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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, easy washing and simple process flow

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-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

[0051] Embodiment 1: Structure and preparation of aluminum ethyl phosphinate

[0052] Add 444.0g (2mol) of aluminum hypophosphite, 1500mL of water 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 pressure regulator Adjust to 2.5MPa and fill in, heat to 72°C, uniformly heat up to 75°C within 4h and use a metering pump to pour in a solution made of 5.0g (0.022mol) ammonium persulfate and 25mL of water, and then keep warm at 75°C After 1 hour, cool and vent, and obtain 2156.2 g of the aluminum ethylphosphinate-water mixed system, which is equivalent to 172.2 g of ethylene absorption (equivalent to 102.5% of the theoretical amount);

[0053]The obtained aluminum ethylphosphinate-water mixed system was heated to 95°C and filtered, washed once with 1000 mL of hot water at 95°C, and the solid was vacuum-dried at 130°C for 5 hours to obtain aluminum...

Embodiment 2

[0058] Example 2: Structure and preparation of aluminum diethylphosphinate

[0059] Add 444g (2mol) of aluminum hypophosphite, 1500mL of water 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 adjust the ethylene through a pressure regulator Charge to 2.5MPa, heat to 72°C, uniformly heat up to 75°C within 4 hours and continuously inject a solution of 5.0g (0.022mol) ammonium persulfate and 25mL water with a metering pump; after 4.5 hours, heat Raise the temperature to 95°C, uniformly raise the temperature to 110°C within 4 hours, and use a metering pump to continuously inject a solution prepared by 15.0g ammonium persulfate and 75mL water, then keep it at 110°C for 1 hour, cool and vent to obtain the diethyl The aluminum-based phosphinate-water mixed system is 2416g, which is equivalent to 342.0g ethylene absorption (101.8% of the theoretical amount).

[0060] The resul...

Embodiment 3

[0066] Example 3: Structure and preparation of aluminum diethylphosphinate

[0067] Add 444.0g (2.00mol) of aluminum hypophosphite and 1500mL of water 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 95°C, within 11 hours, use a metering pump to evenly inject a solution prepared by 20.0g (0.088mol ammonium persulfate) and 100mL water, and evenly raise the temperature to 110°C, then keep it at 110°C for 1 hour, cool and vent. The obtained aluminum diethylphosphinate-water mixed system is 2417.2g, which is equivalent to 343.2g of ethylene absorption (102.1% of the theoretical amount);

[0068] The resulting aluminum diethylphosphinate-water mixed system was filtered, washed once with 1000 mL of water, and the solid was vacuum-dried at 130°C for 5 hours to obtain aluminum diethylphosphinate: 756.1 g, with a yield of 96.93%. The structura...

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Abstract

The invention discloses monoalkyl / dialkyl phosphinate and a preparation method thereof. The method comprises the steps that: 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, 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, 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, a total yield is high, product purity is high, process flow is simple, no organic solvent or other solvent is adopted, and no subsequent processing is needed. 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 ZHUHAI WANTONG CHEM
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