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Dialkyl phosphinic acid salt and preparation method thereof

A technology of dialkyl phosphinate and alkyl phosphinate is applied in the field of dialkyl phosphinate and its preparation, and can solve the problems of easy quenching and deactivation of free radical initiators, long reaction period and the like, Achieve the effect of high yield, short reaction period and simple process flow

Inactive Publication Date: 2013-05-01
GUANGZHOU KINGSKY MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This scheme is carried out in water, and there is less post-treatment, but it makes the free radical initiator easy to quench and deactivate, and the reaction cycle is long

Method used

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  • Dialkyl phosphinic acid salt and preparation method thereof
  • Dialkyl phosphinic acid salt and preparation method thereof
  • Dialkyl phosphinic acid salt and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1: Preparation of high concentration hypophosphorous acid

[0056] Get 400.1g mass fraction to be 50% hypophosphorous acid and 250ml cyclohexane, add in the reaction bottle that oil-water separator and condenser are housed, fill up cyclohexane in oil-water separator;

[0057] Heat and stir under nitrogen protection until azeotropic for about 3 hours, and discharge the water separated at the bottom of the oil-water separator in stages; add the solution in the reaction bottle to a separatory funnel to separate to obtain 222.2 g of the lower liquid, and use acid-base titration to obtain the acid content For: 90.38% (mass fraction).

Embodiment 2

[0058] Example 2: Preparation of high concentration hypophosphorous acid

[0059] Get 400.1g mass fraction 50% hypophosphorous acid and 250ml cyclohexane, add in the reaction bottle that oil-water separator and condenser are housed, fill up cyclohexane in oil-water separator;

[0060] Heat and stir under nitrogen protection until azeotropic for about 4 hours, discharge the water separated at the bottom of the oil-water separator in stages; add the solution in the reaction bottle to a separatory funnel to separate to obtain 212.4 g of the lower layer liquid, and use acid-base titration to obtain the acid content For: 94.07% (mass fraction).

[0061] Get 200.2g of hypophosphorous acid and 200ml methyl alcohol of 94.07% mass fraction, add in the reaction flask that oil-water separator and condenser are housed, and fixed solid calcium chloride is housed in oil-water separator and condenser wherein and in oil-water separator Fill with methanol, heat and stir to azeotrope for 4...

Embodiment 3

[0063] Prepare the high-concentration hypophosphorous acid of 99.49% mass fraction with embodiment 2, get the high-concentration hypophosphorous acid of 99.49% mass fraction

[0064] Add 181.2g (2.732mol), 150ml of benzene and 2.4g (0.014mol, 0.5%mol) of tert-butyl peroxypivalate into the autoclave, seal the autoclave, and replace it with nitrogen (0.5MPa) for 5 times while stirring , and then filled with ethylene to 2.5MPa saturation, heated to 70°C under stirring, and added 4.7g (0.027mol, 1.0%mol) of tert-butyl peroxypivalate and 50ml of benzene evenly within 4 hours. , uniformly warming up to 80° C. within 5 hours, cooling the reactor and venting to obtain 468.8 g of diethylphosphinic acid homogeneous solution containing telomer, acid content: 71.02% (mass fraction);

[0065] Diethylphosphinic acid homogeneous solution 468.8g, extract three times with 300ml water, obtain diethylphosphinic acid aqueous solution altogether

[0066] 1192.3g, the recorded acid content is 24...

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Abstract

The invention discloses a dialkyl phosphinic acid salt with the following structural formula (I). R1 and R2 are the same or different, and represent C2-C6 alkyls; secondary M represents Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr or Sr; m equals to 1-4; and mole percent of a telomer is 0.1-10mol%. The preparation method comprises steps of: a) reacting hypophosphorous acid with high concentration with olefin under the effect of an initiator by using benzene as a solvent to obtain a dialkyl phosphinic acid-organic phase solution; b) removing the organic solvent by water extraction or vacuum distillation, and diluting with water to obtain a dialkyl phosphinic acid aqueous solution; c) neutralizing with an aqueous solution of an alkaline compound to obtain a dialkyl phosphinic acid alkali metal salt aqueous solution; and d) reacting the dialkyl phosphinic acid alkali metal salt aqueous solution with a metal compound aqueous solution to obtain dialkyl phosphinic acid salt. The method provided by the invention employs hypophosphorous acid with high concentration as a raw material and benzene as the solvent to obtain a product containing part of telomer, has a short reaction period only requiring 4-6 h to complete the process, and has a high total yield; the process is simple; and the organic solvent can be recycled.

Description

technical field [0001] The invention relates to a dialkyl phosphinate and a preparation method thereof. Background technique [0002] Dialkylphosphinates, widely used as flame retardants, can be synthesized by different methods. Yuan Chengye et al. in the study of organic phosphine compounds - phosphine oxide reaction - a new method for the synthesis of dihydrocarbyl phosphonic acid and its derivatives (Chinese Science Series B, 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 phosphinate from the reaction of phosphorus trichloride and ethanol Diethyl acid diethyl ester is reacted with self-made Grignard reagent and hydrolyzed to obtain dialkylphosphine oxide, and dialkylphosphine oxide is reacted with oxidant and acidified to obtain d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08K5/5313C08K13/04C08L67/02
Inventor 李积德柴生勇孔蕾陈林卢昌利
Owner GUANGZHOU KINGSKY MATERIAL
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