Purification method of dehydroabietic acid

Abstract

The invention relates to a purification method of dehydroabietic acid, and belongs to the field of chemical engineering. The method is characterized in that disproportionated rosin and absolute ethyl alcohol are mixed to open a special field; 2-neovaricaine with the same quantity as the disproportionated rosin is slowly dripped to perform reaction; after the reaction is finished, water with the same temperature and quantity as a solvent is added. After crystallization for a certain time, preheated petroleum ether is used for extraction while being hot until the ether layer is colourless; cooling and crystallization are performed; suction filtration is performed to obtain a dehydroabietic acid neovaricaine salt coarse body; ethyl alcohol is used for recrystallization to obtain a dehydroabietic acid neovaricaine salt crystal; amine salt is dissolved into the ethyl alcohol; hydrochloric acid is used for acidification until the pH is smaller than 4; a proper amount of distilled water is added for crystallization; cooling and suction filtration are performed to obtain a dehydroabietic acid crude product; the ethyl alcohol is used for recrystallization for 1 to 4 times; suction filtration and drying are performed to obtain a dehydroabietic acid crystal. The method has the advantages that the reaction temperature is lower; the reaction time is shorter; the energy consumption is reduced; the recrystallization time is short; the recrystallization times are few; the whole reaction period is shortened; the product purity reaches up to 98 percent or above.

Description

technical field

[0001] The invention relates to a method for purifying dehydroabietic acid, in particular to a method for purifying dehydroabietic acid assisted by a special field, and belongs to the field of chemical industry. Background technique

[0002] For nearly half a century, the utilization of rosin has been continuously developed from primary products to deep-processed products. Disproportionated rosin is a modified product with a large output and a wide range of uses among rosin deep-processing products. It has the characteristics of high thermal stability, good oxidation resistance, light color, and low brittleness. It has a wide range of applications in industries such as surfactants and fine chemicals, and has achieved considerable results.

[0003] Dehydroabietic acid is one of the main components of disproportionated rosin. It is stable in nature and has a large specific rotation. It is a stable structure containing a tricyclic phenanthrene skeleton structur...

Examples

Embodiment 1

[0026] (1) Add disproportionated rosin to absolute ethanol at a ratio of 0.5g / ml, mix and dissolve under the auxiliary field of microwave and ultraviolet integration at 60°C, and cool to room temperature to obtain a mixed solution;

[0027] (2) Turn on the auxiliary field for microwave-ultraviolet integration, slowly add 2-ethanolamine to the mixed solution with a dropping funnel for reaction, wherein the molar ratio of 2-ethanolamine to disproportionated rosin is 1:1, the reaction temperature is 60°C, and the reaction time is 10min, add isothermal and equal amount of water with absolute ethanol after the reaction finishes;

[0028] (3) After rapid crystallization, extract twice while hot with preheated (60°C) petroleum ether until the ether layer is colorless, cool and crystallize the extract in the lower layer, and filter with suction to obtain the crude dehydroabietic acid ethanolamine salt;

[0029] (4) Recrystallize the crude dehydroabietic acid ethanolamine salt with 10%...

Embodiment 2

[0037] (1) Add disproportionated rosin to absolute ethanol at a ratio of 0.1g / ml, mix and dissolve under the auxiliary field of microwave and ultraviolet integration at 50°C, and cool to room temperature to obtain a mixed solution;

[0038] (2) Turn on the auxiliary field for microwave-ultraviolet integration, slowly add 2-ethanolamine to the mixed solution with a dropping funnel for reaction, wherein the molar ratio of 2-ethanolamine to disproportionated rosin is 2:1, the reaction temperature is 50°C, and the reaction time is 20min, add isothermal and equal amount of water with absolute ethanol after the reaction finishes;

[0039] (3) After rapid crystallization, extract twice while hot with preheated (50°C) petroleum ether until the ether layer is colorless, cool and crystallize the extract in the lower layer, and filter with suction to obtain the crude dehydroabietic acid ethanolamine salt;

[0040] (4) Recrystallize the crude dehydroabietic acid ethanolamine salt with 80%...

Embodiment 3

[0048] (1) Add disproportionated rosin to absolute ethanol at a ratio of 1g / ml, mix and dissolve under the auxiliary field of microwave and ultraviolet integration at 75°C, and cool to room temperature to obtain a mixed solution;

[0049] (2) Turn on the auxiliary field for microwave-ultraviolet integration, slowly add 2-ethanolamine into the mixed solution with a dropping funnel for reaction, wherein the molar ratio of 2-ethanolamine to disproportionated rosin is 3:1, the reaction temperature is 75°C, and the reaction time is 5min, add isothermal and equal amount of water with absolute ethanol after the reaction finishes;

[0050] (3) After rapid crystallization, extract twice while hot with preheated (75°C) petroleum ether until the ether layer is colorless, cool and crystallize the extract in the lower layer, and filter with suction to obtain the crude dehydroabietic acid ethanolamine salt;

[0051] (4) Recrystallize the crude dehydroabietic acid ethanolamine salt with 40% ...

technical field

[0001] The invention relates to a method for purifying dehydroabietic acid, in particular to a method for purifying dehydroabietic acid assisted by a special field, and belongs to the field of chemical industry. Background technique

[0002] For nearly half a century, the utilization of rosin has been continuously developed from primary products to deep-processed products. Disproportionated rosin is a modified product with a large output and a wide range of uses among rosin deep-processing products. It has the characteristics of high thermal stability, good oxidation resistance, light color, and low brittleness. It has a wide range of applications in industries such as surfactants and fine chemicals, and has achieved considerable results.

[0003] Dehydroabietic acid is one of the main components of disproportionated rosin. It is stable in nature and has a large specific rotation. It is a stable structure containing a tricyclic phenanthrene skeleton structur...

Examples

Embodiment 1

[0026] (1) Add disproportionated rosin to absolute ethanol at a ratio of 0.5g / ml, mix and dissolve under the auxiliary field of microwave and ultraviolet integration at 60°C, and cool to room temperature to obtain a mixed solution;

[0027] (2) Turn on the auxiliary field for microwave-ultraviolet integration, slowly add 2-ethanolamine to the mixed solution with a dropping funnel for reaction, wherein the molar ratio of 2-ethanolamine to disproportionated rosin is 1:1, the reaction temperature is 60°C, and the reaction time is 10min, add isothermal and equal amount of water with absolute ethanol after the reaction finishes;

[0028] (3) After rapid crystallization, extract twice while hot with preheated (60°C) petroleum ether until the ether layer is colorless, cool and crystallize the extract in the lower layer, and filter with suction to obtain the crude dehydroabietic acid ethanolamine salt;

[0029] (4) Recrystallize the crude dehydroabietic acid ethanolamine salt with 10%...

Embodiment 2

[0037] (1) Add disproportionated rosin to absolute ethanol at a ratio of 0.1g / ml, mix and dissolve under the auxiliary field of microwave and ultraviolet integration at 50°C, and cool to room temperature to obtain a mixed solution;

[0038] (2) Turn on the auxiliary field for microwave-ultraviolet integration, slowly add 2-ethanolamine to the mixed solution with a dropping funnel for reaction, wherein the molar ratio of 2-ethanolamine to disproportionated rosin is 2:1, the reaction temperature is 50°C, and the reaction time is 20min, add isothermal and equal amount of water with absolute ethanol after the reaction finishes;

[0039] (3) After rapid crystallization, extract twice while hot with preheated (50°C) petroleum ether until the ether layer is colorless, cool and crystallize the extract in the lower layer, and filter with suction to obtain the crude dehydroabietic acid ethanolamine salt;

[0040] (4) Recrystallize the crude dehydroabietic acid ethanolamine salt with 80%...

Embodiment 3

[0048] (1) Add disproportionated rosin to absolute ethanol at a ratio of 1g / ml, mix and dissolve under the auxiliary field of microwave and ultraviolet integration at 75°C, and cool to room temperature to obtain a mixed solution;

[0049] (2) Turn on the auxiliary field for microwave-ultraviolet integration, slowly add 2-ethanolamine into the mixed solution with a dropping funnel for reaction, wherein the molar ratio of 2-ethanolamine to disproportionated rosin is 3:1, the reaction temperature is 75°C, and the reaction time is 5min, add isothermal and equal amount of water with absolute ethanol after the reaction finishes;

[0050] (3) After rapid crystallization, extract twice while hot with preheated (75°C) petroleum ether until the ether layer is colorless, cool and crystallize the extract in the lower layer, and filter with suction to obtain the crude dehydroabietic acid ethanolamine salt;

[0051] (4) Recrystallize the crude dehydroabietic acid ethanolamine salt with 40% ...

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