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Dialkyl phosphinate compound containing active epoxy group as well as preparation and application thereof

A technology of dialkyl phosphinic acid and epoxy group, applied in the field of dialkyl phosphinic acid esters, can solve problems such as inapplicability, and achieve the effect of reducing dosage and good flame retardant performance

Active Publication Date: 2021-05-11
江苏利思德新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, salt compounds are usually solid powders, which cannot be applied to some application systems that require transparency

Method used

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  • Dialkyl phosphinate compound containing active epoxy group as well as preparation and application thereof
  • Dialkyl phosphinate compound containing active epoxy group as well as preparation and application thereof
  • Dialkyl phosphinate compound containing active epoxy group as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1 has the compound preparation in the structure in formula (III)

[0058]

[0059] Add 288g (2mol) sodium diethylphosphinate, 6.0g catalyst polyalkylammonium bromide, 600g epichlorohydrin in the autoclave that stirrer, thermometer are housed, open and stir, pass into nitrogen replacement three times, Raise the temperature to 110-120°C, heat and stir for 10 hours, and then turn on the vacuum to remove unreacted epichlorohydrin. The product was filtered and purified by distillation to obtain 338 g of liquid product with a conversion rate of 95%.

[0060] Characterize by carrying out NMR-P spectrum and NMR-H spectrum to obtained product, the result is as attached figure 1 (phosphorus NMR) and attached figure 2 (Proton NMR). through with image 3 (Sodium diethyl hypophosphite phosphorus NMR) comparison can be known, in figure 1 Among them, the peak between the offset 60-65ppm represents the structure of diethyl hypophosphite, and the newly synthesized co...

Embodiment 2

[0062] Embodiment 2 prepares flame-retardant epoxy material

[0063] 1) the reaction of formula (III) compound and DDS

[0064] Mix the compound of formula (III) prepared in Example 1 and the epoxy resin curing agent DDS uniformly in a certain proportion, take a small amount of samples and test the DSC curve, and judge the reaction between the compound of formula (III) and DDS according to the exothermic peak in the DSC curve. The DSC curve obtained from the test is as follows Image 6 shown.

[0065] From the results, the DSC curve of DDS alone shows that DDS has a melting point peak at 179.3°C due to being a solid, which is an endothermic process; The exothermic peak indicates that the compound of structure (III) undergoes a ring-opening reaction and releases heat; on the DSC curve of the compound of structure (III) and DDS, there are two exothermic peaks, namely 210.0°C and 264.1°C Compared with the exothermic peak of the single structure (III) compound, the peaks are ob...

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Abstract

The invention discloses a dialkyl phosphinate compound containing an active epoxy group, preparation of the dialkyl phosphinate compound and application of the dialkyl phosphinate compound serving as a flame retardant to preparation of a flame-retardant material. The compound is shown as either a formula (I) or a formula (II) which is described in the specification, and in the formula (I) and the formula (II), R1 and R2 are respectively and independently selected from C1-C24 alkyl, cycloalkyl, aryl or alkenyl, R3 is independently selected from C1-C10 linear or branched alkylene, or C6-C10 arylene, alkyl arylene or aryl alkylene, m is an integer of 1-3, and n is an integer of 1-3. The preparation method comprises the following step of: reacting dialkyl phosphinic acid metal salt with a halogenated epoxy compound serving as raw materials. The dialkyl phosphinate compound has the advantages that the dialkyl phosphinate compound has a dialkyl phosphinic acid structure and an epoxy active group structure at the same time; the active epoxy group can be used for preparing alcohol, ester and epoxy resin; and the dialkyl phosphinate compound can be used as a flame retardant, and can be independently used or used after being mixed with other flame retardants.

Description

technical field [0001] The invention relates to the field of dialkyl phosphinates, in particular to a dialkyl phosphinate containing active epoxy groups and its preparation and application. Background technique [0002] Organophosphate is the main species of organophosphorus, which is mainly obtained by reacting phosphoric acid, phosphorous acid, methylphosphonic acid, etc. with alcohol. Common organophosphates include triethyl phosphate, trimethyl phosphite, dimethyl methyl phosphonate, diethyl ethyl phosphonate, etc. [0003] There are few reports on organophosphate esters of hypophosphorous acid, fewer reports on esters of dialkylphosphinic acid, and no reports on dialkylphosphinates containing epoxy groups. Hypophosphorous acid and its derivatives have been widely used because of their good flame retardant properties. But more are the metal salts of hypophosphorous acid and its derivatives (such as the patented technology of CN1660857A, CN106967116A, etc.) with publica...

Claims

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Application Information

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IPC IPC(8): C07F9/655C08K5/5313C08L63/00
CPCC07F9/65505C08K5/5313C08L2201/02C08L63/00
Inventor 李金忠陈章明雷华杨建伟王家凯曹俊华王海峰
Owner 江苏利思德新材料股份有限公司
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