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Flame-retardation sulfur-containing macromolecular triazine charring agent and preparation method thereof

A technology of triazine and char-forming agent, applied in the direction of organic chemistry, etc., can solve the problems of unsatisfactory char-forming effect, limiting the application scope of IFR, limiting the application field of PP, etc., and achieves good char-forming effect and good char-forming efficiency. , the effect of good environmental benefits

Active Publication Date: 2016-11-09
ZHEJIANG XUSEN NON HALOGEN SMOKE FLAME RETARDANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, PP is an extremely flammable material, and the char formation rate is almost 0, and it is easy to melt and drip, which limits the application field of PP.
In order to solve the flammability problem of PP, IFR is gradually applied to polyolefin materials such as polypropylene (PP), and the carbon sources used are mostly pentaerythritol and its series, but the char formation effect in PP is not very ideal, and it has a Disadvantages such as temperature difference, poor water resistance, and easy migration limit the application range of IFR in PP

Method used

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  • Flame-retardation sulfur-containing macromolecular triazine charring agent and preparation method thereof
  • Flame-retardation sulfur-containing macromolecular triazine charring agent and preparation method thereof
  • Flame-retardation sulfur-containing macromolecular triazine charring agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 The structural formula of the carbon forming agent described in Embodiment 1 is:

[0037]

[0038] The preparation method is: add 200ml of acetonitrile and 29.72g (0.1mol) triglycidyl isocyanurate to a 500ml four-neck flask equipped with a stirrer, a thermometer, a constant temperature dropping funnel and a high-efficiency reflux condenser, start stirring, and drop Add 6.11g (0.1mol) of ethanolamine, after dripping, raise the temperature to 30°C, and keep it warm for 1.5h to make the pH of the reaction solution reach 7-8; then add 7.60g (0.1mol) of thiourea, and control the temperature during the addition Do not exceed 50°C, and then reflux for 6 hours to make the pH of the solution reach 7-8. After cooling, filter with suction (solvent recovery), wash with water, dry and pulverize to obtain the product CFA-1; the yield is 98.3% , 1% thermal weight loss decomposition temperature is 265.0 ° C, through FTIR and NMR test analysis, to determine the structure...

Embodiment 2

[0039] Embodiment 2 The structural formula of the carbon forming agent described in Embodiment 2 is:

[0040]

[0041] The preparation method is: add 250ml of acetonitrile and 29.72g (0.1mol) triglycidyl isocyanurate to a 500ml four-neck flask equipped with a stirrer, a thermometer, a constant temperature dropping funnel and a high-efficiency reflux condenser, start stirring, and drop Add 6.11g (0.1mol) ethanolamine, after dripping, raise the temperature to 30°C, and keep it warm for 1.5h to make the pH value of the reaction solution reach 7-8; then add 9.11g (0.1mol) thiosemicarbazide, and control The temperature does not exceed 50°C, and then reflux for 7 hours to make the pH of the solution reach 7-8. After cooling, suction filtration (solvent recovery), washing, drying and crushing, the product CFA-2 is obtained; the yield is 97.5 %, 1% thermal weight loss decomposition temperature is 268.3 ° C, through FTIR and NMR test analysis, to determine the structure of the produ...

Embodiment 3

[0042] Embodiment 3 The structural formula of the carbon forming agent described in Embodiment 3 is:

[0043]

[0044] The preparation method is: add 250ml of water and 29.72g (0.1mol) triglycidyl isocyanurate to a 500ml four-neck flask equipped with a stirrer, a thermometer, a constant temperature dropping funnel and a high-efficiency reflux condenser, start stirring, and drop Add 6.11g (0.1mol) of ethanolamine, after dripping, raise the temperature to 30°C, and keep it warm for 1.5h to make the pH of the reaction solution reach 7-8; then add 13.52g (0.1mol) of dithiobiuret, add Control the temperature in the process not to exceed 50°C, and then reflux for 8 hours to make the pH of the solution reach 7 to 8. After cooling, filter with suction (solvent recovery), wash with water, dry and pulverize to obtain the product CFA-3; The yield is 96.4%, and the decomposition temperature of 1% thermogravimetric loss is 265.4°C. The structure of the product is confirmed by FTIR and N...

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Abstract

The invention relates to a flame-retardation sulfur-containing macromolecular triazine charring agent and a preparation method thereof. The structure of the compound is represented by formula shown in the description; and in the formula, n is greater than 1, X is alcohol amine, and Y is dialkylamine. The preparation method comprises the following steps: adding equimolar alcohol amine to a triglycidyl isocyanurate solution while stirring, heating the obtained solution to a certain temperature, and carrying out a reaction for a period of time to make the pH value of the solution be 7-8; and adding a certain mole of dialkylamine, heating the obtained solution to a certain temperature, carrying out a heat insulation reaction for a period of time to make the pH value of the solution be 7-8, cooling the solution, carrying out suction filtration (solvent recycling), washing the obtained material with water, drying the washed material, and crushing the dried material to obtain the product flame-retardation sulfur-containing macromolecular triazine charring agent. The flame-retardation sulfur-containing macromolecular triazine charring agent is an excellent flame-retardation charring agent, has a charring anti-drip effect, has good compatibility with high-molecular materials, has good heatproof and waterproof property, has excellent processing properties, and can be used as the flame-retardation charring agent of polyethylene (PE), polypropylene (PP) and silicone rubber; and the preparation method has the advantages of cheap and easily available raw materials, low production cost, less device investment, simple production process, and easy large-scale production.

Description

technical field [0001] The invention relates to a sulfur-containing macromolecule triazine flame-retardant char-forming agent compound and a preparation method thereof. The compound can be used as a char-forming agent for materials such as polyethylene (PE), polypropylene (PP), and silicon rubber. Background technique [0002] Intumescent flame retardant (IFR) is a kind of compound environmental protection green flame retardant mainly composed of nitrogen and phosphorus. It does not contain halogen and does not use antimony oxide as a synergist. The system itself has a synergistic effect. When the plastic containing intumescent flame retardant is burned, a carbon foam layer will be formed on the surface, which has the functions of heat insulation, oxygen insulation, smoke suppression, and anti-drip. The generation of corrosive gas is in line with the research and development direction of flame retardants in the future, and has become one of the most active flame retardant re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/36C08K3/32C08L23/12C08L79/04C08G73/06C07D251/30C07D403/14C07D409/14
CPCC07D251/30C07D403/14C07D409/14C08G73/0638C08K3/32C08K5/36C08K2003/323C08L23/12C08L2201/02C08L79/04
Inventor 孟凡一李四新
Owner ZHEJIANG XUSEN NON HALOGEN SMOKE FLAME RETARDANT CO LTD
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