -3 3.20 80.0

4 Agglomerated & silica ad-mixed Comparative Example-5 3.08 77.0
5 **Polymer powder & silica ad-mixed Comparative Example-6 3.16 79.0
6 Polymer & silica wet blended & co-dried Comparative Example-7 1.82 45.4
** Particle are of 50-100 microns, since agglomeration is not happened in the process.
Crush resistance test
100 gms water soluble/ swellable, colloidally dispersible natural and/or synthetic polymer particles of the size 400 - 600 microns tumbled with six SS-316 balls, each of 20 mm dia, weighing 16 gms and rotated at 50 rpm in drums having baffles for a specific time period. To determine the percent crushed particles, it is sieved to find the particles < 400 microns.

No. Polymer Examples % Crushed particles (Particles less than 400 microns )
After 10 min After 20 min. After 30 min. After 40 min.
1 Guar Gum (Natural polymer) Example -1 34.2 36.2 44.7 48.6
Comparative Example -1 36.8 44.1 47.8 51.2

2 Diutan Gum (Natural polymer) Example -2 16.9 17.8 20.8 25.6
Comparative Example -2 19.7 21.4 24.3 31.2

3 AMPS-NNDMA synthetic copolymer Example -3 14.5 18.4 22.2 33.6
Comparative Example -3 17.2 17.8 23.1 32.5

Table B1

It is clearly apparent from Tables A1 above that the silica infused agglomerated polymer particulates of the present invention reveals uniform dispersions and controlled hydration to subsequently yield completely in aqueous systems; the admixed and the co-dried mixture and blends fail both uniform dispersion and controlled hydration tests to immediately solvate in aqueous systems to form a tough outer layer subsequently forming clumps, fish-eyes and gel coated lumps, leading to unhydrated polymer gels getting stranded in the partially hydrated polymer aqueous systems. The crush resistant properties of said polymer particulates are however comparable to the conventional particles in use. Table A1 above also demonstrates the superior water solubility of the silica infused agglomerated polymer particulates of the present invention at low/ambient temperature.

Viscosity test results
Viscosity Test Method using M3600 Viscometer of Grace Instruments:

Test Method 1:
Table C1 to C5: Test sample added to water at ambient temp. in 30 sec. under stirring at 4500 rpm.; stirring continued for further 30 sec.; viscosity checked for 5 mins.; stirring resumed for 30 sec at 4500 rpm.; viscosity checked for further 5 mins. Steps repeated for total 30 mins. viscosity graph plotted.

Test Method 2:
Table C6 to C7: Test sample added to water at ambient temp. in 30 sec. under stirring at 1200 rpm.; stirring continued for further 60 sec.; viscosity checked for 5 mins.; stirring resumed for 30 sec at 1200 rpm.; viscosity checked for further 5 mins. Steps repeated for total 30 mins., viscosity graph plotted.

Table C1: Product doses – 0.3% diutan gum on the basis of polymer content

Time (Minute) 0.3% Diutan gum Example-2 0.3% Diutan gum Comp.Example-2 0.3% Diutan gum Powder
1 9.01 9.59 13.90
2 9.20 9.79 13.32
3 9.99 10.77 13.32
4 11.36 11.55 13.12
5 12.34 13.51 14.10
0.5 min stir
6 18.01 25.06 22.13
7 19.39 27.22 22.91
8 20.76 28.78 24.09
9 21.93 28.98 24.48
10 23.50 28.20 25.06
0.5 min stir
11 32.51 33.88 27.41
12 33.88 35.25 27.02
13 34.66 36.03 26.04
14 35.64 35.83 25.65
15 36.81 35.44 25.65
0.5 min stir
16 42.30 38.58 27.41
17 43.27 39.36 27.02
18 44.06 39.75 26.63
19 44.65 38.58 26.83
20 45.43 39.95 27.02
0.5 min stir
21 48.56 41.12 27.41
22 48.76 41.71 27.22
23 49.15 41.12 26.83
24 49.74 40.73 26.43
25 49.74 41.32 26.43
0.5 min stir
26 51.89 41.32 26.43
27 51.50 43.86 25.85
28 51.30 41.32 25.65
29 51.11 42.30 25.46
30 50.72 40.73 25.46

Table C2: Product doses – 0.5% diutan gum on the basis of polymer content

Time (Minute) 0.5% Diutan gum Example-2 0.5% Diutan gum Comp.Example-2 0.5% Diutan gum Powder
1 10.97 13.51 17.43
2 13.71 15.67 17.82
3 16.64 18.21 18.80
4 22.52 25.46 19.39
5 29.57 32.31 20.17
0.5 min stir
6 54.63 49.74 31.72
7 66.18 52.67 31.53
8 79.70 60.51 32.31
9 92.03 62.07 32.31
10 102.61 65.99 32.31
0.5 min stir
11 124.73 69.91 35.44
12 123.75 74.02 35.25
13 123.17 73.82 35.25
14 121.01 75.78 34.66
15 120.82 78.13 33.88
0.5 min stir
16 126.89 80.87 37.20
17 125.91 80.48 36.42
18 125.71 83.02 37.99
19 126.69 85.18 36.81
20 126.10 85.96 35.25
0.5 min stir
21 122.97 83.61 37.20
22 123.56 84.98 37.01
23 123.36 85.77 36.42
24 122.78 89.10 36.23
25 122.19 90.66 35.64
0.5 min stir
26 122.38 88.90 37.20
27 119.45 84.79 37.40
28 119.25 83.22 37.79
29 119.25 84.98 36.62
30 118.08 87.92 36.62

Table C3: Product doses –1.0 % diutan gum

Time (Minute) 1% Diutan gum Example-2 1% Diutan gum Comp.Example-2 1% Diutan gum Powder
1 25.65 31.53 19.97
2 49.54 61.29 21.54
3 117.10 83.22 26.04
4 170.55 111.61 33.88
5 205.21 130.02 37.01
0.5 min stir
6 257.49 146.66 43.08
7 281.97 144.51 42.30
8 292.94 148.43 41.90
9 281.38 153.52 40.93
10 281.78 158.41 40.53
0.5 min stir
11 283.34 170.16 47.19
12 283.15 168.40 47.58
13 275.90 183.67 47.39
14 275.12 191.70 47.97
15 270.42 191.70 48.17
0.5 min stir
16 280.80 186.02 49.74
17 276.29 183.67 50.32
18 267.09 182.11 50.91
19 263.76 186.22 51.50
20 262.78 188.18 52.48
0.5 min stir
21 261.61 189.74 53.26
22 261.41 182.30 52.87
23 262.78 177.21 53.07
24 264.74 180.34 53.07
25 265.33 179.37 53.26
0.5 min stir
26 270.61 181.71 53.26
27 263.96 177.41 54.24
28 258.67 173.29 54.24
29 253.77 174.08 54.44
30 252.80 171.34 54.63

Table C4: Product doses –1 % AMPS-NNDMA copolymer on the basis of polymer content

Time (Minute) 1% AMPS-NNDMA copolymer Example-4 1% AMPS-NNDMA copolymer Comp.Example-4 1% AMPS-NNDMA copolymer
Powder
1 14.88 15.08 13.90
2 16.25 15.86 13.32
3 17.23 16.84 13.71
4 18.01 17.62 14.10
5 18.80 18.21 14.29
0.5 min stir
6 23.69 21.15 17.04
7 23.50 21.34 16.64
8 23.50 21.34 16.45
9 23.50 21.54 16.64
10 23.50 21.93 17.04
0.5 min stir
11 24.48 22.52 19.19
12 24.28 22.52 19.39
13 24.28 22.52 19.39
14 24.28 22.52 19.39
15 24.28 22.52 19.58
0.5 min stir
16 25.26 23.50 21.15
17 25.26 23.50 20.95
18 25.06 22.91 20.95
19 24.87 22.91 20.95
20 24.67 23.30 21.34
0.5 min stir
21 25.46 23.89 21.74
22 25.26 23.89 21.74
23 25.26 23.50 21.93
24 25.06 23.50 21.93
25 25.06 23.50 21.93
0.5 min stir
26 26.24 24.28 23.11
27 25.65 24.09 22.52
28 25.46 23.89 22.52
29 25.26 23.89 22.52
30 25.26 23.89 22.71

Table C5: Product doses–2% AMPS-NNDMA copolymer on the basis of polymer content.

Time (Minute) 2% AMPS-NNDMA copolymer Example-4 2% AMPS-NNDMA copolymer Comp.Example-4 2% AMPS-NNDMA copolymer
Powder
1 32.31 15.08 21.34
2 38.18 17.04 21.54
3 40.53 18.21 22.13
4 42.88 19.19 22.91
5 44.25 19.78 23.50
6 52.28 28.00 28.00
7 52.28 28.20 28.39
8 51.89 28.39 28.98
9 51.50 28.78 29.76
10 51.50 29.37 30.74
11 52.87 32.51 32.51
12 51.89 32.51 32.90
13 51.30 32.51 33.48
14 50.91 32.51 34.07
15 50.72 32.51 34.46
16 52.48 34.46 36.81
17 51.50 35.05 36.81
18 50.91 35.44 37.20
19 50.91 35.44 37.20
20 50.32 35.25 37.60
21 52.28 38.77 39.75
22 51.50 38.58 39.36
23 50.91 38.58 39.36
24 50.52 38.38 39.75
25 50.32 38.38 39.95
26 51.69 40.53 40.93
27 51.11 40.14 41.32
28 50.72 39.95 41.12
29 50.32 39.75 40.93
30 50.32 39.75 41.12

Table C6: Product doses–0.5% diutan gum with treated silica, on the basis of polymer content

Time (Minute) Example-7 Example-8 Comp. Example-2 Powder
1 11.55 10.97 12.73 14.10
2 11.16 11.55 12.73 14.29
3 11.75 13.12 12.73 15.47
4 14.29 15.86 13.12 16.06
5 15.86 19.39 13.51 17.23
6 33.09 35.83 21.93 35.44
7 35.83 38.58 20.95 35.64
8 38.97 42.69 22.52 34.85
9 41.12 45.43 24.48 35.44
10 44.65 47.97 28.00 35.44
11 48.95 54.44 32.70 41.71
12 51.50 56.39 35.05 40.93
13 51.11 57.96 37.20 39.95
14 52.67 59.72 39.95 39.16
15 53.07 61.09 41.32 38.97
16 57.76 64.62 37.01 41.90
17 56.79 64.81 37.20 41.32
18 56.98 65.60 36.81 39.75
19 56.79 66.18 35.83 39.55
20 57.37 66.38 36.81 38.77
21 59.72 70.69 38.58 40.34
22 59.72 68.93 37.99 39.36
23 59.72 68.14 38.58 38.97
24 59.53 68.14 40.53 38.77
25 59.53 68.34 40.14 38.58
26 59.72 69.51 40.93 38.77
27 59.72 68.73 40.34 38.18
28 59.72 67.75 40.34 37.99
29 58.94 67.56 42.88 37.79
30 58.94 67.36 44.45 37.79

Table C7: Product doses –1.0% diutan gum with treated silica, on the basis of polymer content

Time (Minute) Example-7 Example-8 Comp. Example-2 Powder
1 12.73 16.25 14.29 29.57
2 15.08 24.67 17.23 44.45
3 22.91 49.15 20.17 51.30
4 36.03 75.78 25.65 58.35
5 51.50 101.04 30.16 53.46
6 101.63 172.90 46.02 62.86
7 99.28 184.46 52.48 62.07
8 106.13 185.83 54.24 64.81
9 110.24 183.87 58.35 65.01
10 116.51 187.59 61.29 65.60
11 140.01 211.87 67.56 66.97
12 160.18 206.78 70.30 66.58
13 164.87 204.23 72.06 66.18
14 169.57 200.71 74.80 66.38
15 166.05 200.90 77.15 67.36
16 172.12 200.90 78.91 67.56
17 166.44 203.25 79.30 67.16
18 167.62 203.65 80.28 67.36
19 169.18 201.69 81.46 67.56
20 168.60 200.90 83.22 68.53
21 171.14 200.90 83.42 68.53
22 171.53 202.08 83.61 68.14
23 170.36 203.25 84.20 67.56
24 170.95 203.65 85.57 67.56
25 170.36 202.86 86.35 67.56
26 170.95 202.08 87.92 68.73
27 170.55 201.10 87.14 67.95
28 169.18 200.71 87.53 67.56
29 167.81 200.71 88.12 67.56
30 168.40 200.71 88.70 67.75

The above tabulated results under Tables C1-C7 read with corresponding figures are the obtained results at different dosages of the natural and synthetic polymers.

Table D1: Comparative viscosity table for diutan gum by Test Method 1.
Diutan gum (%age)
0.3% loading 0.5% loading % increase in viscosity upon increasing the loading from 0.3%?0.5% 0.5% loading 1% loading % increase in viscosity upon increasing the loading from 0.5%?1%
Polymer Powder 25.46 36.62 43.83 36.62 54.63 49.18
Polymer Agglomerated (Granules) –Comparative Example-2 40.73 87.92 115.86 87.92 171.34 94.88
Agglomerated & Silica infused polymer particulates of the present invention- Example-2 50.72 118.08 132.80 118.08 252.8 114.09

Table D2: Comparative viscosity table for AMPS-NNDMA copolymer by Test Method 1.
AMPS-NNDMA copolymer(%age)
1% loading 2% loading % increase in viscosity upon increasing the loading from 1%?2%
Polymer Powder 22.71 41.12 81.06
Polymer Agglomerated (Granules) - Comparative Example 4 23.89 39.75 66.38
Agglomerated & Silica infused polymer particulates of the present invention- Example-4 25.26 50.32 99.20

Table D3: Comparative viscosity table for treated silica infused diutan gum polymer by Test Method 2.

Diutan gum (%age)
0.5% loading 1% loading % increase in viscosity upon increasing the loading from 0.5%?1%
Polymer Powder 33.79
67.75
100.5
Polymer Agglomerated (Granules) - Comparative Example 2 44.45
88.70
99.5
Agglomerated & Treated Silica infused polymer particulates of the present invention- Example-7 25.26 168.40 565.4
Agglomerated & Treated Silica infused polymer particulates of the present invention- Example-8 67.36 200.71 197.9

It is also thus clearly evident from the viscosity results in Tables and Figs C1-C7 that for all the plots the silica infused agglomerated polymer particulates of the present invention, as compared to the powder polymer and the agglomerated polymer granules, attained the higher desired viscosity.
It was also observed that the viscosity enhancement for the agglomerated & treated silica infused polymer particulates of the present invention from lower loading to higher loading is highest. Read together with Table A1 it shows that the silica infused agglomerated polymer particulates of the present invention, as compared to the powder polymer, the agglomerated polymer granules, admixed, wet co-dried blend and all others not made in accordance with the present invention, gives clump free easy/even dispersibility displaying properties of controlled hydration and delay in complete yielding to facilitate ease of processibility.

Table and Figs D1 and D2 shows the silica infused agglomerated polymer particulates of the present invention enables making solutions of higher loading/dosage levels delaying complete yielding to enable processibility before complete yielding/viscosity build-up thereby avoiding formation of unhydrated polymer gels getting stranded in the partially hydrated polymer aqueous systems preventing full hydration/viscosity build-up of solutions made using powder polymer and the agglomerated polymer granules.

The following inferences can be drawn from all the above Tables and Figures:
Improved Hydration-
Silica infused agglomerated polymer particulates of the current invention consistently achieves superior yielding of the polymers as demonstrated by the higher viscosities achieved at high as well as low dosage levels (Tables and Figs C1-C7). However, the improvement in the hydration of the silica infused agglomerated polymer particulates vary from polymer to polymer and the dosage levels used.
Uniform Dispersion-
Silica infused agglomerated polymer particulates form fine uniform dispersions (as evident from dispersion data in Table A1 above) in aqueous systems before hydrating and subsequently yields whereas the Powder does not and the Granules does so only moderately. The pictures under Fig. 1 also clearly show the change in particle morphology from polymer powder to agglomerated granules to silica infused and agglomerated polymer particulates.
Table A1 reveals clumping of the polymer particles when polymer powder is added in the aqueous system. Adding agglomerated granules to the aqueous system reduces clumping and gives a dispersion of polymer particles in the system. Adding the silica infused agglomerates to the aqueous system shows no clumping and a very even dispersion of polymer particles in the system.
That infusion with silica gives fine and uniform dispersions is also evident and corroborates the higher degree of hydration achieved as indicated by the higher viscosity achieved (Tables and Figs C1-C7). Uniform and fine dispersions minimizes the formation of clumps, fish-eyes and gel coated lumps, which lead to unhydrated polymer gels getting stranded in the partially hydrated polymer aqueous systems.
Eliminates Over Shear -
Since silica infused agglomerated polymer particulates form fine uniform dispersions (as evident from dispersion data in Table A1 above) in aqueous systems the need for excess stirring and mixing is eliminated thereby eliminating over shear.
Improved Processibility-
The superior dispersion of silica infused agglomerated polymer particulates in aqueous systems (as evident from dispersion data in Table A1 above) also enables cold water solubility and the use of energy efficient standard mixing, processing and transferring equipment to facilitate clump free uniform dispersions leading to controlled hydration, even at high polymer loading, to achieve improved degree of hydration thereby facilitating overall enhanced performance and ease of application of the said polymers.
Processibility Before Complete Hydration-
Because of the fine and uniform dispersions achieved with silica infusion of agglomerated polymer particulates and due to its controlled and delayed hydration, efficient and facile mixing, formulating, blending, processing and pumping can be achieved before the complete hydration and viscosity builds up in aqueous systems.
Higher Loading Of Polymer-
The improved processibility and fine, uniform dispersions of silica infused agglomerated polymer particulates permits higher loading of polymers in aqueous systems, even in cold water, which cannot be achieved using conventional Powder and Granules of the same polymers that clumps, forms fish-eyes and gel coated lumps, which lead to unhydrated polymer gels getting stranded in the partially hydrated polymer aqueous systems and hence the attainment of viscosity gets impaired. Table and Figure D1 clearly indicates that in spite of high polymer loading of 1%, the viscosity achieved is just 55 cps for the powder as against the viscosity achieved of 253 cps for silica infused agglomerated polymer particulates at 25°C.
Therefore the above exemplary studies further confirms clump free easy/even dispersibility of the silica infused agglomerated polymer particulates of the present inventionin aqueous systems even at high polymer loading/ dosage levels together with achievement of unique improved, controlled, as well as uniform and superior hydration in aqueous systems to thereby favour easy processibility over the conventional particles in use. The desired crush resistant characteristics of the silica infused particles of the present advancement are at par with the conventional polymer particles/granules in use thus making it suitable for various end applications and uses requiring crush resistant characteristics.
The amount in weight of water soluble/water swell able natural and/or synthetic polymers :silica only when present in select ratio range of 80 to 99.90 : 0.10 to 20 respectively provides for the silica infused agglomerated polymer particulates of the present invention.
It is thus possible for the present advancement to provide for polymers in the form of at least partially agglomerated non-clumping particles of water soluble/ swellable, colloidally dispersible natural and/or synthetic polymers at least partially infused with silica with or without binders and /or additives. The particles of the present invention is provided in varied particle sizes preferably <3000 microns most preferably 100-1000 microns, which particle size can vary depending upon the polymer and field of application. Advantageously silica infused agglomerated polymer particulates of the present invention disperse in aqueous systems and go into solution without forming clumps or gel-coated lumps and display properties of controlled hydration and delay in complete yielding to facilitate efficient and facile mixing, formulating, blending, processing and pumping before the complete hydration and viscosity builds up in aqueous systems in turn also favouring use of energy efficient standard mixing, processing and transferring equipment for end use/application.