Flame retardants containing melamine structure as well as 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: 2018-06-05
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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  • Flame retardants containing melamine structure as well as preparation method and application thereof
  • Flame retardants containing melamine structure as well as preparation method and application thereof
  • Flame retardants containing melamine structure as well as preparation method and application thereof

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specific Embodiment approach

[0032] Hereinafter, the present invention will be further described in conjunction with the embodiments, but the scope of protection claimed by the present invention is not limited to the scope expressed by the embodiments.

[0033] Instruments and reagents:

[0034] The melting point was measured with X4 melting point meter (produced by Beijing No. 3 Optical Instrument Factory), and the thermometer was not calibrated; 1 H NMR and 13 C NMR is measured by Varian Mercury 400 400MHz nuclear magnetic resonance instrument or Varian Mercury 600 600MHz nuclear magnetic resonance instrument, deuterated chloroform (CDCl 3 ) Or deuterated dimethyl sulfoxide (DMSO-d 6 ) Is the solvent and TMS is the internal standard; MS is determined by FinniganTrace mass spectrometer; elemental analysis is determined by Vario EL III elemental analyzer; the reagents used are domestic (or imported) chemical or analytical pure. The solvents methanol and isopropanol are 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 includes the following experimental steps:

[0037] Under the protection of nitrogen, the compound melamine 1 (0.378g, 3mmol, 3.0eqv.), formic acid 2a (0.046g, 1.0mmol, 1.0eqv.), and formaldehyde 3a (0.030g, 1.0mmol, 1.0eqv.) were added to the reactor in sequence. ), tert-butyl isonitrile 4a (0.091g, 1.1mmol, 1.1eqv.), MeOH:i-PrOH=2:1 (10ml), heated to 50°C and stirred for 30 minutes to dissolve. After dissolving, add the copper complex supported by the catalyst MCM-41 (0.025g), MIL-101 (0.025g) and p-toluenesulfonic acid (0.017g) in sequence. Continue stirring, while the temperature drops to 40℃. After the reaction continues for 24 hours, TLC After the detection reaction is completed, the solvents methanol and ethanol are removed under reduced pressure, and the remainder is filtered, extracted and column chromatography to obtain the target flame retardant Ia with...

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 includes the following experimental steps:

[0046] Under the protection of nitrogen, the compound melamine 1 (0.378g, 3mmol, 3.0eqv.), formic acid 2a (0.046g, 1.0mmol, 1.0eqv.), and formaldehyde 3a (0.030g, 1.0mmol, 1.0eqv.) were added to the reactor in sequence. ), 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. After dissolving, add the copper complex supported by the catalyst MCM-41 (0.025g), MIL-101 (0.025g) and p-toluenesulfonic acid (0.017g) in sequence. Continue stirring, while the temperature drops to 40℃. After the reaction continues for 24 hours, TLC After the detection reaction is completed, the solvents methanol and ethanol are removed under reduced pressure, and the remainder is filtered, extracted and column chromatography to obtain the target flame reta...

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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 kind of flame retardant containing melamine structure, a preparation method and application research thereof. Background technique [0002] Traditional halogen-containing flame-retardant materials have secondary hazards such as smoke, toxic or corrosive gas emission, which poses a serious threat to personal safety. Therefore, it is particularly important to find new halogen-free flame retardants. Melamine-based flame retardants are halogen-free and low-toxic; they have high decomposition temperature and are suitable for processing; they have little impact on mechanical properties; they do not ooze and do not corrode molds; they have excellent flame retardant properties. New high-efficiency flame retardants containing melamine structure have The great development value has caused extensive research. In the UK, Europe and North America and other places, melamine derivatives are used to improve the flame retardant properties of poly...

Claims

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Application Information

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Patent Type & Authority Applications(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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