Flame retardant phosphoryl melamine compound and preparation method thereof

A technology of flame retardant phosphoramidide and phosphoramidide, which is applied in the field of flame retardant phosphoramidine compound and its preparation, can solve the problems of poor permanence, easy migration, easy blooming, etc., and achieve structural stability Good, easy to obtain raw materials, good anti-melt dripping effect

Pending Publication Date: 2022-06-21
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, phosphorus-nitrogen flame retardants are widely developed and applied, such as melamine phosphate, melamine pyrophosphate, melamine polyphosphate, etc. Although the above compounds have good flame retardancy, they are caused by the structure of salt-bonded ionic compounds. The easy ionization characteristics make it easy to absorb moisture, easy to migrate, easy to bloom, and poor in permanence in applications.
Therefore, in order to overcome the shortcomings caused by the above-mentioned ionic bonds, in the design of the molecular structure of the compound, only by changing the salt bond ionic combination of the compound into a stable covalent bond structure can meet the great market application demand

Method used

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  • Flame retardant phosphoryl melamine compound and preparation method thereof
  • Flame retardant phosphoryl melamine compound and preparation method thereof
  • Flame retardant phosphoryl melamine compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 In a 500mL four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a drying tube, under nitrogen protection, add dry melamine sodium salt 29.62g (0.2mol) and 150mL of chloroform, within 30 minutes at room temperature. 30.66g (17.1mL, 0.2mol) of phosphorus oxychloride was added dropwise, after dropping, the temperature was raised to 60°C, refluxed for 6 hours, 3.6mL of water was added dropwise, the reaction was performed for 1 hour until no hydrogen chloride gas was generated, and the temperature was lowered to 30°C, Then add 18 mL of water to dissolve the sodium chloride, suction filtration, rinse the filter cake three times with 60 mL of ice water, compact and drain for each rinse, and vacuum dry at 80 °C to obtain white crystal phosphoramide. . The product yield was 88.3%.

Embodiment 2

[0031] Embodiment 2 In a 500mL four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a drying tube, under nitrogen protection, add dry melamine sodium salt 29.62g (0.2mol) and 180mL of dichloroethane, at room temperature 30.66g (17.1mL, 0.2mol) of phosphorus oxychloride was added dropwise within 30 minutes, after the drop was completed, the temperature was raised to 80°C, the reaction was refluxed for 6 hours, 3.6mL of water was added dropwise, the reaction was performed for 1 hour until no hydrogen chloride gas was generated, and the temperature was cooled to 30 ℃, then add 18 mL of water to dissolve the generated sodium chloride, suction filtration, the filter cake is rinsed three times with 60 mL of ice water, each rinse is compacted and drained, and dried at 80 ℃ in vacuum to obtain white crystalline phosphorus amide. The product yield was 90.5%.

Embodiment 3

[0032] Embodiment 3 In the 500mL four-necked flask equipped with agitator, thermometer, reflux condenser and drying tube, under nitrogen protection, add dry melamine sodium salt 29.62g (0.2mol) and 180mL carbon tetrachloride, at room temperature 30.66g (17.1mL, 0.2mol) of phosphorus oxychloride was added dropwise within 30 minutes, after dropping, the temperature was raised to 75°C, refluxed for 5 hours, 3.6mL of water was added dropwise, the reaction was performed for 1 hour until no hydrogen chloride gas was produced, and the temperature was cooled to 30 ℃, then add 18 mL of water to dissolve the generated sodium chloride, suction filtration, the filter cake is rinsed three times with 60 mL of ice water, each rinse is compacted and drained, and dried at 80 ℃ in vacuum to obtain white crystalline phosphorus amide. The product yield was 86.0%.

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Abstract

The invention relates to a flame retardant phosphoryl melamine compound and a preparation method thereof, the structure of the compound is shown in the following formula: the preparation method comprises the following steps: in an organic solvent, reacting melamine sodium salt with 1-1.1 times of mole of phosphorus oxychloride, and purifying to obtain phosphoryl melamine. The compound disclosed by the invention is stable in structure, high in flame-retardant efficiency, good in expansion charring property and wide in application range, and can be used as a flame retardant of materials such as epoxy resin, unsaturated polyester resin and polyvinyl alcohol; the flame retardant can also be used as a flame retardant for wood, cotton, hemp, paper, cellulose and the like; the process is simple, equipment investment is low, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant phosphoric melamine compound and a preparation method thereof. Specifically, it relates to a flame retardant phosphoryl melamine compound and a preparation method thereof. The compound can be used as a flame retardant for epoxy resin, unsaturated polyester resin, polyvinyl alcohol and other materials; it can also be used as a flame retardant for wood, cotton, hemp, etc. , flame retardant for paper, cellulose, etc. Background technique [0002] At present, with the improvement of environmental protection and human health awareness, the research of new high-efficiency, low-toxicity, halogen-free, and environment-friendly flame retardants has become a hot spot. Among them, phosphorus-nitrogen flame retardants are more developed and applied, such as melamine phosphate, melamine pyrophosphate, melamine polyphosphate, etc. Although the above compounds have good flame retardancy, they are caused by the structure of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6521C08K5/5399C08L67/06C08J5/04C08J5/10
CPCC07F9/6521C08K5/5399C08J5/043C08J5/10C08J2367/06C08K7/14
Inventor 娄帅仲柿成王彦林
Owner SUZHOU UNIV OF SCI & TECH
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