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Oxa-phosphaphenanthrene fire retardant as well as preparation method and application of oxa-phosphaphenanthrene fire retardant

A technology of oxaphosphaphenanthrene and flame retardant, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., and can solve problems such as personal safety threats, application restrictions, and excessive smoke. Achieve the effects of good thermal stability, simple operation and high flame retardant rate

Active Publication Date: 2014-12-24
湖北同广和新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Most of the halogen-containing flame retardant materials have secondary hazards such as smoke, toxic or corrosive gas emission when they burn, which pose a serious threat to personal safety and their application is limited.

Method used

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  • Oxa-phosphaphenanthrene fire retardant as well as preparation method and application of oxa-phosphaphenanthrene fire retardant
  • Oxa-phosphaphenanthrene fire retardant as well as preparation method and application of oxa-phosphaphenanthrene fire retardant
  • Oxa-phosphaphenanthrene fire retardant as well as preparation method and application of oxa-phosphaphenanthrene fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of oxaphosphine phenanthrene flame retardant, the steps are:

[0022] Add p-tert-butylcalix[4]arene (2.96g, 4mmol), p-toluenesulfonate ethoxy-p-benzaldehyde (2.56g, 8mmol) and potassium carbonate (2.20g , 16mmol), stirred and refluxed for 45h, TLC detected that the basic reaction of the raw materials was complete, the solvent was evaporated under reduced pressure, the residue was extracted with hydrochloric acid and chloroform respectively, and the organic layer was washed with sodium bicarbonate solution. The organic layer was separated, dried over anhydrous magnesium sulfate, filtered, and concentrated to form a large amount of precipitates. An appropriate amount of chloroform-methanol mixed solvent was recrystallized to obtain Intermediate I (white solid), with a yield of 85.6%.

[0023] Intermediate I9.44g (10mmol) and DOPO4.32g (20mmol) were placed in a flask, and then 100mL of chloroform and 100mL of anhydrous methanol were added, and the reac...

Embodiment 2

[0030] Increase the p-toluenesulfonate group ethoxy-p-benzaldehyde to 2.62g (8.2mmol), and the others are the same as Example 1, and the yield of intermediate I is 86.8%.

Embodiment 3

[0032] Increase the p-toluenesulfonate group ethoxy p-benzaldehyde to 2.94g (9.2mmol), and the other is the same as Example 1, and the yield of intermediate I is 88.2%.

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Abstract

The invention discloses an oxa-phosphaphenanthrene fire retardant as well as a preparation method and application of the oxa-phosphaphenanthrene fire retardant. The fire retardant has a calyx[4]arene structure; p-tert-butyl calyx[4]arene and p-tosylate ethoxy p-benzaldehyde are prepared into an intermediate I in the presence of K2CO3 and acetonitrile, and the intermediate I reacts with DOPO to obtain a target compound; the compound is white in appearance, has the melting point of 198-200 DEG C and the purity of 98.5% and is good in thermal stability and high in flame retarding rate; the used raw materials are easily available, and a process is advanced and easy for industrialized production. The flame retardant not only can serve as a reactive flame retardant to be used in thermosetting resin such as epoxy resin and polyurethane but also can serve as an additive flame retardant to be used for engineering plastics with relatively high requirement on the heat resistance of the flame retardant.

Description

technical field [0001] The invention belongs to the technical field of DOPO flame retardant compounds, and in particular relates to a oxaphosphine phenanthrene flame retardant containing a calix [4] aromatic ring structure. The application of the flame retardant as an epoxy resin and polyurethane flame retardant additive can also be used Used as an additive flame retardant in engineering plastics. Background technique [0002] Most of the halogen-containing flame retardant materials have secondary hazards such as smoke, toxic or corrosive gas emission during combustion, which pose a serious threat to personal safety, and their application is limited. Flame retardants represented by DOPO have become a hot spot in the research and development and application of environmentally friendly halogen-free flame retardants. The advantages of long-lasting combustion performance. Contents of the invention [0003] The object of the present invention is to overcome the weak points in...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C07F9/6574C08L63/00C08L75/04
CPCC07F9/657172C08K5/5313C08L2201/02C08L63/00C08L75/04
Inventor 李德江刘义稳龚大春陈卫丰刘杨
Owner 湖北同广和新材料有限公司
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