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Method for preparing bis(4-carboxyphenyl) phenyl phosphine oxide (BCPPO)

A technology of phenylphosphine oxide and carboxyphenyl, which is applied in the field of flame retardant materials, can solve the problems of complex synthesis process and high cost, and achieve the effects of high product yield, reduced production cost and high purity

Inactive Publication Date: 2013-10-30
JIANGSU DAMING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its complex synthesis process and high cost, it has not been used in industrial production at present, but its research has become a research hotspot

Method used

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  • Method for preparing bis(4-carboxyphenyl) phenyl phosphine oxide (BCPPO)
  • Method for preparing bis(4-carboxyphenyl) phenyl phosphine oxide (BCPPO)
  • Method for preparing bis(4-carboxyphenyl) phenyl phosphine oxide (BCPPO)

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 在装有搅拌器、温度计和回流冷凝管的1000mL四口瓶中加入106.4g(0.8mol)无水AlCl 3 (分子量:133)、71mL(0.8mol)苯(密度:0.8786g / ml,分子量:78)和210mL(2.4mol)PCl 3 (密度:1.574g / ml,分子量:137),升温至65~68℃反应7h,减压蒸馏出过量的PCl 3 , then add 26g (0.8mol) sulfur powder in batches to the reaction flask, control the temperature not to exceed 80°C, react at 80-82°C for 4h after adding, add 255mL (2.4mol) toluene (density: 0.8669g / ml, molecular weight: 92), slowly warming up to 110-120°C, reacting for 8.5h, distilling off toluene under reduced pressure after the reaction, cooling the reactant to room temperature (about 25°C), slowly pouring into ice water, stirring, to obtain 粘稠固体,用无水乙醇重结晶,得白色固体BMPPS,产率为85.6%。

[0024] Add 32.2g (0.1mol) of BMPPS, 128mL of pyridine and 128mL of water into a 500mL four-necked flask equipped with mechanical stirring, a thermometer and a reflux condenser, stir and heat to 90°C, and add 95g (0.6mol) of KMnO in batches within 3h. 4 ,在96℃反应8h,冷却至室温(25℃左右),过滤,滤液用稀盐酸酸化到pH2,抽滤,得到粗产品,为白色固体。在250mL三口瓶中,将粗产品用适量的N...

Embodiment 2

[0026] 在装有搅拌器、温度计和回流冷凝管的1000mL四口瓶中加入80g(0.6mol)无水AlCl 3 (分子量:133)、53.3mL(0.6mol)苯(密度:0.8786g / ml,分子量:78)和182.8mL(2.1mol)PCl 3 (density: 1.574g / ml, molecular weight: 137), heat up to 68-70°C for 8 hours, and distill off excess PCl under reduced pressure 3 , then add 211g (0.66mol) sulfur powder in batches to the reaction bottle, control the temperature not to exceed 80°C, react at 82-84°C for 4h after adding, add 192ml of toluene (density: 0.8669g / ml, molecular weight: 92), slowly warming up to 110-115°C, reacting for 9h, distilling toluene under reduced pressure after the reaction, cooling the reactant to room temperature (about 25°C), slowly pouring into ice water, stirring to obtain a viscous solid, using Recrystallized from absolute ethanol to obtain white solid BMPPS with a yield of 869%.

[0027] Add 32.2g (0.1mol) of BMPPS, 128mL of pyridine and 128mL of water into a 500mL four-necked flask equipped with mechanical stirring, a thermometer and a reflux condenser, stir an...

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Abstract

The invention discloses a method for preparing bis(4-carboxyphenyl) phenyl phosphine oxide (BCPPO). The method comprises the following steps of: with benzene, phosphorus trichloride, powdered sulfur, methylbenzene and the like as raw materials, carrying out Friedel-Crafts reaction to firstly synthesize bis(4-methylphenyl) phenyl phosphine sulfide (BMPPS); with KMnO4 as an oxidizing agent, carrying out oxidation reaction to finally obtain the BCPPO; and carrying out structural characterization on a product. The method for preparing BCPPO, provided by the invention, is simple in process, high in product yield and purity, simple in purification method and capable of greatly reducing the production cost. The yield of the BCPPO prepared by using the preparation method in the prior art is 79.4%, and the yield of the BCPPO prepared by using the preparation method disclosed by the invention can be up to 88%.

Description

technical field [0001] The invention belongs to the field of flame retardant materials, and relates to a method for preparing a reactive flame retardant bis(4-carboxyphenyl)phenylphosphine oxide (BCPPO). The reactive flame retardant bis(4-carboxyphenyl ) Phenylphosphine oxide has good application effects and prospects in polymer materials (such as PET, PA, PEKK). Background technique [0002] Bis(4-carboxyphenyl)phenylphosphine oxide (BCPPO) is a reactive phosphorus-based flame retardant with excellent performance. It contains two carboxyl groups and flame-retardant element phosphorus in its molecule. The compound is very stable against oxidation and reduction. , has excellent flame retardant properties, and can be used as a reactive flame retardant monomer for various polymer materials such as polyester and polyamide to be introduced into polymers, especially for flame retardant polyester. Studies have shown that the flame retardant is suitable for the application of large...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
Inventor 潘小明仇国才史广平
Owner JIANGSU DAMING TECH
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