2467-03-0Relevant articles and documents
Nano-silica?PVC-bonded N-ethyl sulfamic acid as a recyclable solid catalyst for the hydroxyalkylation of phenol with formaldehyde to bisphenol F
Jiang, Dabo,Zhou, Shuolin,Fu, Zaihui,Xu, Qiong,Xiao, Jiafu,Zheng, Min,Zhong, Wenzhou,Liu, Xianxiang,Kirk, Steven Robert,Yin, Dulin
, p. 1394 - 1403 (2019/09/18)
Sulfamic acid functionalized PVC-coated nano-silica (NS) catalyst (NS?PVC-EDA-SO3H) was prepared via multi-step treatment processes and characterized by FT-IR, N2 adsorption-desorption, TGA/DTG, XRD, TEM, STEM-EDS, as well as acid-base back-titration. The hydroxyalkylation of phenol with formaldehyde to bisphenol F was employed to evaluate in detail its acid catalysis performances. The results indicated that the newly constructed NS?PVC-EDA-SO3H possessed richer short mesoporous to macroporous channels and highly exposed sulfamic acids and could exhibit excellent hydroxyalkylation activity and reusability owing to fast mass transfer and reaction rates for the conversion of substrates, as well as excellent structural and chemical stabilities. This new solid acid was obviously superior to the conventional homogeneous concentrated sulfuric acid and heterogeneous sulfonated resin catalysts in catalytic activity and reusability, which could achieve a remarkable formaldehyde conversion (99.9%) and selectivity of bisphenol F (94.5%) under optimal hydroxyalkylation conditions. Furthermore, it could also be recovered easily and used repeatedly at least nine times without an obvious decrease in activity.
The invention relates to a multi-polyoxymethylene dimethyl ether as raw materials for preparing bisphenol F method
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Paragraph 0031; 0034, (2017/08/25)
The invention relates to a method for preparing bisphenol F by adopting polyoxymethylene dimethyl ethers (PODEn; n is larger than or equal to 2 and smaller than or equal to 8) as a raw material. The method comprises the main step of carrying out a hydroxyl alkylation reaction between phenyl hydroxide and PODEn under the condition of acid catalysis, so as to obtain a target product, wherein the hydroxyl alkylation reaction can be performed in the absence of water or in the presence of water. The method has the advantages that the solubility of PODEn in phenyl hydroxide and water is high, so that a bisphenol F synthesis system serves as a homogeneous-phase system, and is conducive to heat and mass transfer; besides, PODEn has an effect of quantitatively and slowly releasing formaldehyde, so that the hydroxyl alkylation reaction is mild and easy to control, side reactions are less, such by-products as triphenol and phenolic resin are unlikely to generate, and the advantages of high yield and selectivity are achieved.
Highly efficient and recyclable alkylammonium hydrosulfate catalyst for formation of bisphenol F by condensation of phenol with formaldehyde
Xiao, Jiafu,Huang, Hua,Xiang, Weijian,Liao, Wei,Liu, Junyi,She, Xichun,Xu, Qiong,Fu, Zaihui,Kirk, Steven Robert,Yin, Dulin
, p. 92716 - 92722 (2016/10/11)
Several C1-C4 alkylammonium hydrosulfates [R3NH][HSO4] have been conveniently prepared from the cheap raw materials sulfuric acid and alkylamines. Their acidities were measured by chemical titration and determined using UV-vis spectroscopy with a basic indicator 4-nitroaniline. The catalytic performance of these hydrosulfates for the condensation of phenol with formaldehyde to bisphenol F (BPF) was evaluated in detail on a batch reactor. The results indicated that the proposed catalysts are very active for such condensation due to its homogeneous catalysis characteristics in reaction conditions. Among the catalysts examined, [H3NCH2CH2NH3][HSO4]2 shows the best catalytic performance and it can achieve a complete conversion of formaldehyde, providing a higher than 90% selectivity for BPF under the optimal conditions. Furthermore, the catalyst can be recovered from the reaction mixture via an azeotropic distillation with cyclohexane to remove water and then filtration and used repeatedly six times almost without loss of activity, showing an excellent reusability. It is suggested that the present catalytic process combines the characteristics of a homogenized reaction and heterogenized recovery so might provide a highly-efficient, environmentally-friendly and low-cost route for synthesis of bisphenol F.