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A kind of phosphorus-containing acrylate elastomer flame retardant and preparation method thereof

A technology of acrylate and methyl acrylate, applied in the field of phosphorous-containing acrylate elastomer flame retardant and its preparation, and can solve problems such as poor toughness

Active Publication Date: 2021-05-25
苏州斯迈特电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The elastomer flame retardant is expected to be used for flame retardancy and toughening of flame retardant materials, and solve the problem of poor mechanical properties of flame retardant materials, especially poor toughness

Method used

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  • A kind of phosphorus-containing acrylate elastomer flame retardant and preparation method thereof
  • A kind of phosphorus-containing acrylate elastomer flame retardant and preparation method thereof
  • A kind of phosphorus-containing acrylate elastomer flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation method of (diethoxyphosphine) methyl acrylate (DEAMP)

[0028] (1) Add 16.8 g (0.1 mol) of diethyl hydroxymethylphosphonate, 10.1 g (0.1 mol) of dichloromethane (50 mL) and 10.1 g (0.1 mol) of triethylamine into a 250 mL three-necked flask, and place in an ice-salt bath at -5°C React under stirring for 0.5h;

[0029] (2) Mix 9g (0.1mol) of acryloyl chloride and 10mL of dichloromethane evenly and slowly drop them into a three-necked flask. 12h;

[0030] (3) washing with water after the reaction is finished, and rotary evaporation to remove triethylamine salt and unreacted monomers and solvents to obtain an orange-yellow liquid;

[0031] (4) Use ethyl acetate as the mobile phase, purify by neutral silica gel column chromatography, remove ethyl acetate by rotary evaporation at 40-60°C, and finally obtain light yellow (diethoxyphosphine) methyl acrylate (DEAMP) .

Embodiment 2

[0033] Preparation method of phosphorus-containing acrylate elastomer flame retardant

[0034] (1) Mix 20g DEAMP, 0.3g sodium dodecyl sulfate (SDS), 0.3g p-styrene sulfonate (SSS) and 30mL deionized water prepared in Example 1, and carry out at a stirring speed of 600rpm Pre-emulsify for 0.5h.

[0035] (2) Add 20% pre-emulsion, 0.3g SDS, 0.3g SSS, 0.04g potassium persulfate (KPS) and 20mL deionized water into a 150ml four-neck flask, heat it to 78°C in a constant temperature water bath, and keep the speed 150rpm.

[0036] (3) After the blue light appears in the bottle, start to add the remaining pre-emulsion dropwise. After the dropwise addition is completed and react for 4 hours, cool down and discharge, break the emulsion, filter, wash with deionized water for many times, and dry to finally obtain a white phosphorus-containing acrylate elastomer. flame retardant.

[0037] Depend on figure 2 It can be seen that the phosphorus-containing acrylate elastomer flame retardant...

Embodiment 3

[0040] Preparation method of phosphorus-containing acrylate elastomer flame retardant

[0041] (1) Mix 20g DEAMP, 0.2g TAIC, 0.3g SDS, 0.3g SSS and 30mL deionized water prepared in Example 1, and perform pre-emulsification at a stirring speed of 600rpm.

[0042] (2) Then add 20% pre-emulsion, 0.3g SDS, 0.3g SSS, 0.04g KPS and 20mL deionized water into a 150ml four-neck flask, heat it to 78°C in a constant temperature water bath, and keep the rotation speed at 150rpm.

[0043] (3) After the reaction, when the blue light appeared in the bottle, start to add the remaining pre-emulsion dropwise, add the remaining monomer pre-emulsion dropwise, react for 4 hours after the dropwise addition, cool down and discharge the material, break the emulsion, filter, wash and dry with deionized water for many times, Finally, a white phosphorus-containing acrylate elastomer flame retardant is obtained.

[0044] Depend on figure 2 It can be seen that the phosphorus-containing acrylate elastom...

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Abstract

The invention discloses a phosphorus-containing acrylate elastomer flame retardant and a preparation method thereof. The phosphorus-containing acrylate elastomer flame retardant provided by the invention uses (diethoxyphosphine) methyl acrylate (DEAMP) as a flame retardant monomer and is prepared by an emulsion polymerization method. The phosphorus-containing acrylate elastomer flame retardant has the dual characteristics and functions of a flame retardant and an elastomer. Its glass transition temperature is much lower than room temperature, and its initial thermal decomposition temperature is higher than 250 ° C. The residual mass after decomposition is higher than 35 %. The phosphorus-containing acrylate elastomer flame retardant provided by the present invention has both flame retardant and toughening functions when applied, so it is expected to be used for flame retardant materials to solve the problem of mechanical properties of flame retardant materials, especially those with poor toughness. question.

Description

technical field [0001] The invention belongs to the technical field of novel flame retardant design and synthesis, and in particular relates to a phosphorus-containing acrylate elastomer flame retardant and a preparation method thereof. Background technique [0002] At present, the flame retardant modification of polymer materials is still mainly based on the modification of additive flame retardants. Among them, the development of new halogen-free flame retardants has become one of the key technologies in the field of flame retardants. Polyphosphate and polyphosphoramide polymer flame retardants have the characteristics of non-migration, good durability, good weather resistance, high thermal stability, and low volatility. They have been developed and applied to flame retardant materials such as PET, PC, and PA. . However, since these flame retardants are polar polymers and have poor compatibility in polyolefins, they can only solve the problem of additive migration and blo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L43/02C08F230/02C08F226/06C08F212/14C08F2/26C08F2/24C08L67/04C08L5/16C08K3/32C07F9/40
CPCC07F9/4006C08F2/24C08F2/26C08F230/02C08K2003/323C08L43/02C08L67/04C08L2201/02C08L2201/08C08L2205/03C08L2205/06C08F226/06C08F212/14C08L5/16C08K3/32
Inventor 闫莉桑晓明王亚凤
Owner 苏州斯迈特电子科技有限公司
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