A kind of preparation method of poly(aryl ether ketone) and poly(aryl ether ketone)
A technology of aryl ether ketone and benzophenone, which is applied in the field of polymer materials and can solve problems such as dark colors and poor product quality
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[0020] The present invention provides a preparation method of poly(aryl ether ketone), the method comprises:
[0021] Step 1: Mix benzophenone compounds or diacid chloride compounds, hydroxyl-containing compounds and sodium borohydride evenly under the action of a first solvent, heat to 80-150° C. to remove the first solvent to obtain a premix;
[0022] Step 2: Using the premix obtained in Step 1 as a reaction substrate, add the second solvent and carbonate in sequence at 150-160° C., and gradually increase the temperature for reaction to obtain poly(aryl ether ketone).
[0023] According to the present invention, firstly add benzophenone compound or diacid chloride compound, hydroxyl-containing compound, sodium borohydride and the first solvent in turn in the there-necked flask, slowly start and stir to 30-40rpm, after 5-10 minutes the solid All dissolved, speed up the stirring speed to 100-120rpm, stir for 10-15 minutes, thoroughly mix the reaction raw materials, heat the th...
Embodiment 1
[0036] Take a 3000ml three-necked bottle and place it in a heating mantle, insert a metal stirring paddle into the middle of the three-necked bottle, weigh 218.2g (1mol) of 4,4'-difluorobenzophenone from one side of the bottle and add it to the three-necked bottle, weigh 110.1 g (1mol) of hydroquinone is added to the three-necked flask from the same side, weigh 1.892g of sodium borohydride (0.05mol) from the same side and add it to the three-necked flask, measure 800ml of acetone, Add it to the three-necked bottle, slowly start stirring to 30rpm, after 5 minutes all solids are dissolved, speed up the stirring speed to 100rpm, stir for 10 minutes, 4,4'-difluorobenzophenone and hydroquinone are thoroughly mixed evenly. Seal the feeding edge of the three-necked flask, connect the other side (collecting edge) to the straight condenser tube and the collection flask, keep the stirring speed at 100 rpm, heat the three-necked flask to 80°C, and the acetone in the three-necked flask boi...
Embodiment 2
[0043] Prepare poly(aryl ether ketone) a2-a9 according to the steps of Example 1, the difference is that the type of the first solvent in the step 1, the consumption of the first solvent and the consumption of sodium borohydride change, as shown in the table 1 shows:
[0044] Table 1
[0045]
[0046]
[0047] From this, the influence table of orthogonal factors can be obtained, as shown in Table 2
[0048] Table 2
[0049]
[0050] As can be seen from Tables 1 and 2, the amount of sodium borohydride has the greatest influence on the premixing effect, and the influences are ranked as follows: the amount of sodium borohydride>the first solvent>the amount of solvent, so the optimal premixing conditions are: using acetone as For solvent, the ratio of the molar ratio of hydroquinone to sodium borohydride is 1:0.15, and the ratio of the molar mass (mol) of hydroquinone to the amount of solvent (L) is 1:1.
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