Preparation method of dialkyl phosphinic acid and salt thereof

A technology of dialkyl phosphinic acid and dialkyl phosphine, which is applied in the field of preparation of dialkyl phosphinic acid and its salts, can solve the problems of easy quenching and deactivation of free radical initiators, long reaction period, etc. The effect of high purity and simple process flow

Inactive Publication Date: 2013-05-01
GUANGZHOU KINGSKY MATERIAL
View PDF10 Cites 11 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of dialkyl phosphinic acid and salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Preparation of high concentration hypophosphorous acid

[0045] 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;

[0046] Under the protection of nitrogen, heat and stir until azeotropic for about 2 hours, and discharge the water separated at the bottom of the oil-water separator in stages; add the solution in the reaction bottle to the separatory funnel to separate to obtain 249.8 g of the lower layer liquid, and use acid-base titration to obtain the acid content For: 80.25% (mass fraction).

Embodiment 2

[0047] Example 2: Preparation of high concentration hypophosphorous acid

[0048] 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;

[0049] 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: 90.35% (mass fraction).

Embodiment 3

[0050] Embodiment 3: Preparation of high concentration hypophosphorous acid

[0051] 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;

[0052] 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).

[0053] Get the hypophosphorous acid 200.2g and 200ml methyl alcohol that the mass fraction is 94.07%, 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 separation Fill the container with methanol, ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a preparation method of dialkyl phosphinic acid and salts thereof. The method comprises the following steps: reacting hypophosphorous acid with high concentration with olefin under the effect of an initiator to obtain dialkyl phosphinic acid; and then diluting the dialkyl phosphinic acid with water and neutralizing with an aqueous solution of an alkaline compound to obtain a dialkyl phosphinic acid alkali metal salt aqueous solution; and reacting the dialkyl phosphinic acid alkali metal salt aqueous solution with a metal compound aqueous solution to obtain the dialkyl phosphinic acid salt. The concentration of the hypophosphorous acid with high concentration is 80-100%; and the metal compound is compound of Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr and Sr. The invention employs hypophosphorous acid with high concentration as a raw material, which is added with no solvent; a bulk free radical reaction has a quite short reaction cycle requiring only 3-5 h to complete a high pressure synthesis process, and has high total yield; the synthesized dialkyl phosphinic acid product has high concentration and high purity; the process is simple, does not use organic solvent or other solvent; and the salified product does not contain other harmful substance or need any post-treatment.

Description

technical field [0001] The invention relates to a preparation method of dialkylphosphinic acid and salt thereof. Background technique [0002] Dialkylphosphinic acids and their salts, 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 oxid...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07F9/30C08K5/5313C08K7/14C08L67/02C08L101/12
Inventor 李积德柴生勇孔蕾陈林卢昌利
Owner GUANGZHOU KINGSKY MATERIAL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap