Abstract: CHROMIUM OXIDE /NICKEL OXIDE EMBEDDED CHITOSAN-GRAPHITE COMPOSITE RESIN FOR REMOVAL OF COLOR FROM WASTE WATER This research explores the utilization of biomass waste, particularly agricultural residues rich in silica content, for the extraction of silica nanoparticles and their potential combination with zirconium to create a composite material. The resulting composite demonstrates significant adsorption capacity and catalytic activity, facilitating the efficient conversion of biomass into bio-oil. The process involves flash pyrolysis, enabled by high heating rates and short residence durations, which minimizes vapour cracking and maximizes liquid product yields, achieving approximately 70 percent efficiency by weight. Employing silica or hydro silicate with zirconium as a catalyst in bio-oil cracking processes at atmospheric pressure enhances the overall efficiency. Zirconium oxide nanoparticles, obtained via eco-friendly synthesis from plant leaf extracts such as Sambucus canadensis, contribute to the catalytic activity. Furthermore, this research develops into the catalytic upgrading of bio-oil, derived from non-catalytic biomass pyrolysis, to produce biofuels and fuel additives. The upgrading process encompasses low-temperature esterification with alcohols (followed by water separation) or high-temperature gasification, cracking, or hydrotreating processes. Chitosan, a biopolymer derived from chitin, exhibits potential as an effective adsorbent for pollutant removal from wastewater. However, its limited mechanical strength and stability hinder its application in wastewater treatment. The study explores the development of chitosan-based nanocomposites, particularly when combined with graphene oxide, chromium oxide, and nickel oxide, to enhance mechanical strength and stability, consequently improving adsorption efficiency. The synthesis, characterization, adsorption mechanisms, and regeneration potential of these chitosan-based nanocomposites are the focal points of this research.
Description:Field of the invention
The invention leads to chromium oxide /Nickel oxide embedded Chitosan-graphite Composite resin for removal of color from waste water.
Background of the Invention
References which are cited in the present disclosure are not necessarily prior art and therefore their citation does not constitute an admission that such references are prior art in any jurisdiction. All publications, patents and patent applications herein are incorporated by reference to the same extent as if each individual or patent application was specifically and individually indicated to be incorporated by reference.
Several patents have been issued for composite resin but none of these are related to the present invention. For example, TW201819901A relates to a sensor of hydrogen peroxide (H2O2) using the nanocomposite consisting of platinum nanoparticles (PtNPs) with chitosan encapsulated graphite (graphite-CS) composite. The graphite-CS composite was prepared by sonication of pristine graphite in CS in 5% acetic acid. The PtNPs decorated graphite-CS (graphite-CS/PtNPs) composite was prepared by electrodeposition of PtNPs on graphite-CS modified glassy carbon electrode. The modified electrode displays an enhanced reduction peak current for H2O2 when compared with electrodes modified with graphite/PtNPs and PtNPs. The modified electrode exhibits excellent electrocatalytic activity towards the reduction of H2O2, and the amperometric response is linear over the concentration range from 0.25 to 2890 [mu]M.
Another patent, US6989344B2 is directed to the use of aluminum alkyl activators and co-catalysts to improve the performance of chromium-based catalysts. The aluminum alkyls allow for the variable control of polymer molecular weight, control of side branching while possessing desirable productivities, and may be applied to the catalyst directly or separately to the reactor. Adding the alkyl aluminum compound directly to the reactor (in-situ) eliminates induction times.
Another patent, US9819012B2 relates to methods of making high-energy cathode active materials for primary alkaline batteries are described. The primary batteries include a cathode having an alkali-deficient nickel(IV)-containing oxide including one or more metals such as Co, Mg, Al, Ca, Y, Mn, and/or non-metals such as B, Si, Ge or a combination of metal and/or non-metal atoms as dopants partially substituted for Ni and/or Li in the crystal lattice; an anode; a separator between the cathode and the anode; and an alkaline electrolyte solution.
Another patent, US10770609B2 disclosed are multilayer film structures including a layer (B) that includes a crystalline block copolymer composite (CBC) or a specified block copolymer composite (BC), including i) an ethylene polymer (EP) including at least 80 mol % polymerized ethylene; ii) an alpha-olefin-based crystalline polymer (CAOP) and iii) a block copolymer including (a) an ethylene polymer block including at least 80 mol % polymerized ethylene and (b) a crystalline alpha-olefin block (CAOB); and a layer C that includes a polyolefin having at least one melting peak greater than 125 C, the top facial surface of layer C in adhering contact with the bottom facial surface of layer B. Such multilayer film structure preferably includes (A) a seal layer A having a bottom facial surface in adhering contact with the top facial surface of layer B. Such films are suited for use in electronic device (ED) modules including an electronic device such as a PV cell.
Another patent, US7122250B2 relates to a composite resin particle useful as an additive for paints or coatings, powder coatings, cosmetic additives, slush molding resins, spacer for electronic part assembly, standard particles for electric measurement devices, toner, hot melt adhesive as well as other molding materials. Said composite resin particle comprises a resin microparticle (A) depositing on the surface of a resin particle (B) wherein the shape factor (SF-1) of said composite resin particle is 115 to 800. It is also a composite resin particle comprising a resin microparticle (A) depositing on the surface of a resin particle (B) wherein the acid vale of a resin (b) constituting the resin particle (B) is 5 to 100.
Another patent, US10266688B2 relates to surface-modified cellulose nanofibers, which are used to improve fiber-matrix adhesion, resulting in biodegradable nano fibrillated cellulose (NFC)-polyvinyl alcohol (PVOH) composites, which can be used to form structures such as films, with excellent mechanical performance. Particularly, the present invention relates to a bio composite resin composition wherein the surface of cellulose nanofibers has been chemically modified, a method for producing such composite resin composition and a casting-sheet composite body.
Biomass is obtained from waste of biological materials. Biological materials may be dealing plant parts or dead animal or any algae etc. Agricultural waste, especially rice husk or wste left after removing rice from its plant contains higher percentage of silica due to which cattles do not like to eat it. Silica may vary from 15 to 30% in various agri residues. Such biomass is dried and crushed and then silica can be extracted from it. This silica when converted into nano particles along with zirconium then it can give useful composite which has good adsorption capacity and catalytic activity to convert bio mass into bio-oil. The optimisation of the liquid products as an oil known as bio-crude or bio-oil is accomplished with the application of flash pyrolysis. The fast pyrolysis of biomass is made possible by high heating rates and short residence durations. This helps to reduce the amount of vapour cracking that occurs, which in turn maximises the yields of liquid products and achieves efficiencies of up to roughly 70 percent on a weight basis. Using an acid as a catalyst, cracking processes in bio-oils are able to take place even at atmospheric pressure. Silica or hyrdosilicate with Zirconium may play good role of catalyst for same purpose. Zirconium is obtained as oxide nanoparticles by green synthesis of leaf extract of plants like Leaf extract of Sambucus canadensis.
Catalytic upgrading of bio-oil derived from the non-catalytic pyrolysis of biomass can also yield biofuels and fuel additives. This upgrading can be performed by low temperature esterification with alcohols (followed by water separation) or by high temperature gasification, cracking or hydrotreating processes.
Chitosan, a biopolymer derived from chitin, has shown promise as an effective adsorbent for the removal of various pollutants from wastewater. When it is combined with grapheme oxide to form composite with chromium oxide and nickel oxide. However, the low mechanical strength and stability of chitosan restrict its application in wastewater treatment. The development of chitosan-based nanocomposites can overcome these limitations and improve the adsorption efficiency. The research paper focuses on the synthesis and characterization of chitosan-based nanocomposites, along with their adsorption mechanisms and regeneration potential.
The primary object of the present invention is chromium oxide /Nickel oxide embedded Chitosan-graphite Composite resin for removal of color from waste water.
Another object of the present invention is to study chromium oxide /Nickel oxide embedded Chitosan-graphite Composite resin.
Another object of the present invention is to prepare chitosan-graphite Composite resin.
These and other objects and advantages of the present invention will become readily apparent from the following detailed description.
Summary of Invention
This summary is not a comprehensive overview of the disclosure and does not reflect the main/essential features of the establishment or specify the scope of the establishment. Its sole purpose is to present some of the concepts presented here in a simpler way as a precursor to more detailed.
The primary object of the present invention is chromium oxide /Nickel oxide embedded Chitosan-graphite Composite resin for removal of color from waste water.
In some embodiments of the present invention, Soxhlet extraction was employed to prepare the leaf extract. The thimble was filled with the leaf material. The soxhlet's primary chamber received this thimble. On a heating mantle, water was poured into a flask with a round bottom. Following the attachment of the condenser, the soxhlet extractor was fixed to the RB.
In some embodiments of the present invention, water was boiled for two hours after the device was set up in order to obtain the leaf extract. Whatman filter paper was used to filter the resultant extract, which was then placed in a beaker for later use.
In some embodiments of the present invention, to 10 ml of leaf extract, we added 30 ml of 0.01M solution of zirconium oxychloride, then it was stirred for 10 hr until the color change was observed. Color change confirms the formation of nanoparticle. The remaining liquid was dried after which it was calcinated in muffle furnace at 300 c for about 30 minutes. As a result, the brown-colored nanoparticles were obtained.
These and other aspects of the embodiments herein will be better appreciated and understood when considered in concurrence with the following explanation and the accompanying drawings. It should be understood, however, that the following descriptions, while indicating preferred embodiments and numerous specific details thereof, are given by way of illustration and not of limitation. Many changes and modifications may be made within the scope of the embodiments herein without departing from the spirit thereof, and the embodiments herein include all such modifications.
Brief summary of the figures
Figure-1: Sambucus canadensis plant
Figure-2: XRD image
Figure-3: FTIR image
Figure-4: SEM images
Detailed Description
These embodiments are described in sufficient detail to enable those skilled in the art to practice the embodiments and all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In some embodiments of the present invention, chitosan, a biopolymer derived from chitin, has shown promise as an effective adsorbent for the removal of various pollutants from wastewater. When it is combined with grapheme oxide to form composite with chromium oxide and nickel oxide. However, the low mechanical strength and stability of chitosan restrict its application in wastewater treatment.
In some embodiments of the present invention, the development of chitosan-based nanocomposites can overcome these limitations and improve the adsorption efficiency. The research paper focuses on the synthesis and characterization of chitosan-based nanocomposites, along with their adsorption mechanisms and regeneration potential
In some embodiments of the present invention, Soxhlet extraction was employed to prepare the leaf extract. The thimble was filled with the leaf material. The soxhlet's primary chamber received this thimble. On a heating mantle, water was poured into a flask with a round bottom. Following the attachment of the condenser, the soxhlet extractor was fixed to the RB.
In some embodiments of the present invention, water was boiled for two hours after the device was set up in order to obtain the leaf extract. Whatman filter paper was used to filter the resultant extract, which was then placed in a beaker for later use.
In some embodiments of the present invention, to 10 ml of leaf extract, we added 30 ml of 0.01M solution of zirconium oxychloride, then it was stirred for 10 hr until the color change was observed. Color change confirms the formation of nanoparticle. The remaining liquid was dried after which it was calcinated in muffle furnace at 300 c for about 30 minutes. As a result, the brown colored nanoparticles were obtained.
A chromium oxide /nickel oxide embedded chitosan-graphite composite resin for removal of color from waste water comprising the steps of:
using Soxhlet extraction to prepare the leaf extract;
filling the thimble with the leaf material;
receiving the Soxhlet’s primary chamber this thimble;
pouring water into a flask with a round bottom on a heating mantle;
following the attachment of the condenser, the Soxhlet extractor was fixed to the RB;
boiling water for two hours after the device was set up in order to obtain the leaf extract;
using Whatman filter paper to filter the resultant extract, which was then placed in a beaker for later use;
adding to 30 ml of 0.01M solution of zirconium oxychloride to 10 ml of leaf extract;
stirring it for 10 hr until the color change was observed;
color change confirms the formation of nanoparticle;
drying the remaining liquid after which it was calcinated in muffle furnace at 300 c for about 30 minutes; and
obtaining the brown colored nanoparticles.
EXAMPLE 1
Material and Methods
Soxhlet extraction was employed to prepare the leaf extract. The thimble was filled with the leaf material. The Soxhlet’s primary chamber received this thimble. On a heating mantle, water was poured into a flask with a round bottom. Following the attachment of the condenser, the Soxhlet extractor was fixed to the RB. Water was boiled for two hours after the device was set up in order to obtain the leaf extract. Whatman filter paper was used to filter the resultant extract, which was then placed in a beaker for later use.
Preparation of Nanoparticles:
To 10 ml of leaf extract, we added 30 ml of 0.01M solution of zirconium oxychloride, then it was stirred for 10 hr until the colour change was observed. Colour change confirms the formation of nanoparticle. The remaining liquid was dried after which it was calcinated in muffle furnace at 300 c for about 30 minutes. As a result, the brown coloured nanoparticles were obtained.
Characterisation of synthesised nanoparticles:
Several analytical methods were used to characterise the Green Synthesized zirconium oxide Nanoparticles. UV-Vis spectroscopy was utilised to identify ZrO nanoparticles based on their optical characteristics. Powdered XRD investigations were utilised to determine the crystal system and crystalline size of the nanoparticles. The fabrication of nanoparticles' shape and particle size were examined using a scanning electron microscope (Zeiss-evo 18). FTIR was used to examine the surface of ZrO/Sio2 nanoparticles for the presence of various functional groups (Thermo Scientific).
Agri waste i.e. Rice husk which is waste left after removing rice from its plant contains higher percentage of silica due to which cattles do not like to eat it. Silica may vary from 15 to 30% in various agri residues. Such biomass is dried and crushed and then silica can be extracted from it. This silica when converted into nano particles along with zirconium then we get useful composite which has good adsorption capacity and catalytic activity to convert bio mass into bio-oil. It has shown 25 to 35% higher yield.
Development of composite to work as catalyst-
Leaves were collected, crushed and dipped in water and then extract was heated and treated with zirconium nitrate or zirconium chloride or zirconium sulphate solution till color of salt solution is changed, change in colour shows recutiomn of salt into zirconium oxide nano particles. So obtained Silica and zirconium oxide nano particles are mixed in different ratio. Zirconium oxide is taken about 20 to 50% of the Silica and then mixed in a closed vessel or crucible and then heated for 1-3 hrs at 600°C or above to get finely divided nano particles of composite in the range of 10-15 nm. Such prepares composite is used for conversion of biomass into bio -oil then it is observed that conversion efficiency of biomass into bio-oil is increased by 20 -35% as compared to with and without catalyst. And varying the concentration and size of catalyst used.
Result and discussion:
Characterisation of synthesised nanoparticles:
UV-Visible spectroscopy:
The graph below depicts the uv-visible spectrum for zirconium oxide nanoparticles, synthesised from the Sambucus canadensis leaves, where absorption maxima is observed at 370nm, therefore confirming the presence of zirconium oxide nanoparticles.
Crystallographic Analysis:
To study crystalline structure of zirconium oxide/Sio2 nanoparticles, XRD was used. The various bragg peaks were seen at: 28.38°,40.55° 50.51° and 66.37°. Which confirm the formation of crsytalline nanoparticles (Fig 2).
FTIR Spectroscopy and SEM analysis: As can be seen in the image below, SEM was employed to examine the surface morphology, crystallinity, shape, and size of synthesised zirconium oxide nanoparticles. The image makes it evident that nanoparticles are heavily aggregated and nearly irregular in shape.
SEM images (Fig 3-4) of nanoparticles are as shown in the images above, as it can be observed Nps are irregular in shape and slightly agglomerated
ADVANTAGES OF THE INVENTION: By this invention, and by using these prepared catalysts the efficiency of biomass to get converted into bio–oil can be increased to a greater extent by 20 to 35% or more. Cost of process becomes lower. Efficiency increases. This will not only bring the cost but will also give a better yield.
, Claims:
1. A chromium oxide /nickel oxide embedded chitosan-graphite composite resin for removal of color from waste water comprising the steps of:
i. using Soxhlet extraction to prepare the leaf extract;
ii. filling the thimble with the leaf material;
iii. receiving the Soxhlet’s primary chamber this thimble;
iv. pouring water into a flask with a round bottom on a heating mantle;
v. following the attachment of the condenser, the Soxhlet extractor was fixed to the RB;
vi. boiling water for two hours after the device was set up in order to obtain the leaf extract;
vii. using Whatman filter paper to filter the resultant extract, which was then placed in a beaker for later use;
viii. adding to 30 ml of 0.01M solution of zirconium oxychloride to 10 ml of leaf extract;
ix. stirring it for 10 hr until the color change was observed;
x. color change confirms the formation of nanoparticle;
xi. drying the remaining liquid after which it was calcinated in muffle furnace at 300 c for about 30 minutes; and
xii. obtaining the brown colored nanoparticles.
| # | Name | Date |
|---|---|---|
| 1 | 202311062680-STATEMENT OF UNDERTAKING (FORM 3) [18-09-2023(online)].pdf | 2023-09-18 |
| 2 | 202311062680-REQUEST FOR EARLY PUBLICATION(FORM-9) [18-09-2023(online)].pdf | 2023-09-18 |
| 3 | 202311062680-POWER OF AUTHORITY [18-09-2023(online)].pdf | 2023-09-18 |
| 4 | 202311062680-FORM-9 [18-09-2023(online)].pdf | 2023-09-18 |
| 5 | 202311062680-FORM FOR SMALL ENTITY(FORM-28) [18-09-2023(online)].pdf | 2023-09-18 |
| 6 | 202311062680-FORM 1 [18-09-2023(online)].pdf | 2023-09-18 |
| 7 | 202311062680-EVIDENCE FOR REGISTRATION UNDER SSI(FORM-28) [18-09-2023(online)].pdf | 2023-09-18 |
| 8 | 202311062680-EDUCATIONAL INSTITUTION(S) [18-09-2023(online)].pdf | 2023-09-18 |
| 9 | 202311062680-DECLARATION OF INVENTORSHIP (FORM 5) [18-09-2023(online)].pdf | 2023-09-18 |
| 10 | 202311062680-COMPLETE SPECIFICATION [18-09-2023(online)].pdf | 2023-09-18 |
| 11 | 202311062680-FORM 18 [17-06-2025(online)].pdf | 2025-06-17 |