Chinese Journal of Applied Chemistry ›› 2020, Vol. 37 ›› Issue (3): 307-313.DOI: 10.11944/j.issn.1000-0518.2020.03.190233

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Optimal Activation Temperature of γ-Al2O3 for Catalytic Synthesis of Poly(oxy-1,2-ethanediyl)methylphosphonate

SUN Caiyinga,REN Biaobiaoa,DONG Tianheb*(),DAI Qiuboc,XIAO Boa   

  1. a Heilongjiang Key Laboratory of Molecular Design and Preparation of Flame Retarded Materials,College of Chemistry, Chemical Engineering and Resource Utilization/
    b School of Landscape Architecture Northeast Forestry University,Harbin 150040,China
    c Chifeng Product Quality and Mearurement Inspect Institute,Chifeng,Inner Mongolia 024000,China
  • Received:2019-09-03 Accepted:2019-12-13 Published:2020-03-01 Online:2020-03-10
  • Contact: DONG Tianhe
  • Supported by:
    Supported by the Fundamental Research Funds for the Central Universities(No.2572018BK04)

Abstract:

Poly(oxy-1,2-ethanediyl)methylphosphonate(PEMP) as a good flame retardant has lots of benefits such as non-toxic, low smoke, high phosphorus content and better flame retardant effects. γ-Al2O3 is a good catalyst for the condensation of ethylene glycol (EG) and dimethyl phosphate (DMMP) to produce PEMP. However, since γ-Al2O3 is easy to absorb CO2 and water to reduce its catalytic activity, activation is needed before use. The activation temperature affects the catalytic activity of γ-Al2O3. In this paper, γ-Al2O3 was activated at different temperatures from 300 ,400, 500, 600, 700 and 800 ℃. γ-Al2O3 crystal form was analyzed by X-ray difraction (XRD) and its specific surface area, pore diameter and pore volume were measured by Brunauer-Emmett-Teller (BET) method. The change of infrared absorption was analyzed by Fourier transfer infrared (FTIR). The relative contents of Brønsted acid and Lewis acid sites in γ-Al2O3 were determined by pyridine adsorption-FTIR. The purity and viscosity of PEMP catalyzed by γ-Al2O3 were compared, and the optimal activation temperature of γ-Al2O3 was found to be 400, 500 and 600 ℃. At this time, γ-Al2O3 is a typical γ-Al2O3 with large specific surface area and small pore diameter, and the obtained PEMP product has the highest purity.

Key words: poly(oxy-1,2-ethanediyl)methylphosphonate, γ-Al2O3, activation temperature, catalyzed activity