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Synthesis methods of Schiff base phosphazene double-base structure flame retardant and modified polyurethane flame retardant

A polyurethane flame retardant, Schiff base phosphazene technology, applied in the field of flame retardants, can solve the problems of secondary combustion, high temperature burns, etc., achieve the effects of small addition, stable flame retardant performance, and improved mechanical properties

Active Publication Date: 2019-12-13
青岛玉城科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the molten droplets produced during combustion may cause the risk of secondary combustion, as well as problems such as high temperature burns

Method used

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  • Synthesis methods of Schiff base phosphazene double-base structure flame retardant and modified polyurethane flame retardant
  • Synthesis methods of Schiff base phosphazene double-base structure flame retardant and modified polyurethane flame retardant
  • Synthesis methods of Schiff base phosphazene double-base structure flame retardant and modified polyurethane flame retardant

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Experimental program
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preparation example Construction

[0033] A method for synthesizing a Schiff base phosphazene double-base structure flame retardant, comprising the steps of:

[0034] S1. Add 0.16mol p-hydroxybenzaldehyde, 0.25mol potassium carbonate and 200ml tetrahydrofuran into a four-necked round-bottomed flask equipped with a mechanical stirrer, a condenser, a constant pressure funnel and a nitrogen protection device, and pass into the round-bottomed flask High-purity nitrogen, until the flask reaches anaerobic and water-free conditions, start stirring until the reaction system is clear and transparent; dissolve 0.024mol hexachlorocyclotriphosphazene in 100ml tetrahydrofuran, drop it into the reaction vessel through a constant pressure funnel, and then The reaction was stirred and reacted at 65°C for 24 hours, and the crude product obtained from the reaction was subjected to rotary evaporation, water washing, recrystallization and drying to obtain white crystals, which were intermediate products, with a yield of 93.1%;

[...

Embodiment 2

[0056] A method for synthesizing a Schiff base-containing phosphazene double-radical structure flame retardant comprises the following steps:

[0057] S1. Add 0.16mol 2-hydroxypyridine-5-aldehyde, 0.25mol potassium carbonate and 200ml tetrahydrofuran into a four-necked round-bottomed flask equipped with a mechanical stirrer, a condenser tube, a constant pressure funnel and a nitrogen protection device. Introduce high-purity nitrogen into the flask until the anaerobic and water-free conditions are reached in the flask, and start stirring until the reaction system is clear and transparent; dissolve 0.024mol hexachlorocyclotriphosphazene in 100ml tetrahydrofuran, and drop it into the reaction vessel through a constant pressure funnel , then stirred and reacted at 65°C for 24h, and the crude product obtained in the reaction was subjected to rotary evaporation, water washing, recrystallization and drying to obtain a phosphazene-containing intermediate;

[0058] S2. Add 0.02mol of t...

Embodiment 3

[0062] A method for synthesizing a Schiff base-containing phosphazene double-radical structure flame retardant comprises the following steps:

[0063] S1. Add 0.16mol 5-(4-hydroxypiperidine)-2-thiophenecarbaldehyde, 0.25mol potassium carbonate and 200ml tetrahydrofuran into a four-hole round bottom equipped with a mechanical stirrer, condenser tube, constant pressure funnel and nitrogen protection device In the flask, pass high-purity nitrogen gas into the round-bottomed flask until the flask reaches anaerobic and water-free conditions, start stirring until the reaction system is clear and transparent; dissolve 0.024mol hexachlorocyclotriphosphazene in 100ml tetrahydrofuran, and pass Add the funnel dropwise into the reaction vessel, then stir and react at 65°C for 24 hours, and the crude product obtained from the reaction is rotary evaporated, washed with water, recrystallized and dried to obtain the phosphazene-containing intermediate;

[0064] S2. Add 0.02mol of the phosphaz...

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Abstract

The invention discloses a synthesis method of a Schiff base phosphazene double-base structure flame retardant. The synthesis method comprises the following steps: S1, reacting phosphonitrilic chloridetrimer with a compound containing hydroxyl and active carbonyl, a strong alkali and weak acid salt and a solvent to prepare a phosphazene-containing intermediate; S2, reacting the phosphazene-containing intermediate prepared in the step S1 with an alcohol amine compound and a solvent to prepare the Schiff base phosphazene double-base structure flame retardant. A synthesis method of a modified polyurethane flame retardant comprises the step of applying the prepared Schiff base phosphazene double-base structure flame retardant to waterborne polyurethane to prepare a waterborne polyurethane flame retardant containing the hydroxyl-terminated Schiff base phosphazene double-base structure. The Schiff base phosphazene double-base structure flame retardant can effectively improve the flame retardancy and molten drop resistance of a base material; a Schiff base structure contained in the structure of the modified polyurethane flame retardant has certain stability, crosslinking of melt and formation of residual carbon can be promoted, the molten drop resistance of a prepared flame-retardant material is improved, two elements including nitrogen and phosphorus in a phosphazene ring can achieve synergistic flame retardance, and a good flame-retardant effect is achieved.

Description

technical field [0001] The invention relates to the field of flame retardants, more specifically, to a Schiff base phosphazene double-base structure flame retardant and a method for synthesizing a modified polyurethane flame retardant. Background technique [0002] Schiff base compounds mainly refer to a class of organic compounds containing imine or amethyrimine characteristic groups (-RC=N-), usually formed by condensation of amines and active carbonyl groups. Schiff base compounds and their metal complexes have important applications in the fields of biomedicine, catalysis, self-healing materials, and optical sensors. Schiff base compounds with a relatively stable structure can regulate the thermal degradation of materials by forming an ablation surface, and can serve as effective charring agents. In addition, during the combustion process, the flame retardant containing Schiff base structure can quickly cross-link at high temperature, increase the melt viscosity and str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08G18/66C08G18/48C08G18/32C08G18/34
CPCC07F9/65815C08G18/6692C08G18/4833C08G18/348C08G18/3889
Inventor 杜宗良成煦王辉王海波杜晓声
Owner 青岛玉城科技有限公司
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