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Fluorine titanium hybrid flame retardant, and preparation method and application thereof

A flame retardant and curing agent technology, applied in the direction of titanium organic compounds, etc., can solve the problems of harsh reaction conditions and complex formulations, and achieve the effects of simple and mild reaction conditions, simple product purification operations, and high yields

Active Publication Date: 2017-05-31
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing technical scheme of flame-retardant modification of epoxy resin by combining fluorine and titanium elements has defects such as complex formula and harsh reaction conditions.

Method used

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  • Fluorine titanium hybrid flame retardant, and preparation method and application thereof
  • Fluorine titanium hybrid flame retardant, and preparation method and application thereof
  • Fluorine titanium hybrid flame retardant, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 0.336g (0.001mol) of hexafluorobisphenol A and 20mL of ethanol into a 50mL three-necked round-bottomed flask, and then dissolve 0.085g (0.00025mol) of butyl titanate in 3mL of ethanol, and dissolve evenly. The mixture was added dropwise into the above-mentioned three-necked flask, and the reaction was stirred at room temperature for 24 h. After the reaction was completed, the solvent was removed by rotary evaporation to obtain a crude product, which was washed with ethanol three times and freeze-dried to obtain a fluorine-titanium hybrid flame retardant with a yield of about 96%.

[0028] The infrared spectrogram of the fluorine-titanium hybrid flame retardant is shown in figure 1 shown. 994cm -1 The spectrum peak is -Ti-O-C 6 h 4 - The characteristic absorption peak of the group.

Embodiment 2

[0030] Preparation of pure epoxy resin

[0031] Pure epoxy resin was used as the control group. Weighed 20g of epoxy resin E-51, raised the temperature to 90°C, added 5g of curing agent 4,4'-diaminodiphenylmethane, stirred evenly, poured into the mold, and kept at 120°C 5h, then at 140°C for 2h, and finally at 180°C for 2h.

[0032] The oxygen index of the prepared flame-retardant epoxy resin was tested according to the GB / T 2406.2-2009 method to be 25.4%.

[0033] The prepared flame retardant epoxy resin was tested according to the GB / T 2408-2008 method and the results of its vertical burning rating are shown in Table 1.

Embodiment 3

[0035] Weigh 20g of epoxy resin E-51, raise the temperature to 100°C, add 0.25g of the fluorine-titanium hybrid flame retardant prepared in Example 1, the added mass of the flame retardant is calculated according to the mass percentage, the fluorine-titanium hybrid flame retardant is 1% of epoxy resin, while stirring, use vacuum to remove small molecular substances, add 5g of 4,4'-diaminodiphenylmethane after completely dissolving, pour into the mold after stirring, keep at 120°C for 5h, and then Insulate at 140°C for 2 hours, and finally at 180°C for 2 hours, flame retardant epoxy resin.

[0036] The oxygen index of the prepared flame-retardant epoxy resin was tested according to the GB / T 2406.2-2009 method to be 28.9%.

[0037] The prepared flame retardant epoxy resin was tested according to the GB / T 2408-2008 method and the results of its vertical burning rating are shown in Table 1.

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Abstract

The invention discloses a fluorine titanium hybrid flame retardant, and a preparation method and application thereof. The fluorine titanium hybrid flame retardant is characterized in that the fluorine titanium hybrid flame retardant has the molecular structural formula shown in the description, wherein R is CH3CH2CH2CH2 or shown as the description. When the fluorine titanium hybrid flame retardant is used for preparing flame-retardant epoxy resin, the reaction conditions are simple and mild; the yield is high; the product purification operation is simple; the industrialization is easy; the prepared epoxy resin has high transparency; on the premise of ensuring the excellent heat resistance and mechanical property, the flame retardant effect is good; the application range is wide; the environment protection requirements are met.

Description

technical field [0001] The invention belongs to the technical field of organic flame retardant, and in particular relates to a fluorine-titanium hybrid flame retardant and its preparation method and application. Background technique [0002] Epoxy resins include both epoxy-based oligomers and low-molecular-weight compounds containing epoxy groups. Epoxy resin has good mechanical properties, strong adhesion, small curing shrinkage, excellent electrical insulation performance, good processability, excellent stability and chemical resistance. As the resin matrix of adhesives, coatings and composite materials, epoxy resin is widely used in the fields of water conservancy, transportation, machinery, electronics, home appliances, automobiles and aerospace. With the increasing requirements for the reliability and safety of epoxy resin in these fields, especially the heat resistance and flame retardancy have attracted more and more attention. The method widely used to improve the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K5/136C07F7/28
CPCC07F7/28C08L2201/02C08L2201/08C08L2201/10C08K5/136C08L63/00
Inventor 戴李宗吴海洋袁丛辉刘诚李云同吴俣哲罗伟昂陈国荣何凯斌
Owner XIAMEN UNIV
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