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Dialkylhypophosphite and preparation method thereof

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

Inactive Publication Date: 2013-05-08
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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  • Dialkylhypophosphite and preparation method thereof
  • Dialkylhypophosphite and preparation method thereof
  • Dialkylhypophosphite and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1: Preparation of high concentration hypophosphorous acid

[0057] 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;

[0058] 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 223.1 g of the lower layer liquid, and use acid-base titration to obtain the acid content For: 90.31% mass fraction.

Embodiment 2

[0059] Example 2: Preparation of high concentration hypophosphorous acid

[0060] 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;

[0061] 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 212.0 g of the lower layer liquid, and use acid-base titration to obtain the acid content For: 94.09% mass fraction.

[0062] Get 200.2g of hypophosphorous acid and 200ml methyl alcohol of 94.09% mass fraction, add in the reaction bottle that oil-water separator and condenser are housed, and the fixed solid silica gel desiccant is housed in oil-water separator and condenser wherein and in oil-water separator Fill the flask with methanol, heat and ...

Embodiment 3

[0064] Prepare the high-concentration hypophosphorous acid of 99.43% mass fraction with embodiment 2, get the high-concentration hypophosphorous acid of 99.43% mass fraction

[0065] Add 181.6g (2.733mol), 150ml of cyclohexane and 2.4g (0.014mol, 0.5%mol) tert-butyl peroxypivalate into the autoclave, seal the autoclave, and replace it with nitrogen (0.5MPa) under stirring 5 times, then filled with ethylene to 2.5MPa saturation, heated to 70°C under stirring, added 4.7g (0.027mol, 1.0%mol) tert-butyl peroxypivalate and 20ml cyclohexane evenly within 4 hours The prepared solution was evenly heated to 80°C within 5 hours, and the reactor was cooled and emptied to obtain 474.1 g of a homogeneous solution of diethylphosphinic acid containing telomers, acid content: 72.01% (mass fraction) ;

[0066] Diethylphosphinic acid homogeneous solution 474.1g, with 300ml water extraction three times, obtain diethylphosphinic acid aqueous solution altogether

[0067] 1197.3g, the measured ...

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Abstract

The invention discloses a dialkylhypophosphite disclosed as a structural formula (I), wherein R1 and R2 are identical or different and are respectively a C2-6 alkyl group; M is Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr or Sr; m=1-4; and the telomer content is 0.1-10 mol%. The preparation method comprises the following steps: by using cyclohexane and / or cyclohexene as a solvent, reacting high-concentration hypophosphorous acid with alkene under the action of an initiator to obtain dialkylhypophosphorous acid-organic phase solution; extracting with water, or carrying out vacuum distillation to remove the organic solvent and diluting with water, thereby obtaining a dialkylhypophosphorous acid water solution; neutralizing with an alkaline compound water solution to obtain a dialkylhypophosphorous acid alkali metal salt water solution; and reacting the dialkylhypophosphorous acid alkali metal salt water solution with the metal compound water solution to obtain the dialkylhypophosphite. The high-concentration hypophosphorous acid is used as the raw material, and the cyclohexane and / or cyclohexene is used as the solvent to obtain the product containing part of telomer; and thus, the invention has the advantages of very short reaction period (the synthesis can be completed only by 4-6 hours) and high overall yield. The technical 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