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 覃李梅 邓月园 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。本发明提供的方法包括以下步骤：将青蒿蜡油与脱油试剂混合后进行脱油处理,得到脱油青蒿蜡；将所述脱油青蒿蜡、水与盐酸混合后进行除灰处理,得到除灰青蒿蜡；将所述除灰青蒿蜡与脱色剂混合后进行脱色处理,得到精制青蒿蜡。本发明首先利用脱油试剂与青蒿蜡油进行脱油处理,能够有效脱除青蒿蜡油中的脂肪类脂物和树脂类脂物等物质；然后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；最后对除灰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。(The invention relates to the technical field of plant wax refining, in particular to a method for refining sweet wormwood wax. The method provided by the invention comprises the following steps: mixing sweet wormwood wax oil and a deoiling reagent, and then performing deoiling treatment to obtain deoiled sweet wormwood wax; mixing the deoiled sweet wormwood wax, water and hydrochloric acid, and then performing ash removal treatment to obtain ash-removed sweet wormwood wax; and mixing the ash-removed sweet wormwood wax with a decoloring agent, and then decoloring to obtain refined sweet wormwood wax. The method comprises the following steps of firstly, carrying out deoiling treatment on the sweet wormwood wax oil by using a deoiling reagent, so that the substances such as fatty lipid, resin lipid and the like in the sweet wormwood wax oil can be effectively removed; then performing ash removal treatment on the sweet wormwood herb wax oil by using a hydrochloric acid hydration method, so that ash in the sweet wormwood herb wax oil can be effectively removed; and finally, the ash-removed sweet wormwood wax is subjected to decoloration treatment, so that the deep processing value of the obtained refined sweet wormwood wax is favorably improved.)

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

mixing sweet wormwood wax oil and a deoiling reagent, and then performing deoiling treatment to obtain deoiled sweet wormwood wax;

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

and mixing the ash-removed sweet wormwood wax with a decoloring agent, and then decoloring to obtain refined sweet wormwood wax.

2. The refining process of claim 1, wherein the deoiling agent comprises petroleum ether, ethyl acetate, acetone, or n-heptane.

3. The refining method of claim 1 or 2, wherein the dosage ratio of the sweet wormwood wax oil to the deoiling agent is 1 g: (2-10) mL.

4. The refining method according to claim 1, wherein the deoiling treatment is performed at a temperature of 20 to 25 ℃ for 10 to 50 min.

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

6. 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.

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

8. The refining method of claim 7, wherein the dosage ratio of ash-removed sweet wormwood wax to decolorant is 1 g: (0.1-0.4) mL.

9. The refining method according to claim 1, wherein the temperature of the decoloring is 75 to 85 ℃ 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 refine sweet wormwood wax oil, has good deoiling, deashing and decoloring effects and meets the refining requirement.

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 and a deoiling reagent, and then performing deoiling treatment to obtain deoiled sweet wormwood wax;

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

and mixing the ash-removed sweet wormwood wax with a decoloring agent, and then decoloring to obtain refined sweet wormwood wax.

Preferably, the de-oiling agent comprises petroleum ether, ethyl acetate, acetone or n-heptane.

Preferably, the dosage ratio of the sweet wormwood wax oil to the deoiling reagent is 1 g: (2-10) mL.

Preferably, the deoiling treatment is carried out at the temperature of 20-25 ℃ for 10-50 min.

Preferably, the mass concentration of the hydrochloric acid is 30.0-36.5%, and the dosage ratio of the deoiled sweet wormwood wax, 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 decoloring agent comprises hydrogen peroxide, and the mass concentration of the hydrogen peroxide is 25-30%.

Preferably, the dosage ratio of the ash-removing sweet wormwood wax to the decolorizing agent is 1 g: (0.1-0.4) mL.

Preferably, the temperature of the decoloring treatment is 75-85 ℃, 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 and a deoiling reagent, and then performing deoiling treatment to obtain deoiled sweet wormwood wax; mixing the deoiled sweet wormwood wax, water and hydrochloric acid, and then performing ash removal treatment to obtain ash-removed sweet wormwood wax; and mixing the ash-removed sweet wormwood wax with a decoloring agent, and then decoloring to obtain refined sweet wormwood wax. The method comprises the following steps of firstly, carrying out deoiling treatment on the sweet wormwood wax oil by using a deoiling reagent, so that the substances such as fatty lipid, resin lipid and the like in the sweet wormwood wax oil can be effectively removed; then performing ash removal treatment on the sweet wormwood herb wax oil by using a hydrochloric acid hydration method, so that ash in the sweet wormwood herb wax oil can be effectively removed; and finally, the ash-removed sweet wormwood wax is subjected to decoloration treatment, so that the deep processing value of the obtained refined sweet wormwood wax is favorably improved. The results of the examples show that the method provided by the invention has good deoiling, ash removing and decoloring effects when used for refining the sweet wormwood wax oil, and the obtained refined sweet wormwood wax has an acid value of 19.6, a saponification value of 52.3 and an iodine value of 11.2, and meets the refining requirements.

Drawings

Fig. 1 to 4 are color grade charts of artemisia apiacea wax before and after decolorization treatment, wherein fig. 1 is light yellow, fig. 2 is yellow, fig. 3 is yellow brown, and fig. 4 is dark brown.

Detailed Description

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

mixing sweet wormwood wax oil and a deoiling reagent, and then performing deoiling treatment to obtain deoiled sweet wormwood wax;

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

and mixing the ash-removed sweet wormwood wax with 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.

The invention mixes the sweet wormwood wax oil and the deoiling reagent and then carries out deoiling treatment to obtain the deoiled 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 present invention, the deoiling agent preferably includes petroleum ether, ethyl acetate, acetone or n-heptane; the preferred petroleum ether is petroleum ether with a boiling range of 30-60 ℃ or petroleum ether with a boiling range of 60-90 ℃. In the invention, the dosage ratio of the sweet wormwood wax oil to the deoiling reagent is preferably 1 g: (2-10) mL, more preferably 1 g: (6-8) mL.

In the invention, the deoiling treatment temperature is preferably 20-25 ℃, the time is preferably 10-50 min, and more preferably 20-30 min. In the invention, the deoiling treatment is preferably carried out under the condition of stirring, and the stirring speed is preferably 3000-3500 r/min.

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

After the deoiling treatment is finished, the solvent-containing wax is preferably dried in vacuum at the temperature of 50-60 ℃ to constant weight to obtain the deoiled sweet wormwood wax.

In the invention, in the deoiling treatment process, the deoiling reagent is selected according to the solubility characteristics of the sweet wormwood wax and other lipid substances, so that the fat lipid, resin lipid and other substances in the sweet wormwood wax oil can be fully removed, and the high-purity sweet wormwood wax can be obtained.

After the deoiled sweet wormwood wax is obtained, the deoiled sweet wormwood wax, water and hydrochloric acid are mixed and then subjected to ash removal treatment to obtain the ash removal sweet wormwood wax. In the invention, the mass concentration of the hydrochloric acid is preferably 30.0-36.5%, and the dosage ratio of the deoiled sweet wormwood wax, 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 deoiled sweet wormwood wax, water and hydrochloric acid are preferably mixed, the deoiled sweet wormwood wax and the water are heated to 85-95 ℃ to dissolve 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 3800-4000 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 removal sweet wormwood wax) in a molten state, which is beneficial to fully removing the acid contained in the filter cake and ensuring the subsequent decolorization treatment to be carried out smoothly.

In the invention, the de-oiled sweet wormwood wax contains impurities such as colloid ash which is mainly calcium salt and phospholipid and affects the purity, color and performance of the product.

After the ash-removed sweet wormwood wax is obtained, the ash-removed 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 dosage ratio of the ash-removing sweet wormwood wax to the decolorizing agent is preferably 1 g: (0.1-0.4) mL, more preferably 1 g: (0.2-0.3) mL. In the invention, the ash-removed sweet wormwood wax is yellow, and needs to be decolored in order to improve the value of deep processing; because the ash-removed 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.

In the invention, the decoloring treatment is preferably carried out in the presence of an organic solvent, and more preferably, the ash-removed sweet wormwood wax is mixed with the organic solvent, heated to 45-50 ℃ to completely dissolve the ash-removed sweet wormwood wax, and then added with a decoloring agent for decoloring treatment; in the present invention, the organic solvent is preferably colorless gasoline; the dosage ratio of the ash-removing sweet wormwood wax to the organic solvent is preferably 2 g: (10-20) mL, more preferably 2 g: (15-20) mL.

In the invention, the temperature of the decolorization treatment is preferably 60-90 ℃, and more preferably 70-90 ℃; the time is preferably 30 to 120min, and more preferably 60 to 90 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.