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Phosphorus-containing flame retardant with fluorenyl groups and preparation method thereof

A flame retardant, fluorene-based technology, applied in the field of chemical materials, can solve the problem of no relevant reports, and achieve the effects of wide application range, good heat resistance and high yield

Active Publication Date: 2012-01-04
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many types and synthesis methods of polyphosphonate flame retardants, but there are no relevant reports at home and abroad on the research on the synthesis of 9,9-bis(4-hydroxyphenyl)fluorene by solution polymerization.

Method used

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  • Phosphorus-containing flame retardant with fluorenyl groups and preparation method thereof
  • Phosphorus-containing flame retardant with fluorenyl groups and preparation method thereof
  • Phosphorus-containing flame retardant with fluorenyl groups and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Add calcium-type A molecular sieve (5g) into the bottles containing dimethylformamide (473g) and triethylamine (328g) respectively, and use them one day later.

[0029] 2) Dissolve 0.01mol of bisphenol fluorene in 13ml of dimethylformamide, transfer it into a three-neck flask, seal it at 25°C, stir it evenly with magnetic force, add 0.025mol of triethylamine, and continue stirring.

[0030] 3) Add 0.01 mol of phenylphosphonic acid dichloride dissolved in 13 ml of dimethylformamide dropwise at 25°C, keep the system closed and magnetically stirred, and the dropwise addition is completed in 5 minutes.

[0031] 4) Seal and keep warm at 25°C for 1 hour.

[0032] 5) Use a rotary evaporator to remove most of the solvent in the system, and adjust the pH to 6-7 with 0.1mol / L hydrochloric acid. Washing with water for 3 to 5 times, washing with methanol for 3 to 5 times, and drying to obtain polyphenyl phosphonic acid bisphenol fluorene ester.

[0033] The results of its infr...

Embodiment 2

[0036] 1) Add calcium-type A molecular sieve (5g) into the bottles containing tetrahydrofuran (445g) and triethylamine (328g) respectively, and use them one day later.

[0037] 2) Dissolve 0.01mol of bisphenol fluorene in 13ml of tetrahydrofuran, transfer it into a three-necked flask, seal it at 25°C, stir it evenly with a magnetic force, add 0.025mol of triethylamine, and continue stirring.

[0038] 3) 0.01 mol of phenylphosphonic dichloride dissolved in 13 ml of tetrahydrofuran was added dropwise at 0°C, and the system was kept closed with magnetic stirring, and the dropwise addition was completed in 60 minutes.

[0039] 4) Seal and keep warm at 25°C for 1 hour.

[0040] 5) Use a rotary evaporator to remove most of the solvent in the system, and adjust the pH to 6-7 with 0.1mol / L hydrochloric acid. Washing with water for 3 to 5 times, washing with methanol for 3 to 5 times, and drying to obtain polyphenyl phosphonic acid bisphenol fluorene ester.

[0041] Its structural ch...

Embodiment 3

[0043] The synthesis steps were carried out according to Example 1, except that the triethylamine in Example 1 (steps (1) and (2) in Example 1) was replaced by pyridine to obtain polyphenylphosphonic acid bisphenol fluorene ester.

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Abstract

The invention discloses a phosphorus-containing flame retardant with fluorenyl groups and a preparation method thereof, which belong to the field of chemical materials. The flame retardant is a polymer of a structure (I). The flame retardant has relatively higher molecular weight and good compatibility with a polyester substrate and cannot easily shift. Due to the induction of 9,9-bi(4- hydroxyphenyl) fluorene, the defect that the thermal stability of the tradition polymer flame retardant is reduced after a polyester system is added is overcome, and the flame retardant has good flame retarding effect and good flame retarding durability and is favorable to environment-friendliness. The phosphorus-containing flame retardant with fluorenyl groups, provided in the invention, has the advantages of simple preparation method and easily controlled conditions. The phosphorus-containing flame retardant with fluorenyl groups, prepared by the method has broad application range, is suitable for the flame retarding of polyester, polyester alloy, engineering plastics and epoxy resin and can have excellent flame retarding effect. R in the structure (I) is or .

Description

technical field [0001] The invention belongs to the field of chemical materials and relates to the preparation of different phosphorus-containing flame retardants with fluorenyl groups by using a solution polymerization method. Background technique [0002] At present, natural and man-made fires have caused great losses to human property and life safety. According to incomplete statistics, from January to June 2010, there were 73,317 fires in the country (excluding forests, grasslands, army, underground parts of mines), and deaths 656 people were injured, 271 people were injured, and the direct property loss was 792.907 million yuan. Flame retardant has therefore become a hot spot in global research. Flame retardants are functional additives that endow flammable polymers with flame retardancy, and their application methods can generally be divided into additive flame retardants (mainly including inorganic flame retardants, halogenated flame retardants, phosphorus-based flam...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L67/00C08L63/00C08L85/02
Inventor 宋艳朱娜任强李锦春
Owner 溧阳常大技术转移中心有限公司
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