3-trifluoromethyl-4-chlorophenyl paradioxybenzene, its synthesis and polyaryl ether ketone therefrom
A technology of chlorophenylhydroquinone and trifluoromethyl, which is applied in the field of polymer materials and can solve problems such as high melt viscosity, increased processing costs, and limited use range
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Embodiment 1
[0036] 1. Add 98 grams (0.5mol) of 3-trifluoromethyl-4-chlorophenylaniline, 128ml of concentrated hydrochloric acid, and 150ml of water into a 1000ml beaker equipped with mechanical stirring and a thermometer, cool in an ice-salt bath, and control the temperature at - 5°C to 0°C. Put 34.5 grams of sodium nitrite and 100ml of water into a 250ml beaker to fully dissolve it. After 0.5 hours, the sodium nitrite solution was added dropwise at a rate of 0.1 ml / second, and the temperature was controlled from 0°C to 3°C. After 1 hour, an aqueous solution of intermediate product A was obtained with a yield of 70-75%;
[0037] 2. put into 40.5 gram benzoquinones (0.375mol) in 2000ml large beaker, 168 gram sodium bicarbonate (2mol), water 600ml; The aqueous solution of step 1 gained intermediate product A is dripped in with the speed of 0.2ml / second, reaction The temperature is 12-15° C. After 3 hours, filter and wash to obtain the intermediate product B with a yield of 87-90%;
[003...
Embodiment 2
[0040] 1. method is the same as embodiment one, and the charging capacity of 3-trifluoromethyl-4-chloroaniline is expanded to 196 grams (1mol), concentrated hydrochloric acid 128ml, water 150ml add in the 1000ml beaker that mechanical stirring, thermometer are housed, ice Cool in a salt bath and control the temperature at 5°C to 8°C; put 75.9 grams of sodium nitrite (1.1mol) and 200ml of water into a 250ml beaker to fully dissolve it. After 0.5 hours, drop the sodium nitrite solution at a rate of 0.2ml / second, and control the temperature from 0°C to 3°C; after 1 hour, an aqueous solution of intermediate product A is obtained, and the yield is 65-70%;
[0041] 2. Put 108 grams of benzoquinone (1mol), 300 grams of sodium bicarbonate (2mol), and 600ml of water into a 2000ml large beaker; drop the aqueous solution of A at a rate of 0.4ml / second. The reaction temperature is 12-15° C. After 4 hours, it is filtered and washed to obtain the intermediate product B with a yield of more ...
Embodiment 3
[0044] The method is the same as that in Example 1. The feeding amount of aniline is expanded to 390 grams (2 mol), and cooling by directly adding ice is adopted. When the intermediate product A is added to the system, the method of pouring in batches is adopted, and it is divided into 50 batches, each batch is about 100ml, Others are the same as in Example 1, the molar yield is 45-50%, and the melting point is 122°C.
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