Monoalkyl/dialkyl phosphinate and preparation method thereof

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

Inactive Publication Date: 2013-06-26
ZHUHAI WANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the above method obtained is basically a mixture of dialkyl phosphinate or monoalkyl phosphinate and 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

[0047] Embodiment 1: Structure and preparation of aluminum ethyl phosphinate

[0048] Add 444.0g (2mol) of aluminum hypophosphite, 1000mL of toluene and 9.7g (0.04mol) of dibenzoyl peroxide into the high-pressure reactor, seal it, and replace it with nitrogen (0.5MPa) for 5 times while stirring, and then pass ethylene through Adjust the pressure regulator to 2.5MPa and fill it in, heat to 72°C, uniformly heat up to 75°C within 4 hours and inject a solution prepared by 4.8g (0.02mol) dibenzoyl peroxide and 50mL toluene with a metering pump, Then keep the temperature at 75°C for 1 hour, cool and vent to obtain 1538.8 g of aluminum ethylphosphinate-toluene mixed system, which is equivalent to ethylene absorption of 171.0 (equivalent to 101.8% of the theoretical amount).

[0049]The resulting mixed system was filtered, washed once with 1000 mL of hot ethanol, and washed twice with 1000 mL of water, and the resulting filter cake was vacuum-dried at 130°C for 5 hours to obtain alum...

Embodiment 2

[0054] Example 2: Structure and preparation of aluminum diethylphosphinate

[0055] Add 444.2g (2mol) of aluminum hypophosphite, 800mL of toluene and 9.7g (0.04mol) of benzoyl peroxide into the high-pressure reactor, seal it, replace it with nitrogen (0.5MPa) for 5 times while stirring, and then pass ethylene through the regulator Adjust the pressure to 2.5MPa and fill it in, heat to 72°C, uniformly heat up to 75°C within 4 hours and continuously pour in a solution prepared by 4.8g (0.02mol) of benzoyl peroxide and 30mL of toluene with a metering pump; After 4.5 hours, heat up to 105°C, uniformly heat up to 115°C within 4 hours and continuously inject a solution of 11.7g (0.06mol) tert-butyl peroxybenzoate and 100mL toluene with a metering pump; It was kept at ℃ for 1 hour, cooled and evacuated to obtain 1621.2 g of aluminum diethylphosphinate-toluene mixed system, which is equivalent to 345.4 g of ethylene absorption (equivalent to 102.8% of the theoretical amount).

[005...

Embodiment 3

[0062] Example 3: Structure and preparation of aluminum diethylphosphinate

[0063] Add 444.0g (2.00mol) of aluminum hypophosphite and 1000mL of benzene into the high-pressure reactor, seal it, and replace it with nitrogen (0.5MPa) for 5 times while stirring, then adjust ethylene to 2.5MPa through a pressure regulator and fill it in, heat to 105°C, within 11 hours, use a metering pump to evenly inject a solution prepared by 19.4g (0.10mol) tert-butyl peroxybenzoate and 100mL of benzene, and uniformly heat up to 115°C, and then keep it at 115°C for 1 hour , cooled and vented to obtain 1623.3g of aluminum diethylphosphinate-benzene mixed system, which is equivalent to 347.5g of ethylene absorption (equivalent to 103.4% of the theoretical amount).

[0064] The resulting mixed system was filtered, washed once with 1000 mL of ethanol, and then washed twice with 1000 mL of water, and the obtained filter cake was vacuum-dried at 130 °C for 5 hours to obtain aluminum diethylphosphin...

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Abstract

The invention discloses monoalkyl/dialkyl phosphinate and a preparation method thereof. The method comprises the steps that: an organic solvent 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, an organic solvent 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, hypophosphite is directly adopted as a raw material, and the monoalkyl/dialkyl phosphinate is obtained with a one-step method. The reaction period is short, obtained monoalkyl/dialkyl phosphinate can be precisely controlled, a total yield is high, and process floe is simple. 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08K5/5313
CPCC07F9/301C07F9/4816C08K5/5313
Inventor 李积德柴生勇孔蕾陈林卢昌利
Owner ZHUHAI WANTONG CHEM
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