Process for preparing methyl ethylphosphinate and methyl ethylphosphinate aluminum salt

A technology of ethyl methyl ethyl phosphinate and methyl ethyl phosphinic acid, which is applied in the field of dialkyl phosphinate flame retardant materials, can solve the problems of slow reaction rate, undisclosed reaction time, There are no problems such as the possibility of industrialized production, and the effects of high phosphorus content, reduced procedures, and reduced costs are achieved.

Inactive Publication Date: 2019-03-01
LIER CHEM CO LTD +1
View PDF3 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN104693238A discloses a preparation method of alkyl dialkyl phosphinate and dialkyl phosphinate. In the method, dialkyl alkyl phosphinate is heated at a temperature of 60-120° C. and in the presence of a selective catalyst. Reaction produces dialkyl phosphinic acid alkyl ester, and described catalyzer is to be selected from iodine-containing catalyzer and Lewis acid, and described iodine catalyzer comprises elemental iodine, alkyl iodide and alkali metal iodide (particularly potassium iodide); In the patent application, the embodiment uses potassium iodide as a catalyst, and the conversion rate can reach 100%, but it does not disclose the time required for the reaction
[0004] However, when the inventor repeated the method in CN104693238A, he found that when potassium iodide was used as a catalyst, the reaction rate was extremely slow, and the possibility of industrial production was basically not possible.

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
  • Process for preparing methyl ethylphosphinate and methyl ethylphosphinate aluminum salt
  • Process for preparing methyl ethylphosphinate and methyl ethylphosphinate aluminum salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049]

[0050]Add 100g of methyl diethylphosphinate (MDEP, purity 92.1%) and 2g of sodium iodide into a 250mL four-neck flask, protect it with nitrogen, and heat up to 140°C. After 6h, use GC to detect the reaction, and the conversion rate is 99.8%. Distill product, reclaim catalyst, the product methyl ethyl hypophosphite ethyl ester (MEEP) (product GC content 91.9%) that distills out is directly used in next step;

[0051]

[0052] Put 35.95g of anhydrous aluminum trichloride and 400g of trimethylbenzene in a 1L four-necked flask, and add 100g of MEEP dropwise. During the reaction, ethyl chloride gas is generated, which is absorbed by an exhaust device. After the drop is completed, the temperature is raised to 100°C. After reacting for 5 hours, raise the temperature to recover 300 g of trimethylbenzene by distillation; lower the temperature to 70°C, add 600 g of ethanol, react for 1 hour, filter, precipitate and dry to obtain the product with a yield of 96%, and recover...

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 process for preparing methyl ethylphosphinate and methyl ethylphosphinate aluminum salt, and belongs to the technical field of flame-retardant materials, aiming to solve thedifficulty in realization of industrial production of the methyl ethylphosphinate in the prior art. The process for preparing the methyl ethylphosphinate and the methyl ethylphosphinate aluminum saltincludes taking sodium iodide as a catalyst, and reacting methyl diethylphosphinate at the temperature of 80-180 DEG C to generate the methyl ethylphosphinate; reacting the methyl ethylphosphinate with aluminum trichloride in a solvent to obtain the methyl ethylphosphinate aluminum salt. The process has the advantages that the low-purity methyl diethylphosphinate serves as a raw material, the methyl ethylphosphinate is obtained under a moderate condition and at high yield, and industrialization is realized easily; methyl ethylphosphinate aluminum flame retardants with high phosphorus content are further obtained, and are environment-friendly halogen-free flame retardants for polymer materials.

Description

technical field [0001] The invention belongs to the technical field of dialkyl phosphinate flame retardant materials, and in particular relates to a preparation process of ethyl methyl ethyl phosphinate and aluminum methyl ethyl phosphinate. Background technique [0002] Polymer materials (plastics, rubber, synthetic fibers, etc.) are widely used in various fields of human life because of their various types, outstanding performance, light weight, good chemical stability, and low price. However, polymer materials are usually flammable or combustible, which brings great fire hazards. There have been many economic losses and casualties caused by the burning of polymer materials around the world. Therefore, the flame retardancy of polymer materials Higher and higher demands have been put forward. Although halogen-containing flame retardants can meet the flame-retardant requirements of certain materials, they also have a great impact on the environment because they contain halo...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32C08K5/5313
CPCC07F9/3264C08K5/5313
Inventor 岳杰何达左翔程柯
Owner LIER CHEM CO LTD
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