Artemisia annua wax oil sodium copper chlorophyllin and preparation method thereof

Abstract

The invention discloses artemisia annua wax oil sodium copper chlorophyllin and a preparation method thereof. Wax oil is heated and dissolved by absolute ethyl alcohol and stands at the low temperature ranging from -15 DEG C to -5 DEG C, and then a chlorophyll ethanol solution is filtered and collected; vitriol is dropwise added to adjust the pH value to range from 2 to 3, heating reflux is carried out for 20 min to 40 min, a 10% to 20% CuSO4 solution with the volume from 1 to 2 is added into the solution, and suspended de-magging chlorophyllin copper paste sediment is separated out of the solution; the paste sediment washed by water is dissolved by acetone, a 5% sodium hydroxide-ethanol solution is added to adjust the pH value to range from 11 to 12, water bath is carried out at the temperature ranging from 50 DEG C to 70 DEG C for 1 h to 2h, and finally the artemisia annua wax oil sodium copper chlorophyllin is obtained after crystallization. The artemisia annua wax oil has abundant chlorophyll and has the development and utilization value. By means of the preparation method, sodium copper chlorophyllin can be efficiently prepared, and the product quality meets the national standard. The artemisia annua wax oil sodium copper chlorophyllin and the preparation method of the artemisia annua wax oil sodium copper chlorophyllin have the industrial development prospect, and are of important significance in improving the artemisia annua wax oil additional value, broadening the artemisia annua industrial way and protecting environment.

Description

technical field

[0001] The invention relates to a preparation method of copper chlorophyllin sodium, in particular to a method for preparing copper chlorophyllin sodium from Artemisia annua wax oil. Background technique

[0002] Artemisia annua ( Artemisia annua L . ) is an annual herb of the genus Artemisia in the family Asteraceae. It is a traditional Chinese medicine in my country. The value of its active ingredient, artemisinin, in the prevention and treatment of malaria has been recognized and accepted by humans. Artemisia annua wax oil (waxoil) is the initial purification residue of artemisinin extracted from Artemisia annua organic solvent (8# solvent oil), dark in color, strong in smell, semi-solid, rich in volatile oil, chlorophyll, sodium copper chlorophyllin, vegetable wax Such chemical components have important development value. At present, the production of 1 ton of artemisinin can produce about 5 tons of wax oil by-products. According to preliminary estimat...

Examples

Embodiment 1

[0019] (1) Extraction and impurity removal, after the wax oil is heated and dissolved in absolute ethanol, it is allowed to stand at -11°C, and the ethanol solution of chlorophyll is collected by filtration;

[0020] (2) Acidify the copper, add sulfuric acid dropwise to the chlorophyll ethanol solution to adjust the pH to 2.6, heat and reflux for 21 minutes, the solution changes from green to yellow-green, add 1.8 volumes of 19.3% CuSO 4 solution into the solution, the color of the solution changes from yellow-green to dark green, and then continue to heat and reflux for 1.4 hours, the solution precipitates a suspended paste-like precipitate, which generates demagnesified copper chlorophyllin, collects the paste-like precipitate by filtration, and washes with water;

[0021] (3) Neutralize to form a salt, dissolve the pasty precipitate after washing with water, add 5% sodium hydroxide-ethanol solution to adjust the pH to 11.2, and crystallize after 1.8 hours in a water bath at ...

Embodiment 2

[0025] (1) Extraction and impurity removal, after the wax oil is heated and dissolved in absolute ethanol, it is allowed to stand at -14.5°C, and the ethanol solution of chlorophyll is collected by filtration;

[0026] (2) Acidify the copper, add sulfuric acid dropwise to the chlorophyll ethanol solution to adjust the pH to 2.9, heat and reflux for 30 minutes, the solution changes from green to yellow-green, add 1.1 volume of 15% CuSO 4 solution into the solution, the color of the solution changes from yellow-green to dark green, then continue to heat and reflux for 1.8 hours, the solution precipitates a suspended paste-like precipitate, that is, generates demagnesified copper chlorophyllin, collects the paste-like precipitate by filtration, and washes with water;

[0027] (3) Neutralize to form a salt, dissolve the pasty precipitate after washing with acetone, add 5% sodium hydroxide-ethanol solution to adjust the pH to 11.9, crystallize after 1.5 hours in a water bath at 68°C...

Embodiment 3

[0031] (1) Extracting and removing impurities. After the wax oil is heated and dissolved in absolute ethanol, it is allowed to stand at a low temperature of -6°C, and the chlorophyll ethanol solution is collected by filtration;

[0032] (2) Acidify the copper, add dropwise sulfuric acid to the chlorophyll ethanol solution to adjust the pH to 2.1, heat and reflux for 38 minutes, the solution changes from green to yellow-green, add 1.6 volumes of 11% CuSO 4 solution into the solution, the color of the solution changes from yellow-green to dark green, then continue to heat and reflux for 1.1h, the solution precipitates a suspended paste-like precipitate, that is, generates demagnesified copper chlorophyllin, collects the paste-like precipitate by filtration, and washes with water;

[0033] (3) Neutralize to form salt, dissolve the pasty precipitate after washing with acetone, add 5% sodium hydroxide-ethanol solution to adjust pH to 11.7, crystallize after 1.1h in water bath at 50-...

technical field

[0001] The invention relates to a preparation method of copper chlorophyllin sodium, in particular to a method for preparing copper chlorophyllin sodium from Artemisia annua wax oil. Background technique

[0002] Artemisia annua ( Artemisia annua L . ) is an annual herb of the genus Artemisia in the family Asteraceae. It is a traditional Chinese medicine in my country. The value of its active ingredient, artemisinin, in the prevention and treatment of malaria has been recognized and accepted by humans. Artemisia annua wax oil (waxoil) is the initial purification residue of artemisinin extracted from Artemisia annua organic solvent (8# solvent oil), dark in color, strong in smell, semi-solid, rich in volatile oil, chlorophyll, sodium copper chlorophyllin, vegetable wax Such chemical components have important development value. At present, the production of 1 ton of artemisinin can produce about 5 tons of wax oil by-products. According to preliminary estimat...

Examples

Embodiment 1

[0019] (1) Extraction and impurity removal, after the wax oil is heated and dissolved in absolute ethanol, it is allowed to stand at -11°C, and the ethanol solution of chlorophyll is collected by filtration;

[0020] (2) Acidify the copper, add sulfuric acid dropwise to the chlorophyll ethanol solution to adjust the pH to 2.6, heat and reflux for 21 minutes, the solution changes from green to yellow-green, add 1.8 volumes of 19.3% CuSO 4 solution into the solution, the color of the solution changes from yellow-green to dark green, and then continue to heat and reflux for 1.4 hours, the solution precipitates a suspended paste-like precipitate, which generates demagnesified copper chlorophyllin, collects the paste-like precipitate by filtration, and washes with water;

[0021] (3) Neutralize to form a salt, dissolve the pasty precipitate after washing with water, add 5% sodium hydroxide-ethanol solution to adjust the pH to 11.2, and crystallize after 1.8 hours in a water bath at ...

Embodiment 2

[0025] (1) Extraction and impurity removal, after the wax oil is heated and dissolved in absolute ethanol, it is allowed to stand at -14.5°C, and the ethanol solution of chlorophyll is collected by filtration;

[0026] (2) Acidify the copper, add sulfuric acid dropwise to the chlorophyll ethanol solution to adjust the pH to 2.9, heat and reflux for 30 minutes, the solution changes from green to yellow-green, add 1.1 volume of 15% CuSO 4 solution into the solution, the color of the solution changes from yellow-green to dark green, then continue to heat and reflux for 1.8 hours, the solution precipitates a suspended paste-like precipitate, that is, generates demagnesified copper chlorophyllin, collects the paste-like precipitate by filtration, and washes with water;

[0027] (3) Neutralize to form a salt, dissolve the pasty precipitate after washing with acetone, add 5% sodium hydroxide-ethanol solution to adjust the pH to 11.9, crystallize after 1.5 hours in a water bath at 68°C...

Embodiment 3

[0031] (1) Extracting and removing impurities. After the wax oil is heated and dissolved in absolute ethanol, it is allowed to stand at a low temperature of -6°C, and the chlorophyll ethanol solution is collected by filtration;

[0032] (2) Acidify the copper, add dropwise sulfuric acid to the chlorophyll ethanol solution to adjust the pH to 2.1, heat and reflux for 38 minutes, the solution changes from green to yellow-green, add 1.6 volumes of 11% CuSO 4 solution into the solution, the color of the solution changes from yellow-green to dark green, then continue to heat and reflux for 1.1h, the solution precipitates a suspended paste-like precipitate, that is, generates demagnesified copper chlorophyllin, collects the paste-like precipitate by filtration, and washes with water;

[0033] (3) Neutralize to form salt, dissolve the pasty precipitate after washing with acetone, add 5% sodium hydroxide-ethanol solution to adjust pH to 11.7, crystallize after 1.1h in water bath at 50-...