Photoinitiator in benzophenone type of cinnamene oligomer substitution, and preparation method
A technology of photoinitiator and styrene, applied in the field of photoinitiator, can solve the problems of limited promotion and application, cannot be completely replaced, etc., and achieve the effect of wide application prospect, good compatibility and absorption spectrum bandwidth.
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Embodiment 1
[0030] Example 1. Preparation of p-2-hydroxy-2-methyl-1-propionyl polymethylstyrene linear oligomer. Take a dried polymer tube, and equip it with a single-hole rubber stopper and dry short glass The tube and a section of dry rubber tube are connected to an anhydrous and oxygen-free operating system, vacuumed, filled with argon, and repeated three times to remove the air in the test tube. Then turn on the argon system, cool the polymerization tube to 0℃ with an ice bath, and inject 9ml of anhydrous cyclohexane and 4.0ml of dry methylstyrene and 5.4ml of n-butyllithium (2.8M ) Solution, shake well, the solution turns orange-red, after stirring for 30 minutes, add a small amount of methanol to terminate the reaction. The color disappeared immediately. The reaction liquid was added dropwise to 30 ml of methanol, and a white precipitate was immediately formed, which was filtered, washed with methanol and dried to obtain 3.4 g of a white solid with a yield of 92%. .
[0031] Into a 50ml...
Embodiment 2
[0033] Example 2. Preparation of p-2-hydroxy-2-chloromethyl-1-propionyl polyhydroxymethylstyrene linear oligomer
[0034] Into a 2L three-necked flask equipped with a stirrer, a separatory funnel with a calcium chloride drying tube and a reflux condenser with a gas absorption device, add 650ml of dichloroethane, and then add 36g of benzoyl peroxide under stirring With 200 g of hydroxymethyl styrene, the temperature is raised to 60° C. to react for about 5 hours to obtain a polyhydroxymethyl styrene oligomer solution. The temperature was lowered to room temperature, 170 g of anhydrous aluminum trichloride was added in batches under stirring and the temperature was raised to 35°C. Under vigorous stirring, 228 g of 2-chloromethyl propionyl chloride was added dropwise. After the reaction started to emit hydrogen chloride, the heating was stopped, and 2-chloromethyl propionyl chloride was continuously added, which took 4 hours. Then reflux for one hour, cool to room temperature, slowly...
example 3
[0036] Example 3. Preparation of p-1-hydroxy-1-cyclopentylformyl poly(methylstyrene-ethyl methacrylate) linear oligomer
[0037] Into a 1L three-necked flask equipped with a stirrer, a separatory funnel with a calcium chloride drying tube, and a reflux condenser with an absorption gas device, add 350ml carbon disulfide, and add 25g benzoyl peroxide and 150ml formaldehyde under stirring. Methyl styrene and 50 ml ethyl methacrylate, heated to 70° C. and reacted for about 5 hours to obtain a poly(methyl styrene-ethyl methacrylate) solution. The temperature was lowered to room temperature, 140 g of anhydrous aluminum trichloride was added in batches with stirring and the temperature was raised to 35°C. Under vigorous stirring, 115 g of cyclopentylformyl chloride was added dropwise. After the reaction began to emit hydrogen chloride, the heating was stopped, and cyclopentylformyl chloride was continuously added, which took 3h. Then reflux for 2 hours, cool to room temperature, slowly p...
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