18586-39-5Relevant articles and documents
Phosphorous silane coupling agent and preparation method thereof
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Paragraph 0037-0043; 0047; 0048, (2017/08/31)
The invention relates to a phosphorous silane coupling agent and a preparation method thereof and belongs to the technical field of a functional auxiliary agent. The method comprises the following steps: by taking diphenylphosphine (DPP) or diphenyl oxide phosphine (DPOP) or dimethyl phosphine (DMP) and vinyl silane coupling agent as raw materials, and by taking azo or peroxy substance as a catalyst or taking no catalyst, performing addition reaction on DPP, DPO or DMP and vinyl silane coupling agent under a certain temperature, and then collecting the phosphorous silane coupling agent from the reaction mixture after reacting for a period of time. The method provided by the invention has the characteristics of mild reaction condition, easiness in control, high repeatability, high yield, and the like, and is suitable for expanded production. As a novel phosphorous silane coupling agent, the phosphorous silane coupling agent compounded according to the invention not only can promote the compatibility of some inorganic fillers and high molecular materials but also is beneficial to the promotion of the heat stability of the composite material and the reduction of the combustion property of the composite material.
Silica Hybrid Gel Catalysts Containing Group(VIII) Transition Metal Complexes: Preparation, Structural, and Catalytic Properties in the Synthesis of N,N-Dimethylformamide and Methyl Formate from Supercritical Carbon Dioxide
Kroecher, Oliver,Koeppel, Rene A.,Froeba, Michael,Baiker, Alfons
, p. 284 - 298 (2007/10/03)
Sol-gel derived hybrid materials containing group(VIII) transition metal complexes in a porous silica network were prepared and tested for the catalytic synthesis of N,N-dimethylformamide (dmf) and methyl formate (mf) from supercritical carbon dioxide, hydrogen, and dimethylamine and methanol/triethylamine, respectively. Bifunctional silylether phosphines X = Ph2P(CH2)2Si(OEt)3 and Y = Me2P(CH2)2Si(OEt)3 were used as ligands for the preparation of complexes of the type RuCl2X3, RuCl2Y3, MClX3 (M = Ir, Rh), and MCl2X2 (M = Pt, Pd). The silylether complexes were anchored in a silica matrix by co-condensation with Si(OEt)4. The textural and structural properties of the hybrid gels were characterized by means of 31P and 29Si NMR spectroscopy, extended X-ray absorption fine structure (EXAFS), X-ray diffraction (XRD), transmission electron microscopy (TEM), and nitrogen and argon physisorption. 31P NMR spectroscopy confirmed nondestructive immobilization of the Ru, Pt, Pd, Rh, and Ir complexes. TEM and XRD analyses proved the homogeneity and noncrystallinity of the materials. The degree of condensation of the gels and the molecular mixing of the components has been investigated by solid state 29Si NMR spectroscopy. Textural characterization showed that all gels were micro- to mesoporous. EXAFS measurements indicated no metal-metal interactions, confirming that the organometallic complexes were immobilized as monomers. From all catalysts silica matrix stabilized ruthenium complexes exhibited highest activities at 100% selectivity in dmf synthesis from CO2, H2, and dimethylamine. The corresponding turnover frequency (TOF) of 1860 h-1 exceeded those reported so far for heterogeneous catalysts by a factor of 600. In methyl formate synthesis, TOFs up to 115 h-1 were reached.
