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Synthesis of fire retardant tri (bromophenoxy) cyanurate
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A technology of bromophenoxy and cyanurate, applied in the direction of organic chemistry, can solve the problems of large environmental pollution, high cost, and large amount of solvents, and achieve the effect of high safety factor and low cost
Inactive Publication Date: 2008-07-02
NANJING NORMAL UNIVERSITY +1
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[0003] Method 1, the solvents used are organic solvents with low boiling points, which are easy to volatilize and cause great pollution to the environment
When using a single solvent, the amount of solvent required is more and the product yield is lower
Because the organic solvent is volatile, the loss is large and the recovery is small, and the cost of the product is relatively high
In addition, these organic solvents are flammable and explosive substances, which reduces the safety factor of the reaction process.
[0004] Method two, the solvent used is the mixed solvent of dichloromethane and water, although the consumption of organic solvent is reduced, the cost of product is reduced, but because dichloromethane is also flammable and explosive chemicals, still exists in the whole reaction process Security risks
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Embodiment 1
[0017] Embodiment 1 is equipped with agitator, reflux condenser, thermometer, in the reaction flask of constant pressure dropping funnel, add 19.92g tribromophenol, 2.7g sodium hydroxide, 0.5g n-tetrabutylammonium bromide, 52gH 2 O, stir. Dissolve 3.7g of cyanuric chloride in 30ml of chloroform, add the cyanuric chloride chloroform solution dropwise at 20°C to 35°C, and continue the reaction at 40°C to 55°C for 60 minutes after the dropwise addition is completed. Then the solvent was distilled off. Filter, wash with water twice, filter and dry to obtain a white product. The yield is 95%.
Embodiment 2
[0018] Embodiment 2 In the reaction flask that stirrer, reflux condenser, thermometer are housed, constant pressure dropping funnel, add 15.16g dibromophenol, 2.7g sodium hydroxide, 0.5g triethyl benzyl ammonium chloride, 52gH 2 O, stir. Dissolve 3.7g of cyanuric chloride in 25ml of chloroform, add the cyanuric chloride chloroform solution dropwise at 20°C to 35°C, and continue the reaction for 60min after the dropwise addition is completed. Then the solvent was distilled off. Filter, wash with water twice, filter and dry to obtain a white product. The yield is 95%.
Embodiment 3
[0019] Embodiment 3 In the reaction flask equipped with stirrer, reflux condenser, thermometer, and constant pressure dropping funnel, add 10.38g monobromophenol, 2.7g sodium hydroxide, 0.3g triphenylethylphosphonium bromide, 52gH 2 O, stir. Dissolve 3.7g of cyanuric chloride in 20ml of chloroform, add the cyanuric chloride chloroform solution dropwise at 20°C to 35°C, and continue the reaction for 60min after the dropwise addition is completed. Then the solvent was distilled off. Filter, wash with water twice, filter and dry to obtain a white product. The yield is 95%.
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Abstract
The synthesis of fire retardant tri(bromophenoxy) cyanurate inside two-phase solution of water solution and organic solvent includes the following steps: reaction of bromized phenol and sodium hydroxide to produce bromized phenol sodium; and the reaction of bromized phenol sodium and cyanurichloride in the presence of catalyst and at proper temperature to produce tri(bromophenoxy) cyanurate. The catalyst is quaternary ammonium salt and quaternary phosphonium salt, and the proper temperature includes cyanurichloride dropping temperature of 20-35 deg.c and reaction temperature after finishing dropping of 40-55 deg.c. The bromized phenol may be bromophenol, dibromophenol or tribromophenol. The synthesis process of the present invention has high safety and low cost and is suitable for industrial production.
Description
technical field [0001] The invention relates to a method for synthesizing a flame retardant, in particular to a method for synthesizing a flame retardant tris(bromophenoxy)cyanurate. Background technique [0002] Tris(bromophenoxy)cyanurate is an existing flame retardant. From the data currently available, there are two methods for synthesizing this product: (1) using tribromophenol and cyanuric chloride as raw materials, organic solvents such as acetone or ethyl acetate or ethanol as solvents, sodium hydroxide Make a catalyst to synthesize the target product. (2) Tribromophenol is first reacted with aqueous sodium hydroxide solution to make sodium tribromophenolate aqueous solution, and then reacts with cyanuric chloride dichloromethane solution to obtain the target product. [0003] Method 1, the solvents used are all low-boiling organic solvents, which are easy to volatilize and cause great pollution to the environment. When using a single solvent, the amount of solven...
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