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A class of flame retardant containing melamine structure, preparation method and application thereof

A melamine and flame retardant technology, applied in the field of flame retardants, can solve the problems of slow application and development of flame retardants, complex synthesis process, low yield, etc., and achieve high use value, high reaction efficiency, and low preparation cost Effect

Active Publication Date: 2020-02-11
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the application and development of flame retardants containing melamine structure are relatively slow, and there are few products that have been put into commercial production, and there are disadvantages such as complex synthesis process, low yield and high price.

Method used

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  • A class of flame retardant containing melamine structure, preparation method and application thereof
  • A class of flame retardant containing melamine structure, preparation method and application thereof
  • A class of flame retardant containing melamine structure, preparation method and application thereof

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Effect test

specific Embodiment approach

[0032] The present invention will be further described below in conjunction with the examples, but the protection scope of the present invention is not limited to the scope expressed in the examples.

[0033] Instruments and reagents:

[0034] The melting point was measured with an X4 melting point apparatus (produced by Beijing Third Optical Instrument Factory), and the thermometer was not calibrated; 1 H NMR and 13 C NMR is measured with Varian Mercury 400 type 400MHz nuclear magnetic resonance instrument or Varian Mercury 600 type 600MHz nuclear magnetic resonance instrument, deuterated chloroform (CDCl 3 ) or deuterated dimethyl sulfoxide (DMSO-d 6 ) as the solvent and TMS as the internal standard; MS was determined using a FinniganTrace mass spectrometer; elemental analysis was determined using a Vario EL III elemental analyzer; the reagents used were domestic (or imported) chemically pure or analytically pure. Solvents methanol and isopropanol were dried.

Embodiment 1

[0036] A method for preparing N-(tert-butyl)-2-(N-(4,6-diamino-1,3,5-triazin-2-yl)formamido)acetamide flame retardant, comprising the following experimental steps:

[0037] Under nitrogen protection, compound melamine 1 (0.378g, 3mmol, 3.0eqv.), formic acid 2a (0.046g, 1.0mmol, 1.0eqv.), formaldehyde 3a (0.030g, 1.0mmol, 1.0eqv.) were added to the reactor successively. ), tert-butylisonitrile 4a (0.091g, 1.1mmol, 1.1eqv.), MeOH:i-PrOH=2:1 (10ml), heated to 50°C and stirred for 30 minutes to dissolve it. After dissolving, add the copper complex (0.025g) supported by the catalyst MCM-41, MIL-101 (0.025g) and p-toluenesulfonic acid (0.017g) and continue to stir while the temperature drops to 40°C. After continuing the reaction for 24h, TLC After the detection reaction was completed, the solvents methanol and ethanol were removed under reduced pressure, and the residue was filtered, extracted and column chromatographed to obtain the target flame retardant Ia with a yield of 57.01%...

Embodiment 2

[0045] A method for preparing octyl 2-(2-(N-(4,6-diamino-1,3,5-triazin-2-yl)formamido)acetamido)acetate flame retardant, comprising the following experimental steps:

[0046]Under the protection of nitrogen, compound melamine 1 (0.378g, 3mmol, 3.0eqv.), formic acid 2a (0.046g, 1.0mmol, 1.0eqv.), formaldehyde 3a (0.030g, 1.0mmol, 1.0eqv.) were added to the reactor successively. ), n-octyl acetate isonitrile 4b (0.22 g, 1.1 mmol, 1.1 eqv.), MeOH:i-PrOH=2:1 (10 ml), heated to 50°C and stirred for 30 minutes to dissolve it. After dissolving, add the copper complex (0.025g) supported by the catalyst MCM-41, MIL-101 (0.025g) and p-toluenesulfonic acid (0.017g) and continue stirring while the temperature drops to 40°C. After continuing the reaction for 24h, TLC After the detection reaction was completed, the solvents methanol and ethanol were removed under reduced pressure, and the residue was filtered, extracted and column chromatographed to obtain the target flame retardant Ia with...

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Abstract

The invention relates to flame retardants containing melamine structure as well as a preparation method and application thereof. The chemical structural formula of the flame retardants is shown in thedescription, wherein substituent groups R1, R2 and R3 are any one of hydrogen, tertiary butyl, normal-butyl, cyclohexyl alkyl or chlorine, bromine, methyl, methoxy, nitryl, amino, hydroxy-substitutedaryl or ceteroary. A synthesis method comprises the following steps: carrying out Ugi reaction on carboxylic acid compounds, the melamine, aldehyde compounds and isonitrile compounds in a mixed solvent of methanol and isopropanol at the temperature of 50 DEG C under the concerted catalysis of an MCM-41-loaded copper complex, MIL-101 and p-toluenesulfonic acid; carrying out filtering, extracting and column chromatography on a product to obtain the flame retardants containing the melamine. The invention discloses a novel preparation method with the advantages of simple reaction, few byproductsand better selectivity, which is used for selectively synthesizing the melamine flame retardants. The flame retardants disclosed by the invention have the advantages of good thermal stability, high flame retardancy rate, high purity reaching to 97.2 percent, easily-obtained raw materials, advanced technology and easiness for industrial production.

Description

technical field [0001] The invention relates to a class of flame retardant containing melamine structure, a preparation method and application research thereof. Background technique [0002] When traditional halogen-containing flame retardant materials are burned, secondary hazards such as smoke, toxic or corrosive gases are emitted, which pose a serious threat to personal safety. Therefore, it is particularly important to find new halogen-free flame retardants. Melamine-based flame retardants have the characteristics of halogen-free and low toxicity; high decomposition temperature, suitable for processing; small impact on mechanical properties; The great development value has caused people to study extensively. In the United Kingdom, Europe and North America, melamine derivatives are used to improve the flame retardancy of polyurethane foam, and have been extended to other types of polymers, such as hard polyurethane foam and thermoplastics. Recently, the application test...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/3492C08L63/00C08L75/04B01J31/22C07D251/70
CPCB01J29/0333B01J31/0225B01J31/1616B01J31/1691B01J35/0006C07D251/70C08K5/34922C08L63/00C08L75/04
Inventor 王龙刘娜李德江刘明国黄年玉
Owner CHINA THREE GORGES UNIV
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