Phosphorous flame-retardant water-based alkyd resin and preparation method thereof
A technology of water-based alkyd resin and phosphaphenanthrene, which is applied in the field of preparation of water-based alkyd resin and can solve problems such as complex technical processes
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[0022] The preparation steps of DOPOMA are:
[0023] In a three-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add a mixed solution of tetrahydrofuran and toluene of equal mass, DOPO and maleic anhydride are put in at a material ratio of 1:1.05, stir and heat, and the temperature is 84°C Backflow began to occur when the system was stable and reacted for 9 hours, and the color gradually deepened and turned green. After continuing to react for 24 hours, the color of the system was dark green. After 24 hours of heat preservation reaction, the reaction was stopped and cooled to room temperature. The system is layered, the lower layer is a dark green viscous liquid, and the upper layer is a light yellow clear liquid. The lower layer of viscous liquid is separated and washed with xylene for several times, then dried in an oven at 120°C for 48 hours, taken out and cooled to room temperature to obtain a light yellow Crystalline solid.
[0024] The preparat...
Embodiment 1
[0028] Add 51 parts of soy oil, 30 parts of trimethylolpropane, 20 parts of phthalic anhydride and 3 parts of xylene into a 100ml four-neck flask; blow nitrogen gas, start stirring, slowly raise the temperature, and heat to 180°C; at 160°C, there is a sound of oil splashing and reflux, and the system is a turbid liquid. After the temperature reaches 170°C, the system turns into a yellowish clear liquid after 20 minutes of reaction; Add 5.2 parts of DOPOMA in batches within the last 10 minutes; after the addition, slowly raise the temperature to 200°C for 30 minutes, and then slowly raise the temperature to 210°C; the final temperature of the heat preservation reaction is 210~220°C. As the reaction progresses, the color of the system gradually Deepen and finally turn orange-red; measure the acid value every half hour after the heat preservation reaction for 2 hours. When the temperature is 55mgKOH / g, stop heating, lower the temperature, and drain the xylene in the system; weigh...
Embodiment 2
[0030] Add 51 parts of soy oil, 28 parts of trimethylolpropane, 15 parts of phthalic anhydride and 3 parts of xylene into a 100 ml four-necked flask. Nitrogen was passed, stirring was started, and the temperature was raised slowly. (Heat to 180°C within 30~40min). At 160°C, there was a sound of oil splashing and backflow. The system is a cloudy liquid. After a temperature of 170°C, the reaction system turned into a slightly yellow clear liquid after 20 minutes of reaction. When the system temperature reaches 180°C, start to keep warm for 40 minutes. Add 11.2 copies of DOPOMA in batches within 10 minutes after the end of the heat preservation. After the feeding is completed, slowly raise the temperature to 200°C for 30 minutes, then slowly raise the temperature to 210°C, and the final temperature for the heat preservation reaction is 210~220°C (do not rapidly raise the temperature to 220°C to avoid bumping). As the reaction progressed, the color of the system graduall...
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