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Hybrid modified melamine salt, preparation method and application thereof

A technology of melamine salt and melamine, which is applied in the field of hybrid modified melamine salt, can solve the problems of failing to improve the thermal stability of melamine salt, the thermal decomposition temperature is not significantly improved, the mechanical properties are retained, and the like, so as to avoid a large number of problems. Oxidation, increase special effect, increase the effect of content

Active Publication Date: 2018-08-21
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, document 1: the Chinese patent application number 201310550306.X uses zinc borate to modify melamine cyanurate, which improves production efficiency and reduces the viscosity of the reaction system; document 2: patent CN 107556255 A utilizes organic amine to modify melamine Polyphosphate, obtained a good flame retardant effect and its mechanical properties are well preserved; Document 3 (SiO 2 Preparation of modified melamine cyanurate halogen-free flame retardant[J].Colloid and Polymer,2012,30(4):168-170.) SiO 2 The sol is used to modify melamine cyanurate to obtain in-situ modified melamine cyanurate, which can control its particle size; Document 4 (synthesis of metal ion modified melamine polyphosphate and its effect on glass fiber reinforcement) Flame retardant research of PA66 [D]. Northeast Forestry University, 2007.) Use different metal ions to modify melamine polyphosphate, and then apply it to the flame retardant of nylon 66. Although this method has a high yield, its The flame retardant effect is average, and the improvement is not good
Although the above-mentioned methods have advantages of one kind or another, they all fail to improve the thermal stability of melamine salt, that is, the thermal decomposition temperature has no obvious improvement.

Method used

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  • Hybrid modified melamine salt, preparation method and application thereof
  • Hybrid modified melamine salt, preparation method and application thereof
  • Hybrid modified melamine salt, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] A hybrid modified melamine salt, the preparation steps of which are as follows:

[0049] (1) Preparation of amino-rich graphitic carbon nitride nanosheets:

[0050] 1) First heat the melamine to 330°C at a heating rate of 2°C / min and keep it warm for 2 hours;

[0051] 2) Then raise the temperature to 480°C at a heating rate of 2°C / min and keep it warm for 2h;

[0052] 3) Then raise the temperature to 500° C. at a heating rate of 2° C. / min and keep it warm for 2 hours to obtain amino-rich graphite carbon nitride; the nitrogen content of the prepared amino-rich graphite carbon nitride is 66.5 wt%. Its chemical structure is rich in amino groups, such as figure 1 The shown Fourier transform infrared spectrum is at 2700-3400cm -1 It can be proved by the broad absorption peak at the position that the prepared amino-rich graphitic carbon nitride contains a graphite-like structure, which can also be proved by the sharp peaks near 13.5° and 27.5° in the X-ray diffraction patt...

Embodiment 2

[0060] A hybrid modified melamine salt, the preparation steps of which are as follows:

[0061] (1) Preparation of amino-rich graphitic carbon nitride nanosheets:

[0062] 1) First heat dicyandiamine to 350°C at a heating rate of 22°C / min and keep it warm for 5 hours;

[0063] 2) Then raise the temperature to 490°C at a heating rate of 19°C / min and keep it warm for 8 hours;

[0064] 3) Then raise the temperature to 530° C. at a heating rate of 11.5° C. / min and keep it warm for 9 hours to obtain amino-rich graphite carbon nitride; the nitrogen element content of the prepared amino-rich graphite carbon nitride is 67.3 wt%. Its chemical structure is rich in amino groups, and the obtained amino-rich graphite carbon nitride contains graphite-like structures;

[0065] 4) Completely immerse the amino-rich graphite carbon nitride in liquid oxygen and maintain the temperature T1 and maintain the pressure P1 for 22 minutes;

[0066] 5) Take out the amino-rich graphite carbon nitride ...

Embodiment 3

[0072] A hybrid modified melamine salt, the preparation steps of which are as follows:

[0073] (1) Preparation of amino-rich graphitic carbon nitride nanosheets:

[0074] 1) First heat cyanamide to 300°C at a heating rate of 5°C / min and keep it warm for 6 hours;

[0075] 2) Then raise the temperature to 400°C at a heating rate of 3.5°C / min and keep it warm for 10 hours;

[0076] 3) Then raise the temperature to 550° C. at a heating rate of 18° C. / min and keep it warm for 2 hours to obtain amino-rich graphitic carbon nitride; the nitrogen content of the prepared amino-rich graphitic carbon nitride is 66 wt%. The chemical structure is rich in amino groups, and the prepared amino-rich graphitic carbon nitride contains a graphite-like structure.

[0077] 4) Completely immerse the amino-rich graphite carbon nitride in liquid helium and maintain the temperature T1 and maintain the pressure P1 for 18 minutes;

[0078] 5) Take out the amino-rich graphite carbon nitride and place i...

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Abstract

The invention relates to a hybrid modified melamine salt, a preparation method and application thereof. The preparation method includes: 1) dissolving a melamine salt in a solvent, adding amino-rich graphite carbon nitride nanosheets, and carrying out reaction at 30-150DEG C for 0.5-4h; and 2) at the end of the reaction, conducting filtering, drying and crushing to obtain the hybrid modified melamine salt. Specifically, the amino-rich graphite carbon nitride nanosheets have a nitrogen content of 66-68wt%, the chemical structure is rich in amino, the thickness is 0.5-50nm, and the nanosheets contain a graphite-like structure. The 5wt% thermal weight loss temperature of the product is 20-80DEG C higher than that of non-hybrid modified melamine salts. The product obtained by the invention isalso applied to the field of flame retardant materials, and the flame retardant performance and carbon residue amount are greatly improved. The production raw materials used by the invention are widely available, the synthesis process is simple, the equipment requirements are low, and the product has good thermal stability, good compatibility with a polymer matrix and good flame retardant effect,and has great application prospects.

Description

technical field [0001] The invention belongs to the field of preparation and application of flame retardants, and relates to a hybrid modified melamine salt, a preparation method and application thereof. Background technique [0002] Polycyanamide polysalts, such as melamine polyphosphate, melamine cyanurate, etc., generally have the advantages of high thermal decomposition temperature, low water solubility, low smoke generation and less toxic gas generation. The synergistic and synergistic effect of the compound shows good flame retardant properties, and has become a research hotspot of flame retardants in recent years. It is an important phosphorus-nitrogen flame retardant and has been widely used in polyamide and polyolefin fields. . [0003] Although its application prospect is good, the application limitations of melamine salt are very strong, such as poor compatibility, uneven dispersion, large addition amount and large loss of mechanical properties. [0004] Modific...

Claims

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Application Information

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IPC IPC(8): C08K9/02C08K5/3492C01B21/087C08L77/00C08L23/12C08L23/06
CPCC01B21/087C01P2002/72C01P2002/82C01P2004/24C01P2004/64C08K5/34928C08K9/02C08L2201/02C08L2201/22C08L77/00C08L23/12C08L23/06
Inventor 郭承鑫彭治汉杨灿张宇萱王朝生翟一霖李换换秦铭骏
Owner DONGHUA UNIV
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