2882 犃狏狉犪犿犻 S c & ( ()* & ( (+ )*,-.& $ N'?! 7#,$?, %,4 & ("Q M M, 618307) 5 ) > '@c/ Y > O! R ) c /,( " ) > Q, a) F W (PQ <> )5 9 ) N Avrami ( M O )( ( )* ( +)* (PBS b PDGS), )c/ \]Y R!,Avra mi J- )c/,pdgs)l- ) E ) F N,GS ) F PDGS N!",PDGS).O (!") F PBS b PDGS )c/ \]! 01> R // Q Q 6S Q W6S P M Avrami T 3 2345:TQ323.4;O631 678:A 犇犗犐 :10.11896/j.issn.1005 023X.2018.16.033 犖狅狀犻狊狅狋犺犲狉犿犪犾犆狉狔狊狋犪犾犻狕犪狋犻狅狀犓犻狀犲狋犻犮狊狅犳犅犻狅犱犲犵狉犪犱犪犫犾犲犘狅犾狔 ( 犫狌狋狔犾犲狀犲狊狌犮犮犻狀犪狋犲 ) 犫 犘狅犾狔 ( 犱犻犲狋犺狔犾犲狀犲犵犾狔犮狅犾狊狌犮犮犻狀犪狋犲 ) 犕狌犾狋犻犫犾狅犮犽犆狅狆狅犾狔犿犲狉狊犫狔狋犺犲犃狏狉犪犿犻犪狀犱狋犺犲犕狅 狊犕犲狋犺狅犱狊犈狓犮犾狌狊犻狏犲犾狔 LIShaolong,XU Yi,CHEN Nongtian,YANG Wenfeng (AviationEngineeringInstitute,CivilAviationFlightUniversityofChina,Guanghan618307) 犃犫狊狋狉犪犮狋 Thepolymerprocessingisusualyoperatedundernonisothermalconditions,thestudyonnonisothermalcrystaliza tionbehaviorsofpolymershaveveryimportantlypracticalmeaningforchoosingsuitableprocessingmethod,equipment,temperature andtimetopreparepolymermaterialswithexcelentcomprehensiveordesiredproperties.weinvestigatedtheisothermalcrystaliza tionkineticsofbiodegradablepoly(butylenesuccinate) b poly(diethyleneglycolsuccinate)multiblockcopolymersbytheavramiand themo smethod.theresultsshowedthatavramiandthemo smethodscanbeusedtodescribethenonisothermalcrystalization behaviorsofthefoursamples.thecrystalizationmechanismalmostkeptunchangedwhilethecrystalizationratedecreasedwithan increaseofpdgscontent.theresultsalsodemonstratedthatthedecreaseofcrystalizationrateswasatributedtothediluteefectof PDGSwithanincreaseofPDGScontentinPBS b PDGScopolyesters.ThestudyonthenonisothermalcrystalizationkineticsofPBS b PDGSprovidetheorybasisfortheactualprocessingmolding. 犓犲狔狑狅狉犱狊 poly(butylenesuccinate) b poly(diethyleneglycolsuccinate),nonisothermalcrystalizationkinetics,avrami equation,mo smethod 0 9: Q Q 6S (PBS)U P &,B $114 (# 5 (LDPE) U),EW 9! 5$-32 ( a5 (PE) Q (PP) ), $1.25g/cm 3 (#24 5 6S(PET) U),E a PE PP, F? # PE PP U, #L 6 &,L + Z,XY,T 6 %&"L,T$L, & 0 VH B 3 W XN [1 2] PBSK9 <101,T-30~ 100,6 ayn 9 N ]F%&, & %&F? N R [ %% [3 4] V,T9:Z " Z,I#2 PBS [[9V PBS6FT 4 Z\ ] Z "],L,AQ Q 6^6 MW" 7, "! 7, & c, + Ac,PBSR M F? B [5 6],`a PBSP,L @ S (PHA) U (PLA) 6 S/7, b,pbs`a' * STZ ) " :P 8, PBS N., ]L, b# 2 PBS [2,7 8] `a. # PBS, b 2 PBS # [ :!L(U1233202); ( ) '(Q2018 65); ( ) *(BJ2016 02) + :4,1988',, 7, 89,- E mail:zlishaolong@163.com
N Avrami \]/7# /!( ( )* ( +)*, )c/ 2883 U< H Q [9 11] 9M# E -.,T ) "!6! E 7 6DP 3 F? PBS# [12 13] ), I*# % & B _., a, a7 [14 15] H ' 0 PBS # `a #' *,B G PBS, b R, [16] $]2 PBS,` Q (SA)# W 6 (DEG) Q W6S (HO PDGS OH)H, HO PDGS OH PBS' ", Q Q 6S Q W 6 S (PBS b PDGS) #,? P] HO PDGS OH O 2 # @? P $-. [17] P #T Y (), O,U F 7 8 7, a J P %&T B W V H 3 7 ) ", T 0 ] P, b2%& P M P,6 F $ J + P FB_0 T P,# P, P ) Ma %&7 ),2 L 3 P 8 7, (DSC)2 HO PDGS OH O PBS b PDGS# G PBS P MF? ]' P, $# ] J"# 1 F 1.1 F b Q (SA)$ G,7a A 9 1,4 Q 6 (BD) W 6 (DEG) 4 (CHCl 3 ) 6 $ G,7a 0 9 a @ Kb S (HDI),G $98%,7a@Q AlfaAe sar ; K Q S (Ti(iOPr) 4 )$ 9 M G,7 a @ Q Sigma Aldrich 7 4 $ [ 4 1.2 F c Q #Q 6 Q # W6 )S9Z3, ]Q Q 6S (HO PBS OH)H Q W 6 S (HO PDGS OH)H. C D,D & ( 狀 ( ) 狀 ( 6 )=1 1.2), 7 @ H [18 19] ) ^, - 7 H HO PBS OH HO PDGS OH $ 4380g/ mol 4900g/mol PBS/PDGS ( & $ 93/7 86/14 72/28# @ Kb S(HDI) ', 0 ] PBS b PDGS 7 PBS b PDGS 14 PBS b PDGS 28,$]2, PBSH # HDI,' 0] G PBS,` 2 N@ P M b ] P [17] NR, ' (PDI) EW9! ( 犜 )F? g B_ ( 犜 m) a1 1 G PBS PBS b PDGS# @ Table1 FundamentalparametersofneatPBSand PBS b PDGScopolymers Sample 犕 n/(10-4 g/mol) PDI 犜 / g 犜 m/ NeatPBS 3.5 4.3-36.3 113.1 PBS b PDGS 7 5.7 4.1-35.8 111.7 PBS b PDGS 14 4.6 4.7-35.3 111.2 PBS b PDGS 28 6.1 4.5-34.4 109.0 1.3 ;/ Mc @Q TA DSC Q200, \ 2 G PBS? PBS b PDGS # P, $5mg T N 2 A), N 130 B_, 5 min $,, F (20 /min 10 /min 5 /min 2.5 /min) 20,c F P M 2 '<M 2.1 N' 犇犛犆 :1 T 20 /min 10 /min 5 / min 2.5 /min BAP, T 2 P a 2 * + P, 7P ( 犜 c) :,7 PDGSO # P 9 (: 2) :16F,.,# P,, P, $ P R ),,,,,P,,P ] 2 G PBS PBS b PDGS# P Table2 CharacteristicparametersofneatPBSandits copolymersatdiferentcoolingrates Sample Coolingrate/( /min) 犜 c/ Δ 犎 c/(j/g) NeatPBS 2.5 89.3 63.4 5 85.6 64.1 10 81.1 65.0 20 75.1 65.8 PBS b PDGS 7 2.5 86.0 57.0 5 82.1 58.2 10 77.2 58.7 20 71.0 58.8 PBS b PDGS 14 2.5 79.3 58.4 5 74.8 58.8 10 69.3 59.4 20 62.3 60.0 PBS b PDGS 28 2.5 69.3 49.3 5 65.2 50.6 10 60.2 51.1 20 54.4 51.7 Note:Δ 犎 c heatofcrystalization
2884 Fig.1 :1 G PBS PBS b PDGS# T P DSC NonisothermalcrystalizationcurvesofneatPBSanditscopolymersatdiferentcoolingrates 2 :26F,T, PBS b PDGS# P ( 犜 c) PDGSO $ PDGS, ] PBS' P *,U 0 PDGS,*,2 P, S# P,P :2 G PBS PBS b PDGS# T P Fig.2 Thecrystalizationpeaktemperatureversuscooling rateforneatpbsanditscopolymers 2, (DSC) Y,,6F7 2P 犡狋, : 犜犜 0 犡狋 = d 犎犮 ( d犜 ) d 犎犮 d 犜 犜 ( d犜 ) 犜 0 d 犜 (1)!": 犜 0 犜 P P 7, 犜 P V $ 狋 VP, 犎 c P V $ 狋 V P *+!(1),6F HG PBS?L# T 2P 9 ' (:3) P V ( 狋 )#P ( 犜 ) '6F $: 犜 - 犜 0 狋 = φ (2)!": 犜 P V $ 狋 VP, 犜 0 P, φ?!(1)!(2)6f7 2P V 9 ' : 4 $ G PBS? PBS b PDGS# 犡狋 #P V ': :46X, :, ] P # V Z G PBS T $ 20 /min # 1.2min8] P, U: $ 10 /min 5 /min 2.5 /minv,l] P ) # V $2.0min 3.2min 5.0min,,G PBS< P ] # V, 2aL PBS b PDGS# *F U $ 2.5 /min V,G PBS P ] # 5.0 min, PBS b PDGS 7# # 5.5min,PBS b PDGS 14# # 6.6 min,pbs b PDGS 28# # 7.2min T :,/# P ` [$:G PBS PBS b PDGS 7 PBS b PDGS 14 PBS b PDGS 28 PDGS O, < P ] # V,P # DSC F? P RS [17] 2.2 犃狏狉犪犿犻 c0 Aranmi a P M P, 2, C D Aranmi P M [20 22],L!6 $: 狀 1- 犡狋 =exp(- 犣狋 ) (3)!": 犣 P ; 狀 $ AvramiF,#?! ; 犡狋 $ ) " 狋 V 2P (`!(1) 7 )!(1)52 $: lg[-ln(1- 犡狋 )]=lg 犣 + 狀 lg 狋 (4) Flg[-ln(1- 犡狋 )]2lg 狋 :,67 Avrami, $ 狀, $lg 犣 P P $
xl Ａｖ ｍê>á?, 23&@ùÄ@ùAB&@ ù Ä ù C A B D _ + & + A G ¼ ２８８５ U5 G X ３ q ＰＢＳ m ＰＢＳ ＰＤＧＳ 5'Ä Ê >~'( ~=5 P å=0]9^_ Ｆ ３ Ｒ ｖｃ ｎ ｕ ｍｐ ｕ ｆ ｏ ｎ ＰＢＳｎｄ ｃ ｏｐｏ ｄ ｆ ｆ ｎ ｃ ｏｏ ｎｇ ｇ ｙ ｙｖ ｙｍ X ４ q ＰＢＳ m ＰＢＳ ＰＤＧＳ 5'Ä Ê >~'( å 5 P å=0]9^_ Ｆ ４ Ｒ ｖｃ ｎ ｕｃ ｚ ｏｎ ｍｆ ｏ ｎ ＰＢＳｎｄ ｃ ｏｐｏ ｄ ｆ ｆ ｎ ｃ ｏｏ ｎｇ ｇ ｙ ｙｖ ｙ ｙｍ X ５ 6ð, Ａｖ ｍ)* q ＰＢＳ c ＰＢＳ ＰＤＧＳ 5 '(0ÖWPq ＰＢＳ cv5'ä0 狀 KEFÊF " å 'Ä0 ｎ １ 犡狋 5 狋 0 ] 9 X Ê X í ' ( ｇ ｇ Ø; w º 5 X í ' ( s ] n > ~ ' ( @ A ù q Z U 0 1 9 û Ó _ Ａｖ ｍ) * M Ç, q ＰＢＳ ＰＢＳ ＰＤＧＳ ７ ＰＢＳ ＰＤＧＳ １４ m ＰＢＳ ＰＤＧＳ ２８ 0 ＰＢＳ c ＰＢＳ ＰＤＧＳ 5'Äe90 Î ~ å Ø ; w Ａｖ ｍp: 狀 Kj k6 ３ ８ ３ ９ ４ １ m ５ ２ " åz DEU 0 狀 m 犣 0 K 5 Î ~ å Ø ; w 4 0狀 úã ＰＤＧＳ 0 ]6vÊ/òÖ5'Ä0 åº m犽 0KÄ K² ô Ê P D T B C Ａｖ ｍ) * U 0D;w :0ÖWBp jã'zä0 åº " ３ ûr Ð M x 0 Î ~ å Ø ; w : > ~ Ò ÐMx0 å'( : 犣 K È > ~ ' ( 0 Í ÖÁôÂÌF ÊA 犣 K0D[1 ｍ ｎ 狀 5 Ａｖ ｍp :狀 K ] p ) Õ 5 ' Ä 0 å $ ] + å '
2886 1/ 狀 ( 犽 ), 犽 = 犣,L, $ min -1, ] 狀 HY 犽 9 * F c G,I J $ Y, 犽 PDGSO, PDGS P 3 Avrami 7 G PBS PBS b PDGS# P, M Table3 NonisothermalcrystalizationparameterofneatPBSandPBS b PDGScopolyestersobtainedbytheAvramimethod Sample Coolingrate/( /min) 狀 犣 /min - 狀 犽 /min -1 (1/ 狋 1/2)/min -1 狋 1/2/min NeatPBS 2.5 3.6 3.5 10-2 0.40 0.44 2.28 5 4.1 9.6 10-2 0.57 0.62 1.62 10 4.1 5.5 10-1 0.87 0.94 1.06 20 3.2 3.5 1.48 1.67 0.60 PBS b PDGS 7 2.5 4.5 4.5 10-3 0.30 0.33 3.04 5 3.7 1.5 10-1 0.60 0.60 1.51 10 3.9 7.3 10-1 0.92 0.89 0.99 20 3.6 3.3 1.39 1.54 0.65 PBS b PDGS 14 2.5 4.2 2.8 10-3 0.25 0.27 3.72 5 4.0 3.1 10-2 0.42 0.46 2.18 10 4.3 1.6 10-1 0.66 0.76 1.40 20 3.8 1.8 1.18 1.30 0.77 PBS b PDGS 28 2.5 5.3 3.8 10-4 0.23 0.24 4.12 5 5.5 6.8 10-3 0.40 0.43 2.32 10 5.1 1.8 10-1 0.72 0.72 1.30 20 5.0 1.7 1.11 1.19 0.84 :5 G PBS PBS b PDGS# T Avrami Fig.5 AvramiplotsofforneatPBSanditscopolymersatdiferentcoolingrates P MV,6F )P 犣 c,- 4P V ( 狋 1/2)F?4P V (1/ 狋 1/2), ] P L! <$: 1 2 =1- 狀犡狋 =exp (- 犣狋 ) (5)!$: 狋 1/2= ( ln2 犽 ) 1/ 狀 (6) *+ Avrami, - 7 狀 犣,6F 7 G PBS? PBS b PDGS # PDGSO 9 狋 1/2 1/ 狋 1/2 (3), ):66F
N Avrami \]/7# /!( ( )* ( +)*, )c/ 2887 狋 1/2 1/ 狋 1/2# ' F $ 20 / min$,g PBS PBS b PDGS 7 PBS b PDGS 14 PBS b PDGS 281/ 狋 1/2 $1.67min -1 1.54 min -1 1.30 min -1 1.19 min -1, PDGS O,# 1/ 狋 1/2 I/, 狋 1/2., # P PDGSO :6 PDGSO 2 PBS b PDGS# T 狋 1/2 1/ 狋 1/2-. Fig.6 TheefectofweightfractionofPDGSon 狋 1/2and 1/ 狋 1/2ofPBS b PDGSatvariouscoolingrates 2.3 c T 3 P P M, Avrami Ozawa P,7 ^! [23 24] Avrami $!(4),Ozawa!$: lg[-ln(1- 犡狋 )]=lg 犓 ( 犜 )- 犿 lgφ (7)!": φ $ ; 犡狋 $ $ 犜 V 2P ; 犓 ( 犜 ) $ N,#! % ; 犿 $ OzawaF!(4)#!(7)P 7 T 3!: lgφ =lg 犉 ( 犜 )- 犪 lg 狋 (8)!": φ, 犉 ( 犜 )= [ 犓 ( 犜 )/ 犣 ] 1/ 犿, 犪 = 狀 / 犿, 狀 $ AvramiF, 犿 $ OzawaF 犉 ( 犜 ) P T, V < R 2P # 5 b 犉 ( 犜 )6 F c P, 犉 ( 犜 )., A ' P, 犉 ( 犜 ) /, A 'P UP V, < P # V,Flgφ 2lg 狋 :,7 R' P, $lg 犉 ( 犜 ), $- 犪 :7 5 2P $0.2 0.4 0.5 0.6 0.8 V,G PBS?L# Flgφ 2lg 狋, R' ', T 3 c P G PBS? PBS b PDGS# P M,-/ 7 犉 ( 犜 ) 犪,2 a4 2aG PBS? PBS b PDGS#,T 3F 犪 2P..,2 9., V N 犪., PDGS L # " PBS P 2P, N 犉 ( 犜 ).,, V 7 2 :7 G PBS PBS b PDGS# T P ) "lgφ 2lg 狋 Fig.7 Plotsoflgφversuslg 狋 forneatpbsanditscopolymersduringnonisothermalcrystalization
2888 P # < RY 2P V, PDGSO # 犉 ( 犜 )., # P PDGSO, # Avrami 7 PJRS 4 T 3 7 G PBS PBS b PDGS# P, M Table4 NonisothermalcrystalizationkineticsparametersofneatPBSandPBS b PDGScopolyestersatdiferentdegreesof crystalinitybythemo smethod 犡狋 NeatPBS PBS b PDGS 7 PBS b PDGS 14 PBS b PDGS 28 犉 ( 犜 )/( /min) 犪 犉 ( 犜 )/( /min) 犪 犉 ( 犜 )/( /min) 犪 犉 ( 犜 )/( /min) 犪 0.2 5.0 1.31 6.7 1.33 10.1 1.35 11.8 1.29 0.4 7.0 1.36 8.9 1.35 13.5 1.35 14.3 1.29 0.5 7.9 1.38 10.1 1.37 14.8 1.36 15.5 1.30 0.6 9.0 1.39 11.2 1.38 16.4 1.37 16.6 1.30 0.8 11.2 1.40 13.9 1.41 18.4 1.37 19.0 1.31 3 ' F Avrami T 3 2Q Q 6 S Q W6S # P M ] P,PQ 0 PDGS O,' *,2P, S # P,P Avrami T ( ),G PBS PBS b PDGS 7 PBS b PDGS 14 PBS b PDGS 28 AvramiF 狀 $ 3.8 3.9 4.1 5.2, PDGS # P T 3F 犪 9., PDGS? PBS P 2P, N 犉 ( 犜 ).,, V 7 2 P # < RY 2P V,PDGSO # 犉 ( 犜 )., # P PDGSO, # Avrami 7 P J R S # P, P ) M a PBS b PDGS# 7 ),2L P$B W VH 3 7 : J +, a. %& () 1 FujimakiT.Processabilityandpropertiesofaliphaticpolyesters, BIONOLLE,synthesizedbypolycondensationreaction[J].Poly merdegradationandstability,1998,59(1):209. 2 BikiarisD N,PapageorgiouGZ,AchiliasDS.Synthesisandcom parativebiodegradabilitystudiesofthreepoly(alkylenesuccinate)s [J].PolymerDegradationandStability,2006,91(1):31. 3 BechtholdI,BretzK,KabasciS,etal.Succinicacid:Anewplat formchemicalforbiobasedpolymersfromrenewableresources[j]. ChemicalEngineering & Technology,2008,31(5):647. 4 XuJ,GuoB H.Poly(butylenesuccinate)anditscopolymers:Re search,developmentandindustrialization [J].BiotechnologyJour nal,2010,5(11):1149. 5 TachibanaY,MasudaT,FunabashiM,etal.Chemicalsynthesisof fulybiomass basedpoly(butylenesuccinate)frominedible biomass basedfurfuralandevaluationofitsbiomasscarbonratio [J].Bio macromolecules,2010,11(10):2760. 6 WilkeT,Vorlop K D.Industrialbioconversionofrenewablere sourcesasanalternativetoconventionalchemistry[j].appliedmi crobiologyandbiotechnology,2004,66(2):131. 7 Kim D Y,Kim H W,Chung M G,etal.Biosynthesis,modifica tion,and biodegradation of bacterial medium chain length poly hydroxyalkanoates[j].journalofmicrobiology,2007,45(2):87. 8 Mondrinos M J,DembzynskiR,LuL,etal.Porogen basedsolid freeformfabricationofpolycaprolactone calciumphosphatescafolds fortissueengineering[j].biomaterials,2006,27(25):4399. 9 HeYS,ZengJB,LiSL,etal.Crystalizationbehaviorofpartialy misciblebiodegradablepoly(butylenesuccinate)/poly(ethylenesuc cinate)blends[j].thermochimicaacta,2012,529(1):80. 10 QiuZ,IkeharaT,NishiT.Poly(hydroxybutyrate)/poly(butylene succinate)blends:miscibilityandnonisothermalcrystalization [J]. Polymer,2003,44(8):2503. 11 LiYD,ZengJB,WangXL,etal.Structureandpropertiesofsoy protein/poly(butylenesuccinate)blendswithimprovedcompatibility [J].Biomacromolecules,2008,9(11):3157. 12 GanZ,AbeH,DoiY.Crystalization,melting,andenzymaticdeg radationofbiodegradablepoly(butylenesuccinate co 14 mol,ethy lenesuccinate)copolyester [J].Biomacromolecules,2001,2(1): 313. 13 YanJG,WangXD,YaoM.Moleculardynamicsstudyontheglass transitionbehaviorofpbs [J].MaterialsReview,2012,26(S2):180 (inchinese). Q,,.Q Q 6 S E W 9! $ [J].%&,2012,26( 20):180. 14 TserkiV,MatzinosP,Pavlidou E,etal.Biodegradablealiphatic polyesters.partⅠ.propertiesandbiodegradationofpoly(butylene succinate co butyleneadipate)[j].polymerdegradationandstabili ty,2006,91(2):367. 15 CaoA,OkamuraT,NakayamaK,etal.Studiesonsynthesesand physicalpropertiesofbiodegradablealiphaticpoly(butylenesucci nate co ethylenesuccinate)sandpoly(butylenesuccinate co diethy leneglycolsuccinate)s [J].Polymer Degradationand Stability, 2002,78(1):107. 16 ZhengL,LiC,Huang W,etal.Synthesisofhigh impactbiode gradablemultiblockcopolymerscomprisingofpoly(butylenesucci nate)andpoly(1,2 propylenesuccinate)withhexamethylenediso cyanateaschainextender[j].polymersforadvancedtechnologies, 2011,22:279. ( %2896 )
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