阅读说明：本技术 青蒿蜡的精制方法 (Method for refining sweet wormwood wax ) 是由 蒙衍强 邓月园 覃李梅 于 2019-03-08 设计创作，主要内容包括：本发明涉及植物蜡精制技术领域,具体涉及一种青蒿蜡的精制方法。本发明利用盐酸水化法对青蒿蜡油进行除灰处理,能够有效去除其中的灰分,保证后续提取处理顺利进行；然后对所得除灰青蒿蜡进行提取,对所得含溶剂蜡进行蒸馏,能够充分脱除除灰青蒿蜡中的脂肪类脂物和树脂类脂物等物质,并去除含溶剂蜡中的溶剂,有利于获得纯度较高的青蒿蜡；最后对脱脂青蒿蜡进行脱色处理,有利于提高所得精制青蒿蜡的深加工价值。实施例的结果显示,采用本发明提供的方法对青蒿蜡油进行精制,所得精制青蒿蜡产率高、白度高。(The invention relates to the technical field of plant wax refining, in particular to a method for refining sweet wormwood wax. According to the method, the sweet wormwood wax oil is subjected to ash removal treatment by using a hydrochloric acid hydration method, so that ash in the sweet wormwood wax oil can be effectively removed, and the subsequent extraction treatment is guaranteed to be smoothly carried out; then extracting the ash-removed sweet wormwood wax, distilling the obtained solvent-containing wax, fully removing substances such as fatty lipid, resin lipid and the like in the ash-removed sweet wormwood wax, and removing the solvent in the solvent-containing wax, thereby being beneficial to obtaining the sweet wormwood wax with higher purity; and finally, the degreased sweet wormwood wax is decolorized, which is beneficial to improving the deep processing value of the obtained refined sweet wormwood wax. The results of the examples show that the refined sweet wormwood wax oil refined by the method provided by the invention has high yield and high whiteness.)

1. A method for refining sweet wormwood wax comprises the following steps:

mixing sweet wormwood wax oil, water and hydrochloric acid, and then performing ash removal treatment to obtain ash-removed sweet wormwood wax;

mixing the ash-removed sweet wormwood wax with an extraction reagent, then carrying out extraction treatment, and distilling the obtained solvent-containing wax to obtain degreased sweet wormwood wax;

and mixing the degreased sweet wormwood wax and a decoloring agent, and then decoloring to obtain refined sweet wormwood wax.

2. The refining method as claimed in claim 1, wherein the mass concentration of the hydrochloric acid is 30.0-36.5%, and the ratio of the amount of the sweet wormwood wax oil, the amount of water and the amount of hydrochloric acid is 1 g: (2-4) mL: (1-3) mL.

3. The refining method according to claim 1, wherein the temperature of the ash removal treatment is 85 to 95 ℃ and the time is 40 to 80 min.

4. The refining method of claim 1, wherein the extraction reagent comprises ethyl acetate, aqueous ethanol, isopropanol, or methanol; the mass concentration of the ethanol water solution is 90-98%.

5. The refining method as claimed in claim 1 or 4, wherein the dosage ratio of the ash-removed sweet wormwood wax to the extraction reagent is 1 g: (4-12) mL.

6. The refining method according to claim 1, wherein the temperature of the extraction treatment is 25 to 45 ℃ and the time is 20 to 100 min.

7. The refining method of claim 1, wherein the distillation is performed under a vacuum condition of not more than-750 mmHg.

8. The refining method of claim 1, wherein the decolorant comprises hydrogen peroxide, and the mass concentration of the hydrogen peroxide is 25-30%.

9. The refining method of claim 8, wherein the ratio of the amount of defatted artemisia apiacea wax to the amount of the decolorizer is 3 g: (0.6-1.0) mL.

10. The refining method according to claim 1, wherein the temperature of the decoloring is 85 to 95 ℃ and the time is 50 to 70 min.

Technical Field

The invention relates to the technical field of plant wax refining, in particular to a method for refining sweet wormwood wax.

Background

The artemisinin is applied to the prevention and treatment of malaria, and the effect is excellent. The Artemisia annua L for extracting artemisinin is distributed in various parts of the country, and can grow in hillside, wasteland, forest edge and other areas. The sweet wormwood wax oil (also called sweet wormwood wax crude product) is a primary purified residue of sweet wormwood extracted by an organic solvent, has yellow brown color, fragrant smell and semi-solid state, contains a large amount of chlorophyll, volatile oil, fatty acid, sweet wormwood wax and other organic chemical components, and has high research value. To date, about five tons of sweet wormwood wax oil can be produced by 1 ton of artemisinin, and through preliminary estimation, the sweet wormwood wax oil produced by China every year is about 1000 tons when the artemisinin is produced. However, systematic research on the artemisia apiacea wax oil is not carried out in the artemisinin industry, comprehensive development and utilization are not carried out, most of the artemisia apiacea wax oil is treated as waste, so that serious resource waste is caused, and a series of severe environmental problems are brought. Therefore, in order to avoid environmental pollution, increase the additional value of the artemisia apiacea wax oil and reasonably utilize the artemisia apiacea wax resource, the artemisia apiacea wax oil needs to be refined and researched.

Disclosure of Invention

The invention aims to provide a method for refining sweet wormwood wax, which can be used for refining sweet wormwood wax oil, and the obtained refined sweet wormwood wax has high yield and high whiteness.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a method for refining sweet wormwood wax, which comprises the following steps:

mixing sweet wormwood wax oil, water and hydrochloric acid, and then performing ash removal treatment to obtain ash-removed sweet wormwood wax;

mixing the ash-removed sweet wormwood wax with an extraction reagent, then carrying out extraction treatment, and distilling the obtained solvent-containing wax to obtain degreased sweet wormwood wax;

and mixing the degreased sweet wormwood wax and a decoloring agent, and then decoloring to obtain refined sweet wormwood wax.

Preferably, the mass concentration of the hydrochloric acid is 30.0-36.5%, and the dosage ratio of the sweet wormwood wax oil, the water and the hydrochloric acid is 1 g: (2-4) mL: (1-3) mL.

Preferably, the ash removal treatment temperature is 85-95 ℃ and the time is 40-80 min.

Preferably, the extraction reagent comprises ethyl acetate, aqueous ethanol, isopropanol or methanol; the mass concentration of the ethanol water solution is 90-98%.

Preferably, the dosage ratio of the ash-removing sweet wormwood wax to the extraction reagent is 1 g: (4-12) mL.

Preferably, the temperature of the extraction treatment is 25-45 ℃ and the time is 20-100 min.

Preferably, the distillation is performed under a vacuum condition of not more than-750 mmHg.

Preferably, the decoloring agent comprises hydrogen peroxide, and the mass concentration of the hydrogen peroxide is 25-30%.

Preferably, the dosage ratio of the degreased sweet wormwood wax to the decoloring agent is 3 g: (0.6-1.0) mL.

Preferably, the temperature of the decoloring treatment is 85-95 ℃, and the time is 50-70 min.

The invention provides a method for refining sweet wormwood wax, which comprises the following steps: mixing sweet wormwood wax oil, water and hydrochloric acid, and then performing ash removal treatment to obtain ash-removed sweet wormwood wax; mixing the ash-removed sweet wormwood wax with an extraction reagent, then carrying out extraction treatment, and distilling the obtained solvent-containing wax to obtain degreased sweet wormwood wax; and mixing the degreased sweet wormwood wax and a decoloring agent, and then decoloring to obtain refined sweet wormwood wax. According to the method, the sweet wormwood wax oil is subjected to ash removal treatment by using a hydrochloric acid hydration method, so that ash in the sweet wormwood wax oil can be effectively removed, and the subsequent extraction treatment is guaranteed to be smoothly carried out; then extracting the ash-removed sweet wormwood wax, distilling the obtained solvent-containing wax, fully removing substances such as fatty lipid, resin lipid and the like in the ash-removed sweet wormwood wax, and removing the solvent in the solvent-containing wax, thereby being beneficial to obtaining the sweet wormwood wax with higher purity; and finally, the degreased sweet wormwood wax is decolorized, which is beneficial to improving the deep processing value of the obtained refined sweet wormwood wax. The results of the examples show that the refined sweet wormwood wax oil refined by the method provided by the invention has high yield and high whiteness.

Drawings

FIG. 1 is a schematic representation of defatted sweet wormwood wax of example 1;

FIG. 2 is a schematic representation of the purified Artemisia annua wax of example 1.

Detailed Description

The invention provides a method for refining sweet wormwood wax, which comprises the following steps:

mixing sweet wormwood wax oil, water and hydrochloric acid, and then performing ash removal treatment to obtain ash-removed sweet wormwood wax;

mixing the ash-removed sweet wormwood wax with an extraction reagent, then carrying out extraction treatment, and distilling the obtained solvent-containing wax to obtain degreased sweet wormwood wax;

and mixing the degreased sweet wormwood wax and a decoloring agent, and then decoloring to obtain refined sweet wormwood wax.

In the invention, the sweet wormwood wax oil contains waxy lipoid (sweet wormwood wax), fatty lipoid, resin lipoid, mechanical impurities, water, pigment components, colloid ash which takes calcium salt and phospholipid as main components, and other impurities, and after the sweet wormwood wax is refined by the method provided by the invention, the main component of the refined sweet wormwood wax is the sweet wormwood wax, and the rest components are removed.

According to the invention, the ash removal treatment is carried out after sweet wormwood wax oil, water and hydrochloric acid are mixed, so as to obtain the ash removal sweet wormwood wax. The source of the sweet wormwood wax oil is not particularly limited, and the sweet wormwood wax oil generated in the process of extracting the artemisinin and known by the technical personnel in the field can be adopted; in the embodiment of the invention, the sweet wormwood wax oil generated in the process of extracting artemisinin by Guangxi Mesona Tang pharmaceutical industry Co. In the invention, the mass concentration of the hydrochloric acid is preferably 30.0-36.5%, and the dosage ratio of the sweet wormwood wax oil, the water and the hydrochloric acid is preferably 1 g: (2-4) mL: (1-3) mL, more preferably 1 g: 3mL of: 1 mL.

In the invention, the sweet wormwood wax oil, the water and the hydrochloric acid are preferably mixed, the sweet wormwood wax oil and the water are heated to 85-95 ℃ to dissolve the sweet wormwood wax oil in the water, and then the hydrochloric acid is added; the mixing mode is favorable for fully mixing all the components, and ensures that the subsequent ash removal treatment is smoothly carried out.

In the invention, the ash removal treatment temperature is preferably 85-95 ℃, and more preferably 90-95 ℃; the time is preferably 40 to 80min, and more preferably 60 to 80 min.

In the present invention, the ash removal treatment is preferably performed under stirring conditions; the stirring speed is preferably 3500-4500 r/min, and more preferably 4000 r/min. The invention is beneficial to the full interaction of all components under the condition of rapid stirring, and ensures the efficient operation of ash removal treatment.

After the ash removal treatment is completed, the obtained system is preferably cooled and subjected to suction filtration, the obtained filter cake is washed to be neutral by using boiling water, and the obtained filter cake is dried in vacuum at the temperature of 50-60 ℃ to be constant in weight, so that the ash-removed sweet wormwood wax is obtained. The invention adopts boiling water to wash the filter cake (ash-removed sweet wormwood wax) in a molten state, which is beneficial to fully removing the acid contained in the filter cake and ensuring the subsequent extraction treatment to be carried out smoothly.

In the invention, the existence of impurities such as colloid ash which is mainly calcium salt and phospholipid and the like in the sweet wormwood herb wax oil can influence the purity, color and performance of the product.

After the ash-removed sweet wormwood wax is obtained, the ash-removed sweet wormwood wax and an extraction reagent are mixed and then are subjected to extraction treatment, and the obtained solvent-containing wax is distilled to obtain the degreased sweet wormwood wax. In the invention, the extraction reagent preferably comprises ethyl acetate, ethanol water solution (the mass concentration is preferably 90-95%), isopropanol or methanol, and more preferably methanol; the dosage ratio of the ash-removing sweet wormwood wax to the extraction reagent is preferably 1 g: (4-12) mL, more preferably 1 g: (4-6) mL. In the invention, the temperature of the extraction treatment is preferably 25-45 ℃, and more preferably 35-40 ℃; the time is preferably 20 to 100min, and more preferably 40 to 60 min.

In the present invention, the extraction treatment is preferably performed under ultrasonic conditions; the power of the ultrasonic wave is preferably 500-1000W, and more preferably 800-1000W.

In the present invention, the number of times of the extraction treatment is preferably 1 to 4 times, and more preferably 2 to 3 times. In the present invention, when the number of times of the extraction treatment exceeds 1, it is preferable that the system obtained after the extraction treatment is subjected to centrifugal separation to obtain an oil-containing solvent (the oil-containing solvent can be further distilled and separated after recovery to obtain a fatty oil and a solvent for reuse) and a solvent-containing wax, and the solvent-containing wax is mixed with an extraction reagent and then subjected to the next extraction treatment in the manner described above. In the invention, the rotation speed of centrifugal separation is preferably 3000-3500 r/min, and the time is preferably 10-15 min.

In the extraction treatment process, the extraction reagent is selected according to the dissolution characteristics of the artemisia apiacea wax and other lipid substances, so that the fat lipid substances, the resin lipid substances and other substances in the artemisia apiacea wax can be fully removed, and the artemisia apiacea wax with high purity can be obtained.

After the extraction treatment is finished, the solvent-containing wax is distilled to obtain the degreased sweet wormwood wax. In the present invention, the distillation is preferably performed under a vacuum condition of not more than-750 mmHg; the distillation is preferably carried out in a rotary thin film evaporator. The solvent in the solvent-containing wax is removed by distillation to obtain the degreased sweet wormwood wax.

After the degreased sweet wormwood wax is obtained, the degreased sweet wormwood wax is mixed with a decoloring agent and then is subjected to decoloring treatment, so that the refined sweet wormwood wax is obtained. In the invention, the decoloring agent preferably comprises hydrogen peroxide, and the mass concentration of the hydrogen peroxide is preferably 25-30%; the preferable dosage ratio of the degreased sweet wormwood wax to the decoloring agent is 3 g: (0.6-1.0) mL. In the invention, the degreased sweet wormwood wax is yellow, and needs to be decolored to improve the value of deep processing; because the degreased sweet wormwood wax has high viscosity and is solid, if a solid decoloring agent (such as active carbon or diatomite) is used for decoloring, the decoloring effect is poor, and the separation and removal operation after decoloring is inconvenient, the invention adopts hydrogen peroxide as the decoloring agent, can ensure that the whiteness of the obtained refined sweet wormwood wax reaches 39.8 percent, and has simple post-treatment operation.

In the invention, the decolorization treatment is preferably carried out in the presence of an organic solvent, more preferably, the defatted sweet wormwood wax is mixed with the organic solvent, heated to 45-50 ℃ to completely dissolve the defatted sweet wormwood wax, and then a decolorizing agent is added for decolorization treatment; in the present invention, the organic solvent is preferably colorless gasoline; the preferable dosage ratio of the degreased sweet wormwood wax to the organic solvent is 3 g: (15-30) mL, more preferably 3 g: (20-25) mL.

In the invention, the temperature of the decolorization treatment is preferably 85-95 ℃, and more preferably 90-95 ℃; the time is preferably 50 to 70min, and more preferably 50 to 60 min.

In the present invention, the decoloring treatment is preferably performed under stirring conditions; the stirring speed is preferably 1500-2000 r/min.

After the decoloring treatment is completed, the obtained system is preferably cooled, the system is layered to form a water phase and a solid substance, the solid substance is washed for 3-5 times by using boiling water, and then the solid substance is dried in vacuum at the temperature of 50-60 ℃ to constant weight, so that the refined sweet wormwood wax is obtained. The invention adopts boiling water to wash the solid substance (sweet wormwood wax) in a melting state, which is beneficial to fully removing the impurities such as solvent and the like contained in the solid substance and improving the purity of the solid substance.

The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.