2024年3月15日发(作者：)

Vol.42

高等学校化学学报

CHEMICALJOURNALOFCHINESEUNIVERSITIES

2021年5月

1589~1597

No.5

doi：10.7503/cjcu20200303

原位限域生长策略制备有序介孔碳负载的

超小MoO

3

纳米颗粒

王常耀，王帅，段林林，朱晓航，张兴淼，李

（复旦大学化学系,上海200433）

摘要采用原位限域生长策略制备了一系列有序介孔碳负载的超小MoO

3

纳米颗粒复合物(OMC-US-MoO

3

).其

伟

中,有序介孔碳被用作基质来原位限域MoO

3

纳米晶的生长.依此方法制备的MoO

3

纳米晶具有超小的晶粒尺

寸(<5nm),并在介孔碳骨架内具有良好的分散度.制得的OMC-US-MoO

3

复合物具有可调的比表面积(428~796

m

2

/g)、孔容(0.27~0.62cm

3

/g)、MoO

3

质量分数(4%~27%)和孔径(4.6~5.7nm).当MoO

3

纳米晶的质量分数为7%

表现出优异的环辛烯选择性氧化性能.

关键词有序介孔碳；氧化钼纳米晶；纳米材料；限域生长

中图分类号O611.4文献标志码A

时,所得样品OMC-US-MoO

3

-7具有最大的孔径、最小的孔壁厚度和最规整的介观结构.该样品作为催化剂时,

InsituConfinementGrowthStrategyforOrderedMesoporousCarbon

SupportUltrasmallMoO

3

Nanoparticles

WANGChangyao，WANGShuai，DUANLinlin，ZHUXiaohang，

（DepartmentofChemistry，FudanUniversity，Shanghai200433，China）

ZHANGXingmiao，LIWei

*

Abstract

，aseriesoforderedmesoporouscarbonsupportultrasmallmo⁃

lybdenananoparticles（OMC-US-MoO

3

）compositeswassynthesizedthroughaninsituconfinementgrowth

dmesoporouscarbonwasusedasthematrixtoinsituconfinethegrowthofMoO

3

nanocrystals.

TheobtainedMoO

3

nanocrystalsshowultrasmallparticlesizes（<5nm）andexcellentdispersityonthemeso-

m

2

/g），porevolumes（0.27―0.62cm

3

/g），MoO

3

contents（4%―27%，massfraction）anduniformporesizes

ainedOMC-US-MoO

3

exhibitstunablespecificsurfaceareas（428―796

（4.6―5.7nm）.Asatypicalexample，theobtainedsamplewith7%MoO

3

（denotedasOMC-US-MoO

3

-7）

showsthelargestporesize，ingused

asacatalyst，theOMC-US-MoO

3

-7exhibitsanexcellentcatalyticactivityforselectiveoxidationofcyclooctene

withahighstability.

KeywordsOrderedmesoporouscarbon；MoO

3

nanocrystal；Nanomaterials；Confinementgrowth

UltrasmallparticlesizesandexcellentdispersityoftheMoO

3

activespeciesonsupportmajorly

收稿日期：2020-05-28.网络出版日期：2020-09-24.

基金项目：国家自然科学基金(批准号:21975050)、国家重点研发计划纳米科技重点专项(批准号:2016YFA0204000,

2018YFE0201701)和中国博士后科学基金(批准号:2019M651342)资助.

联系人简介：李伟,男,博士,教授,主要从事介孔材料的合成及应用研究.E-mail:*******************.cn

1590

高等学校化学学报

Vol.42

2］

maceuticalintermediates，etc.

［1，

.Catalyticepoxidationofolefinisoneoftheessentialroutetoproduceepo-

Epoxides，animportantindustrialchemicals，hasbeenwidelyusedinthefieldsoffoodadditives，phar⁃

xides，whidofcatalyst

llcatalysts，preciousmetalofgoldbasedoneillustrates

4］

highactivityforolefinepoxidations

［3，

.However，goldislimitedresourceandveryexpensive，eventhoughit

enumoxide（MoO

3

），asoneofthelowcost，non-toxicandenviron⁃

mentallybenigntransitionmetaloxides，iswidelyusedasheterogeneouscatalysisforFriedel-Craftsalkyla⁃

7］9］

tion

［5］

，hydrogenationreaction

［6，

，epoxidationreaction

［8，

，hydrogenevolutionreaction

［10］

，electrochemical

16］

byseveralgroupswhichhavehighactivityforepoxidationofolefinsinrecentyears

［15，

.

12］14］

energystorageforlithium-ionbatteries

［11，

，andgassensors

［13，

，etc..Gratifyingly，MoO

3

hasbeenreported

ertiesforapplication

［17~20］

.However，thesynthesisandreactionprocessofteneasilycausesserioussintering，

migrationandagglomerationoftheMoO

3

nanoparticles，⁃

hasbeenwidelyusedasanoutstanding

matrixtocontrolthesizeanddispersityofsupportedmetaloxidesattributingtoitsadvantagesofintrinsical

chemicalinertness，highthermalstability，non-toxicandwide-sources

［21~23］

.Molybdenasupportedcarbon

Chengroup

［26］

fabricatedγ-Fe

2

O

3

@C@MoO

3

core-shellstructurednanoparticlesasamagneticallyrecyclable

ItisobviousthatthesizeandmorphologyofMoO

3

activespeciesarecriticalfactorsthataffecttheirprop⁃

25］

havebeenreportedandshowexcellentperformanceasthecatalystforcycloocteneepoxidation

［24，

.Recently，

tedcarbonlayerplayanefficientroleforthestabiliza⁃

rgroup

［8］

alsoreportedacarbonmicrospheres-supportedmolybdenananoparticles

supports，especially，mesoporouscarbonhavebeenreportedonmanycatalyticareas

becauseofitslargesurfacearea，porevolumeandporesize，whichcannotonlyimprovetheloadcapacitybut

lentdispersity.

cr，above-mentionedcatalysts

alsoenlargethereactionprogress，wherethediffusionprocessmaybetherate-limitingstep

［26~28］

.Uptonow，

itisstillurgenttofabricatemesoporouscarbonsupportedMoO

3

catalystwithultrasmallparticlesizeandexcel⁃

MoO

3

）strategy，theorderedmesoporouscarbon

Herein，weconstructanorderedmesoporouscarbonsupportultrasmallMoO

3

nanoparticles（OMC-US-

worksasamatrixtoinsituconfinethegrowthofMoO

3

ainedMoO

3

nanocrystalsshow

（massfraction）ofMoO

3

canbetunedfrom4%to27%.TheobtainedOMC-US-MoO

3

showstunablespecific

ultrasmallparticlesize（<5nm）tent

surfaceareas（428―796m

2

/g），porevolumes（0.27―0.62cm

3

/g）anduniformporesize（4.6―5.7nm）.As

MoO

3

-7exhibitsanexcellentcatalyticactivityforselectiveoxidationofcyclooctenewithahighstability.

atypicalexample，theobtainedsamplewith7%MoO

（

）showslargestporesize，

3

denotedasOMC-US-MoO

3

-7

ingusedasacatalyst，theOMC-US-

1Experimental

1.1

PluronicF127（EO

106

PO

70

EO

106

，M

w

=12600）erschemicalswere

Indetailsynthesisprocedure，1.0gofPluronicF127powderswasaddedinto10.0gofethanolsolution

SynthesisofOrderedMesoporousCarbonSupportUltrasmallMolybdenaNanoparticles

ChemicalsandMaterials

zedwaterwasusedinallexperiments.

1.2

andstirredtoahomogeneousclearsolutionat40℃.Afterwards，5.0gof20%（massfraction）preformed

No.5

王常耀等：原位限域生长策略制备有序介孔碳负载的超小MoO

3

纳米颗粒

1591

phenolicresinsethanolsolutionand1.0mLofperoxomolybdenumprecursorsolutionwereaddedintotheho⁃

mogeneoussystem（5—200mg/mL）.Thepreformedphenolicresinswassynthesizedbasedonthereported

28］

method

［27，

.Peroxomolybdenumprecursorsolution

［29］

waspreparedbydissolvingdifferentcontentsofmolyb⁃

denumtrioxideinto10.0mLof30%turesolutionwaspouredintodishesafter2h

andthenthedisheswereheattreatedat40and100℃for8and20h，respectively，formingtheas-madecom⁃

positesconsistingofPluronicF127，phenolicresins，andMospecies（denotedasas-madesample）.Then，the

calcinationofas-madesamplewasimplementedinatubularfurnaceunderN

2

perature

1℃/min，ainedsampleafterpyrolysiswasnamedasorderedmesoporouscarbon

ofMoO

3

.

1.3ActivityTest

supportultrasmallmolybdenananoparticles（OMC-US-MoO

3

-x），whereinxrepresenttheactualmassfraction

Theselectiveoxidationreactionofcyclooctenewascarriedoutintheround-bottomflask（50mL）.In

programwassetfrom25℃to350℃witharampof1℃/min，maintenancefor3h，andthento600℃with

which，40.0mmolofcyclooctene，40.0mmolof5.5mol/LTBHPindecane，10mgofOMC-US-MoO

3

-7cata⁃

lyst（0.0048mmol/LofMoO

3

），6.0gof1，2-dichloroethaneassolvent，and15.0mmolofchlorobenzeneas

ctiontemperatureis80℃.Atdifferenttimeintervals，conversionwascalculatedby

alystwasreusedafterwashingbywaterand

tconditionwaskeptsametothefirsttimeonthecyclictest.

pleswereanalyzedonanAgilent7890AgaschromatographequippedwithaHP-5column

ues（molofreactedcyclooctenepermolofcatalystandhour）

2ResultsandDiscussion

2.1

Thedevelopedinsituconfinementgrowthstrategyisemployedtothepreparationoforderedmesoporous

SynthesisandCharacterizaiton

carbonsupportultrasmallmolybdenananoparticles（OMC-US-MoO

3

）composites（Fig.1）.Inthesynthesissys⁃

tem，PluronicF127isusedasthestructure-directingagent（soft-template），preformedphenolicresinsisused

ascarbonresource，peroxomolybdenumsolutionisusedasprecursor，andethanol/H

2

Oisusedasco-solvent，

-madesampleandproductOMC-US-MoO

3

compositescanbeobtainedafterheat-treatment

at100and600℃，scontentofMoO

3

intheOMC-US-MoO

3

compositescanbewell

tunedthroughadjustingtheamountofperoxomolybdenumprecursorinthesynthesissystem.

Fig.1IllustrationoftheconstructionofOMC⁃US⁃

MoO

3

compositesviatheinsituconfinement

growthstrategy

Fig.2TGAcurvesoftheOMC⁃US⁃MoO

3

composites

withdifferentMoO

3

contentsobtainedafter

pyrolysisat600℃,respectively

MassfractionofMoO

3

(%):a.4;b.7;c.10;d.16;e.27.

TGAcurves（Fig.2）showthatthemassfractionsofMoO

3

speciesintheOMC-US-MoO

3

compositesare

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高等学校化学学报

Vol.42

4%，7%，10%，16%and27%（Table1），respectively，whenadjustingtheamountofmolybdenumprecursors

slossbelow100℃iscausedbythevolatilizationofadsorbedwaterinthe

tmassincreasementcanbedetectedbetween100and300℃，demonstratingtheexistence

oftraceamountofMoO

2

andabundantMoO

3

sincreasementcanbeattributedtothe

tothemassfractionofMoO

3

speciesinthecomposites.

SampleNo.

1

2

3

4

5

MoO

3

content（%，massfraction）

4

7

10

16

27

oxidationofthetraceamountMoO

2

.Subsequently，thehugemasslossabove300℃canbeobservedattribu-

slossbetween100and600℃isapproximate

Table1StructuralandtexturalparametersforOMC-US-MoO

3

withdifferentcontent

S

BET

（/m

2

·g

-1

）

796

693

652

574

428

V（/cm

3

·g

-1

）

0.62

0.54

0.49

0.41

0.27

D/nm

4.7

5.7

5.5

5.4

4.6

diffractionpeaksat0.391and0.782nm

−1

，and0.412and0.824nm

‒1

，respectively，indexingtothe（100）

and（200）eincreasementofMoO

3

content，theqvaluesofthe（100）diffractionpeaksshiftto0.532，0.617，and0.678nm

−1

，forsamples

tersoffivecompositesarecalculatedtobeabout18.5，17.6，13.6，11.7，and10.7nmwiththeincreased

MoO

3

content，atterns［Fig.3（B）］offivecompositesallshownodiffractionpeaksof

ultrasmallsizeevenatahighMoO

3

contenteffectively.

demonstratesthattheorderedmesoporouscarbonframeworkscanconfinethesizeofMoO

3

nanocrystalstoan

OMC-US-MoO

3

-10，OMC-US-MoO

3

-16，andOMC-US-MoO

3

-27，respondingcellparame⁃

MoO

3

phase，suggestingtheultrasmallparticlesizeofMoO

3

sult

TheSAXSpatterns［Fig.3（A）］ofOMC-US-MoO

3

-4andOMC-US-MoO

3

-7compositesshowtwoscattering

Fig.3SAXS(A)andWA⁃XRD(B)patternsoftheOMC⁃US⁃MoO

3

compositeswithdifferent

MoO

3

contentsobtainedafterpyrolysisat600℃

MassfractionofMoO

3

(%):a.4;b.7;c.10;d.16;e.27.

600℃inN

2

alldisplayrepresentativetype-ⅣcurveswithH2hysteresisloops［Fig.4（A）］，inagreementwith

thepreviouslyreportedorderedmesoporousmaterials

［30~32］

.Sharpcapillarycondensationstepsintherelative

nauer-Emmett-Teller（BET）surfaceareaandporevolumeoffivecompositesarecalculatedand

pressure（p/p

0

）of0.41―0.70areobservedforfivecomposites，demonstratingthenarrowporesizedistribu⁃

faceareaandporevolumedecreasewiththeincreasedMoO

3

content，whichcanbe

rageporesizesoffivecompositesare

alsocalculatedandlistedonTable1fromtheirporesizedistributioncurve［Fig.4（B）］derivedfromthe

rageporesizesare4.7，5.7，5.5，5.4，and4.6nm，

Nitrogenadsorption-desorptionisothermsoffiveOMC-US-MoO

3

compositesobtainedaftercalcinedat

No.5

王常耀等：原位限域生长策略制备有序介孔碳负载的超小MoO

3

纳米颗粒

1593

Fig.4N

2

adsorption⁃desorptionisotherms(A)andporesizedistributions(B)oftheOMC⁃US⁃MoO

3

compositeswithdifferentMoO

3

contentsobtainedafterpyrolysisat600℃

MassfractionofMoO

3

(%):a.4;b.7;c.10;d.16;e.27.

ingtothecellparametersresults，theporewallsoffivecompositesarecalculatedtobe

14.1，11.9，8.1，6.3，and6.1nm，respectively.

y，theregular［100］and［110］directionscanbeclearobservedfromtheSEMimages

SEMimages（Fig.5）showthatOMC-US-MoO

3

-4andOMC-US-MoO

3

-7compositesownthemostregular

ofOMC-US-MoO

3

-7composites［Fig.5（B）and（F）］.Inaddition，themesoporesareopenedandnoobvious

alongthe［100］and［110］directionsmanifestawell-defined2Dhexagonalmesostructuresinagreementwith

rtherincreasementofMoO

3

content，thereg⁃

gesofOMC-US-MoO

3

-7composites［Fig.6（A）—（C）］taken

theresultoftheSAXSpattern［Fig.2（A）］.Thelatticespacingismeasuredtobe0.35nmfromtheHRTEM

image［Fig.6（D）］，attributingtothe（040）crystallineplanesofα-MoO

3

［33］

.TheaveragesizeofMoO

3

nano⁃

US-MoO

3

-7compositesshowsthepresenceofonlyMo，OandCelements［Fig.7（A）］.Thehigh-resolution

stratingtheco-existenceofMo

4+

andMo

6+

species

［34~36］

.TheratioofMo

4+

/Mo

6+

iscalculatedtobeabout13%.

OnlyafewMo

4+

signalscanbedetectedfromthespectrum，inagreementwiththeTGAresults.

Mo

3d

corelevelXPSspectra［Fig.7（B）］showfourpeaksat230.5，232.7，233.6，and235.9eV，demon⁃

crystalsisestimatedtobe（4.1±1.0）veyspectrumoftheOMC-

Fig.5SEMimagesofOMC⁃US⁃MoO

3

compositeswithdifferentMoO

3

contentsobtainedafter

pyrolysisat600℃

MassfractionofMoO

3

(%):(A)4;(B)7;(C)10;(D)16;(E)27.

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高等学校化学学报

Vol.42

Fig.6

Viewedalongthehexagonal（A）andcolumnar（B，C）directionsandHRTEMimage（D）ofarepresentativeMoO

3

nanoparticle.

TEMimagesofOMC⁃US⁃MoO

3

⁃7compositesobtainedafterpyrolysisat600℃

Fig.7SurveyXPSspectrum(A)andhigh⁃resolutionXPSspectraofMo

3d

(B)forOMC⁃US⁃MoO

3

⁃7

compositesobtainedafterpyrolysisat600℃

2.2

impactontheformationoffinalOMC-US-MoO

3

ainedMoO

3

nanocrystalsshowultrasmall

retainedeventhemassfractionofMoO

3

isincreasedto27%.However，theregularmesostructurescanbe

talscanbedetectedfromsamplesobtainedafterpyrolysisat600℃，theunregularmesostructurescanbe

attributedtotheuncontrollableoriginco-assemblyprocess.

2.3SelectiveOxidationofCyclooctene

Theselectiveoxidationreactionofcyclooctenewithhighcatalyticperformanceandstabilityisstillhighly

Basedontheaboveresults，weproposethattheinsituconfinementgrowthstrategyshowsignificant

FormationMechanismStudies

particlesize（<5nm）ructurecanbe

partialdestroyedwiththeincreasedMoO

3

ingtotheresultsthatnolargeMoO

3

nanocrys⁃

r，thestabilityofactivenanoparticlesincatalyticreactionisamajorchallenge，especiallyfor

case，theOMC-US-MoO

3

-7compositesshowmostregular

werecarriedoutusing1，2-dichloroethaneassolventinflaskwithchlorobenzeneasinternalstandardat80℃.

mesostructures，largestporesizes，appropriateholewallsize，MoO

3

，theobtained

OMC-US-MoO

3

-7comctions

TheOMC-US-MoO

3

-7compositescatalystshowsahighTOFvalueof2163h

‒1

whichiscalculatedonthebasis

（>99%）to1，isonwiththereportedheterogeneous

ile，ahighconversion（100%）ofcyclooctene，andselectivity

sentOMC-US-MoO

3

-7catalystshows

No.5

王常耀等：原位限域生长策略制备有序介孔碳负载的超小MoO

3

纳米颗粒

1595

ahigherTOFvaluethanMoO

3

/C

［8］

，MoO

3

/SiO

2

［37］

，Mo-MOFs

［9］

，Mo-MCM-41

［38］

，Mo-SBA-15

［38］

，［Pipera⁃

［39］

zinCH

2

｛MoO（）｝］，andMNP

30

-Si-inic-Mo

［40］

ldbenotedthatcyclooc⁃

2

Salen

n

tenestillgaveabout18%conversion［Fig.8（A）］intheabsenceofcatalystowingtothepresenceofstrong

42］

TBHPoxidants，whichisconsistentwithpreviousreports

［41，

.Further，twoothersubstrates，cyclohexene

andstyrenewerealsotestedunderthesameconditionstotesttheversatilityofOMC-US-MoO

3

-7asanepoxida⁃

singly，theconversionofcyclohexeneto1，2-epoxyclohexanecanreach54%

portingInformationofthispaper）.

Table2

OMC

-

US

-

MoO

3

-

7

MoO

3

/C

MoO

3

/SiO

2

Mo

-

MOFs

Mo

-

MCM

-

41

［PiperazinCH

2

｛MoO（）｝］

2

Salen

n

MNP

30

-

Si

-

inic

-

Mo

*

Mo

-

SBA

-

15

Catalyst

addition，theconversionofstyrenetostyreneoxidecanreach95%in36h，respectively（Fig.S1，seetheSup⁃

CalculatingTOFvalueforepoxidationofcycloocteneandcomparingwithothercatalysts

*

Time/h

2

2

6

7

3

12

24

3

Conv.（%）

52

80

90

93

97

99

95

46

Epoxidesel.（%）

>99

100

100

99

95

93

100

98

TOF/h

-1

2163

［8］

53

［9］

270

［36］

22

［36］

40

［37］

16

［38］

2

［35］

72

halfconversionofthereaction.

.TOFvalues(molofreactedcyclooctenepermolofcatalystandhour)werecalculatedatabout

Fig.8Timecourseplotsofcycloocteneepoxidation(A)andreusability(B)byusingOMC⁃US⁃MoO

3

⁃7com⁃

positesascatalyst

Reactionconditions：40.0mmolofcyclooctene，40.0mmolof5.5mol/LTBHPindecane，10mgofOMC-US-MoO

3

-7

catalyst（0.0048mmol/LofMoO

3

），6.0gof1，2-dichloroethaneassolvent，and15.0mmolofchlorobenzeneasinternal

ctiontemperatureis80℃.

tant，，thehotfiltrationtestwasusedtoassessthepresenceof

BesidetheefficientconversionofcatalystandhighTOFvalues，thestabilityofcatalystisalsoveryimpor⁃

ereactionlastedfor2h，weremovedthecatalystbyhotfiltrationand

ultsshowedthattherewasonlyaslightincreaseincon⁃

version［Fig.8（A）］，recyclingstudy，cycloocteneepoxida⁃

tionwasperformedmaine

catesthatultrasmallMoO

3

nanoparticlessupportedonorderedmesoporouscarbonishighlystableandcanbe

reused，demonstratesitspotentialforindustrialapplications.

clearlyfoundthatobviouschangesareundetectedforcatalyticperformanceafterfiveruns［Fig.8（B）］.Itindi⁃

Thehighconversion，selectively，andtheTOFvalueforthecycloocteneepoxidationreactioncanbe

attributedtotheuniquestructureoftheOMC-US-MoO

3

-hsurfacearea，volume，and

1596

高等学校化学学报

Vol.42

uniformmesoporescannotonlyenrichmentthereactionsubstratebutalsoinfavortothediffusionofsub⁃

rasmallMoO

3

nanocrystalssizeanditsexcellentdispersityintheframeworkscanexposemore

lyandconversion.

sefeaturesarebeneficialtotherapidconversionofsubstratemolecularwithhighselective⁃

3Conclusions

rouscarbonsupportultrasmallmolybdenananoparticles（OMC-US-MoO

3

）dmesoporous

tion，aseriousofOMC-US-MoO

3

compositecanbeobtainedwithcontrollablespecificsurface

uniformporesize（4.6―5.7nm）.ThemesostructurescanberetainedeventheMoO

3

contentashighas27%.

Insummary，aninsituconfinementgrowthstrategywasdevelopedtotheconstructionoforderedmesopo⁃

carbonwasusedasaneffectivematrixtoinsituconfinethegrowthofMoO

3

ainedMoO

3

nanocrystalsshowultrasmallparticlesize（<5nm）andexcellentdispersityonthemesoporouscarbonframe⁃

areas（428―796m

2

/g），porevolumes（0.27―0.62cm

3

/g），MoO

3

contents（4%―27%，massfraction）and

Asatypicalexample，theobtainedsamplewith7%MoO

3

（denotedasOMC-US-MoO

3

-7）showslargestpore

tenewithahighstability.

size，ingusedasacatalyst，the

OMC-US-MoO

3

-7exhibitsanexcellentcatalyticactivity（2163h

−1

forTOF）forselectiveoxidationofcyclooc⁃

SupportingInformation:/CN/10.7503/cjcu20200303.

nalKeyResearchandDevelopmentProgramofChina（Nos.2016YFA0204000，2018YFE0201701）andChina

PostdoctoralScienceFoundation（No.2019M651342）.

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