Preparation method and application of hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant

A hindered phenolic quaternary phosphonium salt and intumescent flame retardant technology, applied in the field of material science, can solve the problems of high flame retardant cost, large amount of IFR addition, poor compatibility, etc., and achieve good processing stability, excellent flame retardant effect, long lasting effect

Active Publication Date: 2016-09-14
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame-retardant PP of this system usually has two defects: first, the compatibility between IFR and PP matrix materials is poor, and second, the amount of IFR added is large, and the flame-retardant cost is high

Method used

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  • Preparation method and application of hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant
  • Preparation method and application of hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant
  • Preparation method and application of hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Synthesis of benzyl chloride hindered phenol: under the protection of N2, add 10 parts of 2,6 di-tert-butylphenol (Zibo Shibang Chemical Co., Ltd. ), 20 parts of paraformaldehyde, 5 parts of n-heptane, 0.01 part of initiator, the temperature was raised to 70°C, and the 2,6 phenol was completely dissolved under magnetic stirring. Add 3 parts of concentrated hydrochloric acid dropwise to the above solution, continue the constant temperature reaction at 70°C for 12 hours, then cool the reaction solution to room temperature, separate the liquids, extract the water phase with 20 parts of ethyl acetate and mix it with the organic layer, and wash the organic layer with deionized water until neutral. properties, washed with saturated brine, dried over anhydrous Na2SO4, recovered solvent by distillation under reduced pressure, and dried under vacuum at 30°C for 12h to obtain hindered phenol containing benzyl chloride.

[0027] FT-IR of the synthesized benzyl hindered phenol ...

Embodiment 2

[0036] The difference between this implementation and Example 1 is that the reaction temperature in step (1) is changed to 80°C, the reaction time is 18h, 17.5 parts of n-heptane, 0.3 parts of initiator, 50 parts of paraformaldehyde, 0.5 parts of hydrochloric acid, 50 parts of ethyl acetate. In step (2), the temperature is 50°C, the reaction time is 3 hours, 12 parts of organic phosphine, 10 parts of n-heptane as solvent, and 50 parts of petroleum ether. In step (3), the temperature of the water bath is 70° C., the reaction time is 24 hours, the volume of deionized water is 500 mL, and the volume of hindered phenolic quaternary phosphonium salt is 4.5 parts. In step (4), the amount of hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant is 22 parts of flame retardant (including 3 parts of hindered phenolic quaternary phosphonium salt modified montmorillonite, polymer 14 parts of amine phosphate, 2 parts of p...

Embodiment 3

[0039] The difference between this implementation and Example 1 is that the reaction temperature in step (1) is changed to 90°C, the reaction time is 24h, 25 parts of n-heptane, 0.1 part of initiator, 100 parts of paraformaldehyde, 1.5 parts of hydrochloric acid, ethyl acetate 30 parts of ester. In step (2), the temperature is 60° C., the reaction time is 4 hours, 10 parts of di-n-heptane as solvent, 30 parts of petroleum ether, and 11 parts of organic phosphine. In step (3), the temperature of the water bath is 80° C., the reaction time is 12 hours, 450 mL of deionized water, and 5.5 parts of hindered phenolic quaternary phosphonium salts. In step (4), the amount of hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant is 26 parts of flame retardant (including 3 parts of hindered phenolic quaternary phosphonium salt modified montmorillonite, 18 parts of amine polyphosphate, 2 parts of pentaerythritol, 3 part...

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Abstract

The invention discloses a preparation method of PP containing a hindered phenol quaternary phosphonium salt-modified montmorillonite-synergistic halogen-free intumescent flame retardant. The preparation method is characterized in that the hindered phenol quaternary phosphonium salt-modified montmorillonite-synergistic halogen-free intumescent flame retardant is added in PP, 22-28 parts of the hindered phenol quaternary phosphonium salt-modified montmorillonite-synergistic halogen-free intumescent flame retardant is added in per 100 parts of PP, and the flame retardant and PP are uniformly mixed through a double-screw extruder to prepare the flame-retardant PP. (1) The molecule of the hindered phenol quaternary phosphonium salt-modified montmorillonite-synergistic halogen-free intumescent flame retardant prepared by the preparation method disclosed by the invention has a hindered phenol antioxidant group and a quaternary phosphonium salt group, also has an efficient oxidation resistance, can exert a synergistic flame-retardant action with an intumescent flame retardant, and has an excellent flame-retardant effect and a low dosage; (2) the hindered phenol quaternary phosphonium salt-modified montmorillonite-synergistic halogen-free intumescent flame retardant disclosed by the invention has the quaternary phosphonium salt and hindered phenol groups in good compatibility with the PP, thus improving the interface bonding performance of montmorillonite and the PP, and the hindered phenol quaternary phosphonium salt-modified montmorillonite-synergistic halogen-free intumescent flame retardant is not liable to volatilize and good in processing stability.

Description

technical field [0001] The invention belongs to the field of material science, in particular to a hindered phenolic quaternary phosphonium salt modified montmorillonite synergistic halogen-free expansion flame retardant. The invention also relates to the preparation method and application of the hindered phenolic quaternary phosphonium salt modified montmorillonite. Background technique [0002] Polypropylene (PP) is a general-purpose resin, light in weight, non-toxic, has excellent electrical insulation performance and chemical corrosion resistance, convenient molding and processing, and low price. It is widely used in electrical appliances, chemicals, machinery, textiles, Construction, furniture, food packaging and other industries. However, PP is a flammable material, its oxygen index (LOI) is only 17-18.5, and a large number of molten droplets are generated during combustion, which can easily spread flames, which limits the application of PP in many fields. The main co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L23/12C08K13/06C08K9/04C08K3/34C08K3/32C08K5/053C08K5/3492
CPCC08K3/32C08K3/346C08K5/053C08K5/34922C08K9/04C08K13/06C08K2003/323C08L2201/02C08L23/12
Inventor 陈卓尹晓刚龚维吴伟王潇梦秦叔浩于杰
Owner GUIZHOU NORMAL UNIVERSITY
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