阅读说明：本技术 一种含有有机酸的液态牛至香酚制备方法及制备装置 (Preparation method and preparation device of liquid oregano phenol containing organic acid ) 是由 胡进成 王芝丽 杨军 邹同高 涂勋亮 于 2021-07-10 设计创作，主要内容包括：本发明涉及畜牧兽药生产制备技术领域,具体公开了一种含有有机酸的液态牛至香酚制备方法及制备装置,通过取牛至进行破碎,得到渣料,之后向提取罐内的纯化水中加入渣料进行浸泡；待浸泡完成后加入有机酸,然后将蒸汽加入提取罐内,进行第一次提纯处理,得到提纯液和残渣；排出提取罐内的提纯液,进行冷却,得到牛至挥发油混合液；向残渣中加入乙醇,将蒸汽再次通入提取罐中,进行第二次提纯处理,得到牛至挥发油醇溶液；混合牛至挥发油混合液和牛至挥发油醇溶液,之后进行油水分离处理,得到液态牛至香酚。通过对破碎后的牛至进行浸泡,以及进行两次提纯处理,以此提高牛至香酚的纯度。(The invention relates to the technical field of animal remedy production and preparation, and particularly discloses a preparation method and a preparation device of liquid oregano phenol containing organic acid, wherein oregano is taken and crushed to obtain slag, and then the slag is added into purified water in an extraction tank for soaking; after soaking, adding organic acid, then adding steam into an extraction tank, and carrying out primary purification treatment to obtain a purified liquid and residues; discharging the purified liquid in the extraction tank, and cooling to obtain volatile oil mixed solution of origanum vulgaris; adding ethanol into the residue, introducing the steam into the extraction tank again, and performing secondary purification treatment to obtain Oregano volatile oil alcoholic solution; mixing the origanum volatile oil mixed solution and the origanum volatile oil alcohol solution, and then carrying out oil-water separation treatment to obtain liquid origanum carvacrol. The purity of the oregano phenol is improved by soaking the crushed oregano and carrying out purification treatment twice.)

1. A method for preparing liquid oregano phenol containing organic acid is characterized by comprising the following steps:

crushing origanum vulgare to obtain slag, and then adding the slag into purified water in an extraction tank for soaking;

after soaking, adding organic acid, then adding steam into the extraction tank, and carrying out first purification treatment to obtain a purified liquid and residues;

discharging the purified liquid in the extraction tank, and cooling to obtain an origanum volatile oil mixed liquid;

adding ethanol into the residue, introducing the steam into the extraction tank again, and performing secondary purification treatment to obtain an origanum volatile oil alcoholic solution;

and mixing the origanum volatile oil mixed solution and the origanum volatile oil alcohol solution, and then carrying out oil-water separation treatment to obtain liquid origanum carvacrol.

2. The method of preparing liquid oregano phenol containing organic acid according to claim 1, wherein the step of adding the slag to the purified water in the extraction tank for soaking comprises:

the soaking time is 8-12 hours.

3. The method of claim 1, wherein the organic acid is one or more of methanesulfonic acid, oxalic acid, acetic acid, and citric acid.

4. The method of claim 1, wherein the first purification step comprises:

and raising the temperature in the extraction tank to 110-130 ℃, pressurizing to 0.3-0.5 MPa, and then carrying out hot reflux for 8-10 hours.

5. The method of producing organic acid-containing liquid oregano phenol according to claim 1, wherein in the step of discharging the purified liquid in the extraction tank and cooling:

and cooling by using a cooler.

6. The method of claim 1, wherein the second purification step comprises:

and raising the temperature in the extraction tank to 100-130 ℃, pressurizing to 0.4-0.5 MPa, and then carrying out hot reflux for 6-8 hours.

7. The apparatus for producing organic acid-containing liquid oreganol according to claim 1, wherein the apparatus further comprises a gas-liquid separator,

including soaking case, support and stirring subassembly, be provided with inlet pipe and discharging pipe on the soaking case, the support with soaking case fixed connection, the stirring subassembly includes driving piece, pivot, bracing piece and stirring piece, the driving piece with soaking case fixed connection, the one end of pivot with the output fixed connection of driving piece, the other end of pivot inserts extremely soak the inside of case, the quantity of bracing piece is two, two the bracing piece respectively with pivot fixed connection, every all be provided with on the bracing piece the stirring piece.

8. The apparatus for producing organic acid-containing liquid oregano phenol according to claim 7,

each stirring piece includes connector and two curb plates, the connector with bracing piece fixed connection, the both ends of connector respectively with two curb plate fixed connection.

Technical Field

The invention relates to the technical field of production and preparation of animal remedy, in particular to a preparation method and a preparation device of liquid oregano phenol containing organic acid.

Background

Oregano is currently the whole plant of oregano, a plant of the family labiatae. The origanum oil is volatile oil obtained by steam distillation of origanum vulgare.

Oregano phenol is an aromatic phenolic substance in oregano oil and mainly contains phenolic components such as thymol and carvacrol. The thymol and the parsley are respectively used singly or mixed according to different proportions, and have better antibacterial, antioxidant and antitumor effects. Therefore, the oregano phenol has wide application in the aspects of pharmaceutical chemicals, flavors and fragrances, and feed additives. However, the purity of oregano phenol extracted from oregano by the existing process method is low.

Disclosure of Invention

The invention aims to provide a preparation method and a preparation device of liquid oregano phenol containing organic acid, and aims to solve the technical problem that the purity of the oregano phenol extracted by the existing process is low.

In order to achieve the above object, the present invention provides a method for preparing liquid oregano phenol containing organic acid, comprising the steps of:

crushing origanum vulgare to obtain slag, and then adding the slag into purified water in an extraction tank for soaking;

after soaking, adding organic acid, then adding steam into the extraction tank, and carrying out first purification treatment to obtain a purified liquid and residues;

discharging the purified liquid in the extraction tank, and cooling to obtain an origanum volatile oil mixed liquid;

adding ethanol into the residue, introducing the steam into the extraction tank again, and performing secondary purification treatment to obtain an origanum volatile oil alcoholic solution;

and mixing the origanum volatile oil mixed solution and the origanum volatile oil alcohol solution, and then carrying out oil-water separation treatment to obtain liquid origanum carvacrol.

Wherein, the step of adding the slag charge into the purified water in the extraction tank for soaking comprises the following steps:

the soaking time is 8-12 hours.

Wherein the organic acid is one or more of methanesulfonic acid, oxalic acid, acetic acid and citric acid.

Wherein, the first purification treatment comprises the following steps:

and raising the temperature in the extraction tank to 110-130 ℃, pressurizing to 0.3-0.5 MPa, and then carrying out hot reflux for 8-10 hours.

Wherein, in the step of discharging and cooling the purified liquid in the extraction tank:

and cooling by using a cooler.

Wherein, the second purification treatment comprises the following steps:

and raising the temperature in the extraction tank to 100-130 ℃, pressurizing to 0.4-0.5 MPa, and then carrying out hot reflux for 6-8 hours.

The invention also provides a preparation device adopting the previous preparation method of the liquid oregano phenol containing the organic acid, which comprises a soaking box, a support and a stirring assembly, wherein a feeding pipe and a discharging pipe are arranged on the soaking box, the support is fixedly connected with the soaking box, the stirring assembly comprises a driving piece, a rotating shaft, two supporting rods and a stirring piece, the driving piece is fixedly connected with the soaking box, one end of the rotating shaft is fixedly connected with the output end of the driving piece, the other end of the rotating shaft is inserted into the soaking box, the number of the supporting rods is two, the two supporting rods are respectively and fixedly connected with the rotating shaft, and the stirring piece is arranged on each supporting rod.

Each stirring piece comprises a connecting body and two side plates, the connecting body is fixedly connected with the supporting rod, and two ends of the connecting body are fixedly connected with the two side plates respectively.

According to the preparation method and the preparation device of the liquid oregano phenol containing the organic acid, oregano is taken and crushed to obtain slag, and then the slag is added into purified water in an extraction tank for soaking; after soaking, adding organic acid, then adding steam into the extraction tank, and carrying out first purification treatment to obtain a purified liquid and residues; discharging the purified liquid in the extraction tank, and cooling to obtain an origanum volatile oil mixed liquid; adding ethanol into the residue, introducing the steam into the extraction tank again, and performing secondary purification treatment to obtain an origanum volatile oil alcoholic solution; and mixing the origanum volatile oil mixed solution and the origanum volatile oil alcohol solution, and then carrying out oil-water separation treatment to obtain liquid origanum carvacrol. The purity of the oregano phenol is improved by soaking the crushed oregano and carrying out purification treatment twice.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart showing the steps of the method for producing liquid oregano phenol containing an organic acid according to the present invention.

FIG. 2 is a schematic view showing the structure of an apparatus for producing liquid oregano phenol containing an organic acid according to the present invention.

Fig. 3 is a cross-sectional view of the a-a line structure of fig. 2 of the present invention.

1-soaking box, 11-feeding pipe, 12-discharging pipe, 2-bracket, 3-stirring component, 31-driving component, 32-rotating shaft, 33-supporting rod, 34-stirring component, 341-connecting body, 342-side plate, 343-vertical rod and 344-horizontal plate.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.

In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

Referring to fig. 1, the present invention provides a method for preparing liquid oregano phenol containing organic acid, comprising the steps of:

s1: crushing origanum vulgare to obtain slag, and then adding the slag into purified water in an extraction tank for soaking;

s2: after soaking, adding organic acid, then adding steam into the extraction tank, and carrying out first purification treatment to obtain a purified liquid and residues;

s3: discharging the purified liquid in the extraction tank, and cooling to obtain an origanum volatile oil mixed liquid;

s4: adding ethanol into the residue, introducing the steam into the extraction tank again, and performing secondary purification treatment to obtain an origanum volatile oil alcoholic solution;

s5: and mixing the origanum volatile oil mixed solution and the origanum volatile oil alcohol solution, and then carrying out oil-water separation treatment to obtain liquid origanum carvacrol.

In this embodiment, before the step of taking and crushing oregano, the oregano needs to be cleaned, and then natural air drying is performed, wherein the cleaning of oregano specifically is as follows: rinsing or rinsing. In the step of taking and crushing oregano: organic acid is also needed to be added when the oregano is crushed. In the soaking process, the slag needs to be stirred. Crushing origanum vulgare to obtain slag, adding the slag into purified water in an extraction tank for soaking for 8-12 hours, adding any one of methanesulfonic acid, oxalic acid, acetic acid and citric acid after soaking is finished, adding steam into the extraction tank, raising the temperature in the extraction tank to 110-130 ℃, pressurizing for 0.3-0.5 MPa, and then performing thermal reflux for 8-10 hours to obtain a purified liquid and residues; discharging the purified liquid in the extraction tank, and cooling by using a cooler to obtain an origanum volatile oil mixed liquid; adding ethanol into the residues, introducing steam into the extraction tank again, raising the temperature in the extraction tank to 100-130 ℃, pressurizing to 0.4-0.5 MPa, and then performing thermal reflux for 6-8 hours to obtain an origanum volatile oil alcoholic solution; and mixing the origanum volatile oil mixed solution and the origanum volatile oil alcohol solution, and then carrying out oil-water separation treatment to obtain liquid origanum carvacrol. The purity of the oregano phenol is improved by soaking the crushed oregano and carrying out purification treatment twice.

Referring to fig. 2 and 3, the present invention further provides a preparation apparatus using the previous preparation method of liquid oregano phenol containing organic acid, including an immersion tank 1, a support 2 and a stirring assembly 3, wherein the immersion tank 1 is provided with a feeding pipe 11 and a discharging pipe 12, the support 2 is fixedly connected to the immersion tank 1, the stirring assembly 3 includes a driving member 31, a rotating shaft 32, two supporting rods 33 and a stirring member 34, the driving member 31 is fixedly connected to the immersion tank 1, one end of the rotating shaft 32 is fixedly connected to an output end of the driving member 31, the other end of the rotating shaft 32 is inserted into the immersion tank 1, the number of the supporting rods 33 is two, the two supporting rods 33 are respectively fixedly connected to the rotating shaft 32, and each supporting rod 33 is provided with the stirring member 34.

Each stirring member 34 includes a connecting body 341 and two side plates 342, the connecting body 341 is fixedly connected to the supporting rod 33, and two ends of the connecting body 341 are respectively fixedly connected to the two side plates 342.

In this embodiment, with the broken back of oregano the slag charge pass through inlet pipe 11 add extremely soak the inside of case 1, then add water, soak, later restart driving piece 31 drives pivot 32 rotates, and then drives bracing piece 33 and stirring piece 34 rotates to this fully mixed of realization slag charge and water does benefit to the purity that promotes the follow-up oregano fragrant phenol of extracting. In addition, the connection body 341 and the two side plates 342 are matched together, so that the mixing is more uniform and sufficient.

Further, each stirring member 34 further includes a vertical rod 343, and two ends of the vertical rod 343 are respectively and fixedly connected with the two side plates 342 and are located between the two side plates 342.

In this embodiment, the vertical bar 343 is provided to further enhance the stirring effect of the stirring bar 34.

Further, a plurality of transverse plates 344 which are distributed at equal intervals are arranged on each vertical rod 343.

In the present embodiment, the plurality of horizontal plates 344 are provided to enhance the stirring effect of the stirrer 34.

While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.