Polyphosphate piperazine and preparation method and application thereof

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...

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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 of inert solvent is more than 3 times of the total weight of piperazine phosphate and phosphoric acid, solvent evaporation and recovery limit the implementation of this scheme

In addition, there are prior art methods for preparing high-purity piperazine pyrophosphate using phosphorus pentoxide, phosphoric acid, glacial acetic acid, and piperazine, but the preparation method has long reaction steps, needs to control the low temperature reaction, and needs Solvent removal, high cost

In addition, there are existing technologies that use ammonium dihydrogen phosphate and piperazine as raw materials to prepare piperazine pyrophosphate. This method uses a solid phosphorus source, which overcomes the common use of liquid phosphoric acid as a phosphorus source, but has the disadvantages of difficult transportation and storage. And high temperature deamination is required, and the release of ammonia gas at high temperature is easy to corrode the equipment

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