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Nanostructured Cellulose Fibres And Method Of Producing The Same

Abstract: Title: NANOSTRUCTURED CELLULOSE FIBERS AND METHOD OF PRODUCING THE SAME  ABSTRACT The present invention relates to cellulose nanofiber yarns obtained from the processing of waste generated during agricultural & fiber manufacturing activities. The nanofiber yarn synthesis involves precleaning of cellulosic waste, preparation of cellulose solution, and extruding nanofibers from the prepared cellulose solution under the influence of a high-magnitude electric field, and subsequent collection and curing treatment to obtain nanofiber yarns. The invention provides a biodegradable, non-toxic, and environment friendly nano fiber yarn of cellulose with desirable textile properties of high tensile strength, dye fastness, moisture absorption, air permeability. 

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Patent Information

Application #
Filing Date
09 September 2022
Publication Number
44/2023
Publication Type
INA
Invention Field
TEXTILE
Status
Email
Parent Application
Patent Number
Legal Status
Grant Date
2025-05-21
Renewal Date

Applicants

Proto9 Materials Private Limited
101, B-Wing, Corporate Centre, Marol Pipeline, Andheri-Kurla Road, Andheri East, Mumbai- 400059, India.

Inventors

1. CHERIAN, Aleena
JN-4, Building No:10, Flat No:7&8, Blue Haven Society, Sector-10, Vashi, Navi Mumbai-400703, India
2. RAHEJA, Anant
B32, Flower Bloom C.H.S., Veera Desai Road, Andheri West, Mumbai- 400047, India.
3. ROHIT NAIK
CORPORATE CENTER, B101, MAROLPIPELINE ROAD, AJIT NAGAR, J BNAGAR, ANDHERI EAST, MUMBAI, MAHARASHTRA400059

Specification

DESC:FIELD OF INVENTION
The present invention relates to a regenerated nanofibers from process and agricultural waste cellulose. Most preferably, the present invention provides a nanofibers using electrospinning method by cellulose regeneration. The nano yarn of cellulose nanofibers produced are with high tensile strength, durability, sustainability, negligible chemical residue, non-toxic, biodegradable, environment friendly, better abrasion resistance, good washing fastness, good absorbency, desired breathability, desirable elasticity, and good dye-ability and colour fastness, easy to process, easy to maintain and engineer. The present invention also provides a process for preparation of a regenerated nanofibers from process waste and agriculture waste cellulose .
BACKGROUND AND PRIORART OF THE INVENTION
Fiber is a unit of matter, natural or manufactured, that forms the basic element of fabrics and other textile structures. Cellulose is a major source for fiber and is most abundant occurring in nature, like plants, bacteria, marine organisms. From plant source in the form of cotton fibers and dry wood. Annually about 180 million. tons of various cellulose pulps are consumed worldwide, most of it in paper and paperboard manufacture. Only about 8 million tons a year of the raw material are being consumed in miscellaneous cellulose manufacturing. Cellulose fibers made from cellulose derived from wood pulp have reduced variation in fiber length, structure, and biochemical makeup, these fibers are more appealing than any other natural fiber.
Variety of processes such as wet, dry and dry-jet-wet spinning, and electrospinning that have been utilized effectively to manufacture continuous cellulose fibers in micro and nano scale dimensions.  Viscose and Lyocell methods are now the only two industrially established technologies for the production of manmade cellulosic fibers. Nonetheless, they reveal difficulties relating to the solvents used during the cellulose dissolution stage. For example, the use of extremely toxic chemicals during the viscose method can be hazardous to human and environmental health. As a result, environmental pollution and safety concerns have become significant problems. The N-methyl morpholine-N-oxide (NMMO)-based Lyocell method, which is presently the sole marketed alternative to viscose spinning, is far more environmentally benign and is a closed loop process with the majority of solvent recovered.
Lyocell is obtained from bamboo and eucalyptus and is more expensive, bit delicate, require special care, and majority of its is mixed with cellulose or cotton to give strength. Because of the rising market demand for bio-based textiles and sustainable fashion products, it is critical to produce chemical-free, environmentally friendly, and long-lasting man-made cellulosic fibers employing green spinning methods.
US20190136415A1 -claims fabric using nano particles, nanoparticle modified cellulose fibers and not nanofibers.
US8962821B2 -Claims method of NaOH with urea for dissolving cellulose at cold temperature -8oC solution, time for dissolving cellulose is 30-40 hrs. H2SO4 and Na2So4 bath, coagulation bath, however does not disclose any method of nano fiber preparation.
CN111793898A-Claims a method of swelling cellulose in water, treating with ethanol and separating and dispersing in THF or NMMO for 16 to 20 hrs, and finally electrostatic spinning to get nanomembrane.
WO2016102782A1-Claims a Wet-Extrusion method of preparation of Cellulose 1 structure nanofibrillated cellulose from bleached birch pulp aligned into Nano fiber yarn, nano cellulose hydrogel obtained from wood pulp is wet extruded to aligned it together with simultaneous stretching.Particularly describes how nozzle and surface alignments are done,
US20060099419A1-Cellulose solution is made by swelling and dissolving cellulose powder in NMMO, Polyvinyl alcohol, Calcium chloride. Multifilament by spinning by nozzle, adding in coagulation bath through air layer. Then solidifying solution, winding multifilament after water washing and drying.
US4246221A-It includes extruding a solution containing a cellulose dissolved in a tertiary amine N-oxide solvent containing a solvent for cellulose to shape the solution as a film or filament, stretching the film or filament while still a solution to orient the molecules and develop film, and precipitating the cellulose from said solution to set the properties thereof without additional drawing. It produce films and gives general process for making film by simple stretching and drawing. Doesn’t include any procedure for nano products and also no electrostatic spinning.
WO2014162062A1- In this lignocellulosic material (lignin containing pulp), dissolved in a distillable DBN based ionic liquid, to a spinning method,wherein the ionic liquid is a diazabicyclononene (DBN)-based ionic liquid. Does not produce nano cellulose fibers.
WO2018104330A1- In this cellulose textile is mechanically disintegrated, treated with reducing agents for swelling at 50-100°C, bleaching using NaOH and Na2S2O4 with oxygen at pH 9-13.5, bleaching with Ozone below pH 6 at temperatures of 60oC to 120oC. After washing with water, recovered cellulose is mixed in the dissolving pulp and used for making a cellulose fiber. Cellulose dissolving pulp is obtained from mixture of wood pulp and solvent. Does not produce nano fibers and process is complex.
WO2017135816A1-Decreasing the degree of polymerization of cellulose from waste cotton to under 1500 by subjecting cotton-containing waste textile to an endocellulase C 3.2.1.4 and applying mechanical energy, adding a cellulose solvent comprising N-methyl morpholine N- oxide (NMMO) or an aqueous mixture of NMMO to obtain a cellulose containing liquid, subjecting the cellulose-containing liquid to a cellulose spinning process to produce cellulose fibers.
JP5676860B2- producing polysaccharide nanofibers from a chitin material, by swelling and partially dissolving chitin substance with mixed solvent of ionic liquid and an organic solvent, and esterification and etherification to the swollen or partially dissolved component and then washing and undergoing mechanical defibrillation to get chitin nanofibers.
Direct electrospinning of cellulose in the DBU-CO2 switchable solvent system-Cellulose; (2021), 28, 6869–6880-Mina Heidari etal- This is an article studying potential of the solvent system and various difficulty to keep the cellulose solution stable over electrospinning process and morphology of the fibers thus obtained.
Evaluation of Electrospinnability of Celluloses Derived from Different Biomass Resources. Fibers and Polymers; (2018), 19(5), 1128-1134-Chen, Y., Teng, N., Chen, H. et al.-systematically understand the dissolvability and Electrospinnability of celluloses derived from different biomass resources selection of cellulose to achieve high efficiency fabrication of ultrafine fiber in electrospinning.
Journal of Applied Polymer Sciences; (2005), 98, 1855–1859-Cellulose Nanofibers Prepared by the N-Methylmorpholine-N-oxide Method by Piotr Kulpinski. Raw spruce cellulose pulp and alpha Cellulose (1 to 4 %) mixed and dissolved in NMMO, water at continuous stirring and heating at 80 °C-100oC and is electrospun at 90°C-100°C.The film formation was caused due to surface tension of the coagulation bath was too high, the process of removing the solvent from the spinning jet was too slow, and the process of piling up the new layers of the non-jet-solidified spinning solution was too fast. All these factors resulted in the fibers sticking together and the creation of films, non woven material, created a net like structure, diameters of about 200 nm and 400 nm.
Polymer, (2006), 47, 5097–5107-Non-woven mats of submicron-sized cellulose fibers (250nm-750nm in diameter) by electrospinning of cellulose solutions. Cellulose dissolved in two solvent systems: (a) lithium chloride (LiCl)/N,N-dimethyl acetamide (DMAc) and (b) N-Methylmorpholine oxide (NMMO)/water, and the effects of (i) solvent system, (ii) the degree of polymerization of cellulose, (iii) spinning conditions, and (iv) post-spinning treatment such as coagulation with water on the miscrostructure of electrospun fibers are investigated. Cellulose fibers obtained from LiCl/DMAc are mostly amorphous. Electrospun cellulose fibers are oxidized by HNO3/H3PO4 and NaNO2.
Recycled cotton is difficult to process due to their shorter lengths which leads to produce product of sub-standard quality compared to their virgin fiber components. However the conversion of chemical cellulose to viscose is commercially known.
All the existing methods for preparing Fibers from natural sources use specifically “Raw wood pulp, or a Cellulose powders or Cellulose powders, or mixture of them.” The Solvents used specifically therein is a enzymes, NaOH, or mixture of LiCl, NMMO in water at high temperatures and continuous stirring and with ageing time of 10 to 20 hrs.
The above prior arts suggests cellulose nano films from agriculture wastes, which are technically difficult to be used for weaving fabrics, textiles or to be knitted or used for blending with another fibers. There is a long awaited need for making nano fiber yarns from agriculture wastes with high tensile strength for making, weaving and knitting into fabrics.
Moreover the nano fibers obtained from mentioned prior arts does lack required morphology. And most often the processes mentioned are just experiments and lab scale processes, and are not practically and industrially viable, suggesting more functional difficulties.
As discussed above, there is need exists in the art to have Nano fiber obtained by electrospinning method from wastes such as bagasse or cotton. Hence, the inventors of the present invention provides an electrospun Nano fiber obtained from bagasse and cotton waste by electrospinning method using minimum non reactive, reusable and regenerable solvent system.
The discussion of documents, acts, materials, devices, articles and the like is included in this specification solely for the purpose of providing a context for the present invention. It is not suggested or represented that any or all of these matters formed part of the prior art base or were common general knowledge in the field relevant to the present invention as it existed before the priority date of each claim of this application.
OBJECTIVES OF THE INVENTION
?A primary objective of the present invention is to develop nano fiber yarn by electrospinning of cellulose from Agriculture and process waste.
?An objective of the present invention is to develop a nano cellulose yarn with high tensile strength, durability and sustainability.
?Another objective of the present invention is to develop a nano cellulose yarn with better abrasion resistance, resilient to multiple washing cycles, good absorbancy, anti-stain, fire-resistance, desired breathability, desirable elasticity and anti-microbial properties.
?Another objective of the present invention is to develop a nano cellulose yarn with good dye-ability and colour fastness, light fastness, perspiration fastness, easy to process, easy to maintain, and engineer further into various formations.
?Another objective of the present invention is to develop a method to produce fibers with higher tensile strength and elongation at break.
?Another objective of the present invention is to develop a cellulose nano fibers amenable to blending with various natural and synthetic fibers.
SUMMARY OF THE INVENTION
Present invention relates to nano fiber obtained from agriculture and process waste with electro spinning method comprising dissolving the natural cellulose in at least a solvent, a co-solvent, with or without co-surfactant and water. Introducing the prepared cellulose solution through syringe needle by application of an electric field to obtain cellulose nano fibers, process parameter maintained throughout electrospinning process including maintenance of distance between needle tip and collector surface was 5-50 cm, Maintenance of Electric voltage between 0 to 30 kV for DC and flow rate between 0.5 to 10 ml/hr. Also it further relates to process for preparing yarn formed by collecting the extruded nano fibers over the rotating spool passing through two different needle angles at one end forming conical shape, imparting twist through rotation of spool and collection of formed yarn immersing into water bath for solidification along with drying and winding.
STATEMENT OF THE INVENTION
Present invention relates to nano fibers using agriculture and process waste cellulose with electro-spinning method comprising dissolving the natural cellulose and introducing the prepared cellulose solution through syringe needle by application of an electric field to obtain cellulose nano fibers. More specifically relates to a method for obtaining nano cellulose fibers from agriculture and process wastes, includes precleaning, preparing cellulose solution by dissolving with a recoverable solvent NMMO with successful electrospinning cellulose solution in syringe needle and application of an electric field to obtain cellulose nano fibers. Maintaining process parameter throughout electrospinning process involving distance between needle tip to collector surface, Electric voltage and flow rate, yarn is form by collecting the extruded cellulose fibers over the rotating spool passing through two different needle angles at one end forming conical shape, imparting twist through rotation of spool and collection of formed yarn immerse into water bath for solidification followed by drying and winding.
BRIEF DESCRIPTION OF DRAWINGS:
For a more complete understanding of the features and advantages of the present invention, reference is now made to the detailed description of the invention along with the accompanying figures and in which:
Figure 1: Assembly.
Figure 2: SEM image of nanoyarn (longitudinal view)
Figure 3: SEM image of nanoyarn (Crosssectional view).
Figure 4: FTIR Spectrum of Nano yarn obtained.
Figure 5 : DSC analysis of cellulose Nano yarn.
DETAILED DESCRIPTION OF THE INVENTION
The making and using of various embodiments of the present invention are discussed in detail below as; it should be appreciated that the present invention provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific embodiments discussed herein are merely illustrative of specific ways to make and use the invention and do not delimit the scope of the invention.
To facilitate the understanding of this invention, a number of terms are defined below. Terms defined herein have meanings as commonly understood by a person of ordinary skill in the areas relevant to the present invention. Terms such as "a", "an" and "the" are not intended to refer to only a singular entity, but include the general class of which a specific example may be used for illustration. The terminology herein is used to describe specific embodiments of the invention, but their usage does not delimit the invention, except as outlined in the claims.
The term “Nano fiber,” as used herein, refers to the cylindrical structures with an outer diameter below 1,000 nm and an aspect ratio the ratio between length and width greater than 50. Term “Electrospinning” is a voltage-driven, fabrication process governed by a specific electrohydrodynamic phenomenon where small fibers are yielded from a polymer solution.
The term “Cellulose,” as used herein, refers to an organic compound with the formula (C6H10O5)n, a polysaccharide consisting of a linear chain of several hundred to many thousands of ß linked D-glucose units. Cellulose is an important structural component of the primary cell wall of a plant, many forms of algae and oomycetes.
Cellulose is mainly used for textiles and paper production. The term “Bagasse,” as used herein, refers to is the dry pulpy fibrous material that remains after crushing sugarcane or sorghum stalks to extract their juice, meaning refuse or trash.
The term “Cotton waste,” as used herein, refers to cotton fibers which are extracted during spinning to clothing production includes blow room droppings, carding droppings, noil, fan waste and flat waste.
The term “NMMO” as used herein refers to N-Methylmorpholine N-oxide, a solvent. The term “DMSO” as used herein refers to Dimethyl sulfoxide an organosulfur compound, a solvent. The term “Yarn” as used herein refers to consolidation of nano fibers and are interchangeably used across the context.
In accordance of the present invention, the Nano fiber can be prepared from agriculture and process cellulose waste by methods selected from electrospinning, drawing, self-assembly, forced spinning and extrusion.
In accordance of the present invention, the Nano fiber is prepared from agriculture and process by an electrospinning method. The nano fiber tenacity is obtained is comparable to the other cellulose fibers.
The present invention relates to a system for manufacturing Nano fibers by electrospinning. As mentioned earlier, there remains a need for the nano cellulose yarns and a method to produce fibers that have high tensile strength, sustainable, negligible chemical residue, non-toxic, biodegradable, and environment friendly. The present disclosure provides a nano cellulose yarn with high tensile strength, durability, sustainability, better abrasion resistance, resilient to multiple washing cycles, good absorbance, desired breathability, desirable elasticity, and anti-microbial properties, good dye-ability and colour fastness, easy to process, and engineer further into various formations. The present disclosure also provides a method to produce nano fibers that may be continuous and aligned to form yarns. The present disclosure also provides the method of producing fibers that may have higher tensile strength ranging between 3 to 15 gm/denier and elongation at break range of 4 to 15 %.
The cellulose nano fiber from natural sources ensured enhanced physical properties and morphology. The formulation not only improved the tensile strength, durability, sustainable, negligible chemical residue, non-toxic, biodegradable but also showed increased sustainability, better abrasion resistance, resilient to multiple washing cycles, good absorbance, desired breathability, desirable elasticity, good dye-ability and colour fastness, easy to process and engineer further into various formations of yarns, fabrics, non-woven, film and felts.
The invention also relates to the process for manufacturing the said nano fibers composition wherein the agriculture and process wastes source may be selected from blow room droppings, carding waste, Neps, comber noil, linters. In one embodiment source contains different percentages of cellulose fiber or lesser fiber content with waste mixture proportion of 30:20:50 respectively to get cellulose content of 80 to 100 %.
In one embodiment the cellulose source have impurities or trash, may be subjected to precleaning processes such as mechanical or chemical, blowing and sorting. In one embodiment the cellulose with impurities are pass through precleaning machines.
In another embodiment the cotton fibers after collection are mix of short fibers, long fibers and Neps (entangled/bundles) which are not directly suitable to prepare yarn in their existing state.
In one embodiment solvents are selected from Non derivatizing solvents, Aqueous solvents, Sodium Hydroxide, Urea, Thiourea, PEG, Lithium Hydroxide, Mineral acids, Molten salt hydrates.
In another embodiment solvents are selected from Organic solvents, N-Methyl Morpholine Oxide/H2O, N-Methyl Morpholine Oxide/DMSO
N,N-dimethylacetamide / lithium chloride (DMA/LiCl).
In one more embodiment solvents are selected from Ionic Liquids, 1-Butyl-3-methylimidazolium chloride (BmimCl),1-Allyl-3-methylimidazolium chloride (AmimCl), 1-Ethyl-3-methylimidazolium acetate (EmimAc)
In one embodiment solvents are selected from Derivatizing solvents, Dinitrogen tetroxide/dimethylformamide (N2O4 /DMF), Carbondisulfide Sodium Hydroxide CS2/NaOH/H2O, Formic Acid, Sulphuric acid, Trifluoroacetic acid, HCOOH/H2SO4, CF3COOH, NMMO (N-Methylmorpholine N-oxide), ionic solvent such as 1-butyl-3-methylimidazolium chloride (BMIMCl), 1-allyl-3-methylimidazolium chloride (AMIMCl)) and the like. More preferably N-Methylmorpholine oxide (NMMO) or Dimethyl sulfoxide (DMSO) or combination of both for dissolution of Cellulose waste fibers. Aqueous NMMO helps in dissolution of cellulose, while DMSO helps in viscosity adjustments.
In other embodiment antioxidants are selected from Propyl Gallate or to prevent thickening of the cellulose solutions and effective flow from injection syringes.
In another embodiment the Flow rate ml/hr is selected from 0.5 to 10 ml/hr, more preferably from 2 to 5 ml/hr, collector assembly may be placed at the distance 5 to 50 cm. More preferably the distance between the syringe needle and the collector is selected from 5 to 25 cm.
In an embodiment the electrospinning is done by application of AC or DC electric field of 0 to 30 kV for DC and 20,000 to 50,000 V by 100 v ratio with spin rate electrode of 25 kV for AC temperature ranges from 20°C to 50°C. In another embodiment the Spinning angle of syringe needle is selected from 25o, 30o, 40o, 45o,50o, 55o, 60o and 65o, more preferably from 45o in horizontal settings.
In another embodiment the solution introduction through one or more nozzles of the spinneret assembly followed by applying an electric charges to obtain cellulose nano fibers.
In one more embodiment the cellulose nanofibers spun from one or more nozzles of the spinneret assembly may be collected by a collector assembly attached to one or more nozzles of the spinneret assembly and the collector assembly may a rotating funnel shaped collector or a stationary collector such as a plate collector, disc collector and the like. In another embodiment, the collector assembly may be placed in ambient atmosphere or immersed in a solvent bath or coagulation bath to obtain a consolidated matrix of fibers. In one embodiment, the coagulant bath of solvent may be hydrophobic, hydrophilic, polar, non-polar, ionic, or a combination in nature wherein the coagulation bath may be maintained at a temperature range from 5°C to 150°C may make the cellulose nanofibers to precipitate, forming a matrix of nanofibers.
As per one of the embodiment winding the cellulose nanofiber yarn obtained onto a spool assembly by means of a winding device/equipment, the winding device may include, but not limited to, drum winding device, precision winding device or the like. The winding device may wind the nanofibers in a form selected from various forms like cone form, cheese form, yarn ball, bobbin and foil. The nanofibers may wind as circumferential, hoop, helical, polar, or other ways suitable for packing and handling of the yarn. In another embodiment of the present disclosure, a dye/additive may be incorporated to endow colour or colour fastness to the obtained cellulose nano fiber yarn.
The present invention is further described with the help of the following examples, which are given by way of illustration all the parts, percent's and ratios are by weight unless otherwise indicated and therefore should not be construed to limit the scope of the invention in any manner.
EXAMPLES: Ingredients of composition in weight percentage range or in other unit in following conditions:
Examples 1: For preparation of the cellulose nanofibers from sugarcane bagasse
Sugarcane bagasse was collected, ground, and sugarcane bagasse powder was obtained. Cellulose was extracted from sugarcane bagasse powder by giving treatment such as dewaxing, alkaline treatment, dilute acid treatment and finally first step and second step of bleaching treatment. The treated samples were dissolved in 0.5 to 5 wt. % ratios of NMMO solvent. The obtained cellulose solution was introduced into the electrospinning machine. The syringe was filled with solution with various process parameters were set with a flow rate 1 to 5 ml/hr and an applied electric potential of 10 to 20 kV (kilo voltage) given to syringe needle. The cellulose nano fibers were electro spun, collected over drum collector and emerged in water bath followed by drying.
Example 2: Electrospun cellulose nano fibers by varying fiber collection assembly
The obtained cellulose solution was introduced to electrospun assembly by varying applied electric potential of 10 to 20 kV (kilo voltage). The electrospun cellulose nano fibers were spun into the coagulation bath. The coagulation bath was prepared by inserting copper sheet into water bath and applying negative voltage. The obtained electrospun cellulose fibers from the coagulation bath were collected followed by drying and samples were tested accordingly.
Example 3: Electro spun cellulose nano fibers from cotton waste
Blow-room cotton waste along with carding short fibers were collected and obtained in a merge form. Various synthesis solution with different ratios in the range of 0.5 to 5 % weight prepared. The trash contained various impurities that made it difficult to dissolve and synthesize solution, hence precleaning was done using machine.
Example 4: Electro spun cellulose nano fibers by using type of waste
The Blow-room cotton waste, draw frame waste along with carding short fibers and comber noil were collected and obtained in a blended form. Solution by varying the ratios of cotton waste were prepared 0.5 % to 5 % wt. Ratios, 2 % wt. was suitable solution to electrospun fibers with optimum fibers formation.
Example 5: Obtaining electro spun cellulose nano fibers by changing the process parameters
Parameters 1 2 3
Flow rate ml/hr. 0.5- 1 1.5-2 2-5
Distance (cm) 10-15 15-20 20-25
Voltage (kV) 10-20 20-30 30-35
Nano fibers obtained at flow rate-0.5-5 ml with distance of 15 to 25 cm at voltage of 10-30 kV
Example 6: Electro spun cellulose nano fibers by dissolution
NMMO (50% wt in water) is used in this invention. Maximum amount of cotton waste was dissolved in this experiment.
Example 7: Characterization of Nano yarn
1) General properties: The nano yarn formed exhibits the following general properties.
Sr.No. Properties Values
1 Fiber diameter (by SEM) 50-300 nm
2 Yarn diameter (by SEM) 80 to 4000 microns
3 Yarn Tenacity (gm/denier) (by Yarn Strength Tester) 3-15
4 Elongation at break (%) 4 to 15
5 Degree of crystallinity (%) (by XRD) 50-65
6 Flexural rigidity (dynes.cm) 3.0-5.0
7 Moisture regains (%) at 65 % R.H Around 12-15

2) SEM: Images shows the longitudinal and cross-sectional view of the nanoyarn composed of cellulose electro spun nanofibers. The fiber size may vary between 50nm to 300 nm while overall nanoyarn can be made with 80-4000 microns.
a) Longitudinal
b) Cross sectional
3) FTIR FTIR spectrum shows presence of cellulose absorption. The broad peak at 3391cm-1 is assigned to hydroxyl groups stretching. Bands at 2906 cm-1 and 1373 cm-1 are assigned to stretching and deformation vibrations of C-H bond in polysaccharide units. The peak at 1030 cm-1 is associated with the C-O-C ring vibration of cellulose molecules. The integrated association of all the peaks clearly confirms that, the nanoyarn made of electro spun nanofibers is purely cellulosic.
4) DSC: Differential scanning calorimetry analysis showing the changes that occur in the nanoyarn and detecting their phase transformation as it heats up. Figure shows that the DSC curve of nanoyarn presents different peaks. Fibre and yarn itself stable at Associated enthalpy peak shows at 243.36oC. which shows that the nanoyarn can stable at temperature equivalent to normal cotton yarn or cellulose.
5) TGA:
TGA analysis was carried out in order to evaluate the degradation behaviour of the nanoyarn. in the Figure illustrates through the TGA curves that there are two degradation stages. The initial one is occurring between 23.30°C to 150°C with a 10.91% weight loss, which indicates the elimination of the existing moisture caused by the hydrophilic character of cellulosic materials content and the removal of certain wax contents from the surface of the fibers. The second weight loss is higher for the raw fibre, it is estimated by 150–350°C with a weight loss of 48.94% respectively, until the temperature of 350°C. the residue at 350 degree is around 1.656 mg which is around 40.13%. This loss corresponds to the decomposition of non cellulose and small quantity of cellulose. Which depicts that, the thermal characteristics of nanoyarn form are slightly improved than that conventional cotton yarn.
All of the compositions and/or methods disclosed and claimed herein can be made and executed without undue experimentation in light of the present disclosure. While the compositions and methods of this invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations may be applied to the compositions and/or methods and in the steps or in the sequence of steps of the method described herein without departing from the concept, spirit and scope of the invention. All such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and concept of the invention as defined by the appended claims. ,CLAIMS:CLAIMS
I Claim, 
1.A nano yarn is made up of nano fibers derived from agricultural residues and process wastes having textile purpose wherein the nano yarn with nano fibers of diameter range 10 to 2000 nm and fiber length of 5 mm to 200 mm, having tensile strength of 3 to 15 gm/denier and elongation at break range of 4-15%, the method comprises of Precleaning, Spinning solution preparation, Nano fiber generation, Nano yarn formation and Winding.

2.The nano yarn from  electrospun cellulose nano fibers as claimed in claim 1, wherein  the nano fiber preparation includes electrospinning, drawing, self-assembly, forced spinning, extrusion by solubilization of cellulosic residues in solvent, Stabilizing the dope solution, Viscosity adjustment and Spinning.

3.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein  the agricultural wastes and process wastes with cellulosic content between 20 to 100 % of the dry weight.

4.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein residues include cellulosic wastes from crop wastes, grain crops, fruit crops, oil seed crops vegetables, flower crops and marine plants.
5.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein the process wastes obtained from industries of sugarcane, Sisal, cotton, jute, hemp, ramie, coir, isora, kapok, elephant grass, fruit pulp, and wood pulp.

6.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein  the said wastes is solubilized in Non derivatizing solvents, Aqueous solvents, Organic Solvents, Ionic Solvents, derivatising solvents selected from or combinations of Sodium Hydroxide, Urea, Thiourea, Lithium Hydroxide, Mineral acids, Molten salt hydrates, N-Methyl Morpholine Oxide, N,N-dimethylacetamide, 1-Butyl-3-methylimidazolium chloride (BmimCl),1-Allyl-3-methylimidazolium chloride (AmimCl), 1-Ethyl-3-methylimidazolium acetate (EmimAc), Dinitrogen, tetroxide, Carbon disulfide, Formic Acid, Sulphuric acid, Trifluoroacetic acid, diethyldibenzylammonium hydroxide, Anhydrous hydrazine, Methylamine, Amines, Sulphur dioxide, Ammonia, Formaldehyde, Thionyl chloride, Formamide.1-butyl-3-methylimidazolium chloride, 1-allyl-3-methylimidazolium chloride, Dimethyl sulfoxide.

7.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein the stabilization of solution is done by addition of antioxidant selected from water soluble or lipid soluble antioxidants, Propyl gallate, Alpha Tocopherol, Hydroxytyrosol.
8.The electrospun cellulose nano fiber yarn as claimed in claim 1, the electrospinning is done by application of AC or DC, wherein DC electric field of 0 to 20 kV/cm across the emitter and collector.

9.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein feed rate to the individual emitter between 0.01 to 10 gm/hr.

10.The electrospun cellulose nano fiber yarn as claimed in claim 1, wherein the nano fibers are collected on rotating collector, which is conical or semiconical, cylindrical, hemispherical in solid or grid form.

Documents

Application Documents

# Name Date
1 202221051680-STATEMENT OF UNDERTAKING (FORM 3) [09-09-2022(online)].pdf 2022-09-09
2 202221051680-PROVISIONAL SPECIFICATION [09-09-2022(online)].pdf 2022-09-09
3 202221051680-FORM FOR STARTUP [09-09-2022(online)].pdf 2022-09-09
4 202221051680-FORM FOR SMALL ENTITY(FORM-28) [09-09-2022(online)].pdf 2022-09-09
5 202221051680-FORM 1 [09-09-2022(online)].pdf 2022-09-09
6 202221051680-EVIDENCE FOR REGISTRATION UNDER SSI(FORM-28) [09-09-2022(online)].pdf 2022-09-09
7 202221051680-EVIDENCE FOR REGISTRATION UNDER SSI [09-09-2022(online)].pdf 2022-09-09
8 202221051680-DECLARATION OF INVENTORSHIP (FORM 5) [09-09-2022(online)].pdf 2022-09-09
9 202221051680-Proof of Right [14-09-2022(online)].pdf 2022-09-14
10 202221051680-FORM-26 [14-09-2022(online)].pdf 2022-09-14
11 202221051680-FORM-26 [07-07-2023(online)].pdf 2023-07-07
12 202221051680-FORM-26 [07-07-2023(online)]-1.pdf 2023-07-07
13 202221051680-Proof of Right [10-07-2023(online)].pdf 2023-07-10
14 202221051680-Proof of Right [10-07-2023(online)]-1.pdf 2023-07-10
15 202221051680-FORM-8 [10-07-2023(online)].pdf 2023-07-10
16 202221051680-FORM-26 [10-07-2023(online)].pdf 2023-07-10
17 202221051680-FORM-26 [10-07-2023(online)]-1.pdf 2023-07-10
18 202221051680-FORM 3 [10-07-2023(online)].pdf 2023-07-10
19 202221051680-FORM 13 [10-07-2023(online)].pdf 2023-07-10
20 202221051680-DRAWING [10-07-2023(online)].pdf 2023-07-10
21 202221051680-CORRESPONDENCE-OTHERS [10-07-2023(online)].pdf 2023-07-10
22 202221051680-COMPLETE SPECIFICATION [10-07-2023(online)].pdf 2023-07-10
23 202221051680-ORIGINAL U-R 6(1A) FORM 26-300623.pdf 2023-09-18
24 Abstract1.jpg 2023-09-20
25 202221051680-ORIGINAL UR 6 1A FORM 1, 3, 5, 8, COPY FORM 9, 13, 26, 30 & 28 COPY-110723.pdf 2023-09-27
26 202221051680-FORM-9 [30-10-2023(online)].pdf 2023-10-30
27 202221051680-STARTUP [06-11-2023(online)].pdf 2023-11-06
28 202221051680-FORM28 [06-11-2023(online)].pdf 2023-11-06
29 202221051680-FORM 18A [06-11-2023(online)].pdf 2023-11-06
30 202221051680-ORIGINAL UR 6(1A) FORM 26-300424.pdf 2024-05-03
32 202221051680-RELEVANT DOCUMENTS [07-05-2024(online)]-1.pdf 2024-05-07
33 202221051680-FORM 13 [07-05-2024(online)].pdf 2024-05-07
34 202221051680-FER.pdf 2024-09-27
35 202221051680-OTHERS [19-12-2024(online)].pdf 2024-12-19
36 202221051680-FORM-26 [19-12-2024(online)].pdf 2024-12-19
37 202221051680-FORM 3 [19-12-2024(online)].pdf 2024-12-19
38 202221051680-FER_SER_REPLY [19-12-2024(online)].pdf 2024-12-19
39 202221051680-COMPLETE SPECIFICATION [19-12-2024(online)].pdf 2024-12-19
40 202221051680-CLAIMS [19-12-2024(online)].pdf 2024-12-19
41 202221051680-Annexure [19-12-2024(online)].pdf 2024-12-19
42 202221051680-ABSTRACT [19-12-2024(online)].pdf 2024-12-19
43 202221051680-US(14)-HearingNotice-(HearingDate-08-04-2025).pdf 2025-03-19
44 202221051680-Written submissions and relevant documents [23-04-2025(online)].pdf 2025-04-23
45 202221051680-RELEVANT DOCUMENTS [05-05-2025(online)].pdf 2025-05-05
46 202221051680-POA [05-05-2025(online)].pdf 2025-05-05
47 202221051680-POA [05-05-2025(online)]-1.pdf 2025-05-05
48 202221051680-MARKED COPIES OF AMENDEMENTS [05-05-2025(online)].pdf 2025-05-05
49 202221051680-MARKED COPIES OF AMENDEMENTS [05-05-2025(online)]-1.pdf 2025-05-05
50 202221051680-FORM 13 [05-05-2025(online)].pdf 2025-05-05
51 202221051680-FORM 13 [05-05-2025(online)]-1.pdf 2025-05-05
52 202221051680-AMENDED DOCUMENTS [05-05-2025(online)].pdf 2025-05-05
53 202221051680-AMENDED DOCUMENTS [05-05-2025(online)]-1.pdf 2025-05-05
54 202221051680-PatentCertificate21-05-2025.pdf 2025-05-21
55 202221051680-IntimationOfGrant21-05-2025.pdf 2025-05-21

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