Title of Invention	A PROCESS OF MANUFACTURING NANOPARTICLES FROM INDUSTRIAL WASTE AND A FILTER FOR ARSENIC REMOVAL HAVING SUCH NANOPARTICLES
Abstract	A process of manufacturing nano particles from industrial waste comprising the steps of collection of mill scale/iron oxide rich waste from HSM Scale Pit/LD Shop and primary grinding in a dry media of such scales to generate less than 150 um particle and secondary grinding of less than 150 um particle to generate less than 50 nm particles and subjecting the particles less than 50 nm to magnetic property test and subsequently VSM hall probe (curie temperature test) and subjecting the particles that pass the above two tests; dispersion test and ultrasonication test followed by size-analysis by FE-SEM/AFM and then image- analysis and subjecting the aggregate of 15-50 nm particle sizes to X-Ray diffraction for qualitative and quantification of the phases present.

Title of Invention

A PROCESS OF MANUFACTURING NANOPARTICLES FROM INDUSTRIAL WASTE AND A FILTER FOR ARSENIC REMOVAL HAVING SUCH NANOPARTICLES

Abstract

A process of manufacturing nano particles from industrial waste comprising the steps of collection of mill scale/iron oxide rich waste from HSM Scale Pit/LD Shop and primary grinding in a dry media of such scales to generate less than 150 um particle and secondary grinding of less than 150 um particle to generate less than 50 nm particles and subjecting the particles less than 50 nm to magnetic property test and subsequently VSM hall probe (curie temperature test) and subjecting the particles that pass the above two tests; dispersion test and ultrasonication test followed by size-analysis by FE-SEM/AFM and then image- analysis and subjecting the aggregate of 15-50 nm particle sizes to X-Ray diffraction for qualitative and quantification of the phases present.

Full Text	FIELD OF THE INVENTION The present invention relates to a process of manufacturing nanoparticles from industrial waste and a filter for arsenic removal having such nanoparticles adaptable to filter of water. BACKGROUND OF THE INVENTION In many areas of country, it was observed the water ejecting out from tube-wells and other wells having contaminated with arsenic. This arsenic contaminated water if consumed by the human being, causes many incurable skin diseases and health hazards and as a result the whole society is being effected by the health hazards. In order to overcome such critical problem, a new idea envisages to develop a filter which will be capable to remove arsenic from arsenic contaminated water and the cheap water filter for domestic and industrial uses. OBJECTS OF THE INVENTION It is therefore, an object of the present invention to propose a process of manufacturing nanoparticles from industrial waste and a filter for arsenic removal having such nanoparticles adaptable to filter of water which eliminates the disadvantages of prior art. Another object of the present invention is to propose a process of manufacturing nanoparticles from industrial waste and a filter for arsenic removal having such nanoparticles adaptable to filter of water which produces filter water and can be consumed safely by human beings. A further object of the present invention is to propose a process of manufacturing nanoparticles from industrial waste and a filter for arsenic removal having such nanoparticles adaptable to filter of water which is cheap. A still further object of the present invention is to propose a process of manufacturing nanoparticles from industrial waste and a filter for arsenic removal having such nanoparticles adaptable to filter of water which is portable and versatile application. An yet further object of the present invention is to propose a process of manufacturing nanoparticles from industrial waste and a filter for arsenic removal having such nanoparticles adaptable to filter of water which is manufactured by the industrial waste. DESCRIPTION OF THE INVENTION The present invention comprising of 3 steps: Step 1- comprising of collection of mill scale from HSM scale pit. These scales are undergone grinding in dry media in a primary millings operating at 60 rpm using steel balls. These grounded materials are screened and less than 150µm size are taken to a secondary milling machine for further processing. Above 150µm are again returned back to primary milling machine for further grinding. The secondary milling machine rotates at 300 rpm using WC ball in dry media. After second grinding the product is again screened. The particles are analysed by FE- SEM. The particles size more than 100nm are again returned back to secondary milling for futher grinding. The product of secondary milling machine are subjected to magnetic property test and subsequently VSM Hall probe, curie temperature test. If the particles are passed above two tests then particles are undergone to particle size analysis by FE-SEM/FM. If the particles are not qualified in above tests, they are returned back in the secondary millings for further grinding. Before particle size analysis, the particles are subjected to a dispersion test and ultra-sonication tests. After particle size analysis by FE- SEM/AFM, the particles are send to image analysis. Step 2: The acceptable range of particles after secondary milling is 15-50 nm. Once this particle size is achieved, the aggregate of particles are subjected to the X-Ray Diffraction for qualitative and quantitative identification of the phases present in the agglomerate. It has been found that, due to high speed secondary milling in air, most of the iron oxides get oxidized to hematite. Pellets of hematite were made by adding 2% bentonite with a calculated mass of hematite powder. These aggregates of hematite are then reduced by hydrogen gas in a tabular furnace operated at 373 degree centigrade. After reduction, the pellets are furnace cooled by flashing the chamber with nitrogen gas at room temperature. After reduction, these pallets are crushed and again subjected to quantitative X- ray diffraction for phase characterization. Once we achieve > 80% magnetite/maghemite, we consider the agglomerate as a precursor for making arsenic filter. Step 3: The particles were taken for making nano-filter. We have adopted two ways of making nano-filter (a) Filter 1: a filter made up of nanoparticles hold by steel-wool kept under external magnetic field (b) Filter 2: a filter made up of CaSO4, 2H2O (Plaster of Paris), SiO2 (coarse sand) and nanoparticles. ; Filter 1: A glass burette were packed with steel wool and kept under external magnetic field of 2 kGauss. Magnetic nanoparticles were dispersed in ethanol using ultrasonication. The dispersion were poured into the packed burette. Due to the presence of external magnetic field, the magnetic nanoparticles got trapped into the steel wool making a large active surface area for filtration. This makes the filter. The clear tailing of was discarded. 500 ml of artificially made As-contaminated water of 70 ppb strength was allowed to pass through the filter and allowed to stay for 10 mins. Later the water was connected and As+3 strength was measured. It was found close to nil. This confirms the action of the filter, (b) a slurry was made using Plaster of Paris, coarse sand and magnetic nanoparticle and hollow cylindrical structure, like an ordinary candle in household water filter was made. This candle was kept in a small waster filter of 1 lit volume and the As-contaminated water was allowed to pass through the filter. Encouraging results close to the observation in (a) was found. WE CLAIM:- 1. A process of manufacturing nano particles from industrial waste comprising the steps of:- - collection of mill scale/iron oxide rich waste from HSM Scale Pit/LD Shop; - primary grinding in a dry media of such scales to generate less than 150 urn particle; - secondary grinding of less than 150 urn particle to generate less than 50 nm particles; - subjecting the particles less than 50 nm to magnetic property test and subsequently VSM hall probe (curie temperature test); - subjecting the particles that pass the above two tests; dispersion test and ultrasonication test followed by size-analysis by FE-SEM/AFM and then image-analysis; - subjecting the aggregate of 15-50 nm particle sizes to X-Ray diffraction for qualitative and quantification of the phases present. 2. A filter for arsenic removal having nano particles manufactured by the process as claimed in claim 1, comprising - a burette packed with steel wool containing nano particles treated with ethanol using ultrasonication, the burette being kept under external magnetic field; characterized in that the magnetic nano particles are trapped into the steel wool, making a large active surface area for filtration. 3. A filter for arsenic removal as claimed in claim 2, wherein said magnetic field has a strength of 2 kGauss and the external magnetic field has no effect other than merely holding the particles within the steel wool. 4. A filter for arsenic removal having nano particles manufactured by the process as claimed in claim 1 comprises a candle made of a mixture of Plaster of Paris, coarse sand and said nano particles, the candle being placed in a water reservoir for arsenic filtration. ABSTRACT A PROCESS OF MANUFACTURING NANO PARTICLES FROM INDUSTRIAL WASTE AND A FILTER FOR ARSENIC REMOVAL HAVING SUCH NANO PARTICLES A process of manufacturing nano particles from industrial waste comprising the steps of collection of mill scale/iron oxide rich waste from HSM Scale Pit/LD Shop and primary grinding in a dry media of such scales to generate less than 150 um particle and secondary grinding of less than 150 um particle to generate less than 50 nm particles and subjecting the particles less than 50 nm to magnetic property test and subsequently VSM hall probe (curie temperature test) and subjecting the particles that pass the above two tests; dispersion test and ultrasonication test followed by size-analysis by FE-SEM/AFM and then image- analysis and subjecting the aggregate of 15-50 nm particle sizes to X-Ray diffraction for qualitative and quantification of the phases present.

Full Text

FIELD OF THE INVENTION
The present invention relates to a process of manufacturing nanoparticles from
industrial waste and a filter for arsenic removal having such nanoparticles
adaptable to filter of water.
BACKGROUND OF THE INVENTION
In many areas of country, it was observed the water ejecting out from tube-wells
and other wells having contaminated with arsenic. This arsenic contaminated
water if consumed by the human being, causes many incurable skin diseases and
health hazards and as a result the whole society is being effected by the health
hazards. In order to overcome such critical problem, a new idea envisages to
develop a filter which will be capable to remove arsenic from arsenic
contaminated water and the cheap water filter for domestic and industrial uses.
OBJECTS OF THE INVENTION
It is therefore, an object of the present invention to propose a process of
manufacturing nanoparticles from industrial waste and a filter for arsenic
removal having such nanoparticles adaptable to filter of water which eliminates
the disadvantages of prior art.
Another object of the present invention is to propose a process of manufacturing
nanoparticles from industrial waste and a filter for arsenic removal having such

nanoparticles adaptable to filter of water which produces filter water and can be
consumed safely by human beings.
A further object of the present invention is to propose a process of
manufacturing nanoparticles from industrial waste and a filter for arsenic
removal having such nanoparticles adaptable to filter of water which is cheap.
A still further object of the present invention is to propose a process of
manufacturing nanoparticles from industrial waste and a filter for arsenic
removal having such nanoparticles adaptable to filter of water which is portable
and versatile application.
An yet further object of the present invention is to propose a process of
manufacturing nanoparticles from industrial waste and a filter for arsenic
removal having such nanoparticles adaptable to filter of water which is
manufactured by the industrial waste.
DESCRIPTION OF THE INVENTION
The present invention comprising of 3 steps:
Step 1- comprising of collection of mill scale from HSM scale pit. These scales are
undergone grinding in dry media in a primary millings operating at 60 rpm using
steel balls. These grounded materials are screened and less than 150µm size are
taken to a secondary milling machine for further processing. Above 150µm are
again returned back to primary milling machine for further grinding. The
secondary milling machine rotates at 300 rpm using WC ball in dry media. After
second grinding the product is again screened. The particles are analysed by FE-
SEM. The particles size more than 100nm are again returned back to secondary

milling for futher grinding. The product of secondary milling machine are
subjected to magnetic property test and subsequently VSM Hall probe, curie
temperature test. If the particles are passed above two tests then particles are
undergone to particle size analysis by FE-SEM/FM. If the particles are not
qualified in above tests, they are returned back in the secondary millings for
further grinding. Before particle size analysis, the particles are subjected to a
dispersion test and ultra-sonication tests. After particle size analysis by FE-
SEM/AFM, the particles are send to image analysis.
Step 2: The acceptable range of particles after secondary milling is 15-50 nm.
Once this particle size is achieved, the aggregate of particles are subjected to the
X-Ray Diffraction for qualitative and quantitative identification of the phases
present in the agglomerate. It has been found that, due to high speed secondary
milling in air, most of the iron oxides get oxidized to hematite. Pellets of hematite
were made by adding 2% bentonite with a calculated mass of hematite powder.
These aggregates of hematite are then reduced by hydrogen gas in a tabular
furnace operated at 373 degree centigrade. After reduction, the pellets are
furnace cooled by flashing the chamber with nitrogen gas at room temperature.
After reduction, these pallets are crushed and again subjected to quantitative X-
ray diffraction for phase characterization. Once we achieve > 80%
magnetite/maghemite, we consider the agglomerate as a precursor for making
arsenic filter.
Step 3: The particles were taken for making nano-filter. We have adopted two
ways of making nano-filter (a) Filter 1: a filter made up of nanoparticles hold by
steel-wool kept under external magnetic field (b) Filter 2: a filter made up of
CaSO4, 2H2O (Plaster of Paris), SiO2 (coarse sand) and nanoparticles.

;
Filter 1: A glass burette were packed with steel wool and kept under external
magnetic field of 2 kGauss. Magnetic nanoparticles were dispersed in ethanol
using ultrasonication. The dispersion were poured into the packed burette. Due
to the presence of external magnetic field, the magnetic nanoparticles got
trapped into the steel wool making a large active surface area for filtration. This
makes the filter. The clear tailing of was discarded. 500 ml of artificially made
As-contaminated water of 70 ppb strength was allowed to pass through the filter
and allowed to stay for 10 mins. Later the water was connected and As+3
strength was measured. It was found close to nil. This confirms the action of the
filter, (b) a slurry was made using Plaster of Paris, coarse sand and magnetic
nanoparticle and hollow cylindrical structure, like an ordinary candle in household
water filter was made. This candle was kept in a small waster filter of 1 lit
volume and the As-contaminated water was allowed to pass through the filter.
Encouraging results close to the observation in (a) was found.

WE CLAIM:-
1. A process of manufacturing nano particles from industrial waste comprising
the steps of:-
- collection of mill scale/iron oxide rich waste from HSM Scale Pit/LD Shop;
- primary grinding in a dry media of such scales to generate less than 150 urn
particle;
- secondary grinding of less than 150 urn particle to generate less than 50 nm
particles;
- subjecting the particles less than 50 nm to magnetic property test and
subsequently VSM hall probe (curie temperature test);
- subjecting the particles that pass the above two tests; dispersion test and
ultrasonication test followed by size-analysis by FE-SEM/AFM and then
image-analysis;
- subjecting the aggregate of 15-50 nm particle sizes to X-Ray diffraction for
qualitative and quantification of the phases present.
2. A filter for arsenic removal having nano particles manufactured by the process
as claimed in claim 1, comprising
- a burette packed with steel wool containing nano particles treated with
ethanol using ultrasonication, the burette being kept under external
magnetic field;

characterized in that the magnetic nano particles are trapped into the steel
wool, making a large active surface area for filtration.
3. A filter for arsenic removal as claimed in claim 2, wherein said magnetic field
has a strength of 2 kGauss and the external magnetic field has no effect other
than merely holding the particles within the steel wool.
4. A filter for arsenic removal having nano particles manufactured by the process
as claimed in claim 1 comprises a candle made of a mixture of Plaster of Paris,
coarse sand and said nano particles, the candle being placed in a water
reservoir for arsenic filtration.

ABSTRACT

A PROCESS OF MANUFACTURING NANO PARTICLES
FROM INDUSTRIAL WASTE AND A FILTER FOR
ARSENIC REMOVAL HAVING SUCH NANO PARTICLES
A process of manufacturing nano particles from industrial waste comprising the
steps of collection of mill scale/iron oxide rich waste from HSM Scale Pit/LD Shop
and primary grinding in a dry media of such scales to generate less than 150 um
particle and secondary grinding of less than 150 um particle to generate less
than 50 nm particles and subjecting the particles less than 50 nm to magnetic
property test and subsequently VSM hall probe (curie temperature test) and
subjecting the particles that pass the above two tests; dispersion test and
ultrasonication test followed by size-analysis by FE-SEM/AFM and then image-
analysis and subjecting the aggregate of 15-50 nm particle sizes to X-Ray
diffraction for qualitative and quantification of the phases present.

Documents:

1632-KOL-2008-(10-02-2012)-ABSTRACT.pdf

1632-KOL-2008-(10-02-2012)-AMANDED CLAIMS.pdf

1632-KOL-2008-(10-02-2012)-CORRESPONDENCE.pdf

1632-KOL-2008-(10-02-2012)-DESCRIPTION (COMPLETE).pdf

1632-KOL-2008-(10-02-2012)-FORM-1.pdf

1632-KOL-2008-(10-02-2012)-FORM-2.pdf

1632-KOL-2008-(10-02-2012)-OTHERS.pdf

1632-kol-2008-abstract.pdf

1632-kol-2008-claims.pdf

1632-KOL-2008-CORRESPONDENCE 1.1.pdf

1632-KOL-2008-CORRESPONDENCE-1.2.pdf

1632-kol-2008-correspondence.pdf

1632-kol-2008-description (complete).pdf

1632-KOL-2008-EXAMINATION REPORT.pdf

1632-KOL-2008-FORM 1 1.1.pdf

1632-kol-2008-form 1.pdf

1632-KOL-2008-FORM 18-1.1.pdf

1632-kol-2008-form 18.pdf

1632-kol-2008-form 2.pdf

1632-KOL-2008-FORM 3-1.1.pdf

1632-kol-2008-form 3.pdf

1632-KOL-2008-GPA-1.1.pdf

1632-kol-2008-gpa.pdf

1632-KOL-2008-GRANTED-ABSTRACT.pdf

1632-KOL-2008-GRANTED-CLAIMS.pdf

1632-KOL-2008-GRANTED-DESCRIPTION (COMPLETE).pdf

1632-KOL-2008-GRANTED-FORM 1.pdf

1632-KOL-2008-GRANTED-FORM 2.pdf

1632-KOL-2008-GRANTED-SPECIFICATION.pdf

1632-KOL-2008-OTHERS.pdf

1632-KOL-2008-REPLY TO EXAMINATION REPORT.pdf

1632-kol-2008-specification.pdf

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Patent Number

252927

Indian Patent Application Number

1632/KOL/2008

PG Journal Number

24/2012

Publication Date

15-Jun-2012

Grant Date

11-Jun-2012

Date of Filing

23-Sep-2008

Name of Patentee

TATA STEEL LIMITED

Applicant Address

RESEARCH AND DEVELOPMENT AND SCIENTIFIC SERVICES DIVISION, JAMSHEDPUR, 831001, INDIA

Inventors:

#	Inventor's Name	Inventor's Address
1	SUBHANKAR DAS BAKSHI	TATA STEEL LIMITED RESEARCH AND DEVELOPMENT AND SCIENTIFIC SERVICES DIVISION, JAMSHEDPUR 831 001, INDIA

PCT International Classification Number

C02F 1/70; A62D 3/30

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA