Study on preparation and factors of amino silicone with low viscosity(2)

Effect of pumpdown time. In principal there will be some small molecules of water, methanol and other volatile fractions produced to impacting performance of PDMS. So it must be vacuum-pumping to improve the purity. As seen in Fig.7, around the pumpdown time from 0 to 150min there was a sharp increment in the viscosity with other factors settled. As it got up to 40min, the extraneous components had been already removed completely. So the best pumpdown time was 40min.

V i s c o s i t y (m P a s )

MM(%)

V i s c o s i t y /(m P a s )

Time/(min)

Fig.6 Effect of the MM’s amount Fig.7 Effect of pumpdown time Structures

analysis. A typical IR spectrum of the synthesized PDMS, as shown in Fig. 8, displayed bands at 3360cm ?1 (-NH 2, stretching), 2851, 2920cm -1(-CH 2, -CH 3, stretching), 1260, 1420cm ?1 (Si-CH 3, stretching), 1020-1110cm ?1 (Si-O-Si, stretching) and 800cm ?1 (CH 3-Si-CH 3, stretching). These bands were characteristics of the desired compounds. Furthermore, the structure of the compounds was further supported by the 1H-NMR spectrum (Fig.9), which gave signals at &0.1ppm (Si-CH 3), 0.52ppm (Si-CH 2), 1.55ppm (CH 2-CH 2), 2.61ppm (NH-CH 2), 2.67ppm (NH-CH 2), and 3.45ppm (NH 2-CH 2). From these characterizations, it evidently confirmed that PDMS had been produced.

40003500300025002000150010005000

20

40

60

80

100

T (%)λ/cm -1ppm (t1)-1.00.01.02.03.04.05.0

500000100000

Fig.8 FTIR spectrum of the PDMS Fig.9 1H-NMR spectrum of the PDMS

Conclusions

Amino value was depended on the amount of resin acceptor YDH-602, having no connection with the process conditions. In all cases, in the previous described reaction conditions, the viscosity for PDMS was mainly determined by reaction temperature, time, the amount of catalyst, accelerating agent and capping agent, pumpdown time. Thus, the process conditions should be confirmed by considering the actual needs. And the optimum ones to get PDMS with less than 100mPas viscosity were as followed: reaction temperature 100-110°C, time 3h, KOH 0.05%, DMSO 0.5% and MM 5-7%, distilling at 110°C/0.095Mpa for 40 min.

Reference

[1] SMA El Ola, R Kotek, WC White: Polymer. Vol.45 (2004), p.3215–3216

[2] M.S.Kim, T. J. Kang: Dimensional and Surface Properties of Plasma and Silicone Treated

Wool Fabric (Textile Research Journal, USA 2002)

[3] S.C. Mehta:Variation in emulsion stabilization behavior of hybrid silicone polymers with

change in molecular structure: Phase diagram study(Journal of Colloid and Interface Science, USA 2009)

[4] Y.Q. Zhuang, X. Ke, X.L. Zhan: Particle kinetics and physical mechanism of microemulsion

polymerization of octamethylcyclotetrasiloxane (Powder Technology, Switzerland 2010)

[5] Y.J.Xu, H.Yin, S.F.Yuan, Z.R.Chen: Film morphology and orientation of amino silicone

adsorbed onto cellulose substrate (Applied Surface Science, Holland 2009)

[6]

M. Cazacu, M. Marcu, A. Vlad, D. Caraiman, C. Racles: Synthesis of functional telechelic

polydimethylsiloxanes by ion-exchangers catalysis (European Polymer Journal, England 1999)

[7] M.C.Burrell: Angle-dependent XPS study of functional group orientation for aminosilicone

polymers adsorbed onto cellulose surfaces(Applied Surface Science , Holland 2004)

[8] Y.B. Zhong, J.M. Xia, S.S. Xing: Piperazinyl the preparation for modified silicone oil with

low-yellowing(Ningbo Chemical Industry, China 2010, In Chinese)

[9] X.Y. Shentu, K.Z. Jiang, L.G. Lu, Z.Y. Hu: Dyeing.Vol.9 (2006), p.33–35.

[10] F.G.Guo: Synthesis, characterization of aminosilicone and its study of microemulsification

(China Leather, China 2005, In Chinese)

Equipment Manufacturing Technology and Automation

10.4028/d92bb21d10a6f524ccbf85c2/AMR.317-319

Study on Preparation and Factors of Amino Silicone with Low Viscosity 10.4028/d92bb21d10a6f524ccbf85c2/AMR.317-319.2449