A kind of synthetic method of two (2-carboxyethyl) phosphonic acid

A technology of carboxyethyl and synthetic methods, which is applied in the field of flame retardants, can solve the problems of poor compatibility with polymers, low flame retardant effect, and high toxicity, and achieve good compatibility, short reaction time, and high performance small effect

Active Publication Date: 2017-05-10
ZHEJIANG SCI-TECH UNIV +1
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, the existing flame retardants have defects such as high toxicity, smoke, little flame retardant effect, and poor compatibility with polymers.

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
  • A kind of synthetic method of two (2-carboxyethyl) phosphonic acid
  • A kind of synthetic method of two (2-carboxyethyl) phosphonic acid
  • A kind of synthetic method of two (2-carboxyethyl) phosphonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The commercially available hypophosphorous acid aqueous solution was distilled under reduced pressure by a rotary evaporator in a water bath at 50° C. to obtain crystalline hypophosphorous acid.

[0030] Under an ice-water bath, 0.28mol (18.4g) of crystalline hypophosphorous acid and 0.28mol (29.71g) of trimethyl orthoformate were added to a three-necked flask, the temperature was raised to 30°C, and the reaction was carried out at this temperature for 2 hours, and then distilled under vacuum to obtain Methanol and methyl formate were removed until a pale yellow solid powder formed.

[0031] At 3°C, 0.84mol (44.52g) of acrylonitrile and 7.7g of catalyst triethylamine were added to the three-necked flask, the temperature was raised to 50°C, and the reaction was carried out for 3h. Then add 0.62mol (62.8g) of concentrated hydrochloric acid (37%), raise the temperature to 90°C, and react for 3h. After the reaction, the solution was cooled, ammonium chloride was removed by...

Embodiment 2

[0033] The commercially available hypophosphorous acid aqueous solution was distilled under reduced pressure by a rotary evaporator in a water bath at 50° C. to obtain crystalline hypophosphorous acid.

[0034] Under an ice-water bath, add 0.28mol (18.4g) of crystalline hypophosphorous acid and 0.31mol (32.90g) of trimethyl orthoformate into a three-necked flask, raise the temperature to 30°C, react at this temperature for 2h, and then distill under vacuum to obtain Methanol and methyl formate were removed until a pale yellow solid powder formed.

[0035] At 3°C, 0.84mol (44.52g) of acrylonitrile and 7.7g of catalyst triethylamine were added to the three-necked flask, the temperature was raised to 50°C, and the reaction was carried out for 3h. Then add 0.62mol (62.8g) of concentrated hydrochloric acid (37%), raise the temperature to 90°C, and react for 3h. After the reaction, the solution was cooled, ammonium chloride was removed by filtration, and then recrystallized in acet...

Embodiment 3

[0037] The commercially available hypophosphorous acid aqueous solution was distilled under reduced pressure by a rotary evaporator in a water bath at 50° C. to obtain crystalline hypophosphorous acid.

[0038] Under an ice-water bath, add 0.28mol (18.4g) of crystalline hypophosphorous acid and 0.34mol (36.08g) of trimethyl orthoformate into a three-necked flask, raise the temperature to 30°C, react at this temperature for 2h, and then distill under vacuum to obtain Methanol and methyl formate were removed until a pale yellow solid powder formed.

[0039] At 3°C, 0.84mol (44.52g) of acrylonitrile and 7.7g of catalyst triethylamine were added to the three-necked flask, the temperature was raised to 50°C, and the reaction was carried out for 3h. Then add 0.62mol (62.8g) of concentrated hydrochloric acid (37%), raise the temperature to 90°C, and react for 3h. After the reaction, the solution was cooled, ammonium chloride was removed by filtration, and recrystallized in acetone / a...

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

PropertyMeasurementUnit
limiting oxygen indexaaaaaaaaaa
Login to view more

Abstract

The invention discloses a synthesis method of bis(2-carboxylethyl)phosphonic acid. The synthesis method comprises mixing hypophosphorous acid and trimethyl orthoformate in an ice water bath, carrying out heating for a reaction, carrying out reduced pressure distillation to remove side products comprising methanol and methyl formate and to obtain an intermediate methyl hypophosphite which is flavescent solid powder, mixing methyl hypophosphite, acrylonitrile and a catalyst in a water bath, carrying out heating for a reaction, adding an excess amount of concentrated hydrochloric acid into the reaction system, carrying out a reaction process, cooling the product, filtering the cooled product to remove NH4Cl, and carrying out recrystallization in acetone and acetic acid to obtain the bis(2-carboxylethyl)phosphonic acid. The synthesis method has the advantages of simple processes, simple conditions, short reaction time and a yield of 50% or more. The bis(2-carboxylethyl)phosphonic acid has the advantages of good stability, small influence on material use performances and long fire resistance.

Description

technical field [0001] The invention relates to the synthesis of an organophosphorus flame retardant, in particular to a synthesis method of bis(2-carboxyethyl)phosphonic acid, and belongs to the field of flame retardants. Background technique [0002] Nylon has been widely used in industrial production and people's daily life because of its superior mechanical properties, heat resistance, corrosion resistance, self-lubrication and good processability. However, nylon is combustible or flammable, and its limiting oxygen index is 24%. Once it encounters a fire source, it will be ignited. Moreover, the burning of nylon will produce a large amount of toxic and corrosive gaseous products and smoke, and the consequences in the fire are very serious. In view of this, countries have paid great attention to the flame retardant treatment of nylon, and are committed to the research and application of flame retardants. [0003] The widely used flame retardants mainly include halogen-b...

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 Patents(China)
IPC IPC(8): C07F9/38
Inventor 冯新星杨敏芬张建春周岚刘梅军张华
Owner ZHEJIANG SCI-TECH UNIV
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