A kind of flame retardant and its preparation method and flame retardant acrylate emulsion using the flame retardant

A technology of acrylate and phosphorus-nitrogen flame retardants, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of physical and mechanical properties of acrylate resins and resin compatibility Poor performance, affecting the stability of acrylate emulsion, etc., to achieve the effect of reducing secondary damage, wide application range, and improving stability

Active Publication Date: 2011-11-30
浙江仙居永固橡胶科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Added flame retardants not only seriously affect the stability of acrylate emulsions, but also reduce the physical and mechanical properties of acrylate resins due to poor resin compatibility

Method used

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  • A kind of flame retardant and its preparation method and flame retardant acrylate emulsion using the flame retardant
  • A kind of flame retardant and its preparation method and flame retardant acrylate emulsion using the flame retardant
  • A kind of flame retardant and its preparation method and flame retardant acrylate emulsion using the flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Synthesis of N-acetamido-2-acrylic acid-2-oxygen-5,5-dimethyl-1,3,2-dioxaphosphorinane

[0026] Add 15.4g (0.1mol) of phosphorus oxychloride and 50mL of chloroform into a four-necked flask, stir the reaction temperature to 35°C, slowly add dropwise a mixture of 10.4g (0.1mol) of neopentyl glycol and 80mL of chloroform, After the addition, the reaction was maintained at 40°C for 3 hours, the chloroform was recovered by distillation under reduced pressure, washed with 25 mL of anhydrous ether, and filtered to obtain a colorless crystalline solid of 2-oxo-2-chloro-5,5-dimethyl -1,3,2-dioxaphosphorinane, the yield is 86.1%, and the purity is 97.1%.

[0027] Add 9.0g (0.15mol) of ethylenediamine and 40mL of chloroform into the three-necked flask, stir, and the temperature of the reaction solution is 0°C, slowly add 18.4g (0.1mol) of the solid (2-oxo-2 -Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane) and 100mL chloroform mixture, after the addition, keep the tempera...

Embodiment 2

[0030] The synthetic operation of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine is the same as in Example 1, N-ethyl-acrylamido-2-oxo- The synthesis operation of 5,5-dimethyl-1,3,2-dioxaphosphorinane is the same as in Example 1. In the reaction of formula (II) compound and maleic anhydride, the amount ratio of the feed material of formula (II) compound and maleic anhydride is 1.0: 1.2, solvent selects acetonitrile for use, 60 ℃ of reaction temperatures, the reaction times is 2 hours, yield was 37.1%.

Embodiment 3

[0032] The synthetic operation of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine is the same as in Example 1, N-acetamido-2-acrylic acid-2-oxo - The synthesis operation of 5,5-dimethyl-1,3,2-dioxaphosphorinane is the same as in Example 1. In the reaction of formula (II) compound and maleic anhydride, the amount ratio of the feed material of formula (II) compound and maleic anhydride is 1.0: 1.5, solvent selects ethyl acetate for use, 30 ℃ of temperature of reaction, the reaction times is 12 hours, The yield was 43.6%.

[0033] Example 3

[0034] The synthetic operation of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine is the same as in Example 1, N-acetamido-2-acrylic acid-2-oxo - The synthesis operation of 5,5-dimethyl-1,3,2-dioxaphosphorinane is the same as in Example 1. In the reaction of formula (II) compound and maleic anhydride, the amount ratio of the feed material of formula (II) compound and maleic anhydride is 1.0: 1.2, solvent is selecte...

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Abstract

The invention discloses a flame retardant and a preparation method thereof, and flame-retardant acrylate emulsion employing the flame retardant, in particular a reactive phosphorus-nitrogen flame retardant, and a preparation method and application thereof. The reactive phosphorus-nitrogen flame retardant has the structure shown as a formula (I). The preparation method comprises the following step of: reacting amine compound containing phosphorus spiro, which is shown as a formula (II) with maleic anhydride to obtain the reactive phosphorus-nitrogen flame retardant. The flame-retardant acrylate emulsion is prepared by emulsion polymerization of the reactive phosphorus-nitrogen flame retardant and acrylate monomers. The reactive phosphorus-nitrogen flame retardant and the acrylate monomers form copolymer to perform flame-retardant modification on acrylate emulsion, and the flame-retardant effect of acrylate resin is improved, the using amount of the flame retardant in polymer materials is reduced and the cost of flame-retardant materials is reduced through synergic flame retardancy of phosphorus and nitrogen elements of the flame retardant.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a reactive phosphorus-nitrogen flame retardant and a preparation method thereof, in particular to a technology for preparing a flame-retardant acrylate emulsion using the flame retardant. Background technique [0002] Acrylate emulsion uses water as the dispersion medium, and is used in coatings, adhesives, printing ink binders, varnishes, etc. It has the advantages of low cost, simple production process, convenient use, non-toxic and safe, and no pollution to the environment. . However, when the acrylate emulsion is used in the field of flame retardancy or flame retardation, it is often necessary to add a halogen-containing flame retardant. This kind of flame retardant has high flame retardant efficiency, but it releases a large amount of toxic hydrogen halide gas when it burns, which not only causes harm to the human body, but also makes it difficult for th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08F220/14C08F220/18C08F220/06C08F230/02
Inventor 黄国波潘富友梁华定葛昌华
Owner 浙江仙居永固橡胶科技有限公司
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