A kind of mono-alkyl/di-alkyl 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 effects of high yield, simple process, and low content of other salts

Inactive Publication Date: 2015-09-30
ZHUHAI WANTONG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of mono-alkyl/di-alkyl phosphinate and preparation method thereof
  • A kind of mono-alkyl/di-alkyl phosphinate and preparation method thereof
  • A kind of mono-alkyl/di-alkyl phosphinate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: Structure and preparation of aluminum ethyl phosphinate

[0051] 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);

[0052] 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 aluminu...

Embodiment 2

[0057] Example 2: Structure and preparation of aluminum diethylphosphinate

[0058] 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).

[0059] The resul...

Embodiment 3

[0065] Example 3: Structure and preparation of aluminum diethylphosphinate

[0066] 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);

[0067] 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

Disclosed is a preparation method for monoalkyl / dialkyl phosphinates, comprising the following steps: using an organic solvent as a reaction medium, a phosphinate is reacted with olefin I under the effect of initiator I at a temperature between 70°C and 90°C to acquire the monoalkyl phosphinate; and, heated to a temperature between 90°C and 110°C, the monoalkyl phosphinate acquired is reacted with olefin II under the effect of initiator II to acquire the dialkyl phosphinate; or, using the organic solvent as a reaction medium, the phosphinate is reacted with olefin III under the effect of initiator III at a temperature between 70°C and 120°C to acquire the dialkyl phosphinate. The phosphinates are Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr or Sr salt of hypophosphorous acid. The present invention uses directly the phosphinate as raw material to acquire the monoalkyl / dialkyl phosphinate in a one-step method, where the reaction cycle is short. This allows for precision control in acquiring the monoalkyl / dialkyl phosphinate, a high total yield, and a simplified process flow. The product salt has a low content of other salts when formed and 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 Patents(China)
IPC IPC(8): C07F9/30C07F9/38C08K5/5313C08K5/5317C08L67/02
CPCC07F9/4816C07F9/301C08L67/02C08K5/5313
Inventor 李积德柴生勇孔蕾陈林卢昌利
Owner ZHUHAI WANTONG CHEM
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