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线形与星形端烃羧基聚二甲基硅氧烷的合成与表征 被引量:4

Synthesis and Characterization of Linear and Star-shaped Carboxyl Acid-Terminated Polydimethylsiloxane
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摘要 利用三步法合成了一系列具有不同臂数的线形和多臂星形端烃羧基聚二甲基硅氧烷(PDMS-MAAx,x=1,2,3,4):首先,以Si—H数量不同的含氢封头剂分别与八甲基环四硅氧烷(D4)开环聚合,制得线形和多臂星形端氢基聚二甲基硅氧烷(PDMS-Hx);继而与甲基丙烯酸甲酯(MMA)进行硅氢加成反应,制得酯基封端的聚二甲基硅氧烷(PDMS-MMAx);最后将酯基在碱性条件下水解,制得PDMS-MAAx。采用FT-IR和1H NMR对三个合成阶段的反应产物进行了跟踪分析,确认了各步产物的结构,并讨论了PDMS-MMAx和PDMS-MAAx的合成条件对产物结构的影响,在此基础上优化了PDMS-MAAx的制备工艺,确定了PDMS-MMAx的最佳合成条件为:Si—H与MMA的量之比为1.0∶1.2、反应温度70~80℃、催化剂摩尔浓度20×10-6~60×10-6、反应时间5 h;PDMS-MMAx水解制备PDMS-MAAx的最佳条件为:NaOH水溶液中NaOH的质量分数为20%、NaOH水溶液以及乙醇的用量分别为PDMS-MMAx体积的3倍和1倍。 A three-step procedure was developed for synthesizing a series of linear and star-shaped car- boxyl-terminated polydimethylsiloxane, i. e. , PDMS -MAAx (x = 1, 2, 3, 4). First, the hydrogen-termina- ted PDMS with virous arms ( PDMS - Hx ) were prepared based on the ring-opening polymerization of octam- ethylcyclotetrasiloxane (D4 ) ; then, methyl methacrylate (MMA) was reacted with PDMS -Hx to prepare es- ter terminated PDMS ( PDMS - MMAx ) ; finally, the terminal ester group was transformed to terminal carboxyl acid based on the hydrolysis reaction of ester under alkaline condition to obtain carboxyl acid terminated PDMS, i. e. , PDMS -MAAx. FT -IR and 1H NMR were employed to confirm the structure of the product in each step of reactions and the effects of synthetic conditions on the structure of the products were discussed. Also, the optimal conditions for the preparation of PDMS - MMAx were with a mole ratio of Si--H and MMA of 1.0: 1.2, and a catalyst molality of 20×10-6~60×10-6 at 70 ~80℃ for 5 hours. The optimal conditions for the preparation of PDMS - MAAx were that 20% mass fraction of NaOH in NaOH solution, and the volume of the NaOH solution and ethanol was threefold and one time of the PDMS - MMAx.
出处 《有机硅材料》 CAS 2013年第2期76-82,共7页 Silicone Material
基金 国家自然科学基金资助项目(51003032 31201552) 华南理工大学中央高校基本科研业务费专项资金项目(2012ZZ0016) 广东省"合生珠江计划"大学生创新实验项目(H11020) 华南理工大学SRP资助项目
关键词 端烃羧基聚二甲基硅氧烷 甲基丙烯酸甲酯 硅氢加成 earboxyl acid terminated polydimethylsiloxane, methyl methacrylate, hydrosilylation
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  • 1黄文润.有机硅材料的市场与产品开发(续八)[J].有机硅材料及应用,1994,8(1):1-11. 被引量:26
  • 2黄文润.有机硅材料的市场与产品开发(续九)[J].有机硅材料及应用,1994,8(2):1-17. 被引量:4
  • 3黄文润.有机硅材料的市场与产品开发(续十二)[J].有机硅材料及应用,1994,8(5):14-16. 被引量:7
  • 4Holden G, Kricheldorf H R, Quirk R P. Thermoplastic elastomers [M].3rd ed. Cincinnati: Harmer Gardner, 2004: 1-5.
  • 5Stadler R, Lucca Freitas L. Thermoplastic elastomers by hydrogen bonding 1. rheological properties of modified polybutadiene [J ]. Colloid Polym. Sci., 1986, 264: 773-778.
  • 6Stadler R, Lucca Freitas L. Thermoplastic elastomers by hydrogen bonding. II. IR-spectroscopic characterization of the hydrogen bonding [J]. Polym. Bull., 1986, 15: 173-179.
  • 7Chino K, Ashiura M. Themoreversible cross-linking rubber using supramolecular hydrogen-bonding networks [J ]. Macromolecules, 2001, 34: 9201-9204.
  • 8Chino K, Ashiura M, Natori J, et al. Thermoreversible crusslinking rubber using suprarnoleeular hydrogen bonding networks [J]. Rubber Chem. Teehnol. , 2002, 75(4): 713-723.
  • 9Chang Y W, Mishra J K, Kim S K, et al. Effect of supramolecular hydrogen bonded network on the properties of maleated ethylene propylene diene rubber/maleated high density polyethylene blend based thermoplastic elastomer [J]. Mater. Lett., 2006, 60: 3118- 3121.
  • 10Peng C C, Abetz V. A simple pathway towards modification of polybutadiene: a new approach to thermoreversible cross-linking rubber comprising supramolecular hydrogen-bonding networks [J]. Macromolecules, 2005, 38: 5575-5580.

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  • 1李静,高中良,刘英浪,郭湘立.双(4-氟苯基)氯甲基甲基硅烷的合成[J].河北工业大学学报,2013,42(2):46-48. 被引量:2
  • 2武江红,杜志平,台秀梅,赵永红,王天壮.乙烯基三(β-甲氧基乙氧基)硅烷原位改性纳米SiO_2的制备与表征[J].中国粉体技术,2013,19(4):5-9. 被引量:3
  • 3谢凯明,王斌,朱春华.巯基改性有机硅防水剂的制备与应用[J].乙醛醋酸化工,2013(3):10-13. 被引量:3
  • 4王国建.在《高分子化学》课程中开展互动式教学的实践与探索[J].高分子通报,2007(1):62-65. 被引量:40
  • 5LIN F, SONG M Z, HE Z Z, et al. Synthesis and struc- tural characterization of methacrylic acid/octadecyl acry- late - graft - poly (methyihydrosiloxane) by hydrosilyla- tion [J]. J Appl Polym Sei, 2008, 107 (6): 3773 - 3780.
  • 6BINDL J, PETERSEN H, BACHHUBER K, et al.Process for the preparation of organosilicon compounds containing carboxyl groups: US, 5504233 [P]. 1996 - 04-02.
  • 7YU N, TAKAO A, TOMOKO A, et al. A novel method of preparation of carboxy - terminated polydimethylsilox- ane and its enhancing effect on transdermal drug penetra- tion [ J]. Makromol Chem Rapid Commun, 1992, 13 (10) : 441 -446.
  • 8COO -RANGER J J, ZELISKO P M, BROOK M A. I- onic silicone surfactants in water - in - oil silicone oil emusions conatining proteins [ J ] . Polym Preprints, 2004, 45 ( 1 ) : 674 - 675.
  • 9O'LENICK A J Jr, PARKINSON J K, ROBERT T T. Silicone alkoxylated esters carboxylates: US, 5296625 [P]. 1994-03-04.
  • 10LANGER M E. Method for making carboxyl aryl termina- ted organosiloxanes : US, 4895965 [ P]. 1990 - 01 - 23.

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