Hybrid modified salt of phosphorus-containing acid, preparation method and application thereof

A technology of modification and phosphoric acid, which is applied in the field of preparation and hybrid modification of phosphoric acid-containing salts, can solve the problems of fire hazard expansion, poor compatibility, difficult industrial application, etc., and achieve the effect of improving decomposition temperature and thermal stability

Active Publication Date: 2018-08-21
DONGHUA UNIV
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  • Application Information

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Problems solved by technology

However, when these phosphoric acid-containing salts are used as flame retardants, there are still many problems, such as poor compatibility with the resin matrix, a certain fire hazard in itself, and a large amount of phosphine is released when it is burned (phosphine is a kind of It is an extremely flammable gas, which releases a large amount of heat during combustion, and these heat releases will also intensify the decomposition of phosphoric acid salts, further expanding the fire hazard caused by it) and other issues
[0004] The current mainstream modification method is the microencapsulation method, such as silicon-coated aluminum hypophosphite, melamine cyanurate-coated aluminum hypophosphite, Chinese patent CN 105860594A and document 1 (Aluminum hypophosphite microencapsulated to improve its safety and application to flame retardant polyamide 6.[J].Journal of Hazardous Materials,2015,294:186-194.), etc. In addition, there are also surface modification methods and ultra-fine methods, such as literature 2 (Effect of surface chemical modification for aluminum hypophosphite with hexa‐(4‐aldehyde‐phenoxy)‐cyclotriphosphazene on the fire retardancy, water resistance, and thermal properties for polyamide 6[J].Polymers for Advanced Technologies,2017. its application in polyurethane elastomer[J].Journal of Applied Polymer Science,2015,132(31).), however, although the above method can effectively improve the flame retardant efficiency of phosphoric acid-containing salts and achieve good flame retardant effects, there are also High cost, complex preparation process, difficult to industrial application and other issues

Method used

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  • Hybrid modified salt of phosphorus-containing acid, preparation method and application thereof
  • Hybrid modified salt of phosphorus-containing acid, preparation method and application thereof
  • Hybrid modified salt of phosphorus-containing acid, preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0055] A kind of hybrid modified phosphoric acid salt, its preparation steps are as follows:

[0056] (1) Preparation of amino-rich graphitic carbon nitride nanosheets:

[0057] 1) First heat the melamine to 330°C at a heating rate of 13.5°C / min and keep it warm for 10h;

[0058] 2) Then raise the temperature to 480°C at a heating rate of 12°C / min and keep it warm for 11 hours;

[0059] 3) Then raise the temperature to 500° C. at a heating rate of 0.5° C. / min and keep it warm for 3 hours to obtain amino-rich graphite carbon nitride; the nitrogen element 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 ...

Embodiment 2

[0067] A kind of hybrid modified phosphoric acid salt, its preparation steps are as follows:

[0068] (1) Preparation of amino-rich graphitic carbon nitride nanosheets:

[0069] 1) First heat dicyandiamine to 350°C at a heating rate of 22°C / min and keep it warm for 5 hours;

[0070] 2) Then raise the temperature to 490°C at a heating rate of 19°C / min and keep it warm for 8 hours;

[0071] 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 prepared amino-rich graphite carbon nitride contains graphite-like structures.

[0072] 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;

[0073] 5) Take out the amino-rich graphite carbon ni...

Embodiment 3

[0079] A kind of hybrid modified phosphoric acid salt, its preparation steps are as follows:

[0080] (1) Preparation of amino-rich graphitic carbon nitride nanosheets:

[0081] 1) First heat cyanamide to 300°C at a heating rate of 5°C / min and keep it warm for 6 hours;

[0082] 2) Then raise the temperature to 400°C at a heating rate of 3.5°C / min and keep it warm for 10 hours;

[0083] 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.

[0084] 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;

[0085] 5) Take out the amino-rich graphite carbon nitride, plac...

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Abstract

The invention relates to a hybrid modified salt of phosphorus-containing acid, a preparation method and application thereof. The preparation method includes: 1) dissolving a phosphorus-containing acidin a solvent, adding amino-rich graphite carbon nitride nanosheets, adjusting the PH value to 3-9, then adding a metal salt and carrying out reaction at 30-150DEG C for 2-12h; and 2) at the end of the reaction, conducting filtering, drying and crushing to obtain the hybrid modified salt of phosphorus-containing acid. The amino-rich graphite carbon nitride nanosheets in the obtained product have anitrogen element 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 product prepared by the method provided by the invention also can be applied to the field of flame retardant materials, and the flame retardance and carbon residue amount are greatly enhanced. The production raw materials used by the invention are widely available, the synthesis process is simple, the equipment requirements are low, and the thermal stability is significantly improved than that of non-hybrid modified salts of phosphorus-containing acid, the prepared product has good compatibility with a polymer matrix, and has better flame retardant effect.

Description

technical field [0001] The invention belongs to the field of preparation and application of flame retardants, and relates to a hybrid modified phosphoric acid-containing salt, a preparation method and application thereof. Background technique [0002] With the rapid development of my country's social economy, the losses caused by fires are also serious year by year. Using flame retardant materials is one of the most important ways to reduce fire hazards. [0003] Phosphoric acid-containing salts such as hypophosphite, phosphinate, phosphate, phosphite, etc. are widely used in polyamide and polyester because of their high phosphorus and aluminum content, good thermal stability, and high flame retardant effect. In the flame retardant of polymer materials. However, when these phosphoric acid-containing salts are used as flame retardants, there are still many problems, such as poor compatibility with the resin matrix, a certain fire hazard in itself, and a large amount of phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/02C08K5/5313C08K3/32C01B21/087C08L67/02C08L23/12C08L77/02
CPCC01B21/087C01P2002/72C01P2002/82C01P2004/24C01P2004/64C08K3/32C08K5/5313C08K9/02C08K2003/329C08L2201/02C08L2201/22C08L67/02C08L23/12C08L77/02
Inventor 郭承鑫彭治汉于海岩唐虹昌洋王朝生秦铭骏李换换翟一霖
Owner DONGHUA UNIV
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