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Zhang L.-J.,East China University of Science and Technology | Zhang L.-J.,Shanghai Kangda New Materials Co. | Lu Q.-T.,Shanghai Kangda New Materials Co. | Hou Y.-B.,Shanghai Kangda New Materials Co. | Ying W.-Y.,East China University of Science and Technology
Gongneng Cailiao/Journal of Functional Materials | Year: 2012

The effect of the activated Raney nickel catalyst composition on the catalytic amination was studied by preparation of trifunctional amine terminated polyether in a magnetically stirred stainless steel autoclave. The experiments indicated that the catalyst with 20% aluminium was more effective for the catalytic amination of polyether polyols, and the total amine of the product was up to 340 mg KOH/g. X-ray diffraction (XRD) was employed to characterize the catalyst properties and the chemical composition was analyzed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The reaction route was deduced on the basis of the products and the off-gas analysis by gas chromatography (GC) and fourier transform infrared spectroscopy (FT-IR). Source


Zhang L.,East China University of Science and Technology | Zhang L.,Shanghai Kangda New Materials Co. | Lu Q.,Shanghai Kangda New Materials Co. | Hou Y.,Shanghai Kangda New Materials Co. | Ying W.,East China University of Science and Technology
Reaction Kinetics, Mechanisms and Catalysis | Year: 2013

A trifunctional amine terminated polyether is synthesized in a magnetically stirred stainless steel autoclave using Raney nickel as a catalyst. The effects of the activation conditions such as the leaching temperature, leaching time, sodium hydroxide concentration and the method of addition of the precursor alloy on the Raney nickel catalyst are studied. The experiments show that 353 K is the preferred leaching temperature to prepare the amine terminated polyether and 120 min is long enough because less aluminum need to be leached from the precursor alloy compared with the conventional Raney nickel catalyst. It is proposed that the effective catalyst should be produced by the leaching of aluminum when CNaOH is 15 wt%, rather than 10 and 20 wt%. X-ray diffraction is employed to characterize the catalyst properties and the chemical composition is analyzed by inductively coupled plasma atomic emission spectrometry. The experiments indicate that the catalyst with 20 wt% aluminum is more effective for the catalytic amination of polyether polyols, and the total amine of the product is up to 340 mgKOH/g, which meets the industrial application requirement. © 2012 Akadémiai Kiadó, Budapest, Hungary. Source


Jiang W.-J.,Shanghai Kangda New Materials Co. | Jiang W.-J.,Fudan University | Yao Q.-S.,Shanghai Kangda New Materials Co. | Fan Z.-Y.,Fudan University | And 2 more authors.
Gongneng Cailiao/Journal of Functional Materials | Year: 2013

The trimellitic anhydride-ethanediol polyester (TEPES) and the trimellitic anhydride-1, 3-butanediol polyester (TBPES) have been synthesized with trimellitic anhydride (TMA), ethanediol (EG) or 1, 3-butanediol (1, 3-BG) as raw materials, and monobutyl tin oxide as the catalyst. The results show that, the hydroxyl value, number average functionality (fn) and weight average functionality (fw) of TEPES are 400.0 mg KOH/g, 6.55 and 7.31, respectively. The hydroxyl value, fn and fw of TEPES are 357.2 mg KOH/g, 5.87 and 6.49, respectively. It can be seen that TEPES has a wider molecular weight distribution than TBPES. 1H NMR spectra and TGA curves reveal that, during the reaction there are not only a single hydroxyl reaction, but also a dihydroxy esterification reaction between dihydroxy alcohol and TMA, which further verify the GPC results. In addition, the synthesized polyester polyols both have a few raw dihydroxy alcohol, which was also identified by TGA. It was indicated that TBPES has a better low temperature thermal stability than TEPES, while its high temperature thermal stability was worse than TEPES. With the same apparent density 60 kg/m3, the PU rigid foams of different polyol synergistic systems, have been prepared with GR-835G, TEPES, TBPES and PM-200, as main raw materials. Comparing to the single system with GR-835G, the compressive modulus of the polyol synergistic system between TEPES and GR-835G, has a greater improvement than that of the polyol synergistic system between TBPES and GR-835G. The compressive strength of PU rigid foams will decrease with TEPES used, however, the compressive properties can be improved using TBPES. Source


Jiang W.-J.,Shanghai Kangda New Materials Co. | Jiang W.-J.,Fudan University | Yao Q.-S.,Shanghai Kangda New Materials Co. | Fan Z.-Y.,Fudan University | And 2 more authors.
Gongneng Cailiao/Journal of Functional Materials | Year: 2013

In this work, the 60 kg/m3 PU rigid foam with high compression performance has been successfully prepared with polyether polyol GR-835G and polymethylene polyphenylisocyanate PM-200 as main raw materials, phenol amine catalyst HP-30 as the catalyst, and H2O as the blowing agent. The results show that, HP-30 can play important roles as not only the trimerization catalyst, but also the blowing agent. The cream time, rise time and gel time of the foaming systems, become shorter with more HP-30, while the apparent densities of the foams have a trend with bigger then smaller, and bigger finally. The H2O dosages need be changed for maintaining the same apparent density with the increase of the HP-30 dosages. However, there was almost no effect to the foaming time and the voscosity of the foaming system with H2O dosage changed under 6wt%. The compression properties of 60 kg/m3 foams can be improved with the HP-30 dosages increased. When the HP-30 dosage is 13pphp, the compressive strength and compressive modulus of the PU rigid foam are 0.772 MPa, 30.0 MPa, respectively. In addition, the possible mechanism of HP-30 has also been disscussed. Source


Zhang L.,Shanghai University of Engineering Science | Zhang L.,Shanghai Kangda New Materials Co. | Yang C.,Shanghai University of Engineering Science | Yao Q.,Shanghai Kangda New Materials Co. | And 3 more authors.
Materials and Manufacturing Processes | Year: 2014

Trifunctional amine-terminated polyether is synthesized continuously over Al2O3-supported Co catalyst in the presence of hydrogen by using a fixed-bed process, and the reactor is 800 ml in volume. The experiments show that the Al2O3-supported Co is effective for the catalytic amination of polyether polyols. When the temperature is 190°C, the pressure is 4 MPa, the total amine of the product is up to 350 mgKOH/g. A ratio (15-20 v%) of hydrogen in the feed, which is a little higher than that required for supported Ni catalyst, is necessary to prevent the undesired side reactions when the amination is performed over Co catalysts. The flow rate exerts a tremendous influence on the degree of amination. The appropriate flow rate for catalytic amination polyether polyols to produce amine-terminated polyether is 0.5 ml/min, where the space time is 0.1 h-1. The total amine of the product is up to 350 mgKOH/g, and the primary amine exceeds 94%, which meets the industrial application requirement. Copyright © 2014 Taylor & Francis Group, LLC. Source

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