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Synthesis method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide

A synthetic method, the technology of phosphaphenanthrene, which is applied in 9 fields, can solve the problems of easy spontaneous combustion of decomposition products, increased difficulty in processing, waste of energy, etc., and achieve the goal of improving the conversion rate of raw materials and product quality, reducing the occurrence of side reactions, and reducing the loss of raw materials Effect

Active Publication Date: 2011-07-20
山东旭锐新材股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is following deficiency in this method: (1) because phosphorus trichloride can be decomposed in a large amount at high temperature, and decomposition product is very easy to spontaneous combustion, there is very big potential safety hazard in actual production process, and decomposes a large amount under high temperature Phosphorous trichloride, wasted raw materials, also increased difficulty for subsequent processing; (2) reaction is carried out under the high temperature for a long time, also has higher requirement to equipment performance; (3) wasted a large amount of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 1000kg of o-phenylphenol and 810kg of phosphorus trichloride to the reactor, add 22kg of catalyst zinc chloride, increase the temperature of the heat transfer oil in the jacket of the reactor body, raise the temperature to 50°C, stir for 2 hours, and lower the temperature Raise the temperature to 100°C for 3 hours, then raise the temperature to 125°C for 6 hours, and then raise the temperature to 150°C for reflux reaction. When the reaction is carried out until there is no reflux, use liquid chromatography to measure the adjacent Phenylphenol content, after adding phosphorus trichloride according to the o-phenylphenol content, continue the reflux reaction, and when the reaction is carried out until there is no reflux, then measure the o-phenylphenol content in the reaction product until the o-phenylphenol content in the reaction product content≤0.1wt%, the reflux reaction ends.

[0026] Transfer the reaction material to the decolorization kettle, and when the temper...

Embodiment 2

[0030] Add 1000kg of o-phenylphenol and 760kg of phosphorus trichloride to the reactor, add 40kg of catalyst zinc chloride, increase the temperature of the heat transfer oil in the jacket of the reactor body, raise the temperature to 45°C, stir and react for 2.5 hours, and lower the temperature Raise the temperature to 100°C for 3.5 hours, then raise the temperature to 120°C for 6.5 hours, and then raise the temperature to 145°C for reflux reaction. When the reaction is carried out until there is no reflux, use liquid chromatography to measure the adjacent Phenylphenol content, after adding phosphorus trichloride according to the o-phenylphenol content, continue the reflux reaction, and when the reaction is carried out until there is no reflux, then measure the o-phenylphenol content in the reaction product until the o-phenylphenol content in the reaction product content≤0.1wt%, the reflux reaction ends.

[0031] Transfer the reaction material to the decolorization kettle, and...

Embodiment 3

[0035] Add 1000kg of o-phenylphenol and 840kg of phosphorus trichloride to the reactor, add 20kg of catalyst zinc chloride, increase the temperature of the heat transfer oil in the jacket of the reactor body, raise the temperature to 55°C, stir and react for 1.5 hours, and lower the temperature Raise the temperature to 110°C for 2.5 hours, then raise the temperature to 130°C for 5.5 hours, then raise the temperature to 160°C for reflux reaction, and use liquid chromatography to measure the adjacent Phenylphenol content, according to the o-phenylphenol content, add phosphorus trichloride and continue the reflux reaction. When the reaction is carried out until there is no reflux, then measure the o-phenylphenol content in the reaction product until the o-phenylphenol content in the reaction product content≤0.1wt%, the reflux reaction ends.

[0036] Transfer the reaction material to the decolorization kettle, and when the temperature is lowered to 80°C, add 1900kg of toluene to d...

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Abstract

The invention discloses a synthesis method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide. The method comprises the following steps: mixing o-phenylphenol and phosphorus trichloride according to a weight ratio of 1:0.75-0.85, adding catalyst to dissolve, reacting at 100-110 DEG C for 2.5-3.5 hours, then reacting at 120-130 DEG C for 5.5-6.5 hours, performing reflux reaction at 140-160 DEG C, dissolving, decoloring, hydrolyzing, removing solvent, performing atmospheric distillation in a distillation kettle at 125-135 DEG C, and then performing reduced pressure distillation under the conditions that the vacuum degree is no less than 0.09MPa and the inner temperature of the distillation kettle is 140-150 DEG C, to obtain the product 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide. Background technique [0002] The new phosphaphenanthrene flame retardant intermediate 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and its derivatives are new halogen-free, low-smoke, low-toxicity, green Flame retardant intermediates, with excellent flame retardant properties, have been widely used in flame retardant applications of synthetic fibers, plastics for electronic equipment, circuit boards, and semiconductor packaging materials. At the same time, DOPO and its derivatives can also be used for chemical modification of polymer materials due to their special functions. In addition, DOPO can also be used as an insecticide, fungicide, curing agent, antioxidant, stabilizer, photoinitiator, binder, blocking agent for harmful metal ions, lightening agent for organic matter, ultraviolet ligh...

Claims

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Application Information

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IPC IPC(8): C07F9/53
Inventor 郝建港丁瑞林段俊彪陶书伟邢海亮
Owner 山东旭锐新材股份有限公司
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