Prepn of fire retardant resorcinol tetraphenyldiphosphate

The technology of resorcinol tetraphenyl diphosphate and triphenyl phosphate is applied in the field of preparation of flame retardants, which can solve the problems of low product yield, seriousness, dark color of crude products, etc., and reduce pollution. , the effect of short reaction time and low energy consumption

Inactive Publication Date: 2007-01-03
ZHENJIANG SANWA FLAME RETARDANT ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Third, the obtained crude product has a darker color and a higher viscosity, and needs to be washed and decolorized many times, causing serious pollution to the environment.
[0004] Method 2, the pure substance of diphenylphosphoryl chloride is difficult to synthesize, and it is easy to generate the mixture of monophenylphosphoryl chloride, diphenylphosphoryl chloride and triphenylphosphoryl chloride. If diphenylphosph

Method used

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  • Prepn of fire retardant resorcinol tetraphenyldiphosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1. add phenol 141.2g in the 250ml four-necked flask that reflux condenser (upper mouth is connected tail gas absorption device), electric stirrer and thermometer are equipped with, catalyzer aluminum trichloride 3.0g. Turn on the condensed water, stir, raise the temperature to 50°C and start adding POCl dropwise 3 76.65g, dropwise finished in 1-1.5 hours, the temperature gradually rose to 80°C during the dropwise addition. Then the temperature was raised to 100° C., kept for 1 hour, then raised to 140° C. for 1 hour, and the heating was stopped.

[0018] Add 27.5g of resorcinol, heat and stir, keep the vacuum below 10mmHg, react at 140-160°C for 60min, collect the phenol, then keep it at 180-220°C for about 90min, and the reaction is over. Stop heating, turn off the vacuum pump when the liquid temperature drops to 120°C, and suction filter while it is hot. The crude product is a yellow or brown transparent liquid, and the by-product phenol is reused. The ...

Embodiment 2

[0019] Embodiment 2. Add phenol 282.3g, catalyzer aluminum trichloride 3.0g in the 500ml four-necked flask that reflux condenser (upper mouth is connected tail gas absorption device), electric stirrer and thermometer are housed. Turn on the condensed water, stir, raise the temperature to 50°C and start adding POCl dropwise 3 153.3g, 1 to 1.5 hours to finish the drop, the temperature gradually rose to 80°C during the dropwise addition, then the temperature rose to 100°C, kept for 1 hour, then rose to 140°C for 1 hour, and stopped heating. Distill under reduced pressure to remove unreacted phenol, and collect components at 240-260° C. under a vacuum of 10 mmHg to obtain 293.0 g with a yield of 90.0%.

[0020] Take TPP68.7g (0.21mol), resorcinol 11.6g (0.105mol), join in the 150ml three-neck flask equipped with magnetic stirrer and thermometer, heat and stir, add 0.3g K 2 CO 3 , with a vacuum degree below 10mmHg, react at 120-130°C for 30 minutes, collect phenol, and then keep...

Embodiment 3

[0021] Embodiment 3. in the 500ml four-necked flask that is equipped with reflux condenser (upper mouth is connected with tail gas absorption device), electric stirrer and thermometer, add phenol 282.3g, catalyzer aluminum trichloride 3.0g. Turn on the condensed water, stir, raise the temperature to 50°C and start adding POCl dropwise 3 153.3g, 1 to 1.5 hours to finish the drop, the temperature gradually rose to 80°C during the dropwise addition, then the temperature rose to 100°C, kept for 1 hour, then rose to 140°C for 1 hour, and stopped heating. Distill under reduced pressure to remove unreacted phenol, and collect components at 240-260° C. under a vacuum of 10 mmHg to obtain 293.0 g with a yield of 90.0%.

[0022] Get TPP68.7g (0.21mol), resorcinol 11.6g (0.105mol), join in the 150ml three-neck flask that magnetic stirrer and thermometer are housed, heat and stir, heat and stir, add 0.2g sodium phenoxide, React at 10mmHg 130-140°C for 30 minutes, collect the phenol, the...

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Abstract

The preparation process of fire retardant resorcinol tetraphenyl diphosphate includes the first step of the reaction between phenol and phosphorus oxychloride in the presence of Lewis acid catalyst and under heating to produce triphenyl phosphate ester; and second step of ester interchange reaction between triphenyl phosphate ester and resorcinol in the conditions of catalysis, heating and decompression to obtain resorcinol tetraphenyl diphosphate. The reaction temperature is 80-260 deg.c; the catalyst for the first step is Lewis acid catalyst; and the catalyst for the second step is Lewis acid catalyst or alkali catalyst in the amount of 0.05-3 wt% of resorcinol. The acid catalyst is selected from MgCl2, ZnCl2, AlCl3 and TiCl4 and the alkali catalyst is selected from NaOH, KOH, Na2CO3, K2CO3 and sodium phenate. The present invention has the advantages of short reaction period, low power consumption, high product yield and less environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of the flame retardant resorcinol tetraphenyl diphosphate. Background technique [0002] Resorcinol tetraphenyl diphosphate is an existing flame retardant. According to the current literature, the synthetic methods reported in the literature mainly contain three kinds: 1. Phosphorus oxychloride reacts with resorcinol to obtain resorcinol tetrachlorobisphosphate, which is then capped with phenol to obtain Target product; 2. Phosphorus oxychloride reacts with phenol to obtain diphenylphosphoryl chloride, then reacts with resorcinol to obtain target product; 3. replace phenol with sodium phenate as raw material, i.e. use sodium phenoxide to resorcinol Tetrachlorobisphosphate was subjected to capping reaction to obtain the product. [0003] Method one, at first, when the first step prepares resorcinol tetrachlorobisphosphate, it is easy to generate p...

Claims

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Application Information

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IPC IPC(8): C09K21/12C07F9/12
Inventor 杨锦飞章庚柱黄东平李戈华顾慧丹
Owner ZHENJIANG SANWA FLAME RETARDANT ENG TECH CO LTD
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