Title of Invention

AN IMPROVED INORGANIC BINDER MATRIX USEFUL FOR COLD BRIQUETTING OF IRON AND STEEL PLANT WASTES

Abstract This invention relates to an improved inorganic binder matrix useful for cold briquetting of iron and steel plant wastes. The present invention particularly relates to the development of an improved binder matrix, consisting of a combination of different in-organic binders, which is useful for making composite briquettes by cold briquetting of steel plant wastes such as iron ore fines, flue dust, mill scale, coke fines and the like. The briquettes, obtained through cold briquetting of iron and steel plant wastes with the improved inorganic binder matrix of the present invention, have adequate green strength, cold-crushing strength and RDI and are suitable as blast furnace charge. The binder is synergistic mixture of inorganic binders essentially consisting of pyrophyllite, cement/granulated slag and activated sodium silicate in a ratio in the range of 5 to 10:5 to 10:3 to 7, respectively.
Full Text This invention relates to a process for the manufacture of composite briquettes of iron and steel plant wastes by cold briquetting. The present invention particularly relates to a process for cold briquetting of steel plant wastes sucii as iron ore fines, flue dust, mill scale, coi^e Tn.^s and the like with an improved binder matrix, consisting of a combination of different in-organic binders, to make composite briquettes. The briquettes thus obtained have adequate green strength, cold-crushing strength and RDI and are suitable as blast furnace charge.
Iron and Steel industries, operating all over he world, produce waste materials like, slag, mill-scale and flue dust besides generating a huge quantity of iron ore and coke fines. These wastes cause a lot of storage and environmental related problems besides wastage of valuable resources. In recciit times, efforts have been m.ade to uti these fines employing agglomeration techniques like, pelletisation and briqueiting as pan of zero waste concept. Worldwide, for the 700 million tons of steel produced annually, an estimated 30 million tons of recycle wastes are generated. A typical Indian integrated steel plant of 3 million tons per annum capacity generates around 100,000 tons of iron oxide fines, 55.000 tons of coke fines. 15,000 tons of flue dust and 17,000 tons of mill-scale.
In the known prior art, a few of the steel plants abroad, specially U.S.A., utilise the ore fines generated during steel making, through briquetting method using various organic and/or inorganic binders.
National Steel Corporation, Great lakes division, Chicago. U.S.A. recycle the revert dust/sludges and other materials generated from iron and steel making process through briquetting using inorganic blast furnace binder containing sodium silicate.

U.S. steel, Gary Works, U.S.A. use molasses-cement as binder to produce briquettes which are used as charge for blast furnace and steel making furnaces. U.S. Steel, Edgar, U.S.A., use cement-molasses binder for briquetting revert materials like basic oxygen furnace (BOF) sludge, flue dust. The molasses based binder system causes operational problems like bad odour and ammonia- phenol build-up in recycle water stream.
Bethlehem Steel Corporation, U.S.A., use cement as binder for extrusion of BOF dust.
National Recovery Systems Inc., U.S.A., developed a process to recycle waste oxides in the steel industry by cold bonded rolled briquettes. National Recovery System USA has developed a briquetting process using an inorganic binder for briquetting steel plant revert materials like BOF dust, BOF sludge and flue dust.
The main disadvantages of the above briquetting processes, referred above, are that the binders used causes (i) bad odour, (ii) ammonia-phenol build up in recycle water system, (iii) requirement of extensive gas cleaning, (iv) lower strength of briquettes at high temperature and (v) decrease in strength of briquettes under reducing atmosphere encountered in blastfurnace. Further the above processes do not use coke fines in briquetting of waste oxides from blast furnace / steel industries.
The main object of the present invention is to provide a process for the manufacture of composite briquettes of iron and steel plant wastes by cold briquetting, which obviates the drawbacks of the hitherto known prior art.

Yet another objective of the present invention is to provide and improved inorganic binder matrix useflil for making briquettes suitable as blast furnace charge.
The improved inorganic binder matrix of the present invention provides synergistic combination of inorganic binders consisting of pyrophiilte, cement / granulated slag and activated sodium silicate, useful for making composite briquettes from steel plant wastes like iron ore fines, flue dust, mill scale, coke fines by cold briquetting.
Accordingly the present invention provides an improved inorganic binder matrix useful for cold briquetting of iron and steel plant wastes, which comprises characterized in that a synergistic mixture of inorganic binders essentially consisting of commercial grade pyrophiilte, cement/granulated slag and activated sodium silicate in a ratio in the range of 5 to 10:5 to 10:3 to 7 by wt., respectively.
In an embodiment of the present invention, the pyrophiilte is of commercial grade.
In another embodiment of the present invention, the cement/granulated slag is of- 100 |i size.
In still another embodiment of the present invention, the granulated slag is an industrial waste / by-product.
In yet another embodiment of the present invention, the cement/granulated slag is of commercial grade.

In a further embodiment of the present invention, the activated sodium silicate is of commercial grade.
The improved inorganic binder matrix of the present invneiton is not a mere admixture but a synergistic mixture having properties which are distinct from the mere aggregation of the properties of the individual ingredients and there is no chemical reaction.
The improved inorganic binder matrix of the present invention provides different combination of inorganic binders in the ratio range as detailed above, useful for making composite briquettes using steel plant wastes like iron ore fines, flue dust, mill scale, coke fines by cold briquetting.
In a co-pending patent application no 1223/del/2002 we have described and claimed a process for the manufacture of composite briquettes of iron and steel plant wastes by cold briquetting with an improved inorganic binder matrix. The steel plant wastes used in cold briquetting are in a combination of iron ore fines of - 6 mm size, flue dust of - 3 mm zide, mill scale of- 6 mm size and coke fines of-6 mm size. The combination of inorganic binders used on the basis of wt% of charge materials are: pyrophilite in the range of 5-10%, cement/granulated slag of (-100 [x size) in the range of 5 - 10% and activated commercial grade sodium silicate (NazO : SiOz == 1:1 ) in the range of 3 - 7%.
The composite briquettes obtained using different binder combinations of the present invention have sufficient green strength (above 4 drops), cold-crushing strength of above 250 kg/briquette from cylindrical briquettes and above 130 kg/briquette fro elliptical briquettes and RDI of below 30%, and are suitable for charging into blast furnace for further processing.

press by applying a vertical compression load of the order of 350-450 kg/cm^ and 100-200 kg/cm^ to obtain the cylindrical and elliptical briquettes, respectively, and curing the such briquettes so obtained, under natural conditions for a period of 3-6 days.
In an embodiment of the present invention, the steel plant wastes are in a combination of iron ore fines of - 6 mm size, flue dust of - 3 mm size, mill scale of - 6 mm size and coke fines of - 6 mm size.
In another embodiment of the present invention, the vertical compression load
used in briquetting machine for making cylindrical briquettes is preferably 400
kg/cm^
In yet another embodiment of the present invention, the vertical compression
load used in briquetting roll press for making elliptical briquettes is preferably
150 kg/cm^
In a further embodiment of the present invention, the composite briquettes
obtained have green strength of above 4 drops, cold-crushing strength of above
250 kg/briquette for cylindrical briquettes and above 130 kg/briquette for
elliptical briquettes and RDI of below 30%, and are suitable for charging into
blast furnace for further processing.
The process steps of the present invention for the manufacture of composite briquettes of iron and steel plant wastes by cold briquetting, comprises of: (i) Dry mixing of iron and steel plant wastes such as iron ore fines, flue dust, mill scale, coke fines. The steel plant wastes used are in a

combination of iron ore fines of - 6 mm size, flue dust of - 3 mm size, mill scale of - 6 mm size and coke fines of- 6 mm size.
(ii) Adding to the dry mix, of iron and steel plant wastes obtained in step (i), a binder m.atrix and subjecting to thorough mixing. The binder matrix essentially consisting of inorganic binders such as pyrophilite, cement / ground granulated slag of steel plant and activated commercial grade sodium silicate (Na20 : SiOa «1:1) and are used in a combination on the basis of wt % of charge materials such as: pyrophilite in the range of 5 - 10%, cement/granulated slag of -100 [i size in the range of 5 - 10% and activated commercial grade sodium silicate (NaiO :Si02 »1:1) in the range of 3 - 7%.
(iii) Adding water to the resultant dry mix, obtained in step (ii), and subjecting to further mixing to obtain a charge mixture dough.
(iv) Cold briquetling the resultant charge mixture dough, obtained in step (iii), by conventional. Cold briquetting of the resultant charge mixture dough to obtain cylindrical briquettes, elliptical briquettes is effected in a briquetting machine, briquetting roll press by applying a vertical compression load of the order of 400 kg/cm^, 150 kg/cm , respectively.
(v) Curing the briquettes so obtained, in step (iv), under natural conditions for a period of about 5 days.
A novel feature of the .present invention is the manufacture of composite briquettes by cold briquetting of iron and steel plant wastes, such as iron ore fines, flue dust, mill scale, coke fines, which are otherwise unutilised and are an environmental hazard. Another novel feature of the present invention is the manufacture of composite briquettes having green strength of above 4 drops, cold-crushing strength of above 250 kg/briquette for cylindrical briquettes and above 130 kg/briquette for elliptical briquettes

and (Reduction degradation Index) RDI of below 30%, and are suitable for charging into blast furnace for further processing. The novel features of the present invention have been realised by the non-obvious inventive step of providing a combination of iron and steel plant wastes as charge materials, such as iron ore fines of - 6 mm size, flue dust of - 3 mm size, mill scale of - 6 mm size and coke fines of - 6 mm size and improved inorganic binder matrix consisting of a combination of inorganic binders used on the basis of wt % of charge materials such as pyrophilite in the range of 5 -10%, cement/granulated slag of steel plant of -100 i^ size in the range of 5 - 10% and activated commercial grade sodium silicate (Na20 :Si02 ~1:1) in the range of 3 - 7%.
In a co-pending patent application no. 1224/del/2002, we have described and claimed an improved inorganic binder matrix useful for cold briquetting of iron and steel plant wastes. The improved inorganic binder matrix enables making composite briquettes using steel plant wastes like iron ore fines, flue dust, mill scale, coke fines by cold briquetting and these briquettes are suitable for charging into blast furnace for further processing. The improved inorganic binder matrix is a novel synergistic mixture of inorganic binders essentially consisting of pyrophilite, cement/granulated slag and activated sodium silicate in a ratio in the range of 5 to 10 : 5 to 10 : 3 to 7, respectively.
The following examples are given to illustrate how the process of the present invention is carried out in actual practice and should not be construed to limit the scope of the invention.

Example-1
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and '^hcn 50g of pyrophilite (5% by weight of charge), 50g of cement (5% by weight of charge) were added and again mixed. 40g of activated sodium silicate (4% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine by applying a vertical compression load of 400 kg/cm^. The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes were found to have green strength of 4 drops, cold crushing strength of 260 kg^riquette after curing and RDI of 23%.
Example-2
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then lOOg of pyrophilite (10% by weight of charge), 50g of cement (5% by weight of charge) were added and again mixed. 40g of activated sodium silicate (4% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine by applying a vertical compression load of 400 kg/cm^. The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes were found to have green strength of 6 drops, cold crushing strength of 265 kg/briquette after curing and RDI of 8%.

Example-3
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then 50g of pyrophilite (5% by weight of charge), lOOg of cement (10% by weight of charge) were added and again mixed. 40g of activated sodium silicate, (4% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine applying a vertical compression load of 400 kg/cm^ The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 4 drops, cold crushing strength of 350 kg/briquette after curing and RDl of 20%.
Example-4
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then 50g of pyrophilite (5% by weight of charge), 50g of ground granulated slag (5% by weight of charge) were added and again mixed. 40g of activated sodium silicate (4%) by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine applying a vertical compression load of 400 kg/cm^. The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes have green strength of 4 drops, cold crushing strength of 280 kg/briquette after curing and RDI of 22%.
Example-5
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then 50g of pyrophilite (5% by weight of charge), lOOg of ground granulated slag (10% by weight of charge) were added and again mixed. 40g of activated sodium silicate (4% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine applying a vertical compression load of 400 kg/cm . The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 5 drops, cold cRishing strength of 285 kg/briquette after curing and RDI of 20%.
Example-6
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then 50g of pyrophilite (5% by weight of charge), 50g of cement (5% by weight of charge) were added and again mixed. 30g of activated sodium silicate (3% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine applying a vertical compression load of 400 kg/cm^. The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 4 drops, cold crushing strength of 265 kg/briquette after curing and RDI of 15%.
Example-7
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then 50g of pyrophilite (5% by weight of charge), 50g of cement (5% by weight of charge) were added and again mixed. 70g of activated sodium silicate (7% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine applying a vertical compression load of 400 kg/cm^. The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 5 drops, cold crushing strength of 350 kg/briquette after curing and PvDI of 9%.
Example-8
750g of iron ore fines, lOOg mill-scale, 50g flue-dust and lOOg coke fines were mixed thoroughly and then 50g of pyrophilite (5% by weight of charge), 50g of ground granulated slag (5% by weight of charge) were added and again mixed. 30g of activated sodium silicate (3% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of cylindrical shape were made using this mix in a briquetting machine applying a vertical compression load of 400 kg/cm'. The cylindrical briquettes obtained were of the size of 28 mm diameter and of 30 mm height. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 4 drops, cold crushing strength of 330 kg/briquette after curing and RDI of 15%.
Example-9
7.5 kg of iron ore fines, 1 kg of mill-scale, 0.5 kg of flue dust and 1 kg of coke fines ere mixed thoroughly and then 0.7 kg of pyrophilite (7% by weight of charge), 0.7 kg of cement (7% by weight of charge) were added and again mixed. 0.5 kg of activated sodium silicate (5% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of elliptical shape were made using this mix in a briquetting roll press by applying a load of 150 kg/cm^. The elliptical briquettes obtained were of 50 mm x 35 mm x 15 mm size. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 5 drops, cold crushing strength of 140 ks/briauette after curing and FDI of 22%.
Example-10
7.5 kg of iron ore fines, 1 kg of mill-scale, 0.5 kg of flue dust and 1 kg of coke fines were mixed thoroughly and then 0.7 kg of pyrophilite (7% by weight of charge), 0.7 kg of ground granulated slag (7% by weight of charge) were added and again mixed. 0.5 kg of activated sodium silicate (5% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of elliptical shape were made using this mix in a briquetting roll press by applying a load of 150 kg/cm^. The elliptical briquettes obtained were of 50 mm X 35 mm x 15 mm size. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 4 drops, cold crushing strength of 188 kg^riquette after curing and RDI of 21%.
Example-11
7.5 kg of iron ore fines, 1 kg of mill-scale, 0.5 kg of flue dust and 1 kg of coke fines were mixed thoroughly and then 0.5 kg of pyrophite (5% by weight of charge), 0.5 kg of cement (5% by weight of charge) were added and again mixed. 0.3 kg of activated sodium silicate (3% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of elliptical shape were made using this mix in a briquetting roll press by applying a load of 150 kg/cm". The elliptical briquettes obtained were of 50 mm x 35 mm x 15 mm size. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 4 drops, cold crushing strength of 145 kg/briquette after curing and RDI of 19%.
Example-12
7.5 kg of iron ore fines, 1 kg of mill-scale, 0.5 kg of flue dust and 1 kg of coke fines were mixed thoroughly and then 0.5 kg of pyrophite (5% by weight of charge), 0.5 kg of ground granulated slag (5% by weight of charge) were added and again mixed. 0.3 kg of activated sodium silicate (3% by weight of charge) was added to the above charge mix and mixed thoroughly by adding suitable amount of water. Composite briquettes of elliptical shape were made using this mix in a briquetting roll press by applying a load of 150 kg/cm^. The elliptical briquettes obtained were of 50 mm X 35 mm x 15 mm size. The briquettes were subjected to natural curing for 5 days. The briquettes had green strength of 4 drops, cold crushing strength of 130 kg/'briquette after curing and RDI of 25%.

The main advantages of the process of the present invention are :
1. Manufacture of composite briquettes by cold briquetting of iron and steel plant wastes, such as iron ore fines, flue dust, mill scale, coke fines, which are otherwise unutilised and are an environmental hazard.
2. The iron and steel plant wastes such as iron ore fines, flue dust, mill scale, coke fines can be cold briquetted and these briquettes are suitable for charging into blast furnace for further processing.
3. The process wherein the briquettes of various shapes such as cylindrical and elliptical briquettes have sufficient green strength, cold crushing strength and RDI for charging into the blast furnace.
4. The composite briquettes of iron and steel plant wastes manufactured by cold briquetting have green strength (above 4 drops), cold-crushing strength of above 250 kg/briquette for cylindrical briquettes and above 130 kg/lDriquette for elliptical briquettes and RDI of below 30%.
5. The process is cost effective.



We Claim:
1. An improved inorganic binder matrix useful for cold briquetting of iron and steel plant wastes, which comprises characterized in that a synergistic mixture of inorganic binders essentially consisting of commercial grade pyrophilite, cement/granulated slag and activated sodium silicate in a ratio in the range of 5 to 10:5 to 10:3 to 7 by wt, respectively.
2. An improved inorganic binder matrix, wherein the cement / granulated slag is of- 100µ size.
3. An improved inorganic binder matrix, wherein the granulated slag is an industrial waste / by-product iron ore fines, flue dust, mill scale, coke fines.
4. An improved inorganic binder matrix, wherein the activated sodium silicate consists of Na2O : SiO2 ≈ 1:1.
5. An improved inorganic binder matrix useful for cold briquetting of iron and steel plant wastes, substantially as herein described with reference to the examples.

Documents:

1224-DEL-2002-Abstract-(10-09-2008).pdf

1224-DEL-2002-Abstract-(26-03-2008).pdf

1224-DEL-2002-Abstract-(30-07-2008).pdf

1224-del-2002-abstract.pdf

1224-DEL-2002-Claims-(10-09-2008).pdf

1224-DEL-2002-Claims-(26-03-2008).pdf

1224-DEL-2002-Claims-(30-07-2008).pdf

1224-del-2002-claims.pdf

1224-DEL-2002-Correspondence-Others-(10-09-2008).pdf

1224-DEL-2002-Correspondence-Others-(26-03-2008).pdf

1224-DEL-2002-Correspondence-Others-(30-07-2008).pdf

1224-del-2002-correspondence-others.pdf

1224-del-2002-correspondence-po.pdf

1224-DEL-2002-Description (Complete)-(10-09-2008).pdf

1224-DEL-2002-Description (Complete)-(26-03-2008).pdf

1224-DEL-2002-Description (Complete)-(30-07-2008).pdf

1224-del-2002-description (complete).pdf

1224-DEL-2002-Form-1-(26-03-2008).pdf

1224-del-2002-form-1.pdf

1224-del-2002-form-18.pdf

1224-DEL-2002-Form-2-(10-09-2008).pdf

1224-DEL-2002-Form-2-(26-03-2008).pdf

1224-del-2002-form-2.pdf

1224-DEL-2002-Form-3-(26-03-2008).pdf

1224-del-2002-form-3.pdf


Patent Number 223618
Indian Patent Application Number 1224/DEL/2002
PG Journal Number 40/2008
Publication Date 03-Oct-2008
Grant Date 18-Sep-2008
Date of Filing 09-Dec-2002
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110001, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 JITENDRA NATH MOHANTY REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
2 HEMANTA KUMAR TRIPATHY REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
3 YERRAMSETTI VENKATA SWAMY REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
4 BHASKARA VENKATA RAMANA MURTHY REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
5 SURESH CHANDRA SAHU REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
6 ANIL KANTA TRIPATHY REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
7 VIBHUTI NARAIN MISRA REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013, ORISSA, INDIA.
PCT International Classification Number C02F 11/14
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA