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One-step Synthesis of Green Epoxy Resin Curing Agent Maleic Rosin Anhydride
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A technology of epoxy resin curing and maleic anhydride, applied in the field of bio-based epoxy resin curing agent preparation
Inactive Publication Date: 2019-07-26
EAST CHINA UNIV OF SCI & TECH
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Embodiment 1
[0010] A. 104g of abietic acid, 34g of maleic anhydride, 1.38g of p-toluenesulfonic acid, and 250mL of glacial acetic acid are put into a titanium reactor with a volume of 1L, and the reactor is installed to ensure good airtightness;
[0011] B. Turn on the stirring, control the speed at 600-700r / min, start to heat up to 190°C, and keep it for 4 hours, and the pressure in the kettle is 0.5MPa when it is stable;
[0012] C. Stop heating, cool to room temperature naturally, recrystallize the product 3 times, and dry to obtain a white solid; the purity of the maleic rosin prepared in this embodiment is 97.3%, and the yield is 73%.
Embodiment 2
[0014] A. 104g of abietic acid, 34g of maleic anhydride, 1.38g of p-toluenesulfonic acid, and 250mL of glacial acetic acid are put into a titanium reactor with a volume of 1L, and the reactor is installed to ensure good airtightness;
[0015] B. Turn on the stirring, control the speed at 600-700r / min, start to heat up to 190°C, and keep it for 2 hours, and the pressure in the kettle is 0.4MPa when it is stable;
[0016] C. Stop heating, cool to room temperature naturally, recrystallize the product 3 times, and dry to obtain a white solid; the purity of the maleic rosin prepared in this embodiment is 97.9%, and the yield is 60%.
Embodiment 3
[0018] A. 104g of abietic acid, 37g of maleic anhydride, 1.41g of p-toluenesulfonic acid, and 250mL of glacial acetic acid are put into a titanium reactor with a volume of 1L, and the reactor is installed to ensure good airtightness;
[0019] B. Turn on the stirring, control the speed at 600-700r / min, start to heat up to 190°C, and keep it for 4 hours, and the pressure in the kettle is 0.5MPa when it is stable;
[0020] C. stop heating, naturally cool to room temperature, recrystallize the product 3 times, and dry to obtain a white solid; the purity of the maleic rosin prepared in this embodiment is 96.3%, and the yield is 74%.
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Abstract
Disclosed is one-step synthesis of a green maleic abietic anhydride epoxy resin curing agent. The invention relates to novel technology of the preparation of an abietic acid derivative containing acid anhydride and carboxyl function groups. Abietic acid and acid derivative are taken as raw materials, acetic acid is taken as a solvent, and under the catalysis of p-toluenesulfonic acid, an isomerization and Diels-Alder reaction is carried out for one-step synthesis of maleic abietic anhydride. The reaction is carried out in a high-pressure reaction vessel provided with heating and stirring at the temperature of 160-200 DEG C for 2-4 h, with the pressure controlled in the range of 0.3-0.8 MPa. A mixture obtained from the reaction is subjected to trinary recrystallization to obtain maleic abietic anhydride (MPA). The synthesis is simple in process, high in conversion rate, and excellent in purity of the product.
Description
technical field [0001] The invention belongs to the technical field of preparation of bio-based epoxy resin curing agent. More specifically, the present invention relates to a kind of with abietic acid as raw material, prepares the preparation method of epoxy resin curing agent maleic abietic anhydride. Background technique [0002] With the development of society, people pay more and more attention to the protection of the environment. There are fewer and fewer non-renewable resources such as petroleum, and the refining and refining of petroleum and other resources will cause huge pollution to the environment, saving non-renewable resources and reducing Environmental pollution has become an important issue for human beings all over the world. However, due to the rapid development of modern science and technology and industrial civilization, human demand for various resources is increasing day by day. Therefore, it is particularly significant for the development and utiliz...
Claims
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