15090-23-0Relevant articles and documents
Synthesis and performance of star-shaped aluminum phosphinate flame retardant
Zou, Liyong,Liu, Jiyan,Liu, Xueqing,Wang, Xiaomeng,Chen, Jia
, p. 1399 - 1409 (2016)
A star-shaped aluminum dimethyl(2,2-dimethyl-1,3-propylene)bis(oxy)bicarbonylethyldiphos phinate (AlCP) was synthesized by esterifying reaction between 2-methy-2,5-dioxo-1,2-oxaphospholane (OP) and neopentyl glycol following by neutralizing with aluminum hydroxide. The structure and composition were confirmed with FTIR, 1H NMR, 31P NMR and X-ray fluorescent spectroscopy. AlCP begins to decompose at 370?°C, matching the initial decomposition temperature of PBT. It endows PBT with desired flame retardancy and anti-dripping property and shows good compatibility with PBT. When the total filler loading is kept at 17, 15–13?mass% AlCP combining with 2–4?mass% MC can make the PBT passing the UL 94 V0 rating and eliminating dripping. In addition, the AlCP has a little influence on the mechanical properties of PBT. The tensile strength and notched impact strength of PBT containing 17?mass% AlCP only reduce by 5.6 and 4?%, respectively, comparing to the pure PBT. The SEM photographs show that AlCP has a good compatibility with PBT. Microcombustion calorimeter, TG-FTIR and SEM results show that AlCP can depress the heating release and promote char forming during combustion and acts mainly in the condensed phase.
Interaction of 2-methyl-2,5-dioxo-1,2-oxaphospholane with trimethylsilyl cyanide
Odinets, I. L.,Antonov, E. A.,Petrovsky, P. V.,Morozik, Yu. I.,Krivolapov, Yu. A.,et al.
, p. 154 - 161 (1993)
The reaction of 2-methyl-2,5-dioxo-1,2-oxaphospholane (1) with trimethylsilyl cyanide was found to give, depending on conditions, three organophosphorus compounds: trimethylsilyl methyl(2-cyanocarbonylethyl)phosphinate (2), trimethylsilyl methyl(3-trimethylsiloxy-3,3-dicyanopropyl)phosphinate (3) and trimethylsilyl methyl(3-trimethyl-siloxy-3-cyano-2-propenyl)phosphinate (4).On hydrolysis of 3 under mild conitions, methyl(3-hydroxy-3,3dicarboxypropyl)phosphinic acid (7) was obtained.The latter is readily decarboxylated on heating to give methyl(3-hydroxy-3-carboxy-propyl)phosphinic acid (8).The interaction of 2 and 4 with water or alcohols gives, correspondingly, methylphosphinic acids (11-13).Methyl(2-oxamoylethyl)phosphinic acid (14) was prepared by successive treatment of propenylphosphinate 4 with HCl gas and water.
Preparation method of 2-carboxyethyl methyl phosphinic acid
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Paragraph 0051-0052; 0060-0063, (2018/06/15)
The invention discloses a preparation method of 2-carboxyethyl methyl phosphinic acid and belongs to the technical field of organic synthesis. The invention aims to provide the preparation method of 2-carboxyethyl methyl phosphinic acid, which is simple in operation, few in byproduct, high in yield and low in cost. The preparation method of 2-carboxyethyl methyl phosphinic acid comprises the following steps: performing reaction on methylphosphoric dichloride and acrylic acid, adding water after reaction, enabling the system to react in a mixed solution of water and an organic solvent, and obtaining 2-carboxyethyl methyl phosphinic acid after reaction. By the method, 2-carboxyethyl methyl phosphinic acid is prepared by a one-pot method efficiently, an intermediate does not need to be separated, the method is simple and safe in operation, the byproducts are few, the yield is high, the purity is high, the production cost of 2-carboxyethyl methyl phosphinic acid is obviously reduced and industrialized production is facilitated.
4 - (hydroxy-(methyl) phosphinyl) - 2-oxo-butyric acid production process
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Paragraph 0060; 0061; 0080; 0082; 0083; 0084; 0085, (2017/02/24)
The invention discloses a preparation method of 4-(hydroxy-(methyl)phosphinyl)-2-oxobutyric acid. The preparation method comprises following steps: synthesis of methylphosphoric dichloride; recovery of diethyl phthalate, synthesis of methyl chloro phosphinic propionyl chloride; synthesis of methoxyl methyl phosphinic methyl propionate; synthesis of 4-(hydroxy-(methyl)phosphinyl)-2-oxobutyric acid; and post treatment. Technology processes of the preparation method are simple; yield is high; production cost is low; and production technology is clean. In addition, when 4-(hydroxy-(methyl)phosphinyl)-2-oxobutyric acid obtained by the preparation method is used for synthesis of weed killer glufosinate-ammonium, levo glufosinate-ammonium with high weed killing function is obtained, so that weed killing effect of glufosinate-ammonium is improved greatly.
