Title of Invention	A PROCESS OF PREPARATION OF NANOSIZED METAL MOLYBDATE PARTICLES
Abstract	A process for the preparation of nanosized metal molybdate particles comprising. refluxing pure metal molybdate in the EDTA salt of amines In aqueous medium to make a homogeneous solution, the mole ratio of metal molybdate: EDTA: organic amine being 1:1 to 4::1 to 4 mixing the said homogeneous solution with fuel and minor amount of polyvlnyl alcohol (PVA) to obtain a homogeneous mixture in aqueous medium, the mole ratio of metal mofybdate : fuel:: PVA is 1:1 to 4:0.5 to 4; drying or spray drying the said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass; calcining the said carbonaceous mass at a temperature range depending on the chemical nature of the system to produce the dried no nosized particles;

Title of Invention

A PROCESS OF PREPARATION OF NANOSIZED METAL MOLYBDATE PARTICLES

Abstract

A process for the preparation of nanosized metal molybdate particles comprising. refluxing pure metal molybdate in the EDTA salt of amines In aqueous medium to make a homogeneous solution, the mole ratio of metal molybdate: EDTA: organic amine being 1:1 to 4::1 to 4 mixing the said homogeneous solution with fuel and minor amount of polyvlnyl alcohol (PVA) to obtain a homogeneous mixture in aqueous medium, the mole ratio of metal mofybdate : fuel:: PVA is 1:1 to 4:0.5 to 4; drying or spray drying the said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass; calcining the said carbonaceous mass at a temperature range depending on the chemical nature of the system to produce the dried no nosized particles;

Full Text	-1A- This invention relates to a process of preparation of nanosized metal molybdate particles. BACKBROUND OF THE INVENTION Previously, fuel based nano particles was synthesized by using hydrazine based pyrophoric chemicals. The method of the prior art had several disadvantages, like toxicity of the reagents and difficulty in controlling high exothermic process and homogeneity of the imiilticsMpemeirei; ffisisstoF1©-OBJECTS OF THE ZNVOfTXON An object of tfh^is invwi!t.ii,!im is to propcisc a novel piroccsB of preparffi-fciofra of nainKosixed fl"olybda1te particles- Another dbject orff t&nis invention is to propose a process whose rate f rressfctiora can lb Yet ajmrathiffijir' tnt>jie?art msf fih}is aiw'SMntiesrs is -fees prcpos® SE cheaper process for- t$nm preparation crff nanosizei HBstsiS raolybdate parf:icie?s- Yet aimotB^fpr otojecct of tihiis invention is. %(D piropose sm &mwi.nmmmnt friendly process-Other object:© amid! advantages of tffrne inventior? will be apparent frdro the flKraisuiintg (dSesoriptian-DETAItEIU DESCRHPTIOBf OIF' TOE ISWENTION rflccords^^ tm tjhiiis ijrcvei^tiorns is prcjjvid!©dl 3 process for the preparation of srua^iosIzesS metal iaol^ttclate particles comprising refluxiinss$ pm ase-fcal isBoIytodsfte in the? EBTA salt of amines in aqueous scrHsdituws 1to BtafcK a hooogenerautis solution; mixireg; tlhifl? said! hofnogeneouts solution ntith fuel md Bnintarr amount T" __ of polyvinyl alcohol to ob&aiira a homogeneous tsixture in aqueoMs CBecEiutm; dryitnxgj ccir sprasy dtyin Bvgponticm ifco (aftstialn -fliif'fy carfocmaceous itnassis; (caltcinimw} the sasiid cairtoomaccecHuis mass a.t a tempeTratmire' ramcie depending ran the chroasicral mjatftsire of t"e sysstera fto pf-csduc^ t#e dried rmanosizofflil particles. In Bcconfaric© wit-f^ "this irswen^lDnw the psiire ^etel gis3l^tsclat;e is refluK"tS in a -first step with fEDTA-salt of ayroioes ±m ami aqueous medis.ES® %m a aaoiayr ratio of- 1st to 4sI to 4 erf sstetasl sKtslyibda&es EDTAsor^amiic: aroiam&w The hoaBogteneoRjs solajrlfcicm thiuis obifcasarned is mi"ed with -fuel aimd! sainor ffisnotwnit of pcslyvinyl alcrohasl in t^ueous mediuffi to obitain a !bcwKogeneaai!S mixture witSu a molar1 iratio o-f is! to 4s"0!5 to * of metal molyfedatesfuel sPVA twith raspect to moirEra- mer aMEitS- l#sefiii WS is taken) correspoimdingi to C H O o TThie hoiraogeirrFeotiis H"i>stiBre fi 12 6 obtadnffisi! is dirsedl ssr- spray dlrietf at a f;ess(p D 10& tero Uffl0 C to ofarifcaimt a flu-ff-fy cjarfoon ace outs uRass^ tutiicft is -^ - ¦-¦ o calcines! at at teaperature rasrs^e erf 25B^l to "^^ C to cistaip the desiTredl mantosiarrod particltffs;- The cmrgantic affliime is sseleert-ed frcM" ethyiERe rfiassjine^ diietfhyleirje triaffiairpCj, tTri©-fc!hya"jrae tetTra"ine¥ diethaoolamuine and tirietihtanol™ amiinie,. Further,, ttits? fuel fus^wd in ttwe- piresesntt invention is Eelectedl from xylose, cBluotKSie,, fructose,, SR.ntcro!Si"f hydrolyzed stanch, sorbitol and! majTfiitcei- The follewingi ftamitssiized a"ffl?t"l nolybdates csnt be prepared by the ™ 3 ™" ¦aforesaid process s i . irtetaS. gKCTlyJh?dat©s a- tABtoOJ 1 hawing a particle size erf 20 to 100 nsfc, wfoer-ffi CA = I Ca" SrB Bsw ZITBB OUI¥ Mi, CO and miixtuVeSf) j to, iTA 4CMo© ) 3 tawimfg a particle si2:e of S0 120 oi"5 #3iB!r# (A Smv Eu, PIT,, Nfd,, Py, H!o, SSd; astrad msixtiuiresK EXAfHSPLE i - CaimoO 4 Frvehly preparedl 1 malm CsJJUoO wss dissoivect in a mixtuire of 1-2 4 mole etttylene "Sia"£ne -^etirascetic: acid asrad 3 mole oif diettsylene trftamirme iirn aa^uiecmts nKdiuna m& t"e total voluw ns 1.5 Itr.. In this. sni>;t8iirett 1 feiol© sius:r*ose Mas addc"l sanid water MSSS addled so that the total woUo/nte became 2 Itris--. In this mixture, 0-CK5 mole PVA emas addled S?K 103K w/v ssijuaeouss osolution.. The resultirir^ solution were th©int ewaporatffl>"jt by heastio^- At tflrne time of evaporation^ the nitrates werre decoaposeofl amwJ ibrewsrs fumes wf rsitrs^eira dioxxdle giss was ewolwed- After conplete (evaporation,, HI vraluminouts fluffy organic: fcss^ed! pir®cuirsoir prawdeir resulted. THiis jptrec:ursor o powder- ons CEsIcS.m)i3;tJi.{aa at 5SSS!! C "for- 2 fen^s-, pr-oduc©d CaBicsO powder 4 witlhi av(£?ris^fe patirtisile siz© less than TS r%m- -4- WE CLAIM: 1. A process for the preparation of nanosized metal molybdate particles comprising. refluxing pure metal molybdate in the EDTA salt of amines in aqueous medium to make a homogeneous solution, the mole ratio of metal molybdate: EDTA: organic amine being 1:1 to 4:1 to 4 mixing the said homogeneous solution with fuel and minor amount of polyvinyl alcohol (PVA) to obtain a homogeneous mixture in aqueous medium, the mole ratio of metal molybdate : fuel:: PVA is 1:1 to 4:0.5 to 4; drying or spray drying (he said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass; calcining the said carbonaceous mass at a temperature range depending on the chemical nature of the system to produce the dried nonosized particles; 2. The process as claimed in claim 1 wherein the homogeneous mixture is dried or spray dried at a temperature In the range of 100 to 180 °C to obtain a carbonaceous mass. 3. The process as claimed in claim 1 wherein the carbonaceous mass is calcined at a temperature in the range of 200 to 600 °C. 4. The process as claimed in claim 1 wherein the organic amine is selected from ethylene dfamine, diethylene trlamine, trtefhytene tetramine, diethanolamine and triethanoiamine. -5- 5. The process as claimed in claim 1 wherein the fuel used is selected from xylose, glucose, fructose, sucrose, hydrolysed starch, sorbitol and manitol. 6. The process as claimed in claim 1 wherein the nanosized metal molybdate particles have a size in the range of 20 to 120 nm. 7. The process as claimed in claim 1 wherein the nanosized metal motybdate particles have a size in the range of 20 to 100 nm. A process for the preparation of nanosized metal molybdate particles comprising. refluxing pure metal molybdate in the EDTA salt of amines In aqueous medium to make a homogeneous solution, the mole ratio of metal molybdate: EDTA: organic amine being 1:1 to 4::1 to 4 mixing the said homogeneous solution with fuel and minor amount of polyvlnyl alcohol (PVA) to obtain a homogeneous mixture in aqueous medium, the mole ratio of metal mofybdate : fuel:: PVA is 1:1 to 4:0.5 to 4; drying or spray drying the said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass; calcining the said carbonaceous mass at a temperature range depending on the chemical nature of the system to produce the dried no nosized particles;

Full Text

-1A-
This invention relates to a process of preparation of nanosized metal molybdate particles. BACKBROUND OF THE INVENTION
Previously, fuel based nano particles was synthesized by using hydrazine based pyrophoric chemicals. The method of the prior art had several disadvantages, like toxicity of the reagents and difficulty in controlling high exothermic process and homogeneity of the imiilticsMpemeirei; ffisisstoF1©-OBJECTS OF THE ZNVOfTXON
An object of tfh^is invwi!t.ii,!im is to propcisc a novel piroccsB of preparffi-fciofra of nainKosixed fl"olybda1te particles-
Another dbject orff t&nis invention is to propose a process whose rate f rressfctiora can lb Yet ajmrathiffijir' tnt>jie?art msf fih}is aiw'SMntiesrs is -fees prcpos® SE cheaper process for- t$nm preparation crff nanosizei HBstsiS raolybdate parf:icie?s-
Yet aimotB^fpr otojecct of tihiis invention is. %(D piropose sm &mwi.nmmmnt friendly process-Other object:© amid! advantages of tffrne inventior? will be apparent frdro the flKraisuiintg (dSesoriptian-DETAItEIU DESCRHPTIOBf OIF' TOE ISWENTION
rflccords^^ tm tjhiiis ijrcvei^tiorns is prcjjvid!©dl 3 process for the preparation of srua^iosIzesS metal iaol^ttclate particles comprising refluxiinss$ pm ase-fcal isBoIytodsfte in the? EBTA salt of amines in aqueous scrHsdituws 1to BtafcK a hooogenerautis solution; mixireg; tlhifl? said! hofnogeneouts solution ntith fuel md Bnintarr amount

*T" __
of polyvinyl alcohol to ob&aiira a homogeneous tsixture in
aqueoMs CBecEiutm;
dryitnxgj ccir sprasy dt*yin Bvgponticm ifco (aftstialn -fliif'fy carfocmaceous itnassis;
(caltcinimw} the sasiid cairtoomaccecHuis mass a.t a tempeTratmire' ramcie
depending ran the chroasicral mjatftsire of t*"e sysstera fto pf-csduc^ t#*e
dried rmanosizofflil particles.
In Bcconfaric© wit-f^ "this irswen^lDnw the psiire ^etel gis3l^tsclat;e is
refluK"tS in a -first step with fEDTA-salt of ayroioes ±m ami aqueous
medis.ES® %m a aaoiayr ratio of- 1st to 4sI to 4 erf sstetasl sKtslyibda&es
EDTAsor^amiic: aroiam&w The hoaBogteneoRjs solajrlfcicm thiuis obifcasarned is
mi"ed with -fuel aimd! sainor ffisnotwnit of pcslyvinyl alcrohasl in t^ueous
mediuffi to obitain a !bcwKogeneaai!S mixture witSu a molar1 iratio o-f is!
to 4s"0!5 to * of metal molyfedatesfuel sPVA twith raspect to moirEra-
mer aMEitS- l#sefiii WS is taken) correspoimdingi to C H O o TThie hoiraogeirrFeotiis H"i>stiBre
fi 12 6 obtadnffisi! is dirsedl ssr- spray dlrietf at a f;ess*(p D
10& tero Uffl0 C to ofarifcaimt a flu-ff-fy cjarfoon ace outs uRass^ tutiicft is
-^ - ¦-¦ o
calcines! at at teaperature rasrs^e erf 25B^l to "^^ C to cistaip the
desiTredl mantosiarrod particltffs;-
The cmrgantic affliime is sseleert-ed frcM" ethyiERe rfiassjine^ diietfhyleirje
triaffiairpCj, tTri©-fc!hya"jrae tetTra"ine¥ diethaoolamuine and tirietihtanol™
amiinie,.
Further,, ttits? fuel fus^wd in ttwe- piresesntt invention is Eelectedl from
xylose, cBluotKSie,, fructose,, SR.ntcro!Si"f hydrolyzed stanch, sorbitol
and! majTfiitcei-
The follewingi ftamitssiized a"ffl?t"l nolybdates csnt be prepared by the

™ 3 ™" ¦aforesaid process s
i . irtetaS. gKCTlyJh?dat©s
a- tABtoOJ 1 hawing a particle size erf 20 to 100 nsfc, wfoer-ffi CA = I Ca" SrB Bsw ZITBB OUI¥ Mi, CO and miixtuVeSf) j
to, iTA 4CMo© ) 3 tawimfg a particle si2:e of S0 120 oi"5 *#3iB!r# (A Smv Eu, PIT,, Nfd,, Py, H!o, SSd; astrad msixtiuiresK
EXAfHSPLE i - CaimoO
4
Frvehly preparedl 1 malm CsJJUoO wss dissoivect in a mixtuire of 1-2
4 mole etttylene "Sia"£ne -^etirascetic: acid asrad 3 mole oif diettsylene
trftamirme iirn aa^uiecmts nKdiuna *m& t*"e total voluw ns 1.5 Itr.. In this. sni>;t8iirett 1 feiol© sius:r*ose Mas addc"l sanid water MSSS addled so that the total woUo/nte became 2 Itris--. In this mixture, 0-CK5 mole PVA emas addled S?K 103K w/v ssijuaeouss osolution.. The resultirir^ solution were th©int ewaporatffl>"jt by heastio^- At tflrne time of evaporation^ the nitrates werre decoaposeofl amwJ ibrewsrs fumes wf rsitrs^eira dioxxdle giss was ewolwed- After conplete (evaporation,, HI vraluminouts fluffy
organic: fcss^ed! pir®cuirsoir prawdeir resulted. THiis jptrec:ursor
o powder- ons CEsIcS.m)i3;tJi.{aa at 5SSS!! C "for- 2 fen^s-, pr-oduc©d CaBicsO powder
4 witlhi av(£?ris^fe patirtisile siz© less than TS r%m-

-4-
WE CLAIM:
1. A process for the preparation of nanosized metal molybdate particles
comprising.
refluxing pure metal molybdate in the EDTA salt of amines in aqueous medium to make a homogeneous solution, the mole ratio of metal molybdate: EDTA: organic amine being 1:1 to 4:1 to 4 mixing the said homogeneous solution with fuel and minor amount of polyvinyl alcohol (PVA) to obtain a homogeneous mixture in aqueous medium, the mole ratio of metal molybdate : fuel:: PVA is 1:1 to 4:0.5 to 4;
drying or spray drying (he said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass;
calcining the said carbonaceous mass at a temperature range depending on the chemical nature of the system to produce the dried nonosized particles;
2. The process as claimed in claim 1 wherein the homogeneous mixture is
dried or spray dried at a temperature In the range of 100 to 180 °C to
obtain a carbonaceous mass.
3. The process as claimed in claim 1 wherein the carbonaceous mass is
calcined at a temperature in the range of 200 to 600 °C.
4. The process as claimed in claim 1 wherein the organic amine is selected
from ethylene dfamine, diethylene trlamine, trtefhytene tetramine,
diethanolamine and triethanoiamine.

-5-
5. The process as claimed in claim 1 wherein the fuel used is selected from
xylose, glucose, fructose, sucrose, hydrolysed starch, sorbitol and manitol.
6. The process as claimed in claim 1 wherein the nanosized metal molybdate
particles have a size in the range of 20 to 120 nm.
7. The process as claimed in claim 1 wherein the nanosized metal motybdate
particles have a size in the range of 20 to 100 nm.
A process for the preparation of nanosized metal molybdate particles comprising.
refluxing pure metal molybdate in the EDTA salt of amines In aqueous medium to make a homogeneous solution, the mole ratio of metal molybdate: EDTA: organic amine being 1:1 to 4::1 to 4 mixing the said homogeneous solution with fuel and minor amount of polyvlnyl alcohol (PVA) to obtain a homogeneous mixture in aqueous medium, the mole ratio of metal mofybdate : fuel:: PVA is 1:1 to 4:0.5 to 4;
drying or spray drying the said homogeneous mixture by simple evaporation to obtain fluffy carbonaceous mass;
calcining the said carbonaceous mass at a temperature range depending on the chemical nature of the system to produce the dried no nosized particles;

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Patent Number

206369

Indian Patent Application Number

01660/CAL/1998

PG Journal Number

17/2007

Publication Date

27-Apr-2007

Grant Date

27-Apr-2007

Date of Filing

17-Sep-1998

Name of Patentee

INDIAN INSTITUTE OF TECHNOLOGY

Applicant Address

KHARAGPUR 721, INDIA

Inventors:

#	Inventor's Name	Inventor's Address
1	PROF P PRAMANIK	DEOARTMENT OF CHEMISTRY, INDIAN INSTITUTE OF TECHNOLOGY KHARAGPUR 721 302, INDIA

PCT International Classification Number

C22B/11/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA