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Production Of High Purity (99.999%) Iron Flakes By Electrolysis

Abstract: The present invention claims a novel process of electrolysis for the consistent production of iron flakes of extremely high purity (99.999%), and with minimal gaseous and other impurities.

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Patent Information

Application #
Filing Date
13 December 2017
Publication Number
24/2019
Publication Type
INA
Invention Field
METALLURGY
Status
Email
Parent Application
Patent Number
Legal Status
Grant Date
2020-11-12
Renewal Date

Applicants

Industrial Metal Powders Pvt. Ltd.
Gat No. 699/1, Koregaon Bhima, Pune-Nagar Road, Shirur, Pune - 412216, Maharashtra, India

Inventors

1. Prakash Kundanmal Dhoka
Gat No. 699/1, Koregaon Bhima, Pune-Nagar Road, Shirur, Pune - 412216, Maharashtra, India
2. Rajendra Keshav Kshirsagar
Gat No. 699/1, Koregaon Bhima, Pune-Nagar Road, Shirur, Pune - 412216, Maharashtra, India
3. Sanjay Kisan Gaikwad
Gat No. 699/1, Koregaon Bhima, Pune-Nagar Road, Shirur, Pune - 412216, Maharashtra, India

Specification

Claims:We claim,

1. A novel method of electrolysis for the consistent production of iron flakes of extremely high purity.
2. The novel method of electrolysis as claimed in claim 1, wherein the said method utilises a novel composition of electrolytic bath, comprising of a homogenous solution of -
i. 50-500 g/L of iron sulphate,
ii. 1-200 g/L of iron chloride, and
iii. 1-100 g/L of ammonium chloride.
3. The novel method of electrolysis as claimed in claim 1, wherein the final electrolysis conditions are preferably set at, but not limited to -
i. pH of 2.0 to 5.0,
ii. Bath temperature of 105°F-155°F,
iii. Current of 400-600 Amps,
iv. Voltage of 1-3 V.
4. The novel method of electrolysis as claimed in claim 1, wherein the said electrolysis is performed in an electrode deposition tank, which is preferably, but not limited to, a rubber lined MS tank.
5. The electrode deposition tank as claimed in claim 4, wherein the electrodes are arranged horizontally within the tank in an alternating manner.
6. The electrodes as claimed in claim 5, wherein the said electrodes are either anodes or cathodes.
7. The cathodes as claimed in claim 6, wherein the said cathodes are preferably composed of stainless steel.
8. The anodes as claimed in claim 7, wherein the said anodes are preferably composed of impure iron.
9. The anodes as claimed in claim 7, wherein the number of anodes is such that it is one more than the number of cathodes in the electrode deposition tank.
10. The electrodes as claimed in claim 5, wherein the distance between the cathode and anode must be maintained at 100-150 mm.
11. The novel method of electrolysis as claimed in claim 1, wherein the process of electrolysis is followed by post-electrolysis steps to ensure uniformity, durability and improved shelf life of the flakes.
12. The post-electrolysis steps as claimed in claim 11, wherein the said steps are -
i. Washing of cathodes with cold and hot water jets,
ii. Passivation of cathodes with commercially obtained cleaning chemicals,
iii. Stripping of iron flakes to separate them from the cathode,
iv. Jaw crushing of iron flakes,
v. Annealing of iron flakes,
vi. Coating of iron flakes with commercially obtained coating materials.

, Description:FIELD OF THE INVENTION:
The present invention describes a method for the production of iron flakes of extremely high purity (99.999%) and with minimal gaseous impurities.

DEFINITIONS:
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used, indicate otherwise.
The expression “Electrode” used hereinafter in this specification refers to, but is not limited to, a conductor through which electricity enters or leaves an object, substance or region.
The expression “Cathode” used hereinafter in this specification refers to, but is not limited to, the negatively charged electrode by which electrons enter an electrical device, substance or region.
The expression “Anode” used hereinafter in this specification refers to, but is not limited to, the positively charged electrode by which electrons leave an electrical device, substance or region.
The expression “Electrolytic bath”; referred to as simply “bath”, used hereinafter in this specification refers to, but is not limited to, a solution or molten substance that conducts electricity.

BACKGROUND
Iron flakes are required for a large number of high end industrial applications, including but not limited to, the manufacture of specialty steels and super alloys; and in the fields of aerospace and nuclear power. With the increasing number of industrial applications of iron flakes in the current day, there is a need for the production of iron flakes of extremely high purity, i.e., the amount of metal and gaseous impurities in the flakes must be minimal. At present, the iron flakes produced are of maximum 99.99% purity – this is not pure enough for the aforementioned high end applications. The present invention elaborates on a method to produce iron flakes of 99.999% purity, with low variation and minimal gaseous impurities.
The method disclosed in the present invention overcomes the drawbacks of and offers several advantages over the currently used techniques of electrolytic production of iron flakes. Embodiments of the present disclosure that surpass the current techniques include but are not limited to – proper surface preparation of cathode and anode, tighter control of electrolytic bath parameters, increased spacing between electrodes and refined washing and passivation processes.
Not only are the iron flakes produced by the present method of a higher quality and purity than the iron flakes yielded by currently used methods, but the method of production employed in this invention is more economical than other methods in current use.

OBJECTS:
The objects of present disclosure are aimed at ameliorating one or more problems of the prior art or to at least provide useful alternatives as listed herein below.
The object of the present invention is to provide an electrolytic method for the production of iron flakes.
Another object of the present invention is to provide a method for the production of iron flakes of extremely high purity (~99.999% pure).

SUMMARY:
Before the present invention is described, it is to be understood that present invention is not limited to particular methodologies and materials described, as these may vary as per the person skilled in the art. It is also to be understood that the terminology used in the description is for the purpose of describing the particular embodiments only, and is not intended to limit the scope of the present invention.
The present invention describes a novel composition of electrolytic bath and electrolysis parameters for the production of iron flakes of extremely high purity (99.999%). The flakes produced have low variation in properties. The process involves post-production (i.e., post-electrolysis) steps of passivation, annealing and coating which are performed in order to improve the shelf life of the flakes, as well as to enhance uniformity and appearance and ensure homogeneity of the flakes.

DETAILED DESCRIPTION:
Before the present invention is described, it is to be understood that this invention is not limited to particular methodologies described, as these may vary as per the person skilled in the art. It is also to be understood that the terminology used in the description is for the purpose of describing the particular embodiments only, and is not intended to limit the scope of the present invention. Throughout this specification, the word “comprise”, or variations such as “comprises” or “comprising”, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps. The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results.

The first requirement for the process of production of iron flakes by electrolysis is the preparation of the electrolytic bath. The bath is composed of chlorides and sulphates of iron and chlorides of ammonia. The typical ranges of concentration of these salts is -
1. 50-500 g/L iron sulphates.
2. 1-200 g/L iron chlorides.
3. 1-100 g/L ammonium chlorides.
The commercially procured salts are dissolved in water in the concentrations detailed above and stirred with the help of stirrers in order to obtain a homogenous solution. This process is performed in the deposition tank.
The pH of the bath solution is maintained at acidic levels (between 2.0-5.0) and the temperature is maintained at 105°F-155°F.

The process of electrolysis is performed in an electrode deposition tank. The tank used in the present invention is rubber lined MS tank. In each tank is a horizontal arrangement of electrodes; such that the number of anodes is one more than the number of cathodes used. The electrodes are arranged in an alternating manner such that a cathode is placed next to an anode, which is placed next to another cathode and so on. In order to produce flakes of the extremely high purity desired, the spacing between the electrodes is of paramount importance. This spacing must be maintained at 100-150 mm. The anodes are made of impure iron and the cathodes of sheets of stainless steel.

Once the bath has been prepared, dummying of the bath solution is carried out over a span of 15 days. The conditions of electrolysis and solutions used are identical to those used during the actual electrolysis. The difference between the dummying period and the actual electrolysis is that only anodes are used during the dummying period (i.e., cathodes are not a part of the set up). During this period, the bath is continually monitored for pH, temperature, voltage and ferrous content by titration. After the dummying period, the dummy products are discarded and fresh anodes and cathodes are installed before actual usage of the bath for the production of iron flakes.

The electrolysis reaction occurring during the actual production process is -
Electrolysis reaction at Cathode Fe2+ + 2e- ? Fe (Metal)
Electrolysis reaction at anode Fe (Metal) ? Fe2- + 2e-
During this process, a current of 500 Amps and a voltage of 2V is applied to the tank.
From the reactions depicted above, it can be understood that ferrous ions are produced at the anode and flow through the bath towards the cathode. At the cathode, the double positive charged ferrous ions pick up two electrons and form iron metal. As the process of electrolysis continues, iron metal gradually gets deposited at the cathode.

During the actual production process, aeration is performed with the help of fixtures fitted into the deposition tanks. This is done in order to ensure uniformity of bath solution. The bath is monitored daily and granules that stick to the edges and bottom are removed at regular intervals. The electrodes are also monitored regularly and replaced when necessary.

Once the flakes are collected after electrolysis, they are subjected to post-production steps (in order to ensure uniformity, homogeneity and to increase storage life). The post-production processes are washing, passivation, annealing and coating. 5-6 days after deposition, the cathodes are removed from the deposition tank and transferred to a washing tank. Washing is a two step process -
• Initial cleaning with a jet of cold water,
• Subsequent cleaning with a jet of hot water.
This process removes all surface impurities. Simultaneous to washing, the flakes are cleaned subjected to passivation. During this process, the bath temperature is maintained at 150-160°F and the cathodes are submerged in cleaning chemicals (commercially obtained), followed by a wash with demineralized water. This process improves the shelf life of the flakes. Post washing and passivation, fan drying of the cathodes is performed. Once the cathodes are dry, the iron flakes are stripped from the cathode sheet. At this stage, the flakes are subjected to a preliminary quality check, then taken for annealing. Annealing is performed so as to remove any internal stresses in the flakes. The process of annealing is carried out in a mesh belt furnace maintained at a temperature of 600-700°F. The flakes are cooled and taken ahead for the final step - coating of the flakes. Coating is performed in order to increase the shelf life of the flakes. Prior to coating, the flakes are given another wash with cleaning chemicals to remove any surface impurities. Coating is done using commercially obtained coating materials. The flakes are now ready for packaging. Another quality check is done prior to packaging.

TECHNICAL ADVANCEMENTS
The technical advancements of the system and method envisaged by the present disclosure include the realization of:
1. A novel electrolytic method for the production of iron flakes of extremely high purity (99.999%).
The disclosure has been described with reference to the accompanying embodiments which do not limit the scope and ambit of the disclosure. The description provided is purely by way of example and illustration.
The embodiments herein above and the various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of the embodiments herein.
The foregoing description of the specific embodiments so fully revealed the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising”, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results.
Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the disclosure, unless there is a statement in the specification, specific to the contrary.
While considerable emphasis has been placed herein on the components and component parts of the preferred embodiments, it will be appreciated that many embodiments can be made and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. These and other changes in the preferred embodiment as well as other embodiments of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.

Documents

Application Documents

# Name Date
1 201721044767-STATEMENT OF UNDERTAKING (FORM 3) [13-12-2017(online)].pdf 2017-12-13
2 201721044767-POWER OF AUTHORITY [13-12-2017(online)].pdf 2017-12-13
3 201721044767-FORM 18 [13-12-2017(online)].pdf 2017-12-13
4 201721044767-FORM 1 [13-12-2017(online)].pdf 2017-12-13
5 201721044767-DECLARATION OF INVENTORSHIP (FORM 5) [13-12-2017(online)].pdf 2017-12-13
6 201721044767-COMPLETE SPECIFICATION [13-12-2017(online)].pdf 2017-12-13
7 201721044767-CLAIMS UNDER RULE 1 (PROVISIO) OF RULE 20 [13-12-2017(online)].pdf 2017-12-13
8 201721044767-FER.pdf 2019-07-05
9 201721044767-RELEVANT DOCUMENTS [27-12-2019(online)].pdf 2019-12-27
10 201721044767-MARKED COPIES OF AMENDEMENTS [27-12-2019(online)].pdf 2019-12-27
11 201721044767-FORM 13 [27-12-2019(online)].pdf 2019-12-27
12 201721044767-AMMENDED DOCUMENTS [27-12-2019(online)].pdf 2019-12-27
13 201721044767-RELEVANT DOCUMENTS [03-01-2020(online)].pdf 2020-01-03
14 201721044767-PETITION UNDER RULE 137 [03-01-2020(online)].pdf 2020-01-03
15 201721044767-OTHERS [03-01-2020(online)].pdf 2020-01-03
16 201721044767-FER_SER_REPLY [03-01-2020(online)].pdf 2020-01-03
17 201721044767-CORRESPONDENCE [03-01-2020(online)].pdf 2020-01-03
18 201721044767-COMPLETE SPECIFICATION [03-01-2020(online)].pdf 2020-01-03
19 201721044767-CLAIMS [03-01-2020(online)].pdf 2020-01-03
20 201721044767-ABSTRACT [03-01-2020(online)].pdf 2020-01-03
21 201721044767-Correspondence to notify the Controller [08-10-2020(online)].pdf 2020-10-08
22 201721044767-Written submissions and relevant documents [21-10-2020(online)].pdf 2020-10-21
23 201721044767-RELEVANT DOCUMENTS [21-10-2020(online)].pdf 2020-10-21
24 201721044767-MARKED COPIES OF AMENDEMENTS [21-10-2020(online)].pdf 2020-10-21
25 201721044767-FORM 13 [21-10-2020(online)].pdf 2020-10-21
26 201721044767-Annexure [21-10-2020(online)].pdf 2020-10-21
27 201721044767-AMMENDED DOCUMENTS [21-10-2020(online)].pdf 2020-10-21
28 201721044767-PatentCertificate12-11-2020.pdf 2020-11-12
29 201721044767-IntimationOfGrant12-11-2020.pdf 2020-11-12
30 201721044767-US(14)-HearingNotice-(HearingDate-12-10-2020).pdf 2021-10-18
31 201721044767-PROOF OF ALTERATION [20-10-2021(online)].pdf 2021-10-20
32 201721044767-RELEVANT DOCUMENTS [21-09-2022(online)].pdf 2022-09-21
33 201721044767-RELEVANT DOCUMENTS [25-09-2023(online)].pdf 2023-09-25
34 201721044767-FORM-27 [06-08-2024(online)].pdf 2024-08-06

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1 2019-07-0117-04-34_03-07-2019.pdf

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