Biphenyl-containing compound liquid crystal epoxy resin and preparation method thereof
An epoxy resin, composite technology, applied in liquid crystal materials, chemical instruments and methods, organic chemistry and other directions, can solve the problems of uneconomical synthesis methods and low yields, improve appearance quality, high reaction conversion rate, prevent The effect of oxidation
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[0028] Example 1
[0029] Step 1: Synthesis of di-p-hydroxybenzoic acid-3,3',5,5'-tetramethoxybiphenyl-4,4'-diester
[0030] Under the protection of nitrogen, p-hydroxybenzoic acid (0.2mol, 27.6g), 3,3',5,5'-tetramethoxybiphenyl-4,4'-diphenol (0.05mol, 15.3g), Methylbenzenesulfonic acid (3mmol, 0.54g) and sulfolane (80ml) were added to a three-necked flask with a stir bar, a water trap and a thermometer and stirred at 220°C for 6h. The water formed during the reaction is continuously removed. After the reaction mixture was cooled to room temperature, it was poured into 500 ml of water, and the filter cake obtained after filtration was washed repeatedly with water and ethanol. Finally, di-p-hydroxybenzoic acid-3,3',5,5'-tetramethoxybiphenyl-4,4'-diester (23.3g) was obtained as a white powder. Yield: 85.4%.
[0031] Step 2: Synthesis of bis(4-(2,3-glycidoxy)benzoic acid)-3,3',5,5'-tetramethoxybiphenyl-4,4'-diester
[0032] Under the protection of nitrogen, the di-p-hydroxybenzoic ac...
Example Embodiment
[0036] Example 2
[0037] The synthesis method of this embodiment is:
[0038]
[0039] Step 1: Synthesis of di-p-hydroxybenzoic acid-3,3',5,5'-tetramethylbiphenyl-4,4'-diester
[0040] Under the protection of nitrogen, p-hydroxybenzoic acid (0.2mol, 27.6g), 3,3',5,5'-tetramethylbiphenol (0.05mol, 12.1g), p-toluenesulfonic acid (5mmol , 0.9g) and sulfolane (50ml) were added to a three-necked flask with a stir bar, water trap and thermometer and stirred at 180°C for 4h. The water formed during the reaction is continuously removed. After the reaction mixture was cooled to room temperature, it was poured into 500 ml of water, and the filter cake obtained after filtration was washed repeatedly with water and ethanol. Finally, di-p-hydroxybenzoic acid-3,3',5,5'-tetramethylbiphenyl-4,4'-diester (19.3g) was obtained as a white powder. Yield: 80.1%.
[0041] Step 2: Synthesis of bis(4-(2,3-glycidoxy)benzoic acid)-3,3',5,5'-tetramethylbiphenyl-4,4'-diester
[0042] Under the protection of n...
Example Embodiment
[0044] Example 3
[0045] The synthesis method of this embodiment is:
[0046]
[0047] image 3
[0048] Step 1: N,N'-bis(4-hydroxyphenylmethylene)-2,2',3,3',5,5',6,6'-octafluorobiphenyl-4,4'- Synthesis of Diamine
[0049] Under the protection of nitrogen, p-hydroxybenzaldehyde (0.2mol, 24.4g), 2,2',3,3',5,5',6,6'-octafluorobiphenyl-4,4'-diamine ( 0.05mol, 16.4g) and dimethyl sulfoxide (40ml) were added to a three-necked flask with a stir bar and a thermometer and stirred at 100°C for 3h. After the reaction mixture was cooled to room temperature, it was poured into 500 ml of water, and the filter cake obtained after filtration was washed repeatedly with water and ethanol. Finally, N,N'-bis(4-hydroxyphenylmethylene)-2,2',3,3',5,5',6,6'-octafluorobiphenyl-4 was obtained as pink powder , 4'-Diamine (25.5g). Yield: 95.2%.
[0050] Step 2: N,N'-bis(4-(2,3-glycidoxy)-phenylmethylene)-2,2',3,3',5,5',6,6' -Synthesis of Octafluorobiphenyl-4,4'-diamine
[0051] Under the protection of nitro...
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