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Preparation method and application of integrated hyperbranched intumescent flame retardant

An intumescent and flame retardant technology, which is applied in the manufacture of fire-resistant and flame-retardant filaments, fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of fiber mechanical property damage, reaction conditions and processes, and easy dispersion. , to achieve improved flame retardant performance, simple and controllable preparation method, and good application prospects

Active Publication Date: 2019-06-28
SHANGHAI JUTONG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN 107840996 A discloses an intumescent flame retardant obtained by compounding various components, but the three components of the compounded IFR are easily dispersed unevenly in the polymer matrix, so they cannot play a good role in synergistic flame retardants. Combustion
Chinese patent CN 107652324 A designed and synthesized a three-source intumescent flame retardant of methylphosphonic acid-piperazine-neopentyl glycol phosphonate, but the reaction conditions and process are more cumbersome and complicated
At present, the dosage of most organic intumescent flame retardants is generally about 10%, which will inevitably cause damage to the mechanical properties of fibers

Method used

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  • Preparation method and application of integrated hyperbranched intumescent flame retardant
  • Preparation method and application of integrated hyperbranched intumescent flame retardant
  • Preparation method and application of integrated hyperbranched intumescent flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation of flame retardant:

[0043] Dissolve 5mmolβ-cyclodextrin, 50mmol maleic anhydride and 50mmol DOPO in 30mL N,N-dimethylformamide, react at 80°C for 12h, cool, filter, wash with absolute ethanol, and dry under vacuum at 60°C to obtain product 1;

[0044] Dissolve 0.4mol melamine and 0.6mol terephthalaldehyde in 100mL of absolute ethanol, heat up to 80°C for reflux reaction for 8h, then add 0.4molDOPO, continue to react for 12h, cool, filter, wash with absolute ethanol, and vacuum dry at 60°C Product 2 is obtained;

[0045]Dissolve 3g of product 1, 2g of product 2, and 0.5g of 4-dimethylaminopyridine in DMF, react at 50°C for 6h, cool, filter, wash with absolute ethanol, and dry under vacuum at 60°C to obtain the target product.

[0046] The obtained compound is detected by infrared, hydrogen nuclear magnetic spectrum and phosphorous spectrum, such as Figure 1-3 As shown, it can be proved that the compound of the present invention is indeed the structure of...

Embodiment 2

[0050] Preparation of flame retardant:

[0051] Dissolve 5mmolβ-cyclodextrin, 25mmol maleic anhydride and 25mmol DOPO in 30mL N,N-dimethylformamide, react at 60°C for 12h, cool, filter, wash with absolute ethanol, and dry under vacuum at 60°C to obtain product 1;

[0052] Dissolve 0.4mol melamine and 0.6mol terephthalaldehyde in 100mL N,N-dimethylformamide, raise the temperature to 80°C for reflux reaction for 8 hours, then add 0.4mol DOPO, continue the reaction for 12 hours, cool, filter and wash with absolute ethanol , Vacuum drying at 60°C to obtain product 2;

[0053] Dissolve 2g of product 1, 1g of product 2, and 0.2g of 4-dimethylaminopyridine in DMF, react at 50°C for 6h, cool, filter, wash with absolute ethanol, and dry in vacuo at 60°C to obtain the target product.

[0054] Referring to the preparation of flame-retardant polyacrylonitrile fibers in Example 1, flame-retardant polyacrylonitrile fibers were prepared. The specific performance parameters are shown in Tab...

Embodiment 3

[0056] Preparation of flame retardant:

[0057] Dissolve 5mmolβ-cyclodextrin, 25mmol maleic anhydride and 25mmol DOPO in 30mL N,N-dimethylformamide, react at 60°C for 12h, cool, filter, wash with absolute ethanol, and dry under vacuum at 60°C to obtain product 1;

[0058] Dissolve 0.4mol melamine and 0.6mol terephthalaldehyde in 100mL dimethyl sulfoxide, raise the temperature to 80°C for reflux reaction for 8 hours, then add 0.6mol DOPO, continue the reaction for 8 hours, cool, filter, wash with absolute ethanol, and heat at 60°C Vacuum drying obtains product 2;

[0059] Dissolve 2g of product 1, 2g of product 2, and 0.5g of 4-dimethylaminopyridine in DMF, react at 50°C for 6h, cool, filter, wash with absolute ethanol, and dry under vacuum at 60°C to obtain the target product.

[0060] Referring to the preparation of flame-retardant polyacrylonitrile fibers in Example 1, flame-retardant polyacrylonitrile fibers were prepared. The specific performance parameters are shown in ...

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Abstract

The invention discloses a preparation method and application of integrated hyperbranched intumescent flame retardant, and belongs to the technical field of halogen-free flame retardance. The preparation method is simple and controllable, and can be used for preparing the integrated hyperbranched intumescent halogen-free flame retardant based on Schiff base reaction. The flame retardant is halogenfree and environment-friendly, and has excellent thermal stability, excellent expansion performance and high flame retarding efficiency; the flame retarding performance of flame-retardant fibers prepared with small dosage can be greatly improved, the limiting oxygen index is 27 or more reaching the level of nonflammable materials; and the flame retardant material cannot damage the mechanical performance of fiber materials, and has a good application prospect.

Description

technical field [0001] The invention relates to a preparation method and application of a three-source integrated hyperbranched intumescent flame retardant, belonging to the technical field of halogen-free flame retardant. Background technique [0002] Textile fibers are widely used in important fields such as automobiles, outdoors, clothing, construction, aerospace, etc., but most fiber materials are highly flammable, easily ignited by external heat sources, and release a large amount of heat and smoke during combustion And poisonous gas, brought great hidden danger to people's life and property safety. The development of high-performance, low-consumption green and environmentally friendly flame retardants is an effective method to improve the added value and safety of fiber products, making them difficult to catch fire or slow down the burning speed. [0003] Most of the traditional flame retardants are halogen flame retardants or derivatives of halogen and other flame re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00D01F1/07D01F6/54
Inventor 付少海王冬彭虹云李敏张丽平田安丽刘明明
Owner SHANGHAI JUTONG IND