Polyphosphate piperazine and preparation method and application thereof

A technology of piperazine polyphosphate and polyphosphoric acid, which is applied in the direction of organic chemistry, can solve the problems of high energy consumption, corrosive equipment, and high equipment requirements, and achieve easy operation and industrialization, good flame retardant effect, and good thermal stability Effect

Active Publication Date: 2019-03-01
HANGZHOU JLS FLAME RETARDANTS CHEM +1
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Problems solved by technology

However, by-products such as sodium chloride and piperazine pyrophosphate sodium salt can be produced during the above two preparation methods, and the by-products cannot be completely eliminated even by washing with water.
[0004] There are also some existing technologies that use piperazine diphosphate aging and devolatilization to prepare piperazine pyrophosphate, but this preparation method requires aging and devolatilization at a high temperature of 200 ° C to 300 ° C, high equipment requirements, high energy consumption of the product, and the product is white. Insufficient degree
In addition, there are existing technologies that use piperazine phosphate and high-temperature aging devolatilization of phosphoric acid to prepare piperazine pyrophosphate, but this preparation method needs to be carried out in the presence of an inert solvent. The reaction temperature of piperazine phosphate and phosphoric acid is 120-260 ° C. And the amount o

Method used

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  • Polyphosphate piperazine and preparation method and application thereof
  • Polyphosphate piperazine and preparation method and application thereof
  • Polyphosphate piperazine and preparation method and application thereof

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preparation example Construction

[0025] The present invention provides a kind of preparation method of piperazine polyphosphate, and the preparation method of piperazine polyphosphate comprises:

[0026] Salt forming step: Stir piperazine for 5 minutes to 30 minutes, then slowly add polyphosphoric acid preheated to 80°C to 100°C, keep the temperature at 45°C to 65°C, and stir for 0.5 hours to 3 hours to obtain the initial piperazine polyphosphate product.

[0027] Aging step: evacuate to a vacuum degree of 1000Pa-2000Pa, replace the inert gas several times and maintain the vacuum degree, continue to stir and heat to 150°C-200°C, and keep it for 1-4 hours to obtain piperazine polyphosphate.

[0028] In the preparation method of this piperazine polyphosphate, the reaction equation of polyphosphoric acid and piperazine is as follows:

[0029]

[0030] Where: n≥2.

[0031] The embodiment of the present invention also provides a kind of piperazine polyphosphate, the molecular structure of piperazine polyphosp...

Embodiment 1

[0035] Add 8.6kg of piperazine into the mixer, under stirring, slowly add 17.71kg of polyphosphoric acid (polymerization degree 2.1, preheated to 90°C) within 5 minutes, the material temperature is controlled at 60-65°C, keep the temperature after adding, continue React for 2 hours. Turn on the vacuum with a vacuum degree of 1000-2000 Pa. After nitrogen replacement for 5 times, keep the vacuum degree, continue stirring and heating to 150-160°C, and then continue aging and devolatilization for 4 hours to obtain piperazine polyphosphate. Cooling, crushing, packaging.

Embodiment 2

[0037] Add 8.6kg of piperazine into the mixer, under stirring, slowly add 18.57kg of polyphosphoric acid (polymerization degree 1.4, preheated to 80°C) within 5 minutes, control the material temperature at 45-50°C, keep the temperature after adding, continue React for 0.5 hours. Turn on the vacuum with a vacuum degree of 1000-2000 Pa. After nitrogen replacement for 5 times, keep the vacuum degree, continue to stir and heat to 190-200°C, then continue aging and devolatilization for 4 hours to obtain piperazine polyphosphate. Cooling, crushing, packaging.

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Abstract

The invention provides a polyphosphate piperazine and a preparation method and application thereof. The preparation method of the poly piperazine phosphate includes a salt forming step and an aging step, wherein the salt forming step includes stirring piperazine for 5-30 minutes, then slowly adding polyphosphoric acid preheated to 80-100 DEG C, maintaining the temperature at 45-65 DEG C, and stirring and reacting for 0.5-3 hours to obtain a primary product of the polyphosphate piperazine; and the aging step includes vacuumizing to a vacuum degree of 1000-2000 Pa, replacing inert gas for multiple times and maintaining the vacuum degree, continuously stirring and heating to 150-200 DEG C, and maintaining for 1-4 hours to obtain the polyphosphate piperazine.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to a piperazine polyphosphate, its preparation method and its application. Background technique [0002] Piperazine polyphosphate has good flame retardant properties and is completely halogen-free. Secondly, piperazine polyphosphate has good water resistance as a high-efficiency flame retardant. Using piperazine polyphosphate as a flame retardant is in line with the current halogen-free environmental protection flame retardant development trend. [0003] However, the commonly used preparation method of piperazine polyphosphate produces more by-products. In the prior art, there is a preparation method in which piperazine pyrophosphate is reacted in an aqueous solution to obtain piperazine pyrophosphate. Because piperazine pyrophosphate is hardly soluble in water, it becomes a precipitate, and the piperazine pyrophosphate product can be obtained by separation. Another pr...

Claims

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Application Information

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IPC IPC(8): C07D295/027C08L23/12C08L23/08C08L53/02C08K5/3462
CPCC07D295/027C08K5/3462C08L23/12C08L53/025C08L2201/02C08L23/0815
Inventor 裘雪阳邵江斌朱峰刘君锭王益锦
Owner HANGZHOU JLS FLAME RETARDANTS CHEM
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