research article preparation and characterization of cetyl...

Research ArticlePreparation and Characterization of Cetyl TrimethylammoniumIntercalated Sericite

Hao Ding1 Yuebo Wang1 Yu Liang1 and Faxiang Qin2

1 Beijing Key Laboratory of Materials Utilization of Nonmetallic Minerals and SolidWastes National Laboratory of Mineral MaterialsSchool of Materials Science and Technology China University of Geosciences Beijing 100083 China

2 1D Nanomaterials Group National Institute for Materials Science 1-2-1 Sengen Tsukuba Ibaraki 305-0047 Japan

Correspondence should be addressed to Hao Ding dinghaocugbeducn

Received 15 August 2014 Accepted 16 October 2014 Published 24 November 2014

Academic Editor Peter Majewski

Copyright copy 2014 Hao Ding et alThis is an open access article distributed under theCreativeCommonsAttribution License whichpermits unrestricted use distribution and reproduction in any medium provided the original work is properly cited

Intercalated sericite was prepared by intercalation of cetyl trimethylammonium bromide (CTAB) into activated sericite through ionexchange with the following two steps the activation of sericite by thermal modification acid activation and sodiummodificationthe ion exchange intercalation of CTA+ into activated sericite Effects of reaction time reaction temperature CTAB quantitykinds of medium and aqueous pH on the intercalation of activated sericite were examined by X-ray diffraction (XRD) analysisFourier transform infrared (FT-IR) spectroscopy differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA)The results indicated that the CTA+ entered sericite interlayers and anchored in the aluminosilicate interlayers through strongelectrostatic attractionThe arrangement of CTA+ in sericite interlayers was that alkyl chain of CTA+mainly tilted at an angle about60∘ (paraffin-type bilayer) and 38∘ (paraffin-type monolayer) with aluminosilicate layers The largest interlayer space was enlargedfrom 09 nm to 52 nmThe intercalated sericite could be used as an excellent layer silicate to prepare clay-polymer nanocomposites

1 Introduction

Clay-polymer nanocomposites prepared by intercalation ofpolymers into the interlayer space of phyllosilicates haveattracted much attention for their remarkable improvementsin material properties as compared with virgin polymersor conventional microcomposites andmacrocompositesTheimprovements include high moduli increased strength andheat resistance decreased gas permeability and flammabilityand increased biodegradability of biodegradable polymers[1ndash3] Clay-polymer nanocomposites have a wide scale ofapplications in a range of key areas such as aerospaceautomobile appliance and electronics waste water treatment[4 5] Focusing on the structure of clay-polymer nanocom-posites they can be classified as intercalated nanocompositesand exfoliated nanocomposites The silicate layers in theformer are not fully separated but presented ordered layeredstructure compared with the latter [4] According to thestrength of interfacial interactions between the polymermatrix and layered silicate clay-polymer nanocomposites canalso be divided into three types namely (a) intercalated

nanocomposites polymer matrix insert into layered silicatein crystallographically regular way regardless of the ratio oflayered silicate to polymer (b) flocculated nanocompositesthey are almost similar to intercalated nanocomposites exceptfor the silicate layers that are flocculated sometimes dueto their hydroxylated edge-edge interaction (c) exfoliatednanocomposites the individual layers are separated into acontinuous polymer matrix with average distances [1]

According to the number and the ratio of sheets in afundamental structural layer the existing cation substitutionsin the octahedrons and tetrahedrons and the resulting chargeof the layers the crystalline clay minerals are classifiedinto seven groups [5 6] The common phyllosilicates usedfor preparation are 2 1 type (montmorillonite vermiculiteand mica) and 1 1 type (kaolinite) Montmorillonite [7ndash12]and vermiculite [13ndash19] have been mostly investigated asadsorbents for wastewater treatment because of its swellingbehavior and excellent ion exchange property Isomorphoussubstitution within silicate layers is responsible for the pres-ence of exchangeable cations within the interlamellar region[6 20] Phyllosilicates are characterized by moderate surface

Hindawi Publishing CorporationAdvances in Materials Science and EngineeringVolume 2014 Article ID 480138 8 pageshttpdxdoiorg1011552014480138

2 Advances in Materials Science and Engineering

Table 1 Chemical composition of the original sericite

Composition SiO2 Al2O3 Fe2O3 TiO2 K2O Na2O CaO MgO SO3 LOI TotalContent (mass ) 4571 2832 304 035 809 071 010 212 0075 447 99555

charge known as the cation exchange capacity (CEC) Thischarge is not locally constant but varies from layer to layerand must be considered as an average value over the wholecrystal [1 21] while excessive CEC will lead to the instabilityof interlayer cation and could not serve as the excellentmatrixmaterials for cation modification

Comparing with other clay minerals sericite holds theadvantages of high moduli stable chemical property highelectrical insulation good ultraviolet ray resistance and soforth [22ndash24] Its structure consisted of layers made up of twoSiAl tetrahedral sheets and a sandwiched octahedral sheetfilled with Al3+ and K+ (mainly) in interlayer It also belongsto 2 1 phyllosilicates however there are a few distinct differ-ences as compared with montmorillonite and vermiculite [525 26] It does not swell in water and hardly has ion exchangecapacity and intercalation property because of its high layercharge producing pretty strong electrostatic force [27] Thedifficult preparation based on sericite explains the lack ofliterature concerning the intercalation or exfoliation of micagroups compared with montmorillonite and vermiculite

Intercalated sericite is important to serve as potentialsorbents in the removalspeciation of various pollutantsin the waste waters and perhaps emerged as a new areaof research in the waste water treatment technologies [2829] Cetyltrimethylammonium bromide (CTAB) a typicalcationic surfactant is often used in the modification of clayto increase to adsorption of matrix and also presents heat-resistant acid and alkali resistance and bactericidal activityThe treatment and activation of sericite increased the quantityof exchangeable cations and the organic modification ofsericite made the preparation of clay-polymer nanocompos-ites based on sericite easier To do this here we proposedthree steps first activating the structure of sericite to make ithave more exchangeable cations and intercalation propertiessecond modifying layered structure of sericite by cationsurfactant such as CTAB third intercalating polymer intoorganic sericite interlayers to exfoliate entirely or partly itslayers

In this paper sericite was activated by thermal modi-fication acid activation and sodium modification and theintercalated sericite was prepared by the intercalation of cetyltrimethylammonium ions (CTA+) into activated sericiteReaction time temperature quantity of intercalation agentreaction medium and pH on intercalation were discussed insericite intercalation

2 Materials and Methods

21 Materials The original sericite (S0) was obtained from

Anhui Province China whose mean size was about 10 120583mThe chemical composition of S

0was listed in Table 1 Cetyl

trimethylammonium bromide (CTAB) with a purity of 99

was provided by Xilong Chem Co China which was usedas cation surfactant

22 Preparation The original powder (S0) was heated at

800∘C in muffle furnace for 1 h The resulting product (S1)

was stirred with nitric acid of 5molL at 95∘C in thermostaticwater bath for 4 h and the product was washed till pH = 7Then the powder (S

2) was reacted with NaCl supersaturated

solution at 95∘C for 3 h and the product was washed andfiltrated till without Clminus (tested by AgNO

3) Finally the

activated sericite (S3) was obtained after drying process

Subsequently a certain amount of S3and the surfactantCTAB

were dispersed in distilled water respectively The mass ratioS3water was 3100 After mixing the dispersion of S

3and

CTAB solution (by magnetic stirring) the dispersion washeated to 80∘C for 24 h and pH was adjusted to neutral andweak acid with HNO

3 And then the turbid liquid was laid

aside for 2 h After that the product was washed with distilledwater (room temperature) till Brminus removed effectively (testedby AgNO

3) The final product (CTA-S) was dried at 80∘C

23 Characterization The X-ray diffraction patterns wereobtained on a Rigaku Rotaflex X-ray powder diffractometeremploying Cu K120572 radiation 40 kV and 100mA The X-raydiffraction (XRD) patterns in the 2120579 range from 1∘ to 10∘ werecollected at 05∘min Middle-infrared transmission spectra(500ndash4000 cmminus1) were collected using a Nicolet Magna-IR750 Fourier transform infrared spectrometer equipped witha Nicolet NicPlan IR Microscope operated with a spectralresolution of 4 cmminus1 Simultaneous collecting DSC and TGAsignals was carried out using a SDTQ600 analyzer (from TAthe US) under air flow and heating the samples from roomtemperature to 1100∘C at 10∘Cmin Mass of the samples wasabout 5mg

Sericite does not belong to the clay minerals in thenarrow sense but it is a hydratable layered silicate with acertain layer charge especially after activation and structuretransformation Cation exchange capacity can be used asa measure of the activity Ammonium chloride-anhydrousethanol method was used in this experiment to determinethe cation exchange capacity of sericite The pH value wasadjusted to 7 during the measurement

The intercalation rate defined as the rate of diffractionpeak intensities which can reflect the change of interlayerspacing before and after the layered silicate is intercalatedand can be used to evaluate the degree of intercalationreaction The intercalation rate can be expressed as follows[31]

IR =119868119888

(119868119888+ 119868119896) (1)

Advances in Materials Science and Engineering 3

0 10 20 30 40 50 60 70

(002

)

(004

) (006

) 1 2 3 4 5 6 7 8 9 10

2120579 (∘)

S3

S2

S1

S0

Figure 1 XRD patterns of S0 S1 S2 and S

3

where 119868119888is intensity of the diffraction peak reflecting the

extended interlayer spacing of layer silicate layer after inter-calation and 119868

119896is intensity of the diffraction peak reflecting

the unextended interlayer spacing of layer silicate layer afterintercalation

The more the extended layer silicate after intercalationthe less the residual unextended layer silicate As for sericitethe layer spacing is reflected by 119889

002value so the intercalation

rate can be calculated using the intensity of (002) reflection

3 Results and Discussion

31 Characterization of Activated Sericite The intensities ofreflections in Figure 1 decreased and becamewider from S

0to

S3 the reflections corresponding to 2120579moved towards lower

degree and 119889002

-value increased slightly The intensities ofthe reflections of S

0weakened which moved towards lower

2120579 angle region after heat treatment but they were stillsharp and narrow This was because with the increase ofroasting temperature the lattice of sericite absorbed moreenergy and lattice vibration enhanced Therefore sericitewas activated preliminary After reacting with nitric acid thecrystallinity of S

2decreased slightly However the layered

structure still retained judging from its 002 reflection existedIt can be concluded that acid activation made S

1much more

activated in crystal lattice without destroying its structureby high concentration of H+ dissolving part of Al3+ at hightemperature Then S

2reacted with Na+ for ion exchange

whose hydration radius was smaller than K+ and provideda CEC of 056meqg which was much larger than that ofS0 007meqg The relative high cation exchange capacity

contributes to the intercalation modification

32 Effects of Reaction Conditions on Intercalation The basalspacing of S

3was 09 nm When S

3and CTAB (15 times

the CEC of S3) were mixed and stirred at 80∘C for 10 h or

4 h the intercalation of CTAB was not observed distinctlyexcept for some protuberances when 2120579 lt 5∘ (Figure 3(a))which indicated that CTAB entered the interlayer spaceswith an erratic arrange When reaction time was extended to

16 h new basal reflections corresponding to 119889002= 43 nm

(2120579 = 2∘) were observed obviously which suggested thatCTAB entered the interlayer spaces with a regular arrangeMoreover the interlayer spaces of (002) plane were evenpartly enlarged to 52 nm when reaction time was 24 h Theintercalation rate was obtained according to formula (1) Theresults were 60 73 76 and 82 corresponding to thefour times (4 h 10 h 16 h and 24 h) Consequently with theincrease of reaction time more doses of surfactant enteredinterlayer spaces and arranged more regularly

The intercalations at different reaction temperatures wereinvestigated (Figure 3(b)) When temperature was low lackof energy was afforded in the reaction [32] And the intensityof new basal reflection (119889

002) was much weaker than that at

higher temperature as well as the intercalation rate With theincrease of temperature the interlayer spaces became largerHowever it decreasedwhen temperaturewas high up to 95∘Cbecause severe high temperature makes CTA+ too active tobe adsorbed and instead easily to desorbed from interlayerspaces which reduced the tendency for ion exchange

Mechanism of CTA+ intercalation into sericite interlayerscan be described as

119883119899+ndashS + 119899N+ larrrarr 119899N+ndashS + 119883+ (2)

where 119883 is all kinds of inorganic cations taking part in theexchange and N is nitrogen in CTAB

The CTAB quantity should be much larger than it sup-posed to be because of the reversible reaction The rightdirection is beneficial to the intercalation [33]

The result shown in Figure 4(a) is a proof for the suc-cessful intercalation of all the samples with different dosesof surfactant With the increase of the CTAB quantity thereflection intensities of new basal spaces became stronger andstronger and the newbasal spaces became increasingly largerCorresponding to 5 times 10 times 15 times and 20 timesthe CEC of S

3 the intercalation rates were 67 69 82

and 64 respectively When the quantity of CTAB was 15times the CEC of S

3 the value of 119889

002was 52 nm the sharp

and distinct 002 reflection suggested that CTA+ in interlayersarranged more regularly than that of others However theintercalated effect turned badwhen the quantitywas 20 timeswhich was induced by the agglomeration of large quantityof CTAB The agglomeration decreased the dispersity andhindered the intercalation reaction Two kinds of mediumwere considered Figure 4(b) showed that the reflection ofthe sample modified with aqueous solution was sharper andstronger than that with n-butanol A 10 higher intercalatedrate was gained using water as the solvent instead of n-butanol It could be explained by reaction of hydroxy in n-butanol with the interlayer exchangeable cations andor thebroken bonds of the aluminosilicate layers which reduced theodds for ion exchange of interlayer cations with CTA+

The influence of pH value on the intercalation mainlyreflects in the ionization of surfactants The hydrolytic reac-tion CTA+ + H

2O 999445999468 CTA-OH + H+ exists in the reaction

medium According to the equation the addition of H+restrains the reaction and thus produces more CTA+ in thesystem which facilitates the intercalation on the contrary


5120583m

(a)

5120583m

(b)

Figure 2 SEM images of sericite (a) before and (b) after intercalation

2 4 6 8 104h

10h

16h

24h

d = 52nm

d = 43nm

d = 24 nm

2120579 (∘)

(a)

1 2 3 4 5 6 7 8 9 10

d = 52nm

d = 52nm

d = 44nm

d = 24 nm

80∘C

95∘C60∘C

2120579 (∘)

(b)

Figure 3 XRD patterns of CTA-S reaction for different (a) time and (b) temperatures

alkaline environment promotes the hydrolysis resulting inreduced reaction rate From this perspective the acidicenvironment is conducive to the intercalation

Five different pH values of reaction medium wereadjusted to investigate the effect of pH value on the inter-calation effect The results shown in Figure 5 indicated thatsericite was intercalated in neutral and weak acid aquaticsolution When pH value of the reaction medium was 1nearly no new reflection was observed and even the originalpeak almost disappeared which was a proof of an unsuccess-ful intercalation This was because the strong acid destroyedthe structure of sericite thus leading to a poor result ofintercalation In the case of intercalation at pH 4 and 7 S

3

was intercalated well and new basal reflection was obtained(Figure 5) In the alkaline medium (pH 9 and 11) no newbasal reflection appeared and in that the quantity of CTA+was too little to intercalate S

3 though alkaline medium was

benefit for the dispersing of sericite

33 Characterization of Modified Sericite The FT-IR spec-tra of original sericite (S

0) pure CTAB and intercalated

sericite (CTA-S the one preparing at optimal conditions)were given in Figure 6 The spectra of CTA-S (Figure 6(c))showed that two new bands at 2918 cmminus1 and 2849 cmminus1appeared which were assigned to the CH

2asymmetric and

symmetric stretching vibration The band of SindashO stretching

vibration (1024 cmminus1) was wider and weaker than that of S0

(Figure 6(a)) which could be assigned to the appearance ofthe band of CndashN and CndashC bending vibration (962 cmminus1 and909 cmminus1) The band at 720 cmminus1 was diagnostic of linearalkyl chain ndash(CH

2)119899ndash when 119899 gt 4 whose disappearance

after the intercalation of modified sericite indicated thatalkyl chains were in interlayers with a twisted shape WhenCTA+ entered the interlayer of sericite the shape of alkylchain twisted to a certain extent due to the impact of twoadjacent layers It was considered that crook of alkyl chainhad little effect on its length in interlayer According to thereflections in XRD patterns of CTA-S (the topper one shownin Figure 4(b)) and the results mentioned above it couldbe concluded that CTA+ entered sericite interlayer and theintercalation was stable due to the strong electrostatic forcebetween CTA+ and layer

The DSC-TGA curves of S0and CTA-S were shown

in Figure 7 respectively There was only one mass loss inthe TGA curve for S

0at 489 at 1100∘C (Figure 7(a))

according to the DSC curve peak at the same temperatureThis mass loss was attributed to the loss of structural waterof S0 Displayed in thermogravimetric curves of Figures 7(b)

7(c) and 7(d) the mass loss of organic modified sericiteincreased with the increase of the dosage of CTABWhen thedosage of CTAB was 15 CEC the mass loss reached 1361Subtracting the 489 interlayer water contained in sericite


1 2 3 4 5 6 7 8 9 10

5CEC

10CEC

15CEC

20CEC

2120579 (∘)

d = 52nm

d = 45 nm

d = 24 nm

(a)

1 2 3 4 5 6 7 8 9 10

Water

2120579 (∘)

d = 52nm

d = 52nm

d = 25 nm

d = 25 nm d = 10 nmn-Butanol

(b)

Figure 4 XRD patterns of CTA-S reaction with different (a) quantities of CTAB and (b) mediums

2 4 6 8 102120579 (∘)

d = 52nm

d = 25 nm

d = 15 nm

d = 24 nm

pH = 11

pH = 9

pH = 7

pH = 1

pH = 4

Figure 5 XRD patterns of CTA-S reaction with different pH

raw materials it could be considered that 872 of the CTABwas in the sericite As for the DSC of CTA-S there werethree endothermic valleys at 100∘C 200∘Csim250∘C and 900∘Cand two obvious exothermic peaks at 250∘Csim300∘C and250∘Csim400∘C After modification temperature of the firstendothermic valley was slightly lower than the original oneThis change indicated that the CTAB went into the sericiteinterlayer through intercalation Then the sericite slice layersurface transformed from hydrophilic to hydrophobic makesthe adsorption capacity of water molecules weaken andtherefore the desorption temperature of interlayer waterlower

Analysis of FT-IR spectra andDSC-TGAcurves indicatedthat intercalator is inserted into sericite interlayer bymeans ofchemical reaction The maximum intercalation capacity canreach to 872 and firm chemical bond was formed betweenCTAB and sericite layer

4000 3500 3000 2500 2000 1500 1000 500

(c)

(b)

3400

473

962

909CTA-S

CTAB 720

1404

1024

1630

1484

2849

2918

3624

(a)

Wavenumbers (cmminus1)

S0

Figure 6 FT-IR spectra of (a) S0 (b) CTAB and (c) CTA-S

34 Microstructures of Modified Sericite There were twoideas about the arrangement of alkyl chains in interlayersof layered silicates One was that the alkyl chains eitherlay parallel to the aluminosilicate layers forming mono orbilayers or radiate away from the layers forming mono orbimolecular arrangements [34] The other was that as forshort chain lengths the molecules were effectively isolatedfrom each other for medium lengths there is various degreeof disorder in plane and interdigitation between layers forlong lengths interlayer order increased leading to a liquid-crystalline polymer [35] It was also considered that with theincrease of CTAB concentration the tail of CTA+ chain beganto radiate away from the aluminosilicate surface and thehead groups distributed on aluminosilicate layers uniformlyand the chains of CTA+ adopt highly ordered arrangementwith a fully stretched all-trans conformation Furthermoreaccording to the viewpoint of Zhu et al [36] there weresix typical arrangements of alkyl chain in interlayer which


Residue

200 400 600 800 1000

86

88

90

92

94

96

98

100

102 120

Hea

t flow

(nW

)

90

60

30

0

Wei

ght (

)

9511 AT1050∘C4814 mg

81781∘C

86312∘C

3971

69624∘C

minus120

minus90

minus60

minus30

Temperature (∘C)Exo up

(a)

Residue

200 400 600 800 100078

84

90

96

102 118

51

Hea

t flow

(nW

)

Wei

ght (

)

Exo up Temperature (∘C)

minus150

minus83

minus16

21420∘C09311

33319∘C304425917∘C

41898∘C

24695∘C

39391∘C 9303 AT1050∘C6003 mg

2402

(b)

5046

3558

2023

Residue8843 AT

Hea

t flow

(mW

)

200 400 600 800 100070

75

80

85

90

95

100 96

60

24

Exo up

Wei

ght (

)

Temperature (∘C)

minus120

minus84

minus48

minus12

21546∘C

25458∘C

42391∘C

23597∘C

39071∘C

35517∘C 1050∘C6872mg

(c)

Residue8639 AT

200 400 600 800 100060

65

70

75

80

85

90

95

100

105

17

10

3

Exo up

Wei

ght (

)

38

31

24

Temperature (∘C)

minus25

minus18

minus11

minus4 Hea

t flow

(mW

)

950∘C

3788

8549

21419∘C

25010∘C

34271∘C

23761∘C23603∘C

33272∘C

4295mg

(d)

Figure 7 DSC-TGA curves and integral curves of TGA of S0(a) and CTA-S modified by different quantities of CTAB (5 CEC (b) 10 CEC

(c) and 15 CEC (d))

were lateral-monolayer (ldquoLrdquo type and ldquoMrdquo type) lateral-bilayer paraffin-typemonolayer pseudotrilayer and paraffin-type bilayer The contrastive SEM images of sericite before(Figure 2(a)) and after (Figure 2(b)) intercalation indicatedthat the sericite slice layer was partly dispersed and strippedafter intercalation modification The disperse and exfoliateextent were not well-proportioned which corresponded tothe previous analysis results that intercalators distributebetween the layers in a variety of forms

The schematic drawing about the size of CTA+ was shownin Figure 8 By synthesizing the points of views above weillustrate the CTA-S prepared in aqueous (the upper oneshown in Figure 4(b)) as an example

There were five major reflections in its XRD pattern The119889-value according to the first reflectionwas 52 nmwhich canbe explained that some of the CTA+ chains were full stretchedand orderly tilted at an angle of 60∘ (Figure 9) The 119889-valuesassociated with the second and the third reflection were25 nm and 24 nm respectively which could be explained bythe fact that some of CTA+ chains were arranged in the typeof paraffin-type monolayer at an angle of 38∘ The 119889-value of

051nm

25 nm

046nm

(a)

067nm

25 nm

041nm

(b)

Figure 8 The schematic drawing about the size of CTA+ (a) sideview and (b) top view [30]

the forth reflection was 12 nm which was lesser than thatof lateral-monolayer Therefore of the second reflection inFigure 4(b) was of the second order The appearance of thelast reflection evidenced the vestigial of S

3 In other words S

3

was not be modified completely in reaction


60∘

38∘

TOT

CTA+

Figure 9 The schematic drawing about the arrangement of CTA+in the interlayer of CTA-S

4 Conclusions

Intercalated sericite was prepared by CTA+ intercalating intoactivated sericite The best intercalated sericite in whichCTA+ enlarged the basal spacing from 09 nm to 52 nm wasprepared under reaction time of 24 h reaction temperatureof 80∘C CTAB quantity of 15 times (by mol) of sericite(according to CEC) and reaction medium of aqueous withpH = 4 The results shown by FT-IR DSC and TG provedthat about half of CTA+ physisorbed on the surface of CTA-S and the rest entered the sericite interlayers and stayedstably The arrangements of CTA+ in sericite interlayers wereconstituted by theCTA+ chainsmainly tilted at an angle about60∘ (paraffin-type bilayer) and 38∘ (paraffin-type monolayer)with layers

Conflict of Interests

The authors declare that there is no conflict of interestsregarding the publication of this paper

Acknowledgment

The authors would like to acknowledge the FundamentalResearch Funds for the Central Universities (2011PY0169) forfinancial support during part of this research

References

[1] S Sinha Ray and M Okamoto ldquoPolymerlayered silicate nano-composites a review from preparation to processingrdquo Progressin Polymer Science vol 28 no 11 pp 1539ndash1641 2003

[2] C Zhao H Qin F Gong M Feng S Zhang and M YangldquoMechanical thermal and flammability properties of polyethy-leneclay nanocompositesrdquo Polymer Degradation and Stabilityvol 87 no 1 pp 183ndash189 2005

[3] H Qin Q Su S Zhang B Zhao and M Yang ldquoThermalstability and flammability of polyamide 66montmorillonitenanocompositesrdquo Polymer vol 44 no 24 pp 7533ndash7538 2003

[4] S Pavlidou and C D Papaspyrides ldquoA review on polymer-layered silicate nanocompositesrdquo Progress in Polymer Science(Oxford) vol 33 no 12 pp 1119ndash1198 2008

[5] S M Lee and D Tiwari ldquoOrgano and inorgano-organo-modified clays in the remediation of aqueous solutions anoverviewrdquo Applied Clay Science vol 59-60 pp 84ndash102 2012

[6] J Konta ldquoClay and man clay raw materials in the service ofmanrdquo Applied Clay Science vol 10 no 4 pp 275ndash335 1995

[7] U C Ugochukwu D A C Manning and C I Fialips ldquoEffectof interlayer cations of montmorillonite on the biodegradationand adsorption of crude oil polycyclic aromatic compoundsrdquoJournal of EnvironmentalManagement vol 142 pp 30ndash35 2014

[8] Z Qin P Yuan S Yang D Liu H He and J Zhu ldquoSilylation ofAl13-intercalated montmorillonite with trimethylchlorosilane

and their adsorption for Orange IIrdquo Applied Clay Science vol99 pp 229ndash236 2014

[9] S Yang M Gao and Z Luo ldquoAdsorption of 2-naphthol on theorgano-montmorillonites modified by Gemini surfactants withdifferent spacersrdquo Chemical Engineering Journal vol 256 pp39ndash50 2014

[10] R Zhang W Yan and C Jing ldquoMechanistic study of PFOSadsorption on kaolinite and montmorilloniterdquo Colloids andSurfaces A vol 462 pp 252ndash258 2014

[11] R Ait-Akbour P Boustingorry F Leroux F Leising and CTaviot-Gueho ldquoAdsorption of PolyCarboxylate Poly(ethyleneglycol) (PCP) esters on Montmorillonite (Mmt) effect ofexchangeable cations (Na+ Mg2+ and Ca2+) and PCPmolecularstructurerdquo Journal of Colloid and Interface Science vol 437 pp227ndash234 2015

[12] I Perassi and L Borgnino ldquoAdsorption and surface precipita-tion of phosphate onto CaCO

3ndashmontmorillonite effect of pH

ionic strength and competition with humic acidrdquo Geodermavol 232ndash234 pp 600ndash608 2014

[13] X Ren Z Zhang H Luo et al ldquoAdsorption of arsenic onmodifiedmontmorilloniterdquoApplied Clay Science vol 97-98 pp17ndash23 2014

[14] F H Do Nascimento and J C Masini ldquoInfluence of humic acidon adsorption of Hg(II) by vermiculiterdquo Journal of Environmen-tal Management vol 143 pp 1ndash7 2014

[15] A Sarı and M Tuzen ldquoAdsorption of silver from aqueoussolution onto raw vermiculite and manganese oxide-modifiedvermiculiterdquo Microporous and Mesoporous Materials vol 170pp 155ndash163 2013

[16] T Hongo S Yoshino A Yamazaki A Yamasaki and SSatokawa ldquoMechanochemical treatment of vermiculite invibration milling and its effect on lead (II) adsorption abilityrdquoApplied Clay Science vol 70 pp 74ndash78 2012

[17] Z-D Wen D-W Gao Z Li and N-Q Ren ldquoEffects ofhumic acid on phthalate adsorption to vermiculiterdquo ChemicalEngineering Journal vol 223 pp 298ndash303 2013

[18] H Long PWu L Yang Z Huang N Zhu and Z Hu ldquoEfficientremoval of cesium from aqueous solution with vermiculite ofenhanced adsorption property through surface modification byethylaminerdquo Journal of Colloid and Interface Science vol 428pp 295ndash301 2014

[19] E Padilla-Ortega R Leyva-Ramos and J Mendoza-BarronldquoRole of electrostatic interactions in the adsorption of cad-mium(II) from aqueous solution onto vermiculiterdquo AppliedClay Science vol 88-89 pp 10ndash17 2014

[20] S W Bailey ldquoInterstratified clay mineralsrdquo in Crystal Structureof Clay Minerals and Their X-Ray Identification G W Brndleyand G Brown Eds pp 1ndash113 Mineralogical Society LondonUK 1980


[21] M Alexandre and P Dubois ldquoPolymer-layered silicate nano-composites preparation properties and uses of a new class ofmaterialsrdquoMaterials Science and Engineering R Reports vol 28no 1 pp 1ndash63 2000

[22] H Ding X Xu N Liang and Y Wang ldquoPreparation sericitenanoflakes by exfoliation of wet ultrafine grindingrdquo AdvancedMaterials Research vol 178 pp 242ndash247 2011

[23] Y-J Shih and Y-H Shen ldquoSwelling of sericite by LiNO3-hydro-

thermal treatmentrdquoApplied Clay Science vol 43 no 2 pp 282ndash288 2009

[24] R A Vaia R K Teukolsky and E P Giannelis ldquoInterlayerstructure and molecular environment of alkylammonium lay-ered silicatesrdquoChemistry ofMaterials vol 6 no 7 pp 1017ndash10221994

[25] F Bergaya and G Lagaly ldquoMechanical properties of clays andclay mineralsrdquo in Developments in Clay Science Handbook ofClay Science vol 1 pp 274ndash260 Elsevier Amsterdam TheNetherlands 2006

[26] H W Ma Industrial Minerals and Rocks Chemical IndustryPress Beijing China 3rd edition 2011

[27] X F Yu B Ram and X C Jiang ldquoParameter setting in a bio-inspired model for dynamic flexible job shop scheduling withsequence-dependent setupsrdquo European Journal of IndustrialEngineering vol 1 no 2 pp 182ndash199 2007

[28] D Tiwari and S M Lee ldquoNovel hybrid materials in theremediation of ground waters contaminated with As(III) andAs(V)rdquo Chemical Engineering Journal vol 204-205 pp 23ndash312012

[29] S-M Koh and J B Dixon ldquoPreparation and application oforgano-minerals as sorbents of phenol benzene and toluenerdquoApplied Clay Science vol 18 no 3-4 pp 111ndash122 2001

[30] R Zhu L Zhu J Zhu and L Xu ldquoStructure of cetyltrimethy-lammonium intercalated hydrobiotiterdquo Applied Clay Sciencevol 42 no 1-2 pp 224ndash231 2008

[31] L J Wang X L Xie N C Chen and C J Hu ldquoEvaluation ofkaolinite intercalation efficiencyrdquo Chinese Journal of InorganicChemistry vol 26 pp 853ndash859 2010

[32] Q M Ye and X F Liu ldquoAnalysis of the microstructure ofthe CTMABmodified organobentoniterdquo Bulletin of the ChineseCeramic Society vol 5 pp 40ndash43 2004

[33] Z M Cui L B Liao G M Chen and M S Yang ldquoOrganicintercalation polymerization and exfoliation of different mont-morillonitesrdquo Journal of the Chinese Ceramic Society vol 33 no5 pp 599ndash603 2005

[34] S Xu and S A Boyd ldquoAlternative model for cationic surfactantadsorption by layer silicatesrdquo Environmental Science and Tech-nology vol 29 no 12 pp 3022ndash3028 1995

[35] R L Virta ldquoTalc and pyrophylliterdquo The American CeramicSociety Bulletin vol 84 pp 25ndash26 2005

[36] J Zhu H He J Guo D Yang and X Xie ldquoArrangementmodels of alkylammonium cations in the interlayer of HDTMA+ pillared montmorillonitesrdquo Chinese Science Bulletin vol 48no 4 pp 368ndash372 2003

Submit your manuscripts athttpwwwhindawicom

ScientificaHindawi Publishing Corporationhttpwwwhindawicom Volume 2014

CorrosionInternational Journal of

Hindawi Publishing Corporationhttpwwwhindawicom Volume 2014

Polymer ScienceInternational Journal of



CeramicsJournal of


CompositesJournal of

NanoparticlesJournal of



International Journal of

Biomaterials


NanoscienceJournal of

TextilesHindawi Publishing Corporation httpwwwhindawicom Volume 2014

Journal of

NanotechnologyHindawi Publishing Corporationhttpwwwhindawicom Volume 2014

Journal of

CrystallographyJournal of


The Scientific World JournalHindawi Publishing Corporation httpwwwhindawicom Volume 2014


CoatingsJournal of

Advances in

Materials Science and EngineeringHindawi Publishing Corporationhttpwwwhindawicom Volume 2014

Smart Materials Research



MetallurgyJournal of


BioMed Research International

MaterialsJournal of


Nano

materials


Journal ofNanomaterials


Table 1 Chemical composition of the original sericite

Composition SiO2 Al2O3 Fe2O3 TiO2 K2O Na2O CaO MgO SO3 LOI TotalContent (mass ) 4571 2832 304 035 809 071 010 212 0075 447 99555

charge known as the cation exchange capacity (CEC) Thischarge is not locally constant but varies from layer to layerand must be considered as an average value over the wholecrystal [1 21] while excessive CEC will lead to the instabilityof interlayer cation and could not serve as the excellentmatrixmaterials for cation modification

Comparing with other clay minerals sericite holds theadvantages of high moduli stable chemical property highelectrical insulation good ultraviolet ray resistance and soforth [22ndash24] Its structure consisted of layers made up of twoSiAl tetrahedral sheets and a sandwiched octahedral sheetfilled with Al3+ and K+ (mainly) in interlayer It also belongsto 2 1 phyllosilicates however there are a few distinct differ-ences as compared with montmorillonite and vermiculite [525 26] It does not swell in water and hardly has ion exchangecapacity and intercalation property because of its high layercharge producing pretty strong electrostatic force [27] Thedifficult preparation based on sericite explains the lack ofliterature concerning the intercalation or exfoliation of micagroups compared with montmorillonite and vermiculite

Intercalated sericite is important to serve as potentialsorbents in the removalspeciation of various pollutantsin the waste waters and perhaps emerged as a new areaof research in the waste water treatment technologies [2829] Cetyltrimethylammonium bromide (CTAB) a typicalcationic surfactant is often used in the modification of clayto increase to adsorption of matrix and also presents heat-resistant acid and alkali resistance and bactericidal activityThe treatment and activation of sericite increased the quantityof exchangeable cations and the organic modification ofsericite made the preparation of clay-polymer nanocompos-ites based on sericite easier To do this here we proposedthree steps first activating the structure of sericite to make ithave more exchangeable cations and intercalation propertiessecond modifying layered structure of sericite by cationsurfactant such as CTAB third intercalating polymer intoorganic sericite interlayers to exfoliate entirely or partly itslayers

In this paper sericite was activated by thermal modi-fication acid activation and sodium modification and theintercalated sericite was prepared by the intercalation of cetyltrimethylammonium ions (CTA+) into activated sericiteReaction time temperature quantity of intercalation agentreaction medium and pH on intercalation were discussed insericite intercalation

2 Materials and Methods

21 Materials The original sericite (S0) was obtained from

Anhui Province China whose mean size was about 10 120583mThe chemical composition of S

0was listed in Table 1 Cetyl

trimethylammonium bromide (CTAB) with a purity of 99

was provided by Xilong Chem Co China which was usedas cation surfactant

22 Preparation The original powder (S0) was heated at

800∘C in muffle furnace for 1 h The resulting product (S1)

was stirred with nitric acid of 5molL at 95∘C in thermostaticwater bath for 4 h and the product was washed till pH = 7Then the powder (S

2) was reacted with NaCl supersaturated

solution at 95∘C for 3 h and the product was washed andfiltrated till without Clminus (tested by AgNO

3) Finally the

activated sericite (S3) was obtained after drying process

Subsequently a certain amount of S3and the surfactantCTAB

were dispersed in distilled water respectively The mass ratioS3water was 3100 After mixing the dispersion of S

3and

CTAB solution (by magnetic stirring) the dispersion washeated to 80∘C for 24 h and pH was adjusted to neutral andweak acid with HNO

3 And then the turbid liquid was laid

aside for 2 h After that the product was washed with distilledwater (room temperature) till Brminus removed effectively (testedby AgNO

3) The final product (CTA-S) was dried at 80∘C

23 Characterization The X-ray diffraction patterns wereobtained on a Rigaku Rotaflex X-ray powder diffractometeremploying Cu K120572 radiation 40 kV and 100mA The X-raydiffraction (XRD) patterns in the 2120579 range from 1∘ to 10∘ werecollected at 05∘min Middle-infrared transmission spectra(500ndash4000 cmminus1) were collected using a Nicolet Magna-IR750 Fourier transform infrared spectrometer equipped witha Nicolet NicPlan IR Microscope operated with a spectralresolution of 4 cmminus1 Simultaneous collecting DSC and TGAsignals was carried out using a SDTQ600 analyzer (from TAthe US) under air flow and heating the samples from roomtemperature to 1100∘C at 10∘Cmin Mass of the samples wasabout 5mg

Sericite does not belong to the clay minerals in thenarrow sense but it is a hydratable layered silicate with acertain layer charge especially after activation and structuretransformation Cation exchange capacity can be used asa measure of the activity Ammonium chloride-anhydrousethanol method was used in this experiment to determinethe cation exchange capacity of sericite The pH value wasadjusted to 7 during the measurement

The intercalation rate defined as the rate of diffractionpeak intensities which can reflect the change of interlayerspacing before and after the layered silicate is intercalatedand can be used to evaluate the degree of intercalationreaction The intercalation rate can be expressed as follows[31]

IR =119868119888

(119868119888+ 119868119896) (1)


0 10 20 30 40 50 60 70

(002

)

(004

) (006

) 1 2 3 4 5 6 7 8 9 10

2120579 (∘)

S3

S2

S1

S0


3










0to








1much more






3was 09 nm When S

3and CTAB (15 times






















5120583m

(a)

5120583m

(b)


2 4 6 8 104h

10h

16h

24h

d = 52nm

d = 43nm

d = 24 nm

2120579 (∘)

(a)

1 2 3 4 5 6 7 8 9 10

d = 52nm

d = 52nm

d = 44nm

d = 24 nm

80∘C

95∘C60∘C

2120579 (∘)

(b)




3







2asymmetric and








0at 489 at 1100∘C (Figure 7(a))




1 2 3 4 5 6 7 8 9 10

5CEC

10CEC

15CEC

20CEC

2120579 (∘)

d = 52nm

d = 45 nm

d = 24 nm

(a)

1 2 3 4 5 6 7 8 9 10

Water

2120579 (∘)

d = 52nm

d = 52nm

d = 25 nm


(b)


2 4 6 8 102120579 (∘)

d = 52nm

d = 25 nm

d = 15 nm

d = 24 nm

pH = 11

pH = 9

pH = 7

pH = 1

pH = 4




4000 3500 3000 2500 2000 1500 1000 500

(c)

(b)

3400

473

962

909CTA-S

CTAB 720

1404

1024

1630

1484

2849

2918

3624

(a)


S0




Residue

200 400 600 800 1000

86

88

90

92

94

96

98

100

102 120

Hea

t flow

(nW

)

90

60

30

0

Wei

ght (

)

9511 AT1050∘C4814 mg

81781∘C

86312∘C

3971

69624∘C

minus120

minus90

minus60

minus30


(a)

Residue

200 400 600 800 100078

84

90

96

102 118

51

Hea

t flow

(nW

)

Wei

ght (

)


minus150

minus83

minus16

21420∘C09311

33319∘C304425917∘C

41898∘C

24695∘C

39391∘C 9303 AT1050∘C6003 mg

2402

(b)

5046

3558

2023

Residue8843 AT

Hea

t flow

(mW

)

200 400 600 800 100070

75

80

85

90

95

100 96

60

24

Exo up

Wei

ght (

)

Temperature (∘C)

minus120

minus84

minus48

minus12

21546∘C

25458∘C

42391∘C

23597∘C

39071∘C

35517∘C 1050∘C6872mg

(c)

Residue8639 AT

200 400 600 800 100060

65

70

75

80

85

90

95

100

105

17

10

3

Exo up

Wei

ght (

)

38

31

24

Temperature (∘C)

minus25

minus18

minus11

minus4 Hea

t flow

(mW

)

950∘C

3788

8549

21419∘C

25010∘C

34271∘C

23761∘C23603∘C

33272∘C

4295mg

(d)


(c) and 15 CEC (d))




051nm

25 nm

046nm

(a)

067nm

25 nm

041nm

(b)



3 In other words S

3



60∘

38∘

TOT

CTA+


4 Conclusions




Acknowledgment


References

















































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




0 10 20 30 40 50 60 70

(002

)

(004

) (006

) 1 2 3 4 5 6 7 8 9 10

2120579 (∘)

S3

S2

S1

S0


3










0to








1much more






3was 09 nm When S

3and CTAB (15 times






















5120583m

(a)

5120583m

(b)


2 4 6 8 104h

10h

16h

24h

d = 52nm

d = 43nm

d = 24 nm

2120579 (∘)

(a)

1 2 3 4 5 6 7 8 9 10

d = 52nm

d = 52nm

d = 44nm

d = 24 nm

80∘C

95∘C60∘C

2120579 (∘)

(b)




3







2asymmetric and








0at 489 at 1100∘C (Figure 7(a))




1 2 3 4 5 6 7 8 9 10

5CEC

10CEC

15CEC

20CEC

2120579 (∘)

d = 52nm

d = 45 nm

d = 24 nm

(a)

1 2 3 4 5 6 7 8 9 10

Water

2120579 (∘)

d = 52nm

d = 52nm

d = 25 nm


(b)


2 4 6 8 102120579 (∘)

d = 52nm

d = 25 nm

d = 15 nm

d = 24 nm

pH = 11

pH = 9

pH = 7

pH = 1

pH = 4




4000 3500 3000 2500 2000 1500 1000 500

(c)

(b)

3400

473

962

909CTA-S

CTAB 720

1404

1024

1630

1484

2849

2918

3624

(a)


S0




Residue

200 400 600 800 1000

86

88

90

92

94

96

98

100

102 120

Hea

t flow

(nW

)

90

60

30

0

Wei

ght (

)

9511 AT1050∘C4814 mg

81781∘C

86312∘C

3971

69624∘C

minus120

minus90

minus60

minus30


(a)

Residue

200 400 600 800 100078

84

90

96

102 118

51

Hea

t flow

(nW

)

Wei

ght (

)


minus150

minus83

minus16

21420∘C09311

33319∘C304425917∘C

41898∘C

24695∘C

39391∘C 9303 AT1050∘C6003 mg

2402

(b)

5046

3558

2023

Residue8843 AT

Hea

t flow

(mW

)

200 400 600 800 100070

75

80

85

90

95

100 96

60

24

Exo up

Wei

ght (

)

Temperature (∘C)

minus120

minus84

minus48

minus12

21546∘C

25458∘C

42391∘C

23597∘C

39071∘C

35517∘C 1050∘C6872mg

(c)

Residue8639 AT

200 400 600 800 100060

65

70

75

80

85

90

95

100

105

17

10

3

Exo up

Wei

ght (

)

38

31

24

Temperature (∘C)

minus25

minus18

minus11

minus4 Hea

t flow

(mW

)

950∘C

3788

8549

21419∘C

25010∘C

34271∘C

23761∘C23603∘C

33272∘C

4295mg

(d)


(c) and 15 CEC (d))




051nm

25 nm

046nm

(a)

067nm

25 nm

041nm

(b)



3 In other words S

3



60∘

38∘

TOT

CTA+


4 Conclusions




Acknowledgment


References

















































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




5120583m

(a)

5120583m

(b)


2 4 6 8 104h

10h

16h

24h

d = 52nm

d = 43nm

d = 24 nm

2120579 (∘)

(a)

1 2 3 4 5 6 7 8 9 10

d = 52nm

d = 52nm

d = 44nm

d = 24 nm

80∘C

95∘C60∘C

2120579 (∘)

(b)




3







2asymmetric and








0at 489 at 1100∘C (Figure 7(a))




1 2 3 4 5 6 7 8 9 10

5CEC

10CEC

15CEC

20CEC

2120579 (∘)

d = 52nm

d = 45 nm

d = 24 nm

(a)

1 2 3 4 5 6 7 8 9 10

Water

2120579 (∘)

d = 52nm

d = 52nm

d = 25 nm


(b)


2 4 6 8 102120579 (∘)

d = 52nm

d = 25 nm

d = 15 nm

d = 24 nm

pH = 11

pH = 9

pH = 7

pH = 1

pH = 4




4000 3500 3000 2500 2000 1500 1000 500

(c)

(b)

3400

473

962

909CTA-S

CTAB 720

1404

1024

1630

1484

2849

2918

3624

(a)


S0




Residue

200 400 600 800 1000

86

88

90

92

94

96

98

100

102 120

Hea

t flow

(nW

)

90

60

30

0

Wei

ght (

)

9511 AT1050∘C4814 mg

81781∘C

86312∘C

3971

69624∘C

minus120

minus90

minus60

minus30


(a)

Residue

200 400 600 800 100078

84

90

96

102 118

51

Hea

t flow

(nW

)

Wei

ght (

)


minus150

minus83

minus16

21420∘C09311

33319∘C304425917∘C

41898∘C

24695∘C

39391∘C 9303 AT1050∘C6003 mg

2402

(b)

5046

3558

2023

Residue8843 AT

Hea

t flow

(mW

)

200 400 600 800 100070

75

80

85

90

95

100 96

60

24

Exo up

Wei

ght (

)

Temperature (∘C)

minus120

minus84

minus48

minus12

21546∘C

25458∘C

42391∘C

23597∘C

39071∘C

35517∘C 1050∘C6872mg

(c)

Residue8639 AT

200 400 600 800 100060

65

70

75

80

85

90

95

100

105

17

10

3

Exo up

Wei

ght (

)

38

31

24

Temperature (∘C)

minus25

minus18

minus11

minus4 Hea

t flow

(mW

)

950∘C

3788

8549

21419∘C

25010∘C

34271∘C

23761∘C23603∘C

33272∘C

4295mg

(d)


(c) and 15 CEC (d))




051nm

25 nm

046nm

(a)

067nm

25 nm

041nm

(b)



3 In other words S

3



60∘

38∘

TOT

CTA+


4 Conclusions




Acknowledgment


References

















































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




1 2 3 4 5 6 7 8 9 10

5CEC

10CEC

15CEC

20CEC

2120579 (∘)

d = 52nm

d = 45 nm

d = 24 nm

(a)

1 2 3 4 5 6 7 8 9 10

Water

2120579 (∘)

d = 52nm

d = 52nm

d = 25 nm


(b)


2 4 6 8 102120579 (∘)

d = 52nm

d = 25 nm

d = 15 nm

d = 24 nm

pH = 11

pH = 9

pH = 7

pH = 1

pH = 4




4000 3500 3000 2500 2000 1500 1000 500

(c)

(b)

3400

473

962

909CTA-S

CTAB 720

1404

1024

1630

1484

2849

2918

3624

(a)


S0




Residue

200 400 600 800 1000

86

88

90

92

94

96

98

100

102 120

Hea

t flow

(nW

)

90

60

30

0

Wei

ght (

)

9511 AT1050∘C4814 mg

81781∘C

86312∘C

3971

69624∘C

minus120

minus90

minus60

minus30


(a)

Residue

200 400 600 800 100078

84

90

96

102 118

51

Hea

t flow

(nW

)

Wei

ght (

)


minus150

minus83

minus16

21420∘C09311

33319∘C304425917∘C

41898∘C

24695∘C

39391∘C 9303 AT1050∘C6003 mg

2402

(b)

5046

3558

2023

Residue8843 AT

Hea

t flow

(mW

)

200 400 600 800 100070

75

80

85

90

95

100 96

60

24

Exo up

Wei

ght (

)

Temperature (∘C)

minus120

minus84

minus48

minus12

21546∘C

25458∘C

42391∘C

23597∘C

39071∘C

35517∘C 1050∘C6872mg

(c)

Residue8639 AT

200 400 600 800 100060

65

70

75

80

85

90

95

100

105

17

10

3

Exo up

Wei

ght (

)

38

31

24

Temperature (∘C)

minus25

minus18

minus11

minus4 Hea

t flow

(mW

)

950∘C

3788

8549

21419∘C

25010∘C

34271∘C

23761∘C23603∘C

33272∘C

4295mg

(d)


(c) and 15 CEC (d))




051nm

25 nm

046nm

(a)

067nm

25 nm

041nm

(b)



3 In other words S

3



60∘

38∘

TOT

CTA+


4 Conclusions




Acknowledgment


References

















































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




Residue

200 400 600 800 1000

86

88

90

92

94

96

98

100

102 120

Hea

t flow

(nW

)

90

60

30

0

Wei

ght (

)

9511 AT1050∘C4814 mg

81781∘C

86312∘C

3971

69624∘C

minus120

minus90

minus60

minus30


(a)

Residue

200 400 600 800 100078

84

90

96

102 118

51

Hea

t flow

(nW

)

Wei

ght (

)


minus150

minus83

minus16

21420∘C09311

33319∘C304425917∘C

41898∘C

24695∘C

39391∘C 9303 AT1050∘C6003 mg

2402

(b)

5046

3558

2023

Residue8843 AT

Hea

t flow

(mW

)

200 400 600 800 100070

75

80

85

90

95

100 96

60

24

Exo up

Wei

ght (

)

Temperature (∘C)

minus120

minus84

minus48

minus12

21546∘C

25458∘C

42391∘C

23597∘C

39071∘C

35517∘C 1050∘C6872mg

(c)

Residue8639 AT

200 400 600 800 100060

65

70

75

80

85

90

95

100

105

17

10

3

Exo up

Wei

ght (

)

38

31

24

Temperature (∘C)

minus25

minus18

minus11

minus4 Hea

t flow

(mW

)

950∘C

3788

8549

21419∘C

25010∘C

34271∘C

23761∘C23603∘C

33272∘C

4295mg

(d)


(c) and 15 CEC (d))




051nm

25 nm

046nm

(a)

067nm

25 nm

041nm

(b)



3 In other words S

3



60∘

38∘

TOT

CTA+


4 Conclusions




Acknowledgment


References

















































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




60∘

38∘

TOT

CTA+


4 Conclusions




Acknowledgment


References

















































CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials




























CeramicsJournal of







Biomaterials




Journal of


Journal of





CoatingsJournal of

Advances in








MaterialsJournal of


Nano

materials



research article preparation and characterization of cetyl...

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