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DOPO derivative and preparation method thereof

A technology of derivatives and oxides, which is applied in the field of organic synthesis, can solve the problems of polymer material application popularization restrictions, high-temperature deformation of polymer materials, and flammability, and achieve the effects of avoiding harsh preparation conditions, mild reaction conditions, and simple operation

Active Publication Date: 2015-05-13
DAQING BRANCH OF HEILONGJIANG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Polymer materials have been widely used in daily life, and partially or completely replaced metal or inorganic non-metallic materials in some fields. restricted

Method used

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  • DOPO derivative and preparation method thereof
  • DOPO derivative and preparation method thereof
  • DOPO derivative and preparation method thereof

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Experimental program
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specific Embodiment approach 1

[0015] Specific embodiment 1: The structural formula of DOPO derivatives in this embodiment is

[0016] Its preparation method is carried out according to the following steps:

[0017] Step 1. Mix 10mmol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1mmol anhydrous potassium carbonate, and 10mmol hexachlorocyclotrimeric phosphazene (HCCP), Add 50mL of N,N-dimethylformamide, then stir at room temperature (25°C) until the substrate DOPO disappears (monitored by TLC) to stop the reaction;

[0018] Step 2, then poured into saturated brine and stirred, extracted three times with 50 mL of dichloromethane, combined the extracts and dried with anhydrous magnesium sulfate for 12 hours, concentrated to dryness with a rotary evaporator to obtain a light yellow solid, and then recrystallized with ethyl acetate , to obtain DOPO derivatives (DOPO-HCCP).

[0019] The reaction equation of the present embodiment is:

[0020]

[0021] The DOPO derivative obtained in this em...

specific Embodiment approach 2

[0023] Specific embodiment two: the difference between this embodiment and specific embodiment one is: adopt triethylamine to replace anhydrous potassium carbonate. Other steps and parameters are the same as in the first embodiment.

[0024] The DOPO derivative obtained in this embodiment is a white solid with a spiro ring structure, the yield is 70%, and the maximum thermal decomposition temperature is 370°C.

specific Embodiment approach 3

[0025] Specific embodiment three: the difference between this embodiment and specific embodiment one is: Potassium tert-butoxide is used to replace anhydrous potassium carbonate. Other steps and parameters are the same as in the first embodiment.

[0026] The DOPO derivative obtained in this embodiment is a white solid with a spiro ring structure, the yield is 65%, and the maximum thermal decomposition temperature is 370°C.

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Abstract

The invention discloses a DOPO derivative and a preparation method thereof, and belongs to the technical field of organic synthesis. According to the preparation method disclosed by the invention, a spiral structure is formed by activating a hydrogen bond and phosphonitrile compounds on a DOPO aromatic ring, and is novel and abundant in functional groups. The structural formula of the DOPO derivative disclosed by the invention is specified in the description. A preparation method of the DOPO derivative disclosed by the invention comprises the following steps: 1, mixing 10mmol of DOPO, 1mmol of a catalyst and 10mmol of HCCP, adding 50mL of an organic solvent, and stirring at a room temperature to completely react; 2. pouring a mixture obtained from the step 1 in saturated table salt and stirring, extracting with dichloromethane for three times, mixing extracts and drying with anhydrous magnesium sulphate, concentrating to be dry, and then recrystallizing to obtain the DOPO derivative. The DOPO derivative disclosed by the invention is shorter in reaction route, moderate in experiment conditions and easy to purify, the highest decomposition temperature can achieve about 370 DEG C, and the DOPO derivative can be used as a flame retardant.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis; in particular, it relates to a 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (abbreviated as DOPO) derivative and a preparation method thereof. Background technique [0002] Polymer materials have been widely used in daily life, and partially or completely replaced metal or inorganic non-metallic materials in some fields. limit. Therefore, the flame retardancy of polymer materials has been paid more and more attention by people. Due to the limitation of the chemical composition of polymer materials, the most practical and effective way to make polymer materials flame retardant is to add flame retardants. Flame retardants are additives used to improve the flame resistance of materials, that is, to prevent materials from being ignited and to inhibit flame propagation. [0003] Grafting small molecule branched or blended flame retardants with flame retardant properties in polymer ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08K5/5399
Inventor 高宝昌崔宝玉田媛
Owner DAQING BRANCH OF HEILONGJIANG ACAD OF SCI
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