Diethyl phosphinate fire retardation agent preparation method

A technology of diethyl phosphinate and diethyl phosphinic acid is applied in the field of preparation of diethyl phosphinate flame retardants without monoethyl phosphinic acid group, and can solve the problem of no diethyl phosphinate. Problems such as detailed data of aluminum base phosphinate, complex process, and increased process procedures

Active Publication Date: 2013-09-25
TAIZHOU BAILLY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Chinese patent CN101624401 A reports a method for preparing dialkylphosphine by free radical reaction between olefin and phosphine under the action of an initiator, and then preparing dialkylphosphinic acid through oxide oxidation and other processes. The cost is high, and there is no report on the preparation of dialkylphosphinic acid and its salts by the alkylation of light olefins and phosphine
Chinese patent CN101048344 A reports the method of removing monoalkylphosphinic acid salts by alkali washing to achieve purification of dialkylphosphinic acid and its salts. In 2011, Yang Li of Nankai University reported in "Chemical Reagents" that the method used in strong acid conditions The following methods for preparing aluminum diethylphosphinate with higher purity, there is no detailed data on aluminum diethylphosphinate, both methods are resolved during post-processing and the product does not contain mono-alkylphosphinate According to the report of Chinese patent CN101891762 A jointly applied by Yang Li and others, there is no solution to remove the method of monoalkylphosphinic acid or monoalkylphosphinate
However, regardless of the use of alkali washing method or the preparation of relatively pure dialkylphosphinic acid and its salts under strong acid, the process procedure is increased, especially the treatment of waste liquid is troublesome.

Method used

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  • Diethyl phosphinate fire retardation agent preparation method
  • Diethyl phosphinate fire retardation agent preparation method
  • Diethyl phosphinate fire retardation agent preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 212g of sodium hypophosphite, 120g of acetic acid and 44g of ethylene glycol monomethyl ether into an 800mL acid-resistant and pressure-resistant reactor that can be heated and cooled, heat the materials in the reactor to 80°C, and pass ethylene into the reactor through a pressure reducing valve and make the pressure in the kettle reach 1MPa, add the mixture composed of 20g of azobisisobutyronitrile, 0.4g of copper complex and 44g of ethylene glycol monomethyl ether in batches under stirring at 800 rpm, add the initiator During the process, the ethylene pressure in the reactor should not be lower than 0.8MPa, the temperature should not be higher than 90°C, and the addition should be completed within 10 hours. Reactor is cooled to room temperature, excess ethylene is fed into bromine water to recover when the pressure is released, and finally the dissolved ethylene is driven out of the liquid with nitrogen to obtain a product with a total weight of 558g (theoretical 5...

Embodiment 2

[0054] Add 212g of sodium hypophosphite, 185g of propionic acid and 44g of ethylene glycol monobutyl ether into an 800mL acid-resistant and pressure-resistant reactor that can be heated and cooled, heat the materials in the reactor to 80°C, and feed ethylene into the reaction through a pressure reducing valve. In the kettle and make the pressure in the kettle reach 1MPa, add the mixture consisting of 20g of azobisisobutyronitrile, 0.4g of copper complex and 44g of ethylene glycol monobutyl ether in batches at 800 rpm, add the initiator During the process, the ethylene pressure in the reactor should not be lower than 0.6MPa, the temperature should not be higher than 95°C, and the addition should be completed within 10 hours. Reactor is cooled to room temperature, excess ethylene is fed into bromine water to reclaim during decompression, finally drives away dissolved ethylene in the liquid with nitrogen, obtains the product of total weight 589g (theoretical 582.4g), corresponding...

Embodiment 3

[0060] Add 424g of sodium hypophosphite, 250g of acetic acid and 100g of butyl ether into a 1500mL acid-resistant and pressure-resistant reactor that can be heated and cooled. When the internal pressure reaches 1.2MPa, add a mixture of 30g di-tert-butyl peroxide, 0.6g copper complex and 100g butyl ether in batches at 600 rpm, and keep the ethylene pressure in the reaction kettle during the process of adding the initiator. Lower than 0.6MPa, the temperature is not higher than 100°C, and the addition is completed within 16 hours. Reactor is cooled to room temperature, excess ethylene is fed into bromine water recovery during decompression, finally drives away the dissolved ethylene in the liquid with nitrogen, obtains the product of gross weight 1112.0g (theoretical 1108.6g), is equivalent to consuming 227.4g ethylene absorption ( Theoretical absorption of ethylene 224g).

[0061] The resulting product is moved into a still, and the mixture of butyl ether and acetic acid is rec...

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Abstract

The present invention relates to a preparation method of a diethyl phosphinate fire retardation agent for a polymer material, wherein the diethyl phosphinate fire retardation agent does not contain monoethyl phosphinate. The preparation method comprises that: hypophosphorous acid and/or hypophosphite, an organic acid and an organic solvent are subjected to a reaction under a condition of ethylene gas introduction, the obtained material and an initiation system formed by an initiator, an auxiliary initiator and an organic solvent are subjected to a reaction to obtain monoethyl hypophosphorous acid-free diethyl hypophosphorous acid and organic acid sodium, and the diethyl hypophosphorous acid, the organic acid sodium and a metal compound are subjected to a reaction to obtain the monoethyl phosphinate-free diethyl phosphinate fire retardation agent. With the preparation method, a hypophosphorous acid and/or hypophosphite conversion rate can be 100%, and the finally obtained diethyl hypophosphorous acid and the salt thereof do not contain the monoethyl hypophosphorous acid group.

Description

technical field [0001] The invention relates to the fields of fine organic chemical industry and macromolecular materials, in particular to a method for preparing a diethylphosphinate flame retardant without monoethylphosphinic acid groups used in macromolecular materials. technical background [0002] Diethylphosphinate flame retardants without monoethylphosphinic acid groups have the following structural features: [0003] [0004] where R 1 and R 2 Both are ethyl, n is 1~4, M is aluminum, zinc, magnesium, antimony, aluminum, zinc, magnesium, antimony, scandium, yttrium, titanium, zirconium, vanadium, niobium, chromium, molybdenum, manganese, iron, cobalt , nickel, cadmium, germanium, tin, lanthanum, pavement, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and other metal ions. [0005] The product density of this kind of flame retardant is low, the amount of addition is small when used, the color is go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 刘治国汪静莉朱建华焦德荣谢滋东钟柳
Owner TAIZHOU BAILLY CHEM CO LTD
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