Title of Invention

A PROCESS OF PREPARATION OF NANOSIZED METAL VANADATE PARTICLES

Abstract A process for the preparation of nanosized metal van date particles comprising mixing ammonium van ad ate with formic acid and hydrazine hydrate a mole ratio of ammonium van ad ate; formic acid: hydrazine hydrate of 1:1-4:0.025 - 4, produce vanadyl formate; mixing said vandyl formate with metal nitrate(s), fuel and minor amount of polyvmyl alcohol in aqueous medium to obtain a homogeneous mixture; drying or spray drying the said homogenous mixture by simple evaporation to obtain fluffy carbonaceous mass; calcining the said carbonaceous mass depending on the chemical nature of the system to produce the dried nanosized particles.
Full Text
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This imsvention relates to a process of preparation of nanosized metal wanadlate particles. BACKBROUTO OF TTHE INVENTION
Previously, fuel tossed ntasno paHicles was synthesized! by using Ihytihrazime based pyropthoric chemcals. The raethod of the prior art had sveral dispelvantages, like toxicitry of the reagents snd (dififiemity in (cornitrolillin is h:ii An objject of' t;htiis itrnvereifciran) is to propose a nowel procress- of
prepai aifcioni of ini.'sintosised nttetal v asm ad ate particles.
AnavfcheTT nttojecft o-ff tfeiiis ifrnveinttiomt is to propose a process ratoose
rate imtf ira?ac1tiLoni (cam Ibe sBsonjitliUy (control led for- getifcJLncji cBtesired
fiBOrplhiolcr y of itM& pffir"feii.c 1 es.
Vet smotheir (nbjjsHEit (mf tthtis inrention is tra propose a crlheafxier
process for tfutB prepariasftirant oiF im parfciicles-
Yet aimottiwrr object c -ff th fis iinventicm is to propose aam enwiirQnRent
frifendfly pmcwiess-
Other- oojjcciifcs airartl ariJvBirutacfie'S of t-H iimvencfciomi will toe apparent
frosit t*ne wirasuiifBg dJiesciriptioirc-
DETflilLE(c) DEHCREPTION OF THHE. IMVEJWTION
AcconrfiiB cy to thtii.s irmveirotinmi is provided! a process foir tlhie preparation of intaimosiscefca Bwe-tal wanadate particles {comprising fBiiKiiinQ acBffrawrcilium wansdlatei wiii.-frh formiic acidl aodl hy.'idlrasiioffi hrvcPrffite to prodhiifce wainitadyU foiraiat;(r);
mixing said! vanadisfl fiamatE witBs metal nitirateCsJ v fiuiel affnd! Bsimor

__ T1
smotutnt of ptolywinyl alcohol in aapi&ous medium to obtk&iin) a Ihtomo e-
meows, flrjisctfuupe;
drying oir spray dJiryiny the sasid IhiOBto e internes mixture? itoy siimple
evaporation to ofolfcairnt fluffy carbotntaceous mass;
(calfcAmarftinxgi tfhxe said CE a ribwort J OE?O(U 5 mssss depeinidiiing csri (WtTtce- cfh)ffl?n ical
mature oif Mite systpui to pradkietE? th(c) dried tntarsosiartBd particles.
In accordance with this iimv-'effutjioirs,, tlbe irasEnos-ized! B6*1fcaI vaireadate
particles mre pr-epasfietdf tf7)Trou#T) the fomnaticBn of wars cByl foraat(c),
obt-asinssHdl b 1 eeixiBT afiifiDDTTiiujwB wanadate wii-fch fonniic acid) aimdt Ihiydira-
zinie hydrsibe iimt a fcsolam iratio rff A si *o -4S0-.Z5 to 4- The? reaction
D
mixtume is IbeaifcEed ait a tewper ¦for a; p iriiocJ! o1F t -fco. fi.* hrs
cv -VP tC
The vaanadyl -fcBrnrtstfte itlhtus obitaiirnfffll is fimixedl wi*h ai metal niittrafte,
The vanadyl formate and metal
.¦fuel, pjolyviimyl alcroffnol itn affpiieodRs aedlAuaitg .iwi-fch mm molar raifcio of nitrate
1 to 2: 1 to 3 are mixed
in ord TT -to ol 1fcas.m met-aJ waoadaites of tMe in a
fonnuli ff%(VO ) _ Tihi(r) hofBtogtemteoiuis mixttutre is dried oir sjpiray dried
4- X o
at ;a ttcfmpeiratmiire iifnt tttnc? ran(c)(c) of lfifflf to 10$ C to tatotaiirfl s -fluffy
cartocwmacecKLfis* ctia;ssK wftaiichi is calcined! a& a teuurperaiifcure itm t:-!he
o rant|p mt 2M fto The BiBorajsiacietd meitatl wamtadaits? particles fh*aw
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and maimi&oi.
The fol Jxmlmgs jraanosizeaJi a ffl?1fca"ll vantad sites cars be prepared fby the
aforesaid purracess 2
i . Meifcat warn) ad a. "fees
a. EA ¥O 2 Jw **hi ire €A =¦ (%" CSB, Sirf 3Ba, Co, litflfi " Dutn Zmt snd
3 4 2
mixfeLnret b- CB'yO 1T fcrffueirffi? SBt ~ Al. B Cirfl Fc, ffikre, V, Bafe-eairifch eleiments asid
This iiimvemjtioim, wmSl mraw toe expiaiiwd iim ceiresa-feer* derail iwifefht tfie help of t#B -folltowiffiKg oora~.Ii 9iitioQ exaople.
EXAMPLE 1 - WO 4
i,3 nsmle Y O €fR*l 225.0 was dJissaalved inn conereimt-Tra-tedi imiti ic
2 3 acid solution I2!S I nsU tro pirodutce VCNO I soltuttioirn- 1 Bffiole airano-
3 3 tniuwii wansidlate wras ollissolvsed itnt 4 nole -fforsfflic: acidJ. In
¦ this -ffor aiic ancidl /mis;-trt.fiew # mole hydra:2rirBffi? hydrate dfFtil 5i!3J,BOJ& JS iw;as •slowly ffiddlffid seiradl -(Khie solwifcicHm was i"e-ffliui3fiffi?(di -ffoir i &itir- at; 120 C to
prcxriluce? wffimactjfl sialit(tm) Vai adlyl salt: Mas mitsced! witdhi Y€WO > SDIILI-
3 3 titm- In ttiis tniixKtuine, 2-5 mrcsle sucrose was addferf aimd tMjatwir was
addffid so ttlhaifc the tofcali woluine beeainne? 2 Itrs-- In tthtis nixturv, 0-05 mails P S was add(c) voluroifreooiB iFIuiFfy oingafmic ttoasedf pireciuiirsor powder was TretsHutlted-
o This pirectutiTEiOir pioiwdeir 01m calfciraaifciafra at 5*?# C -for1 2 lh Trs jprodlmred
YVO pratwdeir wiltttj ffiwejrage patrticle size less than 60 rwn. 4

-4-WE CLAIM:
1. A process for the preparation of na no sized metal vanadate particles
comprising
mixing ammonium vanadate with formic acid and hydra sine hydrate a mole ratio of ammonium vanadate: formic acid: hydrazine hydrate of 1:1-4:0.025 - 4, produce vanadyt formate;
mixing said vandyl formate with metai nitrate9s), fuel and minor amount of poly vinyl alcohol in aqueous medium to obtain a homogeneous mixture;
drying or spray drying the said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass;
calcining the said carbonaceous mass depending on the chemical nature of the system to produce the dried nanosized particles.
2. The process as claimed in claim 1 wherein said mixture of ammonium
vanadate, formic acid and hydrazine hydrate is heated for a period ranging
from 1 to 6 hrs.
3. The process as claimed in claim 1 wherein said mixture of ammonium
vanadate, formic acid and hydrazine hydrate is heated at a temperature in
the range of 60 to 150 °C.
4. The process as claimed In claim 1 wherein the homogeneous mixture
comprises vanadyl formate and metal nitrate, in a mole ratio of 1 to 2:1 to
3 for a metal vanadate of formula My (VOnK
2.
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5. The process as claimed in claim 1 wherein said homogeneous mixture is
dried or spray dried at a temperature in it\e range of 100 to 180 QC.
6. The process as claimed in claim 1 wherein said carbonaceous mass in
calcined at a temperature in the range of 200 to 600 °C.
7. The process as claimed in claim 1 wherein said metal nitrate is selected
from magnesium nitrate, calcium nitrate, strontium nitrate, barium nitrate,
cobalt nitrate, nickel nitrate, copper nitrate, zinc nitrate, aluminium nitrate,
chromium nitrate, ferric nitrate, manganous nitrate, ytrium nitrate and
nitrates of the rare elements, singly or in mixtures.
8. The process as claimed In claim 1 wherein said fuel Is selected from
xylose, glucose, fructose, sucrose, hydrofyzed starch, sorbitol and manttol.
9. The process as claimed in claim 1 wherein said nanoslzed metal vanadate
particles have a particle size of 20 to 80 nm.
A process for the preparation of nanosized metal van date particles comprising mixing ammonium van ad ate with formic acid and hydrazine hydrate a mole ratio of ammonium van ad ate; formic acid: hydrazine hydrate of 1:1-4:0.025 - 4, produce vanadyl formate; mixing said vandyl formate with metal nitrate(s), fuel and minor amount of polyvmyl alcohol in aqueous medium to obtain a homogeneous mixture; drying or spray drying the said homogenous mixture by simple evaporation to obtain fluffy carbonaceous mass; calcining the said carbonaceous mass depending on the chemical nature of the system to produce the dried nanosized particles.



Documents:

01659-cal-1998 abstract.pdf

01659-cal-1998 claims.pdf

01659-cal-1998 correspondence.pdf

01659-cal-1998 description(complete).pdf

01659-cal-1998 description(provisional).pdf

01659-cal-1998 form-1.pdf

01659-cal-1998 form-2.pdf

01659-cal-1998 form-3.pdf

01659-cal-1998 form-5.pdf

01659-cal-1998 g.p.a.pdf

01659-cal-1998 letters patent.pdf

1659-CAL-1998-FORM 27.pdf

1659-cal-1998-granted-abstract.pdf

1659-cal-1998-granted-claims.pdf

1659-cal-1998-granted-description (complete).pdf

1659-cal-1998-granted-form 2.pdf

1659-cal-1998-granted-specification.pdf


Patent Number 208960
Indian Patent Application Number 1659/CAL/1998
PG Journal Number 33/2007
Publication Date 17-Aug-2007
Grant Date 16-Aug-2007
Date of Filing 17-Sep-1998
Name of Patentee INDIAN INSTITUTE OF TECHNOLOGY
Applicant Address KHARAGPUR 721 302,INDIA
Inventors:
# Inventor's Name Inventor's Address
1 PROF. P. PRAMANIK INDIAN INSTITUTE OF TECHNOLOGY,KHARAGPUR 721 302,INDIA
PCT International Classification Number C01B 13/14
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA