Prepn. of expanding halide-free fire-retardant and products thereof

The technology of an intumescent flame retardant and a phase transfer catalyst is applied in the field of flame retardant preparation, and can solve the problems of not easy to be affected by coloration and decomposition mechanical properties, easy to color decomposition mechanical properties, and unstable flame retardant effect.

Active Publication Date: 2006-09-20
HANGZHOU JLS FLAME RETARDANTS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The present invention aims at the disadvantages of the prior art and the disadvantages of easy migration in plastics, poor heat resistance, easy coloring and decomposition, great influence on the mechanical properties of plastics and the use of compounding, which makes the flame retardant effect unstable, and provides a plastic in plastics. Not easy to migrate; good heat resistance, not easy to color and decompose, less impact on the mechanical properties of plastics, and a preparation method and product of an intumescent halogen-free flame retardant with stable flame retardant effect

Method used

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  • Prepn. of expanding halide-free fire-retardant and products thereof
  • Prepn. of expanding halide-free fire-retardant and products thereof
  • Prepn. of expanding halide-free fire-retardant and products thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0161] 1. Add phosphorus pentoxide (P 2 o 5 Content ≥ 98%) 4347 grams, add diammonium hydrogen phosphate (ammonium dihydrogen phosphate content ≥ 95%) 3631.6 grams simultaneously, stir and heat, and pass 20 minutes of 0.1 liters / minute of ammonia, and keep the ammonia pressure at 0.2Mpa. When it rises to 250°C, it becomes a viscous syrupy liquid, and when kept at 250°C for 1 hour, it becomes a white solid powder.

[0162] 2. Under stirring, pass 0.2 L / min of nitrogen gas, cool to 50° C., pulverize and sieve to obtain compound (III).

[0163] 3. At -5°C, add 1000 grams of (III) to 3 liters of 85% ethanol, stir for 30 minutes, add 0.2 grams of benzyltriphenylphosphine hydroxide activated with pyridine, and add 230 grams of it evenly under stirring The nitrogen-containing triazine polymer was reacted for 3 hours, filtered, dried, and pulverized to obtain 1217 grams of an expandable halogen-free flame retardant. The yield was 98.94%. The water solubility is 0.24g / 100g water, a...

Embodiment 2

[0165] At -5°C, add 1000 grams of (III) to 3 liters of 85% ethanol, stir for 30 minutes, add 0.2 grams of benzyltriphenylphosphine hydroxide activated with pyridine, and add 26 grams of morphine evenly under stirring , 78 grams of melamine and 45 piperazine, reacted for 2 hours, filtered, dried, and pulverized to obtain 1068 grams of expandable halogen-free flame retardant, with a yield of 92.95%, water solubility of 0.63g / 100g water, and TGA thermal decomposition temperature of 210.56 ℃.

Embodiment 3

[0167] At -5°C, add 1000 grams of (III) to 3 liters of 85% ethanol, stir for 30 minutes, add 0.2 grams of benzyltriphenylphosphine hydroxide activated with pyridine, and evenly add 120 grams of nitrogen-containing The triazine polymer was reacted for 3 hours, filtered, dried and pulverized to obtain 1110 g of expandable halogen-free flame retardant with a yield of 99.10%. Water solubility is 0.45g / 100g water, TGA thermal decomposition temperature is 254.25℃

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Abstract

This invention relates to a method to prepare a flame retardant and its product, and especially relates to a method to prepare graft nitrogenous heterocyclic compounds with P-O backbones from phosphorus pentoxide and ammonium dihydrophosphate, a method to prepare nonhalogen intumescent flame retardant for polyolefin and its product. The nonhalogen intumescent flame retardant produced in this invention has following advantages compared to nonhalogen intumescent flame retardants produced by current techniques: a) two-step method is adopted so that production time is shortened, temperature is lowered, operation is simple and energy cost is low; b) phase transmission catalyst is solid-liquid system so that grafting efficiency of oxygen-containing amine is ensured; c) crystallization is accelerated by the introduction of ammonia and tightly and perfectly crystallized nonhalogen intumescent flame retardant backbone intermediate can be obtained.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant and its products; in particular, to a method for preparing a P-O main chain by using phosphorus pentoxide and ammonium dihydrogen phosphate, grafting nitrogen-containing heterocyclic compounds, and preparing a halogen-free flame retardant for polyolefins. Preparation method and product of intumescent flame retardant. Background technique [0002] Intumescent halogen-free flame retardants are mainly used in polyolefins, such as polypropylene, polyethylene, and EVA. The prior art halogen-free intumescent flame retardants have poor compatibility with polyolefins and have a great influence on the notched impact strength of polyolefins. At the same time, it has the disadvantage of poor water resistance. In the water immersion test at 70°C for 168 hours, the extraction rate is high, and it cannot meet the flame retardant requirements of UL94 V0. [0003] There are three main methods for prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/32C08K5/52
Inventor 裘雪阳朱峰吴伟俊
Owner HANGZHOU JLS FLAME RETARDANTS CHEM
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