33 5 Vol. 33, No. 5 2 0 0 5 5 J OURNAL OF T H E CHIN ESE CERAMIC SOCIET Y May, 2 0 0 5 1, 1 2, (1., 100083 ; 2., 100024) : 2 (polypropylene,pp), PP/ ( scanning elec2 tron microscope, SEM),Fourier PP/ SEM : A 174 FR 693 1. 5 % 1. 0 % 80 PP/ 0. 3 kj/ m 2, 30 %, FR 693 1 MPa,2 : ; ; ; ; : T G985 : A : 0454 5648 (2005) 05 0659 06 SURFACE MODIFICATION OF ULTRA2FINE BRUCITE POWDER BY SILANE COUPL ING AGENT DU Gaoxiang 1, Z H EN G S huilin 1, L I Yang 2 (1. Department of Chemistry and Environment Engineering, China University of Mining and Technology, Beijing 100083 ; 2. Beijing University of Technology, Beijing 100024, China) Abstract : Surface2modified ultra2fine brucite powder is a kind of environment2f riendly fire2retardant of polymer. The ultra2fine brucite powder was surface2treated with two kinds of silane (A 174 and FR 693), and then filled into polypropylene ( PP) as a kind of fire2retardant aimed. The effect of modification by silane on the properties of PP/ brucite composite material was stud2 ied. The effect and modification mechanism were investigated by means of Fourier transfer infrared analysis, scanning electron microscopy of brucite powder and the f resh new surface of PP/ brucite. The result s show that the optimal dosage of brucite powde for silane A 174 and silane FR 693 is 1. 5 % and 1. 0 % in mass respectively and the temperature of surface treatment is 80. It indicates that the surface modification can enhance the izod impact strength of PP/ Mg (O H) 2 composite material by 0. 3 kj/ m 2, the bend modulus about 30 %, and the retardant degree is enhanced to V 0 from V 1. The tensile strength of the composite material surface modified with silane FR break of the material are not improved by both silane. 693 can be increased 1 MPa. The bending strength and elongation at Key words : brucite ; magnesium hydroxide ; surface modification ; silane coupling agent ; polypropylene, : 2004 07 29 : 2004 11 24 : (1976 ),, : (1956 ),,,, Received date : 2004 07 29. Approved date : 2004 11 24. First author : DU Gaoxiang (1976 ), male,postgraduate student for E doctor degree. mail : dugaox @sohu. com Correspondent author : ZHENG Shuilin(1956 ), male, doctor, professor. E mail : shuilinzh @sina. com. cn
660 2005,, [ 1,2 ],,, 6 cm, 5 ml,, [3 ], PP/ (, ) : PP 100 [4,5 ] ; 0. 3 ; 120 ; PP PP/ : PP, 100 ;, 0. 3 (polypropylene,pp) ;,5 : 1 PP/, 1. 1 ( scanning elect ro n micro scope, SEM) :MgO 64. 03 % ; CaO 0. 63 % ; SiO2 2. 56 % ; Fe2 O3, KBr 1. 48 % ;700 31. 30 %, Fourier ( Fourier transfer A 174 inf rared, F TIR) SEM FR 693,,, 1. 2 Fourier, WQ F 410, 2, S 450,, SHL 35 2. 1,, IS75PN II 2. 1. 1,,, Stanto n Red2 croft, Tarlin Scientific [6 ] 80 1,CZF 2,,XJ 300A,,D LL 10000, 1. 3 200 g/ L, A 174,FR 693, 50 min, 0. 25 g, 50 ml 10 min, 25 ml, 180 190 PP 1, PP/ Fig. 1 Effect of dosages of silane on the settling time of brucite powder in kerosene
33 5 : 661 ( ) d50 = 1. 03 m, d97 = 2. 05 m 1, 2, 2, A 174 1. 5 %, 10. 0 h 52. 2 h, ; FR 693 1. 0 %, 2 Fig. 2 Effect of surface modified temperatures on the 48. 3 h, set2 tling time of brucite powder in kerosene, A 174 FR 693 1. 5 % 1. 0 % Mass ratio of silane to brucite : A 174,1. 5 % ; FR 693, 2. 1. 2, 2. 2 PP 2 A 174,FR 693 [7 ], PP, 1. 5 % 1. 0 % PP 120 %, d50 = 0. 80 m, d97 = 1. 5 m PP/, 2 PP, 1 PP 1. 2 d50 = 1. 03 m, d97 = 2. 05 m 1,, PP/ 80,A 174 FR 693, 3 % 2 1, 2 10. 9 kj / m 2,,, 30 % 2, PP/ 80 FR 693 Material Izod impact strength/ (kj m - 2 ) 1. 0 % 1 PP/ Table 1 Mechanics and f ire2retardant properties of PP/ brucite composite materials Tensile strength/ MPa Elongation at break/ % Bending strengt h/ MPa Bending modulus/ MPa Oxygen index/ % Melted drops when burning Smoking situation when burning UL94 retardant degree PP (pure) 15. 0 35. 4 > 50 48. 3 1 351 19. 4 Many Thick smoke Less PP/ brucite (non2 modified) PP/ brucite (modified by A 174) PP/ brucite (modified by FR 693) PP/ brucite (MA GNIFIN H10) 10. 6 28. 3 3 42. 1 4 315 26. 3 No Little smoke V 1 10. 9 27. 5 2. 45 40. 9 5 620 30. 1 No No V 0 10. 9 29. 3 2. 5 42. 8 5 837 30. 7 No No V 0 8. 6 18. 6 1. 4 3 120 No No V 0 Note : The izod impact strength of materials is measured according to the standard of GB/ T1843 1996, tensile strength and elongation at break according to the standard of GB/ T1040 92, bend properties according to the standard of GB/ T9431 2000. The oxygen index is measured according to the standard of AST2 MD 2863 and the UL94 retardant degree according to the standard of ANSI/ UL94 1985. The melted drops and smoking situation are obtained by observa2 tion when the materials are burning. MA GNIFIN H10 is a kind of brucite products of MARTIN Co. Ltd.
662 2005 PP/ 1 MPa, A 174 2 Martin, 1,, PP 19. 4 26. 3, V 1,, PP 2 30. 1 30. 7,, V 1 V 0,,, 2. 3 2. 3. 1 SEM, 2 SEM, 3 3,, SEM 2,,,,,, 3 SEM, Fig. 3 SEM ( scanning electron microscope) photographs 2. 3. 2 F TIR 2 of brucite powders, 2 F TIR 970. 24 cm - 1 889. 23 cm - 1, 4 4,3 697. 73 cm - 1 OH, 1 645. 36 cm - 1 ;1 429. 33 cm - 1 ;450 cm - 1 Mg O 4 F TIR 1 384. 96 cm - 1 CO3 2 -,, 2, CO2 1 087. 91 cm - 1 OCH3 1 190 cm - 1,
33 5 : 663 4 FTIR Fig. 4 FTIR spectra of brucite powders modified by siliane coupling agent s 1 Sample of non2modification ; 2 Sample modified by A 693 174 ; 3 Sample modified by FR F TIR, 1 645. 36 cm - 1 1 384. 96 cm - 1, 1 429. 33 cm - 1 5 PP/ SEM 1 458. 26 cm - 1, Fig. 5 SEM photographs of PP/ brucite composite mate2, rials Si O Mg 2. 3. 3 PP SEM F TIR,, PP, 2 PP 5. 0 % PP, : SEM, 5 5a, PP, PP, PP 100 m, PP, 3 5a PP (1) A 174 FR 693,, PP 5b, PP PP, :A 174 FR 693
664 2005 1. 5 % 1. 0 %, 80 (2) A 174 FR 693 PP/ FR 693 1 MPa, A 174 2 PP/ : [1 ] WEBER M. Mineral flame retardant s overview and future trends[j ]. Ind Miner, 2000 (2) :19 28. [ 2 ],,. ogy, 2002. 11, 34 40. [J ]., 2002, 25 ( ) :10 13. DU Gaoxiang, ZHEN G Shuilin, L I Yang. Non2Met Miner (in Chinese), 2002, 25 (suppl) :10 13. [3 ]. [J ].,1996 (2) : 33 35. LU Kaijun. J Miner Protection Use (in Chinese), 1996 ( 2) : 33 35. [ 4 ]. [J ].,1997,26 (1) :5 9. GUO Ruxin. Sea Salt Lake Chem Technol (in Chinese),1997, 26 (1) :5 9. [ 5 ],,,. [J ]., 2001, 20 (5) :500 502. NI Zhongbin, CHEN Mingqing, YAN G Cheng, et al. J Wuxi Light Ind Univ(in Chinese), 2001, 20 (5) :500 502. [ 6 ]. [ D]. :, 2002. 11, 34 40. DU Gaoxiang. The preparation of super2fine and surface modi2 fied brucite powder filler used as a kind of fire2retardant (in Chinese, dissertation). Beijing : Beijing University of Technol2 [ 7 ],,,. ( REC) PP/ Mg (O H) 2 [J ]., 2001, 10 :57 60. FEN G Jiachun, CHEN Mingcai, ZHAN G Xiuju, et al. Chin Plast (in Chinese), 2001,10 :57 60. 33 5 2005 5 ( 1957 ) Journal of the Chinese Ceramic Society Vol. 33, No. 5, May, 2005 (monthly, started in 1957) : : Sponsor : The Chinese Ceramic Society Editor in Chief : GAN Fuxi : Responsible Editors : CH EN Tianpeng ; YU Baoting : ; Edited and Published by Editorial Department of Journal of the :, 100831 Chinese Ceramic Society : (010) 88376444 ; 68352977 : (010) 68342016 E mail :jccs @ceramsoc. com E mail :jccs @ceramsoc. com : Http :/ / www. ceramsoc. com ; : : ( 399, 100044) ISSN 0454 5648 : CN 11 2310/ TQ Responsible Institution : China Association for Science and Technology Baiwanzhuang, Beijing 100831, China Tel : (010) 88376444 ; 68352977 Fax : (010) 68342016 Overseas Distributed by gsyxb. periodicals. net. cn ; gxyb. chinajournal. net. cn China International Book Trading Corporation ( P. O. Box 399, Beijing 100044, China) :25 2005 5 BM57 2-695 0583