1068-07-1Relevant articles and documents
Free radical reaction of α-haloalkylphosphonates with alkenes and alkynes: A new approach to modified phosphonates
Balczewski,Mikolajczyk
, p. 392 - 396 (1995)
A new approach to the synthesis of phosphonates 3 functionalized in the α- and γ-phosphonate positions by alkyl, ethoxy, butoxy, acetoxy, acetyl and cyanide groups and allylphosphonate 6 is described. It is based on the radical reaction of α-halosubstituted phosphonates 1 (X = Cl, Br, I) with the terminally unsubstituted alkenes 2 (1-heptene, ethoxyethene, butoxyethene, acetoxyethene, acrylonitrile, methyl vinyl ketone) and alkyne 5 (hept-1-yne). The reaction involving the tin hydride method (Bu3SnH/AIBN) was more effective with alkenes than with alkynes (40-72% versus 20-30%). With electron-rich alkenes, chloro- and bromomethylphosphonates 1 (X = Cl, Br) gave higher yields than iodomethylphosphonate 1 (X = I). Diethyl methylphosphonate 4, as a reduction product of 1, accompanied 3 and 6 in the above reactions. The yield of 4 could be reduced by optimizing the reaction conditions.
A solution-based approach to composite dielectric films of surface functionalized CaCu3Ti4O12 and P(VDF-HFP)
Ehrhardt, Claudia,Fettkenhauer, Christian,Glenneberg, Jens,Muenchgesang, Wolfram,Leipner, Hartmut S.,Diestelhorst, Martin,Lemm, Sebastian,Beige, Horst,Ebbinghaus, Stefan G.
, p. 2266 - 2274 (2014)
High permittivity CaCu3Ti4O12/ poly(vinylidenefluoride-co-hexafluoropropylene) P(VDF-HFP) nanocomposites were investigated as dielectrics for film capacitors. CaCu3Ti 4O12 was synthesized by two different soft-chemistry methods, namely, decomposition of a citrate precursor and a recently developed lactate precursor to identify a preferable route to nanometer scale spherical particles with an increased interfacial area. A ball-milling step was applied to break particle agglomerates and to enhance particle distribution in the composite films. To improve the wetting of the CaCu3Ti 4O12 oxide particles and the polymer, a variety of surfactants, e.g. carbonic acid, silane, sulfonic acid and phosphonic acid were investigated. A successful oxide surface functionalization was achieved by 2,3,4,5,6-pentafluorobenzyl phosphonic acid, leading to stable bonds and good structural compatibility between the surfactant and the highly fluorinated polymer matrix. The films were prepared from composite dispersions by a spin-coating technique and can be formed out of powders from both precursors, but the citrate method is preferable due to milder synthesis conditions and improved film homogeneity. The use of ball-milled powders as the oxide component results in homogeneous particle distributions even near to the percolation threshold. In addition, such fine-ground particles lead to homogeneous film thickness and decreased film roughness. Dielectric measurements at different frequencies revealed an enhancement in the relative permittivity by a factor of 5 compared to the pure polymer while the dielectric losses remained very low.
Maier
, p. 1190,1193 (1965)
Method for preparing n-octylphosphonic acid
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Paragraph 0020, (2016/11/17)
The invention provides a method for preparing n-octylphosphonic acid. The method includes the following steps that firstly, n-octylphosphonic acid ester and concentrated hydrochloric acid are added into a reaction kettle, 98% sulfuric acid is added dropwise, stirring is continuously carried out, after sulfuric acid is completely added dropwise, the temperature is raised to 115-118 DEG C and kept for 25-35 hours, the mixture is naturally cooled to 55-65 DEG C, the materials are discharged from the reaction kettle after reaction, the reacted materials are cooled to 25-35 DEG C and is placed for 12 hours or above at the temperature of 25-35 DEG C, and a n-octylphosphonic acid crude product is obtained through centrifugal separation; secondly, the n-octylphosphonic acid crude product is recrystallized to obtain n-octylphosphonic acid. An acid catalyst used in hydrolysis reaction in the preparing process of n-octylphosphonic acid is a mixture of hydrochloric acid and sulfuric acid, is cheap and easy to obtain, and makes hydrolysis of ester thorough.
Non-metallic compd. Bisphosphonic acid crosslinked layered manufacturing method
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Paragraph 0117, (2017/01/02)
PROBLEM TO BE SOLVED: To provide a novel noncrosslinking type layered phosphonic acid metal compound which has high crystallinity and a uniformly introduced multicomponent phosphonic acid and is free of a fluorine atom, and to provide a method for the production of the same.SOLUTION: The method for the production of the noncrosslinking type layered phosphonic acid metal compound includes a reaction step of reacting two or more monophosphonic acids or derivatives thereof having predetermined conditions with a metal source that can generate a hexacoordinated metal atom ion to be a central atom (M) of a metal oxide octahedron upon reaction in the presence of a sulfuric acid catalyst. The noncrosslinking type layered phosphonic acid metal compound obtained by the production method is also provided.