Form2
The Patents Act, 1970
&
The Patents rule, 2003
The complete Specification
(See Section 10 rule 13)
Synthesis of aluminium nanoparticles from waste packaging aluminium foil by Ceriops tagal stem
extract

The field of invention;
The field of invention relates to a method for preparation of Aluminium nanoparticles, more particularly the method of preparation relates to waste aluminium foil by employing aqueous plant extract;
Background of invention and prior art;
Aluminum foil is made by rolling pure aluminum metal into very thin sheets, followed by annealing to achieve dead-folding properties (a crease or fold made in the film will stay in place), which allows it to be folded tightly. Moreover, aluminum foil is available in a wide range of thicknesses, with thinner foils used to wrap food and thicker foils used for trays. Like ail aluminum packaging, foil provides an excellent barrier to moisture, air, odours, light, and microorganisms.
Lamination of packaging involves the binding of aluminum foil to paper or plastic film to improve barrier properties. Thin gauges facilitate application. Although lamination to plastic enables heat sealability, the seal does not completely bar moisture and air. Because laminated aluminum is relatively expensive, it is typically used to package high value foods such as dried soups, herbs, and spices. A less expensive alternative to laminated packaging is metallized film. Metallized films are plastics containing a thin layer of aluminum metal (Fellows and Axtell 2002). These films have improved barrier properties to moisture, oils, air, and odors, and the highly reflective surface of the aluminum is attractive to consumers. More flexible than laminated films, metallized films are mainly used to package snacks. Although the individual components of laminates and metalized films are technically recyclable, the difficulty in sorting and separating the material precludes economically feasible recycling.
Multilayer packaging is very difficult to recycle because it contains many different polymers. It has become an 'unmanageable' quotient in municipal solid waste management. Complex packaging materials or plastic lined with foils or laminated plastics are product and consumer friendly but at the same time they are proving a major threat to environment as they pose a huge problem in recycling. Co-mingled aluminum and plastic are used on large scale in packaging food materials (Kennethmarsh, And Betty Bugusu, 2007),
PolyAI is completely non-degradable. It emits toxic fumes on burning and causes infertility of soil, if it gets imbedded in it, reducing permeability, porosity and fertility of the soil. Packaging materials degradation also leads in formation of greenhouse gasses C02, and release of toxin (e.g. vinyl chloride monomer) and the scarring of landscape (e.g. mining pits) (Road Map on Management of Wastes in India 2010).

U.S. Patent No. 6,872,459 teaches that aluminium foil is effective as a barrier material. Since use of an aluminium foil will seemingly bring the concern on the environment, the various attempts in which the practical alternative to an aluminium foil is developed have been made. The alternative has the barrier which was excellent in oxygen gas and aroma, and is easily scrapped after use. Therefore, it is an object of the present invention to use waste aluminium foils to prepare aluminium nanoparticles by using an aqueous aluminium extract;
Object of the present invention;
It is an object of the present invention to provide a method for preparation of aluminium
nanoparticles form waste aluminium foils,
It is also an object of the present invention to provide a method for preparation of aluminium
nanoparticles form waste aluminium foils by using aqueous plant extract,
It is also an object of the present invention to provide a method for preparation of aluminium
nanoparticles form waste aluminium foils by using aqueous stem extract of Ceriops tagal,
It is also an object of the invention to provide rapid eco-friendly method for preparation of
nanoparticles from waste aluminium foil.
Description of drawings and figures,
Fig. 1. Fig 1: UV-Visible spectrum of standard solutions
Fig 2: UV-Visible spectra of 15% autoclaved Aluminium foil solution at 60°C.
Fig 3: UV-Visible spectra of 10% Unautoclaved Aluminium foil solution at 50°C.
Fig 4. SEM (A) and EDAX (B) micrograph (15% autoclaved Aluminium foil at 60°C.)
Fig 5. SEM (A) and EDAX (B) micrograph (10% Unautoclaved Aluminium foil solution at 50°C)
Fig 6: FTIR spectra of 10% aqueous Ceriops tagal stem extract (CTSE)
Fig 7: FTIR spectra of 15% autoclaved Aluminium foil after challenging with 10% CTSE
Fig 8: FTIR spectra of 10% Unautoclaved Aluminium foil solution after challenging with 10% CTSE
Summary of the invention;
In one of the aspects of the invention it is provided that stable aluminium nanoparticles are synthesized from waste aluminium foil (used in packaging industry) using aqueous stem extract of Ceriops tagal. Optimisation and characterisation studies indicate that maximum rate of synthesis was obtained by challenging 10% aqueous stem extract of Ceriops tagal with 15% autoclaved and 10% unautoclaved waste aluminium foil solution respectively. Scanning electron microscopy (SEM),

energy-dispersive spectroscopy (EDX), ATR-FTIR and UV-visible absorption spectroscopy confirmed the formation of aluminium nanoparticles. Concentration of waste aluminium foil solution, time course and temperature played a major role in synthesis process.
Detailed description of the invention;
In one of the aspects of the invention it is provided that preparation of extract is done using C. tagal stem, C. tagal stem was collected from the Gorai creek, Mumbai, chopped, dried at 40° C and pulverized. Ultra-pure water produced by Milli Q system was used throughout the experiment.
Aqueous C tagal stem extract (CTSE) was prepared by soaking 10 gm of stem powder in 100ml MilliQ water for 10 mins and then the mixture was boiled at 100° C for 10 mins. The freshly prepared extract was filtered through Whatman filter paper No.l.
In the other aspect of the invention it is provided that preparations of solutions from waste aluminium foil which is collected from municipal waste,
Waste aluminium foil was washed thoroughly and shredded into small pieces. Aqueous autoclaved and un-autoclaved solutions of 5 %, 10% and 15% were prepared as follows - 5,10 and 15 gm of shredded waste aluminium foil was mixed with 100 ml MilliQ water respectively and autoclaved; while un-autoclaved solutions with same concentrations were prepared by boiling them at 100°C for 10 mins. These autoclaved and unautoclaved solutions were filtered and reacted with 10% C. tagal stem extract.
In another aspect of the invention synthesis of nanoparticles was initiated by adding 5ml of 10% CTSE in 95 ml aqueous autoclaved and un-autoclaved solutions respectively. Ail the reactions were carried out at static condition. Formation of aluminium nanoparticles was monitored as a function of time by measuring UV-Vis spectra using UV-1650CP Schimadzu spectrophotometer operated at lnm resolution. Effect of temperature on rate of synthesis was studied by carrying out the reactions at Room temperature (R.T.), 50°C and 60°C in water bath.
In one of the important aspects of the invention solvent selected is water or optionally lower alcohols C1-C2;
In the one of the aspect of the invention municipal waste aluminium laminated includes, coated polymers films used for packaging the of the dry, liquid, semisolid food materials; In an another aspect of the invention confirmation of the formation of aluminium nanoparticles is carried out by following analytical techniques;

SEM and energy dispersive spectroscopy measurements:
Size and surface morphology of bio-reduced nanoparticles was determined by scanning electron microscope. Individual nanoparticles solutions were mounted rigidly on specimen stub, after which films were allowed to stand for 2 mins and excess solution was blotted. An energy dispersive spectrum was recorded with SEM.
Attenuated total reflections Fourier transform infrared (ATR-FTIR) Spectroscopy:
ATR-FTIR spectrum of CTSE before and after reduction of metal ions was obtained using FTIR (Perkin Elmer) Frontier spectrophotometer. 10% plant extract and supernatant of bio-reduced samples was subjected to IR source 400 cm-1- 4000 cm-1.
Visual observations and UV-Visible spectroscopy
Bio-reduction to aluminium nanoparticles in presence of CTSE was monitored as a function of time using UV-Visible spectroscopy with various concentrations and temperature. Mere autoclaving and boiling of solutions did not lead to synthesis of aluminium nanoparticles (Fig 1). Table 1 gives information about the fastest synthesis of nanoparticles at optimum concentration, temperature and time. Depending on the concentrations, temperature and time the best synthesis of aluminium nanoparticles was with 15% autoclaved solution at 4hrs with surface plasmon resonance (SPR) peak of absorption spectra at 505nm (Fig.2). While for unautoclaved solution best synthesis was achieved with 10% solution at 24 hr with absorption peak at 503 (Fig.3). Maximum bio-reduction of autoclaved and unautoclaved solutions was achieved at 60°C and 50°C respectively.
Intense brown colour was observed after aluminum nanoparticles formation. Bio-reduction to nanoparticles was very rapid; onset of colour change was seen within 5-10 minutes and more than 90% of reduction was achieved within lhr for both solutions. The differences in the redox potential and solubility of metal ions are most likely to be considered for rate of synthesis of nanoparticles formation. The pH of plant extract affects the binding trend of ions to functional groups of biomass and subsequently the shape and size of nanoparticles during synthesis. The pH of CTSE extract was 7. Although the reaction was fast at higher temperature and low at lower temperature with slight colour variation, indicating the dependence of temperature on bio-reduction process, no significant difference was observed in peaks.
SEM and energy dispersive spectroscopy measurements
SEM micrograph confirmed the synthesis of nanoparticles. For elemental analysis of nanoparticles, a signature spectrum from the atoms in the nanoparticles was obtained by EDS. Nanoparticles

synthesized were almost spherical with a small percentage being ellipsoidal. From the few particle images we found that the size (diameter) varied from 87 nm to 115 nm and 125 nm to 226 nm for nanoparticles synthesized employing autoclaved (Fig 4) and un-autoclaved solutions (Fig 5) respectively. It was clear from the measurements that the biosynthesized nanoparticles were poly-dispersed. A signature spectrum corresponding to aluminium atom in the nanoparticles was obtained by EDS. Weak signals from oxygen, were also seen which may have originated from the bio-molecules bound to the surface of the nanoparticles.
ATR-FTIR-. ATR-FT1R spectroscopic studies were carried out to identify the functional group involved in capping and efficient stabilization of the metal nanoparticles. FTIR absorption spectra of CTSE showed prominent bands at 3306.92 cm-1, 2130.79 cm"1 1634.84 cm-1 and 403.38 cm-1 (Fig.6). The intense broad stretching at 3306.02 cm-1 arises due to the free O-H groups present in alcohols and phenols, weak stretch at 2130.79 cm"1 is due to C= C from alkynes while IR peak at 1634.85 cm-1 could be assigned to characteristic asymmetrical stretch of carboxylate group and the characteristic peak at 403.38 cm"1 can be attributed to C-N-C in amines. The shifting of peaks occurred after synthesis of nanoparticles (Fig.7 and Fig. 8). Based on the band shift it can be seen that alkynes and amines are involved in the synthesis of above nanoparticles. Therefore, the synthesized nanoparticles were surrounded by proteins and metabolites such as terpenoids having functional groups of alcohols, phenols etc. CTSE is mainly composed of terpenoids, flavonoids, alkaloids and ployphenols which may play an important role in reduction, stabilization and assembly of synthesized nanoparticles.
Examples;
1.0 Isolation of bioactive components from Ceriops tagal;
An aqueous stem extract was prepared by soaking 10.0 gm of stem powder in 100ml MilliQ water, for 10 min and then the mixture was boiled at 100° C for 10 min. The freshly prepared extract was obtained by filtering it through Whatman filter paper No. 1. The filtrate obtained from extraction of stem of the Ceriops tagal contains the bioactive components includes high number of terpenoids and flavonoids, believed to add stability and increased productivity of nanoparticles; the filtrate is collected for the synthesis of metal nanoparticles from the packaging materials;
2.0 Synthesis of aluminium nanoparticles from autoclaved aluminium foil;

15.0 gm of shredded waste aluminium foil was mixed with 100 ml MilliQ water and autoclaved. In 95ml autoclaved solution of aluminium foil; 5.0 ml of the solution of bio-reducing agents isolated from the Ceriops tagal stem extract (CTSE) is added, the mixture of solution is kept at the temperature about 60 °C for about 4.0 hrs;
3.0 Synthesis of aluminium nanoparticles from unautoclaved aluminium foils; 10.0 gm of shredded waste aluminium foil was mixed with 100 ml MilliQ water and boiled at 100°C for about 10 min. In 95ml unautoclaved solution of aluminium foil; 5.0 ml of the solution of bio-reducing agents isolated from the Ceriops tagal stem extract (CTSE) is added, the mixture of solution is kept at the temperature about 50 °C for about 4.0 hrs;
The formation of aluminium nanoparticles in autoclaved and un-autoclaved solution of aluminium is monitored by the change in colour of the mixture of solution and measuring absorbance by using UV -visible spectroscopy;

(a) isolation of bioactive components from plant parts in a solvent,
(b) shredding the aluminium foil in to small pieces,
(c) soaking the packaging material used for aluminium foil in a water for a predetermined time;
(d) optionally heating in an autoclave at an elevated temperature;
(e) reacting the soaked and autoclaved shredded the aluminium foil with the bioactive components isolated from the plant parts at a pH in the range of 6-8 and at an elevated temperature;
(f) monitoring the synthesis of metal nanoparticles from aluminium foils used for food packaging by using UV-visible spectrophotometer,
(g) characterization of metal nanoparticles formed by analytical techniques;
2. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim1 wherein from waste aluminium foils obtained from municipal waste aluminium laminated includes, coated polymers films used for packaging the of the dry, liquid, semisolid food materials;
3. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 wherein plant selected is Ceriops tagal,
4. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 wherein stem, leaves, roots;
5. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 wherein stem,
6. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 wherein stem is having terpenoids and flavonoids;
7. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 wherein solvent is water, methanol, ethanol.
8. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 temperature is 50-60 °C;

9. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 temperature is 50-60 °C;
10. A method for green preparation of aluminum nanoparticles from waste aluminium foils obtained from municipal waste according to claim 1 ratio Ceriops tagal, steam extract to solution of the aluminum foil is 5:95 v/v;