Preparation method of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and intermediate of DOPO

An o-phenylphenol and compound technology, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, and organic chemistry, etc. problems, to achieve the effect of simplifying production operations

Active Publication Date: 2018-01-09
LIER CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

First of all, in the process of preparing CDOP, if the excessive amount of phosphorus trichloride is too much, it is easy to cause side reactions, which not only causes difficulties in the purification of intermediate products, but also affects the reaction yield and the purity of the final product; for this reason, the existing preparation The method usually adopts the mode of adding phosphorus trichloride in batches during the reaction proc

Method used

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  • Preparation method of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and intermediate of DOPO
  • Preparation method of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and intermediate of DOPO
  • Preparation method of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and intermediate of DOPO

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Example Embodiment

[0046] Example 1 Preparation of DOPO using the method of the present invention

[0047] 1. Add 100g o-phenylphenol (1eq, 0.588mol), 1g anhydrous zinc chloride (0.0125eq, 0.0073mol) and 80.7g phosphorus trichloride (1eq, 0.588mol) into a 500mL four-necked flask, and heat to After reacting at 100°C for 2 hours, the temperature was continued to rise to 160°C for 2 hours. HPLC detected that the reaction was complete, and the reaction solution was directly used in the next reaction.

[0048] 2. Add 150 g of toluene and 5 g of diatomaceous earth to the upper reaction solution, stir at room temperature for 0.5 h, and filter to obtain a colorless clear liquid. 50 g of purified water was added to the filtrate, and the temperature was heated to reflux for 4 hours. TLC detected that the reaction was complete. Cool down to 0°C, vigorously stir to precipitate a white solid, filter, wash the filter cake twice with 50g purified water, the filter cake is detected as a mixture of HPPA-DOPO (detect...

Example Embodiment

[0051] Example 2 Preparation of DOPO using the method of the present invention

[0052] 1. Add 100g o-phenylphenol (1eq, 0.588mol), 1g anhydrous zinc chloride (0.0125eq, 0.0073mol) and 112.98g phosphorus trichloride (1.4eq) into a 500mL four-neck flask, and heat to 80℃ After reacting for 2 hours, the temperature was continued to rise to 180°C for 2 hours. HPLC detected that the reaction was complete, and the reaction solution was directly used in the next reaction.

[0053] 2. Add 150 g of toluene and 5 g of diatomaceous earth to the upper reaction solution, stir at room temperature for 0.5 h, and filter to obtain a colorless clear liquid. 50 g of purified water was added to the filtrate, and the temperature was heated to reflux for 4 hours. TLC detected that the reaction was complete. The temperature was lowered to 0°C, a white solid was precipitated out with vigorous stirring, and filtered. The filter cake was washed twice with 50 g purified water, and the filter cake was collec...

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Abstract

The invention relates to a preparation method of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and an intermediate of DOPO and belongs to the field of chemistry. Aiming at solving the technical problems, the invention provides the preparation method of the DOPO intermediate CDOP; the method comprises the following steps: raising the temperature of a mixture of o-phenylphenol, zinc chloride and phosphorus trichloride to 60 DEG C to 140 DEG C and carrying out esterification reaction; continually raising the temperature to 160 DEG C to 220 DEG C and reacting to obtain the product. Byadopting the preparation method provided by the invention, the phosphorus trichloride can be added in one step in a material feeding process and the excessive phosphorus trichloride and reaction byproducts do not need to be removed by decompressing and distilling after the reaction is finished, so that the production operation is greatly simplified; compared with an existing technology, the preparation method has remarkable advantages.

Description

technical field [0001] The invention relates to a preparation method of DOPO and its intermediate, belonging to the field of chemistry. Background technique [0002] 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, referred to as DOPO, molecular formula C 12 h 9 PO 2 , CAS No.: 35948-25-5, molecular weight 216.2, melting point 117-121°C, white flaky or powdery solid. The flame retardant synthesized by DOPO and its derivatives has the characteristics of high efficiency, no halogen, less smoke, low toxicity, no migration, and long-lasting flame retardant performance. It is a new type of halogen-free and environmentally friendly flame retardant developed in recent years. At present, its synthesis and application have attracted extensive attention. [0003] The synthetic route of DOPO is as follows: [0004] [0005] Mainly comprise the following steps: 1, ortho-phenylphenol OPP and phosphorus trichloride under the effect of catalyst (such as zinc chloride) one-pot es...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C07F9/6574
Inventor 姚中伟王福雄程柯
Owner LIER CHEM CO LTD
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