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STUDIES ON THE SYNTHESIS OF BUTADIENE/ISOPRENE/STYRENE POLYMER INITIATED BY DILITHIUM INITIATORS

Author: LiYang
Tutor: YangJinZong;GuMingChu;HongDingYi
School: Dalian University of Technology
Course: Fine Chemicals
Keywords: Dilithium Initiator Butadiene lsoprene Styrene Homo-polymer Stereo-block-polymer Block Copolymer Terpolymer
CLC: O632
Type: PhD thesis
Year: 2000
Downloads: 316
Quote: 8
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Executive Summary


During the last few years, the focus on development of alkyllithium initiator gradually shafted from monolithium to dilithium or multilithium or mixed-lithium initiators. Among them, the dilithium initiator was developed very fast and increasingly attracted extensive attentions since the dissolution problem of the dilithium initiator in non-polar solvent had been overcome. Dilithium initiator possessed the incomparable advantages over monolithium in preparing lithium-initiated polymers, among them, the most important characteristic was that the symmetrical polymer could be synthesized when the initiation, propagation and termination of the chain occurred at two ends at the same time. Combined with the features of anionic active polymerization, the dilithium initiator already created a new growth point in technology of lithium-initiated polymer through its application in the ternary copolymerization field of butadiene-isoprene-styrene. At present, the dilithium initiator manufactured by Dow Company, USA, was known as the best commercialized product in comprehensive properties, however, there still existed problems which remain to be resolved, such as non-single solvent system, slow initiation speed, inferior solubility and long preparation time, Under the precondition of ensuring the advantages such as good solubility, uniform functionality, fast initiation speed, single solvent system, simplified preparation technology, short synthesis time and low cost, the present thesis developed two kinds of dilithium initiators. One was the dilithium oligomer prepared via addition reaction of diene, named as diene addition type dilithium; the novel initiator reached the current international level in the technical indexes and formed proprietary technology. The other was dilithium oligomer prepared through substitution reaction of dihalogenated alkane, named as dihalogenated alkane substitution type dilithium. Thanks to the breakthrough in the understanding against the traditional concept of dilithium, the development of the dihalogenated alkane substitution type dilithium was injected with the fresh vigor proceeding from facilitating the practical application on industrial scale, making the initiator meet the requirements in application and realizing the localization of the initiators. Based on the philosophy of macromolecular design throughout the thesis, the author fully utilized the monomers of butadiene, isoprene and styrene produced in bulk to synthesize a series of novel copolymers with the dilithium as initiator, cyclohexane as solvent and diethylene glycol dimethyl ether / tetramethyl ethylenediamine as polar additive. Following were the typical block copolymers as prepared, including the polybutadiene, polyisoprene, 1,2-1,4-1 ,2-stereo-triblock polybutadiene, 3,4-1 ,4-3,4-stereo-triblock polyisoprene, symmetrical two-end tapered block copolymer of butadiene/styrene, symmetrical two-end tapered block copolymer of isoprene/styrene and symmetrical two-end tapered block terpolymer of butadiene/isoprene/styrene. Furthermore, this thesis also studied systematically the kinetic behaviour and heat effect in the polymerization process. The microstructure, sequential arrangement and morphology as well as the mechanical properties of the polymers mentioned above were also investigated in detail. From the summary of the full thesis, it came to the conclusions that: 1. The dihalogenated alkane substitution type dilithium was one kind of initiator that possessed pret

Full-text Catalog


The Chinese summary     13-20
preface     20-22
Chapter 1 dilithium initiator agents and butadiene / isoprene / styrene polymer technology progress   the   22-75 the
1.1 bifunctional The group alkyl lithium initiator technology progress     the 22-60 type
1.1.1 Electron Transfer     23-27
1.1.2 Dual halogenated alkanes replace type     27-32
1.1.3 double bond forming     32-47
1.1.4 abroad dilithium initiator technical progress     47-50
1.1.5 dilithium initiator agent technology progress     50-53
1.1.6 Summary and recommendations     53
1.1.7 References     53-60
1.2 butadiene / isoprene / styrene polymer technology progress     60-73
1.2.1 L-SIBR the developed     the 60-63 1.2.2 S-SIBR
developed    
1.2.3 LB 63-66 -SIBR development     66-70
1.2.4 SB-SIBR the, developed     70
1.2.5 few suggestions     70-72 < br /> 1.2.6 References     72-73
the 1.3 topic selection and research ideas     73-75
2 the Diene plus molding dilithium initiator developed     75-97
2.1 Introduction     75
2.2 routings     75-76
2.3 Experimental     76-87
2.3.1 of raw materials and refined     76-77
2.3.2 dual ketone synthesis     77-78
2. 3.3 diene synthesis     78
2.3.4 dual lithium synthesis     78
2.3.5 Analysis and Characterization     78-87 < br /> 2.4 Results and discussion     87-95
2.4.1 reaction time of     87-88
2.4.2 solvent     88
2.4.3 polar additives affect   the   88-92
2.4.4 single lithium species affect     92
2.4 .5 oligomerization and oligomerization degree of control     92-93
the 2.4.6 control functionality     93-94
2.4.7 polymerization     94-95
2.5 Conclusion     95-97
Chapter 3 double haloalkane replace type dilithium initiator developed     97-116
3.1 Introduction     97
3.2 Experimental     97-104
3.2.1 of raw materials and refined     97-98
3.2 .2 dilithium initiator synthesis     98
3.2.3 Analysis and Characterization   the   98-104
3.3 Results and Discussion     104-114 < br /> 3.3.1 solvent system selection     104-105
3.3.2 ethyl ether content, control     105-109
3.3.3 gathered degree of control     109-111
3.3.4 Stability Control   the   111-114
3.4 Conclusion     114-116
first the 4 chapters the polybutadiene developed     116-141
4.1 Introduction     116
4.2 Experimental     116-118
4.2 a .1 of raw and refined     116-117
4.2.2 synthetic     117
4.2.3 Analysis and Characterization     117-118
4.3 Results and discussion     study the
4.3.1 kinetics, 118-140     118-129
4.3.2 polymerization, the reaction process thermal effects     129 -131
4.3.3 Structure and performance     131-140
4.4 Conclusion nbsp a;   140-141
Chapter 5 stereoregular polybutadiene triblock Development     141-155
5.1 Introduction     141-142
5.2 Experimental     142-143
5.2.1 raw materials and refined     142
5.2.2 synthetic     142-143
5.2.3 Analysis and Characterization     143
5.3 Results and Discussion     143-154
5.3.1 kinetics, process research     143-145
5.3.2 polymerization process thermal effects     145-146 < br /> 5.3.3 Structure and Properties of     the
146-154 5.4 Conclusion     154-155
Chapter 6 the polyisoprene developed     155-180
6.1 Introduction     155
the 6.2 experiment     155-156
6.2.1 raw and refined     155 - 156
6.2.2 synthetic     156
6.2.3 Analysis and Characterization     156
6.3 Results and discussion     156-176
6.3.1-kinetic Research     156-165
6.3.2 polymerization, the thermal effects of the reaction     165-167
6.3.3 structure with Performance Research     167-176
6.4 Conclusion     176-180
stereotriblock the the triblock polyisoprene development     180-203 < br /> 7.1 Introduction     180
7.2 Experimental     180-182
7.2.1 of raw and refined     180-181
7.2.2 synthetic     181
7.2.3 Analysis and Characterization     181-182
7.3 Results and discussion     182-197
7.3.1 kinetics studies     182-188
7.3.2 Structure and Properties of     188-197
7.4 Conclusion     197 - 203
Chapter 8 symmetric double-ended transition state butadiene / styrene block copolymer developed     203-234
8.1 Introduction     203
8.2 Experimental     203-205
8.2.1 of raw and refined   the   203-204
8.2.2 synthetic     204
8 2.3 Analysis and characterization     204-205
8.3 Results and discussion     study the
8.3.1 kinetics, 205-232     205-213
8.3.2 thermal effects     213-214
8.3.3 structure and performance     214-232
8.4 Conclusion     232 - 234
Chapter 9 symmetrical double-ended transition state isoprene / styrene block copolymer developed     234-262
9.1 Introduction     234
9.2 Experimental     234-236
9.2.1 of raw and refined    . 234-235,
9.2.2 synthetic     235
9.2.3 Analysis and characterization     235-236
9.3 Results and discussion     236-257
9.3.1 kinetics studies     236 - 245
9.3.2 polymerization process thermal effects     245-246
9.3.3 Structure and Properties of     246-257
9.4 Conclusion     257-262
Chapter 10 symmetrical double-ended transition state butadiene / isoprene / styrene block copolymer developed     262-285
10. 1 Introduction     262
10.2 experimental     the 262-264 the
10.2.1 of raw materials and Refining    
10.2.2 262-263, synthesis     263
10.2.3 Analysis and characterization     263-264
10.3 Results and discussion     264-282
10.3. a kinetic study     264-273
10.3.2 Structure and Properties     273-282
10.4 Conclusion     282-285
first Diene 11 chapters plus molding the dilithium system butadiene / styrene polymer developed     285-314
11.1 preface nbsp,;   285
11.2 experimental     285-287
11.2.1 raw materials and refined     285-286
11.2.2 synthesis     286
11.2.3 Analysis and Characterization     286-287
11.3 Results and discussion     287-312
11.3.1 the polybutadiene developed     287-298
11.3.2 symmetrical double-ended transition state butadiene / styrene block copolymer developed     298-312
11.4 Conclusion     312-314
first Chapter 12 dilithium system butadiene / isoprene / styrene polymer patent chain formation     314-330
Chapter 13 Summary and Outlook     330-334
The papers published in Appendix 1 doctoral dissertation during   the   334-338
Appendix doctoral dissertation during the application of the patent     338-343
Appendix 3 Summary of innovation     343-344
Appendix 4 Acknowledgements     344

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