Method for preparing piperazine pyrophosphate

A technology of piperazine pyrophosphate and piperazine phosphate, which is applied in the field of preparation of piperazine pyrophosphate, can solve the problems of increasing production energy consumption, achieve the effects of reducing heating energy consumption, reducing process steps, and cheap preparation

Active Publication Date: 2012-01-04
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of solvent, the method needs to carry out solid-liquid separation for product desolvation; and because heating is required during preparation, production energy consumption is also increased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 250mL vacuum kneader, at a speed of 40rpm, add 80g of piperazine phosphate, and spray 50g of 85wt% phosphoric acid into the kneading kettle during the heating process. After spraying, vacuumize and heat up to 270°C to continue dehydration After condensation reaction for 1 hour, 113.4 g of white powder of piperazine pyrophosphate was obtained, the sodium content was 0 ppm, the decomposition temperature was 341° C., and the purity was 100%.

Embodiment 2

[0028] In the 150L pressurized kneader, under the condition that the rotating speed is 60rpm, first add 48kg of piperazine phosphate, pressurize and protect the kneading kettle with nitrogen, and spray 30.1kg of 85wt% phosphoric acid into the kettle during the heating process, and the temperature reaches After 150°C, the dehydration condensation reaction was carried out for 3 hours to obtain 68.1 kg of white powder of piperazine pyrophosphate, with a sodium content of 0 ppm, a decomposition temperature of 345°C, and a purity of 98.7%.

Embodiment 3

[0030] In the extruder, under the condition that the rotation speed is 100rpm and the barrel temperature is 150°C-240°C (direction from the feed port to the die), piperazine phosphate and phosphoric acid are added to the feed port in an equimolar ratio, and the The section is vacuumized, and a white powder of piperazine pyrophosphate is obtained at the die, with a sodium content of 0 ppm, a decomposition temperature of 335° C., and a purity of 99%.

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Abstract

The invention discloses a method for preparing piperazine pyrophosphate. The method is a method A or a method B; in the method A, piperazine sulfate and phosphoric acid are mixed in a molar ratio of 1:1 in a reaction device and the mixture is subjected to dehydration condensation at the temperature of between 150 and 300 DEG C to form the piperazine pyrophosphate; and in the method B, piperazine sulfate and phosphoric acid are subjected to dehydration condensation in a molar ratio of 1:1 at the temperature of between 120 and 260 DEG C in a reaction device in the presence of an inert solvent, wherein the inert solvent has the boiling point of more than or equal to 100 DEG C, and the using amount of the inert solvent is more than three times the total weight of the piperazine sulfate and the phosphoric acid.

Description

technical field [0001] The invention relates to a preparation method of piperazine pyrophosphate, in particular to a method for preparing piperazine pyrophosphate through dehydration condensation by using piperazine pyrophosphate. Background technique [0002] Piperazine pyrophosphate (piperazine pyrophosphate), as an important component of halogen-free additive flame retardant, has excellent flame retardant effect, and now it is getting more and more attention from the flame retardant industry. At one time, some new Preparation. [0003] In the prior art, Japanese Patent Laid-Open No. 47-88791, U.S. Patent US 3810850, and U.S. Patent No. 4599375 respectively disclose methods for preparing piperazine pyrophosphate by reacting in aqueous solution. Piperazine pyrophosphate becomes a precipitate due to its poor solubility in water product, the piperazine pyrophosphate product can be obtained by separation. But above-mentioned method can not remove the sodium chloride and pipe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/027
Inventor 陈涛郝冬梅陈崇伟尹亮林倬仕刘彦明
Owner SHANGHAI RES INST OF CHEM IND
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