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Charring agent with beta-crystal inducing nucleation effect, and synthetic method thereof

A technology of nucleation and synthesis method, which is applied in the field of intumescent flame retardant products, can solve problems such as low char formation, poor thermal stability, and great influence on mechanical properties, achieve high char formation rate, improve mechanical properties, and reduce absorption tidal effect

Inactive Publication Date: 2017-07-25
SHUNDE POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a kind of carbon-forming agent with β crystal in view of the shortcomings of existing triazine char-forming agents, such as low char-forming amount, poor thermal stability and poor compatibility with polypropylene, which have a great influence on the mechanical properties of composite materials. A char-forming agent that induces nucleation and its synthesis method. The product obtained in the present invention has a high char-forming amount, good thermal stability, and can induce a certain amount of β crystals, thereby changing the aggregated state structure of the polypropylene composite material and realizing The purpose of improving both flame retardancy and mechanical properties

Method used

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  • Charring agent with beta-crystal inducing nucleation effect, and synthetic method thereof
  • Charring agent with beta-crystal inducing nucleation effect, and synthetic method thereof
  • Charring agent with beta-crystal inducing nucleation effect, and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 500ml three-necked bottle equipped with a thermometer, a stirrer, and a constant pressure dropping funnel, add 36.90 g (0.2 mol) of cyanuric chloride, then add 100 ml of acetone, place the three-necked bottle in an ice bath, and stir fully to make Cyanuric chloride is evenly dispersed, and a mixture of 18.62g (0.2mol) of aniline and 20.24g (0.2mol) of triethylamine is added dropwise to the three-necked flask, the reaction temperature is controlled at -5 - 5°C, and the reaction time is 1 -2 hours, add water to precipitate, wash, and dry in vacuum to obtain a monobasic substitute for cyanuric chloride.

[0028] Add cyanuric chloride monobasic substitute (0.2 mol) into a 500mL three-necked flask equipped with a reflux heating and cooling tube, a stirrer, and a constant-pressure dropping funnel, and drop 12.02 g (0.2mol) into the three-necked flask with a constant-pressure funnel. The mixture of ethylenediamine and 40.48g (0.4mol) triethylamine controls the dropping ra...

Embodiment 2

[0031] In a 500ml three-necked bottle equipped with a thermometer, a stirrer, and a constant pressure dropping funnel, add 92.25g (0.2mol) of cyanuric chloride, then add 100ml of acetone, place the three-necked bottle in an ice bath, and stir fully to make Cyanuric chloride is evenly dispersed, add 46.56g (0.2mol) cyclohexylamine dropwise to the three-necked bottle, dissolve 11.22g (0.1mol) triethylenediamine in 50ml distilled water, add dropwise with a constant pressure funnel, and control the pH at 5-7, the reaction temperature is controlled at -5-5°C, the reaction time is 1-2 hours, adding water to precipitate, washing, and vacuum drying to obtain a monobasic cyanuric chloride substitute.

[0032] Add cyanuric chloride monobasic substitute (0.2 mol) into a 500mL three-necked flask equipped with a reflux heating and cooling tube, a stirrer, and a constant-pressure dropping funnel, and drop 17.63g (0.2mol) into the three-necked flask with a constant-pressure funnel The mixtur...

Embodiment 3

[0034] In a 500ml three-necked bottle equipped with a thermometer, a stirrer, and a constant pressure dropping funnel, add 36.90 g (0.2 mol) of cyanuric chloride, then add 100 ml of acetone, place the three-necked bottle in an ice bath, and stir fully to make Cyanuric chloride is evenly dispersed, and a mixture of 18.62g (0.2mol) of aniline and 20.24g (0.2mol) of triethylamine is added dropwise to the three-necked flask, the reaction temperature is controlled at -5 - 5°C, and the reaction time is 1 -2 hours, add water to precipitate, wash, and dry in vacuum to obtain a monobasic substitute for cyanuric chloride.

[0035] Add cyanuric chloride monobasic substitute (0.2 mol) into a 500mL three-necked flask equipped with a reflux heating and cooling tube, a stirrer, and a constant-pressure dropping funnel, and add 22.02 g (0.2mol) dropwise to the three-necked flask with a constant-pressure funnel. The mixture of hydroquinone and 40.48g (0.4mol) triethylamine controls the dropping...

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PUM

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Abstract

The invention relates to a charring agent having a beta-crystal inducing nucleation effect, and a synthetic method thereof. The method comprises the following steps: adding a solvent into a vessel, cooling the solvent in a freezing reactor or ice bath to -5-5 DEG C, adding cyanuric chloride, and uniformly stirring the solvent and the cyanuric chloride to obtain a mixed solution; dropwise adding a rigid group-containing reactant and an acid binding agent solution to the mixed solution, carrying out a reaction at -5-5 DEG C for 1-3 h, and separating the obtained reaction product to obtain a monobasic substituent; and dropwise adding a diamine or diol substance and the acid binding agent to a reaction container provided with the monobasic substituent, rising the temperature to 40-60 DEG C, carrying out a reaction for 1-3 h, rising the temperature to a solvent refluxing temperature, and carrying out a reaction for 5-8 h to obtain the charring agent. The charring agent has the advantages of high charring capacity, good thermal stability, and induction of a certain amount of beta-crystals to change the aggregation structure of a polypropylene composite material.

Description

technical field [0001] The invention belongs to the technical field of intumescent flame-retardant products, in particular, the invention relates to a char-forming agent containing a triazine structure and a rigid group and capable of inducing polypropylene to form certain beta crystals and a synthesis method thereof. Background technique [0002] The wide application of polypropylene and its composite materials has brought great convenience to people's production and life. However, polypropylene is a flammable material, which limits its use in places with flame retardant requirements. Therefore, it is very important to implement flame retardant modification of polypropylene, and flame retardants have also become one of the important additives for the application of polymer materials. . [0003] Traditional high-efficiency flame retardants generally contain halogens, especially bromine, which have high flame retardant efficiency. When such flame retardants are compounded wi...

Claims

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Application Information

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IPC IPC(8): C08G73/02C08G65/40C08L79/02C08L71/10C08L23/12
CPCC08G73/0273C08G65/4006C08G65/4081C08L23/12C08L2201/02C08L2205/242C08L79/02C08L71/00
Inventor 冯才敏黄健光梁敏仪刘洪波
Owner SHUNDE POLYTECHNIC
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