Title of Invention

PROCESS OF MAKING PAINT COMPOSITIONS USING PHOSPHATE SLUDGE

Abstract

Novel aqueous and powder coating compositions are revealed herein. The novelty of the invention lies in the use of waste Ferric Phosphate (FeP04) sludge obtained from metal pretreatment zinc phophating process. The disclosed coating compositions are made using the sludge as such and after treating the sludge to neutralize and dry it. Processes of making paint compositions using waste phosphate sludge, a by-product obtained from zinc phosphating metal pretreatment process, for making useful paint compositions comprising mixing wet or dry waste phosphate sludge (1-90%) with dispersing agent (0.5-2.00%), emulsifier (0.01-5%), Wetting Agents (0.05 -0.30%), Freeze-thaw stabiliser (0-5%), thickner (1-3%), pigments (1-50%), biocidal additives (0.01-20%), binder (5-50%) and water (0-20%), resin (5-80%), matting hardener (0-10%), flow control agent (0-2%), degassing agent (0-2%), pigments (1-30%), plasticizer (0-2%), anticaking agent (0.02-2%), additives and / or water

Full Text

FORM 2 THE PATENT ACT 1970 (39 Of 1970) The Patents Rules, 2003 COMPLETE SPECIFICATION See Section 10, and rule 13) 1. TITLE OF INVENTION PROCESS OF MAKING PAINT COMPOSITION USING PHOSPHATE SLUDGE AND PAINT COMPOSITIONS THEREFROM 2. APPLICANT(S) a) Name b) Nationality c) Address : GOODLASS NEROLAC PAINTS LIMITED : INDIAN Company GANPATRAO KADAM MARG, LOWER PAREL, MUMBAI - 4 00 013 3. PREAMBLE TO THE DESCRIPTION The following specification particularly describes the invention and the manner in which it is to be performed : - Process of making Paint Composition Using Phosphate Sludge and Paint Compositions Therefrom Background of Invention For protecting iron/steel sheets from corrosion, Zinc Phosphating pretreatment process of these sheets is carried out in various Industries. Zinc phosphate pretreatment process provides a corrosion resistant base for subsequent coating films. The byproduct of this Zinc phosphating process is a Pale Yellow colored sludge. This sludge mainly comprises of Ferric Phosphate (FePo4). The phosphating and sludge formation reaction can be explained as follows: PHOSPHATE COATING REACTION Currently voluminous amounts of the waste sludge are being disposed off as land fills, adding to the environmental burden. The sludge, a product of chemical reaction, is of consistent quality. The dried sludge is cream colored, insoluble in water and most industrial solvents. The properties of the phosphate sludge make it suitable for use in paint formulations as a Pigment / Extender / Additive / Mattening agent. Owing to the color of the sludge, paint can be made in yellow and other shades. The sludge may be used as available or it may be treated to make it more suitable for use in paints. The principal object of this invention is therefore to manufacture Paint Composition from Phosphate Sludge and method of making the same. Another object of this invention is to provide a Cost effective method of preparing Paint. Still further object is to provide different paint compositions using the Phosphate Sludge. 2 Accordingly, there are provided Paint Compositions comprising about 1 to 90% of Phosphate Sludge as Pigment/ Extender /Additive/ Mattening agent with water based or solvent based polymer binder, thickener, additive and suitable solvents. A method of making the above Paint Composition based on Phosphate Sludge by mixing the Sludge in suitable proportions to give a fine stable coating dispersion in a suitable waterborne or organic solvent borne film forming medium. The sludge may be used as available or it may be treated to make it more suitable for use in Paints. Summary of the invention Novel aqueous and powder coating compositions are described herein. The novelty of the invention lies in the use of waste Ferric Phosphate (FePo4) sludge obtained from metal pretreatment zinc phophating process. The disclosed coating compositions are made using the sludge as such and after treating the sludge to neutralize and dry it. Detailed description of the invention The sludge as such is composed of fine paste and small lumps, has a pale yellow appearance and contains phosphoric acid and water. Aqueous coating compositions have been formulated with the sludge sample as such. Additionally, the sludge sample may be pretreated in various ways to make it suitable for use in more different coatings compositions. The following constitutes one such process to treat the phosphate sludge. This is not exhaustive; other methods may be employed to treat the sludge. Sludge pretreatment Equal quantities of the sludge and deionised water was mixed. The pH of the solution is raised to pH7 by addition of Soda ash and /or triethyl amine and or sodium hydroxide and / or potassium hydroxide and / or mono ethanol amine, under constant stirring. This neutralized mixture thus obtained is filtered with a vacuum filter. The filtrate is given at least three washings with deionised water. The resultant filtrate was dried at 105°C. The properties of the dried sludge are as follows: Physical properties Sludge Appearance Cream Solubility Insoluble in water & most industrial solvents Volatile content 0.10%-0.5% Specific gravity 2.60-2.90 Novel aqueous and powder coating compositions are disclosed herein, formulated using the phosphate sludge as such and after pretreatment. 3 The Aqueous Coating Compositions were formulated comprising Phosphate sludge (1-90%), Dispersing agent (0.5-2.00%), Emulsifier (0.01-5%), Freeze-thaw stabiliser (0-5%), Thickner (1-3%), Pigments (5-50%), Biocidal additives (0.01-20%), Adjuvants (0.01-20%), Binder (5-50%), and remaining water to make a coating composition. The powder coating compositions were formulated comprising dry pretreated waste phosphate sludge in powder form (1-50%) with resin (5-80%), matting hardener (0-10%), flow control agent (0-2%), degassing agent (0-2%), pigments (1-30%), plasticizer (0-2%), anticaking agent (0.02-2%), Examples : The following examples A to V constitute some aqueous coating formulations based on the above experimental work. This is not an exhaustive list of the formulations made. 4 5 6 7 AQUEOUS COATING RAW MATERIALS 1 Water 2 Wet Sludge (as such) 3 Pretreated Dry Sludge 4 Synthetic Yellow oxide Pigment 5 Synthetic Red oxide Pigment 6 Synthetic Red oxide Pigment 7 Cellulosic Thickner 8 TiO2 Pigment 9 XanthanGum 10 iodo propynyl butyl carbamate, carbendazim, N'-(3,4-dichlorophenyl)-N,N-dimethyl-urea, 2-n-octyl-4-isothiazolin-3-one 11 Sodium hydroxide 12 Liquor Ammonia 13 Sodium Poly acrylate 14 Ammonium salt of Polyacrylic Acid, ammonium polyacrylate, sodium salt of Maleic acid/di-isobutylene copolymer 15 Tetra sodium pyro phosphate, Tetra potassium pyro phosphate ,Sodium Hexa meta Phosphate 16. Non ionic Emulsifier (Alkyl aryl sulphonate, Nonyl phenol ethylene oxide condensate.) 17 Glycolic Freeze thaw Stabiliser 18 Dipentene 19 5-chloro-2-metyl-4-isothiazolin-3-one,2-metyl-4-isothiazolin-one1.5%, 2-benzisothiazolin-3-one 20 Carbendazim, Octyliso thiazolinone, iodopropynyl butyl carbamate 21 Acrylic Thickner 22 Binder( polymer such as Acrylics/vinyls/styrene- acrylic/polyurethanes/ synthetic distemper binder.) 23 Silicon Based Additive 8 Manufacturing Process: Example 1 Using Pretreated Dry sludge: To make coating composition, Sand mill is Used. 9 Take a clean container. Add about 70% of the water. Add under slow speed additives like(13,14,18 ), emulsifier(16 ), Glycolic Freeze staw stabiliser (17), 50% of Defomer(23), add( 11,12) check pH and adjust to pH7.5. Add Thickner(7,9) mix for 30 minutes. Add powder(3,4,5,6,8) and run at High speed (peripheral speed of 5-18 m/sec) for 30 minutes. Pass the resultant slurry through sand mill, Keep a flow rate of 200-300 Kg/hr. Check finish with appropriate addition of binder and water in small sample of slurry and then applying by brush Cool to below 55°C add remaining ingredients under slow speed such as biocides (19,20), Binder(22), remaining Defoamer (23),thickner(21) and remaining water. Tint with appropriate colourant.if particular shade is required. Example 2 Using sludge as such : To make the coating composition, Sand mill is Used. 10 Take a clean container. Add Sludge (2) mix for 15 minutes. Add under slow speed additives like (13,14,18), emulsifier (16), Glycolic Freeze staw stabiliser (17), 50% of the Defomer(23), add (11,12) check pH and adjust to pH7.5,Thickner(7, 9) mix for 30 minutes. Add powder (4,5, 6,8) and run at High speed (peripheral speed of 5-18 m/sec) for 30 minutes. Pass through sand mill, Keeping a flow rate of 200-300 Kg/hr. Check finish with appropriate addition of binder and water in small sample of slurry and then applying by brush. Cool to below 55°C add remaining ingredients such as biocodes (19,20), Binder(22), remaining Defoamer (23), thickner(21) and remaining water, under slow speed. Tint with appropriate colourant, if particular shade is required. The following examples PC-A to PC-D constitute some powder coating formulations based on the above experimental work. This is not an exhaustive list of the formulations made. 11 POWDER COATING RAW MATERIALS 24 Pretreated Dry Sludge 25 bisphenol A based epoxy resin, carboxyl terminated polyester resin, hydroxyl terminated polyester resin, 26 carboxyl terminated polyester resin (interior grade), hydroxyl terminated polyester resin, glycydyl acrylics, carboxyl or hydroxyl terminated acrylics 27 Carboxyl terminated polyester resin (Exterior Grade), glycydyl acrylics, carboxyl or hydroxyl terminated acrylics 28 pyromellitic acid monophylnylimidazoline salt, Dicynadiamide derivatives, glycydyl acrylics 29 Triglycidyl isocyanurate 30 Polyacrylate absorbed on silicon dioxide 31 Bezoyl Phenyl carbinol 32 Polyethylene wax 33 PTFE modified Polyethylene Wax 34 Titanium. Di Oxide (Rutile) 35 Carbon black 36 Synthetic Yellow oxide 37 Synthetic Red oxide 38 Barium Sulphate 39 Epoxidised soyabean oil 40 Silicon dioxide, aluminium oxide 12 Example 3 Using Pretreated Dry sludge : Block Diagram of the Process : 13 WE CLAIM: 1. A process of making a paint composition using waste phosphate sludge, a by-product obtained from zinc phosphating metal pretreatment process, for making useful paint compositions comprising mixing wet waste phosphate sludge (1-90%) with dispersing agent (0.5-2.00%), emulsifier (0.01-5%),Wetting Agents (0.05 -0.30%), Freeze-thaw stabiliser (0-5%), thickner (1-3%), pigments (1-50%), biocidal additives (0.01-20%), binder (5-50%) and water (0-20%) in a reactor with high speed dispersion for half an hour subsequently grinding the mixture in a sand mixer at flow rate 200 to 300 kg per hour, cooled below 55°C and mixing additives at a slow speed for half an hour for adjusting the required viscosity to obtained useful paint composition. 2. The process as claimed in claim 1, wherein the waste phosphate sludge is pretreated in demineralised water with Soda ash and /or triethyl amine and or sodium hydroxide and / or potassium hydroxide and / or mono ethanol amine achieve pH7, filtered under vaccum and washed with demineralised water. 3. The process as claimed in claim 2, wherein the pretreated dry sludge in powder form is used for making for making useful paint compositions comprising mixing dry pretreated waste phosphate sludge (1-70%) with dispersing agent (0.5-2.00%), emulsifier (0.01-5%),Wetting Agents (0.05 -0.30%) Freeze-thaw stabiliser (0-5%), thickner (1-3%), pigments (1-50%), biocidal additives (0.01-20%), binder (5-50%) and remaining water to make 100% in a reactor with high speed dispersion for half an hour subsequently grinding the mixture in a sand mixer at flow rate 200 to 300 kg per hour, cooled below 55°C and mixing additives at a slow speed for half an hour for adjusting the required viscosity to obtained useful paint composition. 4. The process as claimed in claim 1, wherein the dispersing agent are selected individually and / or in combination from the group consisting of Ammonium salt of Polyacrylic Acid, ammonium polyacrylate, Na salt of Maleic acid/di-isobutylene copolymer 5. The process as claimed in claim 1, wherein the emulsifier are selected individually and / or in combination from the group consisting of Alkyl aryl sulphonate, Nonyl phenol ethylene oxide condensate. 6. The process as claimed in claim 1, wherein the Wetting Agents are selected individually and/or in combination from group consisting of Tetra sodium pyro phosphate, Tetra potassium pyro phosphate, Sodium Hexa meta Phosphate. 7. The process as claimed in claim 1, wherein the biocidal additives are selected individually and/or in combination from group consisting of 5-chloro-2-metyl-4-isothiazolin-3-one,2-metyl-4-isothiazolin-one 1.5%, 2-benzisothiazolin-3-one, iodo propynyl butyl carbamate, carbendazim, N'-(3,4-dichlorophenyl)-N,N-dimethyl-urea, 2-n-octyl-4-isothiazolin-3-one 8. The process as claimed in claim 1, wherein the Binders are selected individually and/or in combination from group consisting of Acrylics/ vinyls/ styrene-acrylic/ polyurethanes/ synthetic distemper binder. 14 9. The process as claimed in claim 3, wherein the dispersing agent are selected individually and / or in combination from the group consisting of Ammonium salt of Polyacrylic Acid, ammonium polyacrylate, Na salt of Maleic acid/di-isobutylene copolymer 10. The process as claimed in claim 3, wherein the emulsifier are selected individually and / or in combination from the group consisting of Alkyl aryl sulphonate, Nonyl phenol ethylene oxide condensate. 11. The process as claimed in claim 3, wherein the Wetting Agents are selected individually and/or in combination from group consisting of Tetra sodium pyro phosphate, Tetra potassium pyro phosphate, Sodium Hexa meta Phosphate. 12 The process as claimed in claim 3, wherein the biocidal additives are selected individually and/or in combination from group consisting of 5-chloro-2-metyl-4-isothiazolin-3-one,2-metyl-4-isothiazolin-one 1.5%, 2-benzisothiazolin-3-one, iodo propynyl butyl carbamate, carbendazim, N'-(3,4-dichlorophenyl)-N,N-dimethyl-urea, 2-n-octyl-4-isothiazolin-3-one 13. The process as claimed in claim 3, wherein the Binders are selected individually and/or in combination from group consisting of Acrylics/vinyls/styrene-acrylic/polyurethanes. 14. The process as claimed in claim 2, wherein the pretreated dry sludge in powder form is used for making useful paint compositions comprising mixing dry pretreated waste phosphate sludge in powder form (1-50%) with resin (5-60%), matting hardener (0-10%), flow control agent (0-2%), degassing agent (0-2%), pigments (1-20%), plasticizer (0-2%), anticaking agent (0.02-2%), powder coating raw material wherein the process comprises premixing all the solid raw materials in a mixer at a speed 150 to 250 r.p.m. for 3 minutes extruding through an extruder maintained 100°C at a rate of 200 to 300 kg per hour and subsequently cooling the molten extrudate at 5°C-10°C and mixing of resultant flakes with anticaking agent and other additives in a mixer for 5 to 10 minutes and grinding in a grinder to obtain powder coating composition of desired particle size. 15. The process as claimed in claim 2, wherein the pretreated dry sludge in powder form is used for making useful paint compositions comprising mixing dry pretreated waste phosphate sludge in powder form (1-50%) with resin (5-80%), matting hardener (0-10%), flow control agent (0-2%), degassing agent (0-2%), pigments (1-30%), plasticizer (0-2%), anticaking agent (0.02-2%), powder coating additives wherein the process comprises premixing all the solid raw materials in a mixer at a speed 150 to 250 r.p.m. for 3 minutes extruding through an extruder maintained 100-130°C at a rate of 200 to 300 kg per hour and subsequently cooling the molten extrudate at 5°C-10°C and mixing of resultant flakes with anticaking agent or other additives in a mixer for 5 to 10 minutes and grinding in a grinder to obtain powder coating composition of desired particle size. 16. The process as claimed in claim 15 wherein the resin is selected individually and / or in combination from the group compromising bisphenol A based epoxy resin, carboxyl terminated polyester resin, hydroxyl terminated polyester resin, glycydyl acrylics, carboxyl or hydroxyl terminated acrylics. 15 17 .The process as claimed in claim 15 wherein the matting hardner is selected individually and / or in combination from the group compromising pyromellitic acid monophylnylimidazoline salt, Dicynadiamide derivatives, glycydyl acrylics. 18 .The process as claimed in claim 15 wherein the anti-caking agent is selected individually and / or in combination from the group compromising silicon dioxide, aluminium oxide. 19 .The process as claimed in claim 15 wherein the additives are selected individually and / or in combination from the group compromising Triglycidyl isocyanurate, Polyacrylate absorbed on silicon dioxide, Bezoyl Phynyl carbinol, polyethylene tetrafluoride modified wax, Polyethylene wax. HARISHCHANDRA MEGHRAJ BHARUKA MANAGING DIRECTOR GOODLASS NEROLAC PAINTS LTD. 16 this 16th day of February, 2006. ABSTRACT: Novel aqueous and powder coating compositions are revealed herein. The novelty of the invention lies in the use of waste Ferric Phosphate (FeP04) sludge obtained from metal pretreatment zinc phophating process. The disclosed coating compositions are made using the sludge as such and after treating the sludge to neutralize and dry it. Processes of making paint compositions using waste phosphate sludge, a by-product obtained from zinc phosphating metal pretreatment process, for making useful paint compositions comprising mixing wet or dry waste phosphate sludge (1-90%) with dispersing agent (0.5-2.00%), emulsifier (0.01-5%), Wetting Agents (0.05 -0.30%), Freeze-thaw stabiliser (0-5%), thickner (1-3%), pigments (1-50%), biocidal additives (0.01-20%), binder (5-50%) and water (0-20%), resin (5-80%), matting hardener (0-10%), flow control agent (0-2%), degassing agent (0-2%), pigments (1-30%), plasticizer (0-2%), anticaking agent (0.02-2%), additives and / or water To, The controller of Patents, The Patent Office, Mumbai. 2 0 FEB 2006 17

Documents:

181-mum-2005-abstract (complete).doc

181-mum-2005-abstract (complete).pdf

181-mum-2005-abstract(11-03-2008).doc

181-mum-2005-abstract(11-03-2008).pdf

181-mum-2005-cancelled pages(11-03-2008).pdf

181-mum-2005-claims (complete).doc

181-mum-2005-claims (complete).pdf

181-mum-2005-claims(granted)-(11-03-2008).doc

181-mum-2005-claims(granted)-(11-03-2008).pdf

181-mum-2005-correspondence(ipo)-(16-07-2008).pdf

181-mum-2005-correspondence-received-ver-100806.pdf

181-mum-2005-correspondence-received-ver-170206.pdf

181-mum-2005-correspondence-received-ver-180205.pdf

181-mum-2005-correspondence1(17-06-2008).pdf

181-mum-2005-correspondence2(21-02-2006).pdf

181-mum-2005-correspondence3(06-11-2006).pdf

181-mum-2005-correspondence4(11-08-2006).pdf

181-mum-2005-description (complete).pdf

181-mum-2005-description (provisional).pdf

181-mum-2005-form 1(11-03-2008).pdf

181-mum-2005-form 13(11-08-2006).pdf

181-mum-2005-form 13(18-06-2008).pdf

181-mum-2005-form 18(04-12-2006).pdf

181-mum-2005-form 18(06-11-2006).pdf

181-mum-2005-form 2(granted)-(11-03-2008).doc

181-mum-2005-form 2(granted)-(11-03-2008).pdf

181-mum-2005-form 26(18-07-2007).pdf

181-mum-2005-form 26(24-08-2006).pdf

181-mum-2005-form 3(11-03-2008).pdf

181-mum-2005-form 5(11-03-2008).pdf

181-mum-2005-form 5(20-02-2006).pdf

181-mum-2005-form-1.pdf

181-mum-2005-form-13.pdf

181-mum-2005-form-2 (complete).doc

181-mum-2005-form-2 (complete).pdf

181-mum-2005-form-2 (provisional).doc

181-mum-2005-form-2 (provisional).pdf

181-mum-2005-form-3.pdf

181-mum-2005-form-5.pdf

181-mum-2005-power of attoreny(18-06-2008).pdf