Preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof

A technology of monoethylphosphinic acid and diethylphosphinic acid, which is applied in the field of preparation of diethylphosphinic acid and its salts, can solve the problems of complex process, high cost, waste water, etc., and achieve good removal effect, Ease of recycling and simple waste liquid treatment

Active Publication Date: 2015-04-01
成都美域高制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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 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 prepari

Method used

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  • Preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof
  • Preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof
  • Preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof

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Example Embodiment

[0055] Example 1

[0056] Dissolve sodium hypophosphite monohydrate (2mol) and acetic anhydride (2mol) in 44ml ethylene glycol monomethyl ether, then add a catalytic amount of glacial acetic acid (0.1mol) with stirring, and add anhydrous after stirring at room temperature for 2 hours Sulfuric acid (1mol), after adding anhydrous sulfuric acid, cool to 15°C and let stand for 1 hour, filter and recover sodium sulfate to obtain anhydrous hypophosphorous acid solution;

[0057] Transfer the anhydrous hypophosphorous acid solution into an acid-resistant and pressure-resistant reactor with a constant-pressure dripping device, pass ethylene gas, and make the pressure in the kettle reach 1MPa, and separate from the constant-pressure dripping device under stirring at 1800r / min. Add in batches an initiating mixture composed of 20g of azobisisobutyronitrile, 0.4g of copper complex and 44ml of ethylene glycol monomethyl ether. During the dripping of the initiating mixture, keep the ethylene pre...

Example Embodiment

[0064] Example 2

[0065] Dissolve sodium hypophosphite monohydrate (2mol) and acetic anhydride (2mol) in 44ml ethylene glycol monomethyl ether, then add catalytic amount of propionic acid (0.05mol) under stirring, and add 98% after stirring for 3 hours at room temperature Concentrated sulfuric acid (1mol), after adding 98% concentrated sulfuric acid, cool to 10°C and stand for 2.5 hours, filter and recover sodium sulfate to obtain anhydrous hypophosphorous acid solution;

[0066] Transfer the anhydrous hypophosphorous acid solution to an acid-resistant and pressure-resistant reactor with a constant-pressure dripping device, pass ethylene gas, and make the pressure in the kettle reach 1.2MPa, and stir from the constant-pressure dripping device at 800r / min. Add in batches an initiating mixture composed of 20g of azobisisobutyronitrile, 0.4g of copper complex and 44ml of ethylene glycol monomethyl ether, and keep the ethylene pressure in the reactor not less than 0.6 during the dripp...

Example Embodiment

[0072] Example 3

[0073] Dissolve sodium hypophosphite monohydrate (2mol) and acetic anhydride (2.2mol) in 55ml dioxane, then add a catalytic amount of isovaleric acid (2mol) under stirring, and add 98.4% of isovaleric acid (2mol) under stirring at room temperature for 0.5 hours Concentrated sulfuric acid (1.2mol), after adding concentrated sulfuric acid, cool down to 5°C and let stand for 6 hours, filter and recover sodium sulfate to obtain anhydrous hypophosphorous acid solution;

[0074] Transfer the anhydrous hypophosphorous acid solution into an acid-resistant and pressure-resistant reactor with a constant-pressure dripping device, pass ethylene gas, and make the pressure in the kettle reach 0.1MPa, and stir from the constant-pressure dripping device at 1800r / min. Add in batches an initiation mixture composed of 20g azobisisobutyronitrile, 0.4g copper complex and 44ml ethylene glycol monomethyl ether, and keep the ethylene pressure in the reactor not less than 0.1 during the ...

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Abstract

The invention relates to the field of fine organic chemical industry and polymer materials, and particularly relates to a preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof. The preparation method of diethyl phosphinic acid comprises the following steps: uniformly mixing sodium hypophosphite monohydrate, acetic anhydride and organic solvent; adding organic acid and concentrated sulfuric acid or anhydrous sulfuric acid; cooling and standing; filtering and recovering sodium sulfate to obtain an anhydrous phosphinic acid organic acid solution; adding ethylene and dropwise adding a trigger mixture to obtain a first mixture; and distilling and recovering the organic acid and the organic solvent to obtain a product. The preparation method is simple and easy to implement, the monoethyl phosphinic acid is completely converted into diethyl phosphinic acid, and the prepared diethyl phosphinic acid does not contain the monoethyl phosphinic acid group. In the invention, the diethyl phosphinic acid without the monoethyl phosphinic acid group serves as a reactant and reacts with a metal compound, the obtained diethyl phosphinate does not contain impurities such as organic sodium salt, and the generated waste liquid is simple to dispose.

Description

technical field [0001] The invention relates to the fields of fine organic chemical industry and macromolecular materials, in particular to a preparation method of diethylphosphinic acid and its salts without monoethylphosphinic acid groups. Background technique [0002] Diethylphosphinic acid and salts thereof that do not contain monoethylphosphinic acid groups have the structural characteristics of the following formulas (I) and (II): [0003] [0004] R in the formulas (I) and (II) 1 and R 2 Both are ethyl, n in formula (II) is 1-4, M is 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 whe...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 刘治国钟柳林羿成王小宁
Owner 成都美域高制药有限公司
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