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Method for preparing silicon-containing phosphonitrile modified ammonium polyphosphate flame retardant and application in flame-retardant polyolefin

A technology of ammonium polyphosphate and silicon-containing phosphazene, which is applied in the field of flame-retardant materials, can solve problems such as poor effect, poor compatibility, and penetration, and achieve the effects of improved heat release rate, mild preparation conditions, and good mechanical properties

Inactive Publication Date: 2012-08-01
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

APP is a flame retardant developed by Monsanto Company of the United States in 1965. It has the advantages of large phosphorus content, high nitrogen content, good thermal stability, low moisture absorption, low toxicity, and smoke suppression. It is often used in intumescent flame retardant systems; However, the effect of APP alone on the flame retardant modification of polymers is not good.
[0003] People have found in long-term use that APP also has many shortcomings, such as: poor compatibility with certain materials, penetration, migration, moisture absorption, etc.; reduce the strength and heat resistance of flame-retardant products, etc.
Therefore, people have adopted various methods to modify APP, including the use of coupling agents such as organic silicon, etc., but the existing modification methods still have problems such as osmosis migration and affecting the mechanical properties of products.

Method used

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  • Method for preparing silicon-containing phosphonitrile modified ammonium polyphosphate flame retardant and application in flame-retardant polyolefin
  • Method for preparing silicon-containing phosphonitrile modified ammonium polyphosphate flame retardant and application in flame-retardant polyolefin

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Bake the ammonium polyphosphate APP-JLS in a vacuum oven at 80°C for 6 hours; dissolve APESP in absolute ethanol and mix thoroughly in a three-necked flask, the mass ratio of APESP to absolute ethanol is 1:5; then bake Add dry ammonium polyphosphate to the absolute ethanol solution of APESP, the mass ratio of APESP to APP is 1:7, stir and heat up to 50°C, after 40 minutes, remove the absolute ethanol, and then in a vacuum oven at 80°C Baked for 8 hours, and finally crushed into powder to obtain APESP modified ammonium polyphosphate flame retardant.

[0025] The modified ammonium polyphosphate flame retardant prepared by the above steps and polypropylene S1003 were compounded according to the ratio of 30:70 in mass ratio, and 0.1% of 1010 antioxidant and 0.2% of 168 antioxidant were added in mass ratio, squeezed The outlet temperature conditions were 170°C, 175°C, 180°C, 185°C, 180°C, 175°C, and the injection molding temperature conditions were 195°C, 195°C, 190°C, 185°C...

Embodiment 2

[0029] Bake the ammonium polyphosphate APP-JLS in an electric blast oven at 100°C for 4 hours; dissolve APESP in anhydrous methanol and mix thoroughly in a three-necked flask, the mass ratio of APESP to anhydrous methanol is 1:10; then Add the dried ammonium polyphosphate to the anhydrous methanol solution of APESP, the mass ratio of APESP to APP is 1:4, stir and heat up to 50°C, after 30 minutes, remove the anhydrous methanol, and then place in a vacuum oven for 80 Bake at ℃ for 12 hours, and finally pulverize into powder to obtain APESP modified ammonium polyphosphate flame retardant.

[0030] The modified ammonium polyphosphate flame retardant prepared by the above steps and polypropylene T30S were compounded according to the ratio of 30:70 in mass ratio, and 0.1% of 1010 antioxidant and 0.2% of 168 antioxidant were added in mass ratio, squeezed The outlet temperature conditions were 170°C, 175°C, 180°C, 185°C, 180°C, 175°C, and the injection molding temperature conditions ...

Embodiment 3

[0034] Dry the ammonium polyphosphate APP2100 in a vacuum oven at 80°C for 6 hours; dissolve APESP in absolute ethanol and mix thoroughly in a three-necked flask, the mass ratio of APESP to absolute ethanol is 1:2; then dry the Add ammonium polyphosphate to the absolute ethanol solution of APESP, the mass ratio of APESP to APP is 1:3, stir and heat up to 40°C, after 40 minutes, remove the absolute ethanol, and then dry in a vacuum oven at 80°C After 6 hours, it was finally crushed into powder to obtain APESP modified ammonium polyphosphate flame retardant.

[0035] Compound the modified ammonium polyphosphate flame retardant prepared by the above steps, polypropylene S1003 according to the ratio of 28:72 in mass ratio, add 0.1% of 1010 antioxidant and 0.2% of 168 antioxidant in mass ratio, squeeze The outlet temperature conditions were 170°C, 175°C, 180°C, 185°C, 180°C, 175°C, and the injection molding temperature conditions were 195°C, 195°C, 190°C, 185°C, 180°C to obtain fla...

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Abstract

The invention relates to a method for preparing a silicon-containing phosphonitrile modified ammonium polyphosphate flame retardant and application in flame-retardant polyolefin, and belongs to the technical field of flame-retardant materials. The method comprises the following steps of: adding ammonium polyphosphate (APP) into an aminopropyl ethoxy silane polymer (APESP) solution system, removing a solvent, drying, and thus obtaining the modified ammonium polyphosphate flame retardant. The novel collaborative inflaming-retarding modified APP flame retardant integrating phosphorus / nitrogen / silicon elements is prepared by modifying the surface of the APP through the silicon-containing nitrile APESP; the method is mild in preparation conditions, easy to control, good in repeatability and high in yield, and is suitable for expanded production; and when the flame retardant is applied to a polyolefin flame-retardant system, oxygen index, vertical burning level and heat release rate of the obtained polyolefin are remarkably improved, and good mechanical property is kept.

Description

technical field [0001] The invention relates to a preparation method of a novel flame retardant obtained by modifying the surface of ammonium polyphosphate with silicon-containing phosphazene and its application in flame-retardant polyolefin. The flame retardant contains phosphorus, nitrogen and silicon elements at the same time , belonging to a self-synergistic flame retardant system; at the same time, the flame retardant is added to a flame retardant polyolefin system, which can improve the compatibility and flame retardant performance of the system, and belongs to the technical field of flame retardant materials. Background technique [0002] The halogen-free intumescent flame retardant based on ammonium polyphosphate (APP) has become a hot spot in the current research of flame retardant technology due to its non-toxicity, low smoke and no droplet when burning. APP is a flame retardant developed by Monsanto Company of the United States in 1965. It has the advantages of la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/00C09C3/12C08K9/10C08K9/06C08K3/32C08K13/06C08L23/00C08L23/12
Inventor 李定华杨荣杰何兰岚秦兆鲁
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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