DOPO-modified cyclophosphazene fire retardant and preparation and application thereof

A DOPO-CH2OH, flame retardant technology, applied in the direction of flame retardant fibers, textiles and papermaking, chemical instruments and methods, etc., can solve the problem of affecting the physical and mechanical properties of the matrix, the large amount of flame retardants added, and the large amount of flame retardants used and other issues, to achieve the effect of environmental protection, good flame retardancy, and halogen-free

Inactive Publication Date: 2017-02-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the added amount of blended flame retardant is relatively large, which will affect the physical and mechanical properties of the substrate, etc.; as a flame retardant for finishing, there are also problems of large dosage and low utilization rate.

Method used

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  • DOPO-modified cyclophosphazene fire retardant and preparation and application thereof
  • DOPO-modified cyclophosphazene fire retardant and preparation and application thereof
  • DOPO-modified cyclophosphazene fire retardant and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] DOPO-CH 2 Preparation of OH

[0029] Add DOPO 216g (1.0mol) and ethanol 600mL into a four-neck flask (1L) equipped with a mechanical stirrer, reflux condenser, addition funnel and thermometer, heat the reaction mixture to 70°C, and add 36 90g (1.1mol) of ~38% formaldehyde aqueous solution was added in about 30 minutes. The reactant was heated to 80° C., kept for 6 hours, cooled, filtered with suction, washed, and dried to obtain a white solid product.

[0030]

[0031] (2) Preparation of DOPO modified cyclophosphazene flame retardant (DOPO-TPN)

[0032] Add 100ml of chloroform into a four-necked flask (250mL) equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel, and then add DOPO-CH 2 14.76g (0.06mol) of OH and 3.48g (0.01mol) of hexachlorocyclotriphosphazene, and the reaction mixture was heated to reflux at 65°C. 6.06 g (0.05 mol) of triethylamine (Et3N) was added dropwise, and the addition was completed in about 1 hour, an...

Embodiment 2

[0035] (1)DOPO-CH 2 Preparation of OH

[0036] Add DOPO 216g (1.0mol) and methanol 500mL into a four-neck flask (1L) equipped with a mechanical stirrer, reflux condenser, addition funnel and thermometer, heat the reaction mixture to 70°C, and add formaldehyde dropwise under stirring 90g (1.1mol) of the aqueous solution was added in about 30 minutes. The reactant was heated to 80° C., kept for 6 hours, cooled, filtered with suction, washed, and dried to obtain a white solid product.

[0037] (2) Preparation of DOPO-TPN

[0038] Add 200ml of tetrahydrofuran into a four-neck flask equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel, and then add DOPO-CH 2 14.76g (0.06mol) of OH and 3.48g (0.01mol) of hexachlorocyclotriphosphazene, and the reaction mixture was heated to reflux at 65°C. Join K 2 CO 3 5.0g (0.036mol) was kept under reflux to continue stirring for 48h. After the reaction was finished, unreacted substances were removed b...

Embodiment 3

[0040] 5 g of DOPO-TPN prepared in Example 1 and 95 g of polyester pellets were mixed and extruded in a twin-screw extruder, and then tableted to obtain blended flame retardant polyester chips with a flame retardant content of about 5%.

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Abstract

The invention relates to a DOPO-modified cyclophosphazene fire retardant and preparation and application thereof. The structural formula of the fire retardant is as shown in the specification. According to the preparation, a DOPO hydroxymethyl derivative DOPO-CH2OH, phosphonitrilic chloride trimer and an acid binding agent react in a solvent so as to obtain the fire retardant. The DOPO-modified cyclophosphazene fire retardant is used as a blending additive flame retardant to be applied to thermosetting or thermoplastic polymers, or is used as a fire retardant for after-treatment to be applied in flame-proof treatment of textile. The prepared fire retardant is a phosphorus-nitrogen type fire retardant, and has good flame resistance, contains no halogen and is beneficial to environmental protection.

Description

technical field [0001] The invention belongs to the field of flame retardant materials and their preparation and application, in particular to a DOPO modified cyclophosphazene flame retardant and its preparation and application. Background technique [0002] DOPO and its derivatives are a class of halogen-free phosphorus-containing flame retardants with excellent flame retardant properties. DOPO derivatives are often used as a blending additive flame retardant for epoxy resins or as a curing agent for epoxy resins to prepare flame-retardant epoxy resins; they can also be copolymerized or blended to prepare flame-retardant polyesters. Generally, the added amount of blended flame retardant is relatively large, which will affect the physical and mechanical properties of the substrate; as a flame retardant for finishing, there is also a problem of large dosage and low utilization rate. Therefore, it is necessary to improve the flame retardant efficiency of the flame retardant a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08K5/5399C08L67/00D06M13/44D06M15/01D06M15/09D06M101/32
CPCC07F9/659C08K5/5399C08L2201/02D06M13/44D06M15/01D06M15/09D06M2101/32D06M2200/30C08L67/00
Inventor 方寅春周翔吴亚容邢志奇
Owner DONGHUA UNIV
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