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Monoalkyl/dialkyl phosphinate and preparation method thereof

A technology of alkyl phosphinate and mono-alkyl, applied in the field of mono-alkyl/di-alkyl phosphinate and its preparation, can solve the problem that it is difficult to obtain mono-alkyl phosphinate or hypophosphorous acid , to achieve the effect of high yield, low salt content and easy washing

Inactive Publication Date: 2013-06-26
GUANGZHOU KINGSKY MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the above-mentioned method obtained is basically dialkyl phosphinate, it is difficult to obtain relatively high content of monoalkyl phosphinate or hypophosphorous acid

Method used

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  • Monoalkyl/dialkyl phosphinate and preparation method thereof
  • Monoalkyl/dialkyl phosphinate and preparation method thereof
  • Monoalkyl/dialkyl phosphinate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1: Structure and preparation of aluminum ethyl phosphinate

[0047] Add 444.1g (2mol) of aluminum hypophosphite, 500mL of water, 500mL of ethanol and 10.0g, 0.044mol of ammonium persulfate into the high-pressure reactor, seal it, and replace it with nitrogen (0.5MPa) for 5 times while stirring, and then pass ethylene through the regulator Adjust the pressure regulator to 2.5MPa and fill it in, heat it to 72°C, uniformly heat up to 75°C within 4h and use a metering pump to inject 5.0g, 0.022mol ammonium persulfate and 30mL water into the solution, and then at 75°C Insulate for 1 hour, cool and vent to obtain a mixed system of 1559.6g, which is equivalent to 175.5g of ethylene absorption (104.5% of the theoretical amount);

[0048] The resulting mixed system was filtered, washed twice with 1000 mL of water, and the obtained filter cake was vacuum-dried at 130° C. for 5 hours to obtain aluminum ethyl phosphinate: 583.7 g, with a yield of 95.37%, wherein the stru...

Embodiment 2

[0053] Example 2: Structure and preparation of aluminum diethylphosphinate

[0054] Add 444g (2mol) of aluminum hypophosphite, 300mL of water, 700mL of ethanol and 10.0g, 0.044mol of ammonium persulfate into the high-pressure reactor, seal it, replace it with nitrogen (0.5MPa) for 5 times while stirring, and then pass ethylene through the pressure regulator Adjust to 2.5MPa and fill it in, heat to 72°C, uniformly heat up to 75°C within 4 hours and use a metering pump to continuously inject 5.0g, 0.022mol of ammonium persulfate and 30mL of water into the solution; after 4.5 hours, Heat up to 95°C, uniformly heat up to 110°C within 4 hours, and use a metering pump to continuously inject a solution prepared by 15.0g ammonium persulfate and 90mL water, then keep warm at 110°C for 1 hour, cool and vent to obtain a mixed system 1794.1g, equivalent to 347.1g of ethylene absorption (103.3% of theoretical amount);

[0055] The resulting mixed system was filtered, washed twice with 100...

Embodiment 3

[0061] Example 3: Structure and preparation of aluminum diethylphosphinate

[0062] Add 444.0g (2.00mol) of aluminum hypophosphite, 500mL of water and 500mL of methanol into the high-pressure reactor, seal it, and replace it with nitrogen (0.5MPa) for 5 times while stirring, then adjust the ethylene to 2.5MPa through a pressure regulator and fill it with 20.0 g, 0.088 mol of ammonium persulfate and 120 mL of water are evenly poured into the solution within 9 hours with a metering pump, and the temperature is evenly raised to 110 ° C, and then kept at 110 ° C for 1 hour, cooled Vented to obtain 1832.1g of the mixed system, which is equivalent to 353.1g of ethylene absorption (105.1% of the theoretical amount);

[0063] The resulting mixed system was filtered, washed twice with 1000 mL of water, and the obtained filter cake was vacuum-dried at 130°C for 5 hours to obtain aluminum diethylphosphinate: 751.0 g, yield 96.27%, wherein, aluminum diethylphosphinate The structural form...

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Abstract

The invention discloses monoalkyl / dialkyl phosphinate and a preparation method thereof. The method comprises the steps that: organic solvent-water is adopted as a reaction medium; under the effect of an initiator I, hypophosphite is subjected to a reaction with alkene I under a temperature of 70-90 DEG C, such that monoalkyl phosphinate is obtained; the temperature is increased to 90-110 DEG C by heating; the obtained monoalkyl phosphinate is subjected to a reaction with alkene II under the effect of an initiator II, such that dialkyl phosphinate is obtained; Or, organic solvent-water is adopted as a reaction medium; under the effect of an initiator III, hypophosphite is subjected to a reaction with alkene III under a temperature of 70-120 DEG C, such that dialkyl phosphinate is obtained. The hypophosphite is hypophosphorous acid salt of Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr, or Sr. According to the invention, the reaction period is short, obtained monoalkyl / dialkyl phosphinate can be precisely controlled, a total yield is high, and product purity is high. When the product is salified, the contents of other salts are low. The product is easy to wash.

Description

technical field [0001] The invention relates to a mono-alkyl / di-alkyl phosphinate and a preparation method thereof. Background technique [0002] Mono- and di-alkylphosphinates, widely used as flame retardants, can be synthesized by different methods. Yuan Chengye et al. in the study of organophosphorus compounds - oxidative phosphorylation reaction - a new method for the synthesis of dihydrocarbyl phosphonic acid and its derivatives (Chinese Science B series, 1984, 12, 1088~1092) and Lin Qiang et al. in the synthesis of dihydrocarbyl phosphine oxide Quantitative synthesis of phosphinic acid (Journal of Central South University (Natural Science Edition), 1987, 18 (6), 697) described the Grignard reagent method to generate diethyl phosphinate and phosphinic acid from the reaction of phosphorus trichloride and ethanol Diethyl ester is reacted with self-made Grignard reagent and hydrolyzed to obtain dialkylphosphine oxide, and dialkylphosphine oxide can be reacted with oxidant...

Claims

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Application Information

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IPC IPC(8): C07F9/30C07F9/38C08K5/5313C08K5/5317C08L67/02
CPCC07F9/301C07F9/4816C08K5/5313
Inventor 李积德柴生勇孔蕾陈林卢昌利
Owner GUANGZHOU KINGSKY MATERIAL
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