From 2
The Patents Act 1970,
(39 of 1970)
&
The Patents Rule, 2003
Complete specification
Title of Invention
A METHOD OF PREPARATION OF ZnO NANOPARTICLES BY CO-PRECIPITATION METHOD USING BLACK TIGER PRAWNS (PENAEUS MONODON) EXTRACT
Applicants:
1) Name: Dr Rajesh C Patil
2) Nationality: Indian
3) Address: Bhavan's College, Andheri (West), Mumbai 400058, Maharashtra, India
Inventors:

l.Dr Rajesh C Patil Indian Bhavan's College, Andheri (West), Mumbai 400058, MAH Elphinstone College, Mumbai 400001, MAH
2.Dhanashree Talekar Indian B/122, Dwarka, IC Colony, Borivali (West), Mumbai 400103, MAH
3.Dr Shantaj Mulchand Deshbhratar
4.Dr Anita S Jadhav Indian
Indian Bhawani Hazarimal Somani College, Chowpatty, Mumbai 400007, MAH
ICLES MJ College, Sector 9 A Vashi, Navi Mumbai, MAH
5.Dr Manisha N Kulkarni Indian Ismail Yusuf State Govt College,
6.Dr A SKulkami Indian Jogeshwari (East) Mumbai 400060, MAH
Block no 104, Laxmi Narayan Apts, Bandar Road, Ratnagiri,
415612, MAH
7.Prof Athoiba Singh Elangbam Indian BVU-Rajiv Gandhi Institute of ITBT, Katraj, Pune 46, MAH
8.Ms Archana Sambhajirao Injal Indian Dept of Bio-technology, Gogate-Joglekar College, Ratnagiri, 415612, MAH

The following specification particularly describes the invention and the manner in which it is to be performed

Field of invention
The field of invention relates to the method for preparation of Zinc Oxide nanoparticles, more particularly it relates to Zinc Oxide nanoparticles from the co-precipitation method by using biological extract obtained from Prawns (Penaeus Monodori)
Background of invention and prior art
Nanoparticles are particles ranging in size from 3 nm to 1 micron in diameter. "Nano" is a prefix which means one billionth (10-9) part of something, in recent years, the field of nanoparticles has grown due to their unique properties. Many industries utilize nanoparticles, for example the electronics industry, medical science, material science, and environmental science. Noble metal nanoparticles have found widespread use in several technological applications and various wet chemical methods have been reported. See, X. Wang and Y. Li, Chem. Commun, 2007,2901
There is great interest in synthesizing metal and semiconductor nanoparticles due to their extraordinary properties, which differ from those of the corresponding bulk material. An example of a nanoparticle is nanoscale zero valent iron (nZVI). Generally, nanoparticles are synthesized in three ways: physically by crushing larger particles, chemically by precipitation, and through gas condensation. Chemical generation is highly varied and can incorporate laser pyrolysis, flame synthesis, combustion, and sol gel approaches. See, U.S. Pat. No. 6,881,490 (Apr. 19, 2005) N. Kambe, Y. D. Blum, B. Chaloner-Gill, S. Chiruvolu, S. Kumar, D. B. MacQueen, Examples of mechanical processes for producing nanoparticles include mechanical attrition (e.g., ball milling), crushing of sponge iron powder, and thermal quenching. Examples of chemical processes for producing nanoparticles include precipitation techniques, sol-gel processes, and inverse-micelle methods. Other chemical or chemically-related processes include gas precipitation with a compressed fluid anti-solvent, and generation of particles from gas saturated solutions condensation methods, evaporation techniques, gas anti-solvent recrystallization techniques. The commercial significance of nanoparticles is limited by the nanoparticle synthesis process, which is generally energy intensive or requires toxic chemical solvents and is costly.
Therefore, in the present invention efforts are made to provide an alternative cost effect, environmentally friendly method for generation of Zinc oxide nanoparticles, the method is provided by using the co-precipitation method by using biological extract obtained from Prawns {Penaeus Monodori),
Object of the invention
It is an object of the invention to provide a method for preparation of Zinc Oxide nanoparticles
It is also an object of the invention is to provide a method for preparation of Zinc Oxide nanoparticles by using biological material such as extract prepared from the tiger prawn {Penaeus Monodon) as co-precipitant

It is also object of the invention to provide a method for safe, environmentally friendly method for preparing ZnO nanoparticles
It is also an object of the invention to provide a method for preparation of ZnO nanoparticles which is cost-effective
It is one of the object of the invention is to provide anti-microbial activity of ZnO nanoparticles
It is also an object of the invention to provide a method for preparation of ZnO nanoparticles which gives ZnO having compatibility for medical and pharmaceutical applications as well as large scale commercial production because of its pollution free and eco-friendly nature
Summary of the invention
In one of the aspect of the invention it is provided that the process for preparing Nanoparticles from ZnO is provided, the process involves co-precipitation method. 0.02 M aqueous solution of zinc acetate di-hydrate is put into 100 ml of distilled water under vigorous stirring. After 10 min stirring, 3mL-5ml of extract prepared from the prawn is added the above solution. After addition of extract, 2.0 M aqueous sodium hydroxide solution is introduced into the above aqueous solution drop wise, resulting in a white aqueous solution at pH 12, which is then placed on magnetic stirrer for 2 hr. The precipitate is then taken out and washed repeatedly with distilled water followed by ethanol to remove the impurities for the final products. Then a white powder is obtained after drying at 60 °C in vacuum oven overnight.
In an another aspect of the invention Characterization of ZnO is done by Transmission electron microscopy (TEM) and Scanning electron microscopy (SEM) and UV-Vis Spectrophotometer.
Further, the ZnO nanoparticles prepared are studied for the Antibacterial activity of synthesized Zn Materials used for antimicrobial activity of zinc oxide nanoparticles are Nutrient agar slants, petriplates, Cork borer, zinc oxide nanoparticle sample, Salmonella typhi, salmonella paratyphi A and Salmonella paratyphi B. Agar diffusion method used for antimicrobial activity of zinc oxide nanoparticles.
Detailed description of the invention
In one of the aspect of the invention zinc compounds selected from organic or inorganic salts such as Zinc organic and inorganic salts such as Zinc gluconate, Zinc pyrithione, Zinc ricinoleate, Zinc stearate, zinc chloride, zinc sulphate, Zinc sulphide, zinc acetate di-hydrate are used, having concentration in the range of Molar standard solution rages from 0.1-2.0M are used,
Alkali hydroxide mainly selected from sodium or potassium hydroxide is used having the concentration in the rage of 1.0-3.0M.

Biological extract is prepared from Black Tiger Prawns {Penaeus Monodon) extract, which is prepared by using the Black Tiger Prawns (Penaeus Monodon) grinding that into the grinder and the same is filtered through filter paper, the filtrate obtained is called as extract, the concentration of the biological extract used is preferably from 3.0-5.0 %, v/v;
In one of the aspect of ZnO are prepared by co-precipitation method. 0.02 M aqueous solution of zinc acetate di-hydrate is put into 100 ml of distilled water under vigorous stirring. After 10 min stirring, 3mLof biological extract from Black Tiger Prawns {Penaeus Monodon) is added the above solution. After addition of extract, 2.0 M aqueous sodium hydroxide solution is introduced into the above aqueous solution drop wise, resulting in a white aqueous solution at pH 12, which were then placed on magnetic stirrer for 2 hr. The precipitate is then taken out and washed repeatedly with distilled water followed by ethanol to remove the impurities for the final products. Then a white powder was obtained after drying at 60 °C in vacuum oven overnight.
The results obtained are as tabulated below:

Samples Element Zinc in ppm
0.5% ZnO-NPs 9,789.5
0.5% Zinc Acetate Dihydrate 5500
0.5% prawns extract 67.8
In an another aspect of the invention Characterization of synthesized ZnO is provided by Transmission electron microscopy (TEM), scanning electron microscopy (SEM), UV-Vis Spectrophotometer.
1. Transmission electron microscopy (TEM)
TEM image shows ZnO nanoparticles with average size of nm. Inset shows Selective area electron diffraction (SAED) pattern exhibits a set of rings containing spots suggesting that nanoparticles have a larger grain size of about 25-34nm, uniform shape and polycrystalline in nature. A TEM image was recorded by dissolving the as-synthesized powder sample in ethanol and then placed a drop ethanolic solution on the surface of copper grid.
2. Scanning electron microscopy (SEM)
The morphology of ZnO NPs with little agglomeration having sizes about 28nm throughout the carbon coated copper grid and average particles size and shape in the range of nm. Scanning electron microscopy (SEM) image reveals that the particles are of flakes in nature as depicted in the figure.
3. UV-Vis Spectrophotometer
Optical properties of the ZnO nanostructure sample were revealed by UV-Vis spectrum spectrophotometer at room temperature. It can be seen from the Fig. 6 that there was intensive absorption in the ultraviolet band. The Characteristic peak at about 360 nm of ZnO was observed at room temperature.
In an another aspect of the invention it is provided that the antimicrobial activity of the ZnO nanoparticles formed is studied

Antibacterial activity of synthesized ZnO nanoparticles on
i) Salmonella typhi
ii) Salmonella paratyphi A
in) Salmonella paratyphi B

Bioactive agent Zone of inhibition (mm)
Salmonella typhi Salmonella paratyphi
A Salmonella paratyphi B
ZnONPs 1% 41 30 25
Zn acetate 1% - - -
Zndustl% - - -
Extract - - -
Examples
Preparation of ZnO nanoparticles by using biological extract from Black Tiger Prawns (Penaeus Monodon) by co-precipitation method
Example 1
0.02 M aqueous solution of zinc acetate di-hydrate is put into 100 ml of distilled water under vigorous stirring. After 10 min stirring, 3mL biological extract from Black Tiger Prawns {Penaeus Monodon) of is added the above solution. After addition of extract, 2.0 M aqueous sodium hydroxide solution is introduced into the above aqueous solution drop wise, resulting in a white aqueous solution at pH 12, which were then placed on magnetic stirrer for 2 hr. The precipitate is then taken out and washed repeatedly with distilled water followed by ethanol to remove the impurities for the final products. Then a white powder was obtained after drying at 60°C in vacuum oven overnight.
Example 2
Preparation of ZnO nanoparticles from electroplating waste by co-precipitation method; 0. 2 M aqueous solution of zinc sulphate is put into 100 ml of distilled water under vigorous stirring. After 10 min stirring, 5mL of biological extract from Black Tiger Prawns {Penaeus Monodon) is added the above solution. After addition of extract, 2.0 M aqueous potassium hydroxide solution is introduced into the above aqueous solution drop wise, resulting in a white aqueous solution at pH 12, which were then placed on magnetic stirrer for 2 hr. The precipitate is then taken out and washed repeatedly with distilled water followed by ethanol to remove the impurities for the final products. Then a white powder was obtained after drying at 60 °C in vacuum oven overnight.

Exam pie 3
Preparation of ZnO nanoparticles from electroplating waste by co-precipitation method; 0, 2 M aqueous solution of zinc gluconate is put into 100 ml of distilled water under vigorous stirring. After 10 min stirring, 5mLof biological extract from Black Tiger Prawns {Penaeus Monodon) is added the above solution. After addition of extract, 2.0 M aqueous potassium hydroxide solution is introduced into the above aqueous solution drop wise, resulting in a white aqueous solution at pH 12, which were then placed on magnetic stirrer for 2 hr. The precipitate is then taken out and washed repeatedly with distilled water followed by ethanol to remove the impurities for the final products. Then a white powder was obtained after drying at 60 °C in vacuum oven overnight.
Description of drawing and Figures
Fig.l synthesis by Co-precipitation method;
Fig.2 Black Tiger Prawns {Penaeus Monodon), inset - extract;
Fig.3 TEM image shows ZnO nanoparticles in as-prepared sample with Black Tiger
Prawns {Penaeus Monodon) extract and inset shows selective area electron
diffraction (SAED) pattern; Fig.4 SEM image shows the particles are nano-flower in nature; Fig. 5 Uv-vis spectra of ZnO nanoparticles; Fig.6 Antibacterial activity of synthesized ZnO nanoparticles on
Salmonella typhi, Salmonella paratyphi A, Salmonella paratyphi B

Claims
We claim:
1. A method for preparation of ZnO nanoparticles by co-precipitation by using extract from Penaeus Monodon comprising
(a) co-precipitation of zinc salt aqueous extract Penaeus Monodon;
(b) with drop wise addition of alkali hydroxide;
(c) maintaining alkaline pH;

(d) stirring magnetic stirrer for 2 hr;
(e) washing repeatedly with distilled water and ethanol to remove the impurities for the final products,
(f) drying under vaccum the white powder at 60 °C in vacuum oven overnight to obtain white powder of ZnO nanoparticles;

2. A method for preparation of ZnO nanoparticles by co-precipitation by using extract from Penaeus Monodon according to claim 1 wherein zinc salt is selected from Zinc gluconate, Zinc pyrithione, Zinc ricinoleate, Zinc stearate, zinc chloride, zinc sulphate, Zinc sulphide, zinc acetate di-hydrate.
3. A method for preparation of ZnO nanoparticles by co-precipitation by using extract from Penaeus Monodon according to claim 1 wherein molar concentration of zinc salt is 0.1-2.0M.
4. A method for preparation of ZnO nanoparticles by co-precipitation by using extract from Penaeus Monodon according to claim 1 wherein alkali hydroxide is sodium or potassium hydroxide.
5. A method for preparation of ZnO nanoparticles by co-precipitation by using extract from Penaeus Monodon according to claim 1 wherein concentration of alkali hydroxide is 1.0-3.0M
6. A method for preparation of ZnO nanoparticles by co-precipitation by using extract from Penaeus Monodon according to claim 1 wherein alkaline pH is up to 12.