Phosphorus-containing polyaspartic acid ester as well as preparation method and application thereof
A technology of aspartate and dichlorophosphoric acid, applied in polyurea/polyurethane coatings, chemical instruments and methods, coatings, etc., can solve the problems of improving the flame retardant properties of polyaspartate.
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Embodiment 1
[0082]
[0083] (1) to the reflux condenser, stirring, thermometer, connected with N 2 Add 148.9g (1.0mol) of methyl dichlorophosphate and 223.4g of solvent ethanol to the reaction bottle of the gas pipeline and place it in an ice-water bath. Slowly add 34.1g (2.0mol) of liquid ammonia under a nitrogen atmosphere for 1 hour, and heat it after the addition is complete. Reflux at 85°C for 3 hours to obtain an amination reaction liquid, and the conversion rate of methyl dichlorophosphate is >99% as monitored by GC.
[0084] (2) in N 2 Atmosphere, add 253.0g (2.5mol) triethylamine to the above reaction solution, stir at room temperature for 2 hours to adjust the pH to not less than 7, add 17.6g ferrocene, and stir 351.3g (2.04mol, C= C / -NH 2 =1.02) Diethyl maleate was slowly added to the reactor at a uniform speed within 1h, and the feed rate was controlled so that the temperature of the system was around 50°C. After the addition was completed, the reactor was heated to 90°C ...
Embodiment 2
[0088]
[0089] (1) to the reflux condenser, stirring, thermometer, connected with N 2 Add 162.9g (1.0mol) of ethyl dichlorophosphate and 244.4g of solvent ethanol to the reaction bottle of the gas pipeline and place it in an ice-water bath. Slowly add 34.1g (2.0mol) of liquid ammonia under a nitrogen atmosphere for 1 hour. After the addition is complete, , heated to 80° C. for reflux reaction for 5 hours to obtain an amination reaction liquid, and the conversion rate of ethyl dichlorophosphate was >99% as monitored by GC.
[0090] (2) in N 2 Atmosphere, add 253.0g (2.5mol) triethylamine to the above reaction solution, stir at room temperature for 2h to adjust the pH to not less than 7, add 7g of cobalt chloride; 378.8g (2.2mol, C=C / -NH 2 = 1.1) Diethyl maleate was slowly and uniformly added to the reaction kettle within 0.5h, and the feeding rate was controlled to keep the system temperature at about 30°C. After the addition was completed, the reaction kettle was heated...
Embodiment 3
[0094]
[0095] (1) With reflux condenser, stirring, thermometer, connected with N 2 Add 161.0g (1.0mol) of isopropyl dichlorophosphoric acid and 325.8g of solvent petroleum ether into the reaction bottle of the gas line pipe and place it in an ice-water bath. Slowly add 34.1g (2.0mol) of liquid ammonia under a nitrogen atmosphere for 3 hours, and the addition is complete Then heated to 68° C. for reflux reaction for 2 hours to obtain an amination reaction liquid, and the conversion rate of isopropyl dichlorophosphoric acid was >99% as monitored by GC.
[0096] (2) in N 2 Atmosphere, add 253.0g (2.5mol) triethylamine to the above reaction solution, stir at room temperature for 2h to adjust the pH to not less than 7, then add 35.2g zinc chloride; 413.3g (2.4mol, C= C / -NH 2 =1.2) Diethyl maleate was slowly added to the reactor at a uniform speed within 2 hours, and the feeding rate was controlled so that the system temperature was around 50°C. After the addition was completed...
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