Preparation and application of diphenylphosphinic acid chloride_Kain Industrial Additive

Background and overview^[1]

Diphenylphosphinic acid chloride can be used to prepare composite retarding water-reducing agents for concrete, flame retardants diphenylphosphinic acid-N-cage phosphate ester amine compounds, etc. It can be prepared from diphenylphosphine chloride and Preparation by trifluoromethanesulfonic acid reaction.

Preparation^[1]

Put 27.8g triphenylphosphine oxide, 88.2g diphenylphosphine chloride (the mass ratio of the two is 1:3.17), and 0.56g trifluoromethanesulfonic acid (triphenyl 2% of the mass of base phosphine oxide), raise the temperature to 150°C, and keep it warm for 12 hours. After cooling to room temperature, turn on the vacuum pump. After the vacuum degree reaches 0.098Mpa, slowly raise the temperature to intercept the mixture of diphenylphosphine chloride and diphenylphosphinic acid chloride.

Apply^[2-3]

Application 1,

CN201710971195.8 discloses a composite retarding water-reducing agent for long-distance pumping of concrete, which relates to the technical field of concrete additives and is made of the following raw materials in parts by weight: 35-45 parts of naphthalene series water-reducing agent , 10-15 parts of soil-grade polyglutamic acid, 5-10 parts of nano-powder, 5-10 parts of ultra-fine wollastonite powder, 1-5 parts of crospovidone, 1-5 parts of polydipentaerythritol hexaacrylate parts, 1-5 parts of trimethylolpropane triglycidyl ether, 0.5-2 parts of sodium gluconate, and 0.5-2 parts of diphenylphosphinic acid chloride. The retarded water-reducing agent prepared by the invention has good water-reducing effect, good water retention, low bleeding rate and low gas content; it can effectively delay the hydration process of cement and adjust the setting time so that the initial setting time is about 8 hours. The final setting time is about 10 hours.

Application 2,

CN201811145924.5 relates to a flame retardant diphenylphosphinate-N-cage phosphate ester amine compound and its preparation method. The structure of the compound is as shown in the following formula: The preparation method is: adding Cage phosphate ester amine and triethylamine, use nitrogen to drive out the air in the reactor, add diphenylphosphinic acid chloride dropwise within 1 hour at 20°C, limit the molar ratio of the reaction materials to diphenylphosphinic acid chloride ∶ Cage phosphate ester amine: triethylamine = 1:1:1-1:1.2:1, control the dropping temperature not to be higher than 50℃, after the dropwise addition is completed, raise the temperature to 80-110℃, reflux for 4-6 hours. Afterwards, it was cooled and filtered, washed with water, and dried under vacuum to obtain a light yellow solid diphenylphosphinic acid-N-cage phosphate ester amine. The compound of the present invention is an excellent phosphorus-nitrogen synergistic flame retardant and is suitable for use as a flame retardant for polyamide, polyester, polyurethane, fiberglass, polyolefin and other materials. The process is simple, the equipment investment is small, and it is easy to realize industrial production.

References

[1]CN201810201659.1 A method for preparing triphenylphosphine by reduction

[2]CN201710971195.8 A composite retarding water-reducing agent for long-distance pumping of concrete

[3]CN201811145924.5 flame retardant diphenylphosphinate-N-cage phosphate ester amine compound and preparation method thereof