Benzene ring-containing cross-linking agent and preparation method thereof
A technology of cross-linking agent and benzene ring, applied in the field of cross-linking agent containing benzene ring and its preparation, can solve the problems of few types of cross-linking agent, low purity, inability to meet the photolithography process, etc., and improve light absorption performance and purity. High, Moderate Yield Effects
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[0022] The invention provides a cross-linking agent containing a benzene ring and a preparation method thereof, wherein the method comprises: uniformly mixing tetramethylol glycoluril, a benzene series containing a hydroxyl group, and an alcohol compound in an organic solvent, Add an acid catalyst under stirring and carry out a temperature rise reaction. After the reaction is completed, lower it to room temperature to obtain a reaction solution; separation to obtain a cross-linking agent solution containing benzene rings; removing the solvent in the cross-linking agent solution containing benzene rings to obtain a high-purity cross-linking agent containing benzene rings.
[0023] Specifically, the benzene series containing hydroxyl group is one or more of phenol and benzyl alcohol, the alcohol compound is one or more of methanol and ethanol, and the acid catalyst is an inorganic acid. Described organic solvent is ethyl acetate, methylene dichloride, one or more in normal hexan...
Embodiment 1
[0028] Add 24.6g of tetramethylol glycoluril, 18.8g of phenol, 7.2g of methyl alcohol, and 100g of normal hexane in a four-necked flask equipped with condensing reflux, and then add 2ml of concentrated hydrochloric acid under stirring. At the same time, the temperature was raised to 50°C for constant temperature reaction for 3 hours. After the reaction, the temperature was lowered to room temperature, and then the pH of the reaction solution was adjusted to 7 with NaOH aqueous solution, and the n-hexane in the reaction solution was removed. Carry out column treatment in petroleum ether: ethyl acetate = 100:1 as developing solvent, and finally remove the solvent from the reaction solution after passing the column to obtain 38 g of colorless viscous liquid, which is colorless and viscous The liquid is 1,3-diphenoxy-4,6-dimethoxymethyl glycoluril with a purity of 97.73% and a yield of 85.9%.
Embodiment 2
[0030] Add 24.6g of tetramethylol glycoluril, 21.6g of benzyl alcohol, 7.2g of methanol, and 100g of n-hexane into a four-necked flask equipped with condensing reflux, and then add 2ml of concentrated sulfuric acid under stirring At the same time, the temperature was raised to 50°C for a constant temperature reaction for 3 hours. After the reaction was completed, the temperature was lowered to room temperature, and then the pH of the reaction solution was adjusted to 7 with NaOH aqueous solution, and the n-hexane in the reaction solution was removed. The solution was subjected to column treatment with petroleum ether: ethyl acetate = 100:1 as a developing solvent, and finally the reaction solution after passing the column was subjected to solvent removal to obtain 30 g of a colorless viscous liquid. The thick liquid is 1,3-diphenoxy-4,6-dimethoxymethyl glycoluril with a purity of 98.56% and a yield of 63.8%.
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