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Novel piperazine pyrophosphate flame retardant and preparation method thereof

A piperazine pyrophosphate and flame retardant technology, which is applied in the field of flame retardants, can solve the problems of easy agglomeration of flame retardants, reduced flame retardant efficiency, and restrictions on the application of piperazine flame retardants, and achieve good dispersion performance, Effect of improving flame retardancy and mechanical properties

Pending Publication Date: 2021-04-20
浙江富锦新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the prior art, there is a technology for preparing piperazine phosphate flame retardants. Although piperazine phosphate has been successfully prepared, the compatibility between the flame retardant and the plastic matrix is ​​poor, and the flame retardant itself is easy to agglomerate, resulting in The dispersion of flame retardants in the plastic matrix becomes poor, which eventually leads to a decrease in flame retardant efficiency and a significant decrease in other properties of the plastic matrix after flame retardant modification, which limits the further application of piperazine flame retardants

Method used

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  • Novel piperazine pyrophosphate flame retardant and preparation method thereof
  • Novel piperazine pyrophosphate flame retardant and preparation method thereof

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Effect test

Embodiment 1

[0035] A novel piperazine pyrophosphate flame retardant and a preparation method thereof, is characterized in that it comprises the following steps:

[0036]Step 1: Add 100kg of distilled water, 15kg of 2-piperazine carboxylic acid, and 34kg of phosphoric acid into the reaction kettle, pass nitrogen into the reaction kettle, fully remove the air, stir at 100r / min for 30min to fully dissolve the materials, and heat the reaction solution to 80°C , reacted for 2 hours, then lowered the temperature to 0°C, white crystals were precipitated, washed with ice distilled water, and filtered under reduced pressure to obtain white crystals, then put the obtained white crystals into a conical dryer, dried at 100°C for 4 hours, and removed water, then Transfer the powder to a vacuum kneader, raise the temperature to 220°C, keep it warm for 60 minutes, and then cool to room temperature to obtain pyrophosphate piperazine powder;

[0037] Step 2, react 3kg of diallylamine, 30kg of pyrophosphat...

Embodiment 2

[0041] A novel piperazine pyrophosphate flame retardant and a preparation method thereof, is characterized in that it comprises the following steps:

[0042] Step 1: Add 109kg of distilled water, 15kg of 2-piperazinone, and 35kg of phosphoric acid into the reaction kettle, feed nitrogen into the reaction kettle, fully remove the air, stir at 133r / min for 36min to fully dissolve the materials, and heat the reaction solution to 83°C. Reacted for 2 hours, then lowered the temperature to 2°C, white crystals were precipitated, washed with ice distilled water, and filtered under reduced pressure to obtain white crystals, then put the obtained white crystals into a conical dryer, dried at 103°C for 3 hours, and removed water, then put Transfer the powder to a vacuum kneader, raise the temperature to 228°C, keep it warm for 47 minutes, and then cool to room temperature to obtain pyrophosphate piperazine powder;

[0043] Step 2, react 4kg of diallylamine, 32kg of pyrophosphate piperazi...

Embodiment 3

[0047] A novel piperazine pyrophosphate flame retardant and a preparation method thereof, is characterized in that it comprises the following steps:

[0048] Step 1: Add 115kg of distilled water, 15kg of piperazine, and 37kg of phosphoric acid into the reaction kettle, pass nitrogen into the reaction kettle, fully remove the air, stir at 176r / min for 47min to fully dissolve the materials, heat the reaction solution to 85°C, and react for 2h , then lower the temperature to 3°C, white crystals are precipitated, washed with ice distilled water, and filtered under reduced pressure to obtain white crystals, then put the obtained white crystals in a conical dryer, dry at 106°C for 2 hours, remove moisture, and then transfer the powder In a vacuum kneader, raise the temperature to 235°C, keep it warm for 42 minutes, and then cool to room temperature to obtain pyrophosphate piperazine powder;

[0049] Step 2, react 7 powders, 0.9kg of dispersion stabilizer at 77°C for 0.9h;

[0050] ...

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Abstract

The invention discloses a novel piperazine pyrophosphate flame retardant and a preparation method thereof. The preparation method comprises the following steps: 1, adding distilled water, piperazinyl monomers and phosphoric acid into a reaction kettle in parts by mass, heating a reaction solution to 80-90 DEG C and reacting for 2h; reducing the temperature to 0-5 DEG C, separating out white crystals, and obtaining pyrophosphate piperazine powder; and carrying out surface polymerization reaction on the piperazine pyrophosphate, copper acrylate and (2, 7-octadiene-1-yl) succinic anhydride to obtain the novel piperazine pyrophosphate flame retardant.

Description

technical field [0001] The invention relates to the field of flame retardants, in particular to a novel piperazine pyrophosphate flame retardant and a preparation method thereof. Background technique [0002] With the continuous promotion of the application of polymer material technology, polymer materials have gradually replaced various metals and inorganic non-metallic materials with their high cost performance, and have gradually entered thousands of households. However, most polymer materials are easily It is flammable, and it will release a lot of heat when it burns. It has high smoke density and smoke toxicity, and the burning speed is fast. There are great safety hazards. It can be seen that the flame retardant modification of polymer materials is of great significance. [0003] At present, the flame retardant modification of polymer materials is mainly by adding flame retardants to the materials. According to whether the flame retardants contain halogen, flame retard...

Claims

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Application Information

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IPC IPC(8): C08G79/04C07F9/6509C08L63/00C08L85/02C08K5/3462
Inventor 方孝汉
Owner 浙江富锦新材料有限公司
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