阅读说明：本技术 一种橙皮苷碱浸提液脱色除杂的方法 (Method for decoloring and decontaminating hesperidin alkaline leaching solution ) 是由 林楚潮 张勇 康辉 林雄水 于 2021-11-01 设计创作，主要内容包括：本发明提供了一种橙皮苷碱浸提液脱色除杂的方法,属于橙皮苷生产技术领域,所述方法包括以下步骤：采用陶瓷膜对橙皮苷碱浸提液进行脱色除杂,得到含有橙皮苷的透析液；所述陶瓷膜的截留精度≤80nm；所述脱色除杂的压强为≥0.2MPa。本发明中,橙皮苷碱浸提液经过陶瓷膜脱色除杂得到的橙皮苷陶瓷膜透析液中蛋白质、色素、果胶含量降低,透光率提高,提高了等电结晶橙皮苷产品纯度,增加了生产附加值,降低了生产成本。(The invention provides a method for decoloring and decontaminating hesperidin alkaline leaching solution, belonging to the technical field of hesperidin production and comprising the following steps: carrying out decoloration and impurity removal on the hesperidin alkali leaching solution by adopting a ceramic membrane to obtain a dialysate containing hesperidin; the interception precision of the ceramic membrane is less than or equal to 80 nm; the pressure of the decolorization and impurity removal is more than or equal to 0.2 MPa. In the invention, the content of protein, pigment and pectin in the hesperidin ceramic membrane dialysate obtained by decoloring and removing impurities from the hesperidin alkali leaching solution through the ceramic membrane is reduced, the light transmittance is improved, the purity of the isoelectric crystallization hesperidin product is improved, the production additional value is increased, and the production cost is reduced.)

1. A method for decoloring and decontaminating hesperidin alkaline leaching solution comprises the following steps:

carrying out decoloration and impurity removal on the hesperidin alkali leaching solution by adopting a ceramic membrane to obtain a dialysate containing hesperidin; the interception precision of the ceramic membrane is less than or equal to 80 nm; the pressure of the decolorization and impurity removal is more than or equal to 0.2 MPa.

2. The method according to claim 1, wherein the pressure for decoloring and impurity removal is 0.2-0.5 MPa.

3. The method according to claim 1 or 2, wherein the temperature for decoloring and impurity removal is 40-50 ℃.

4. The method according to claim 1, wherein the ceramic membrane comprises a cylindrical support (1) and a membrane layer (2); the cylindrical support body is provided with a cylindrical through hole (3) in the length direction; the film layer (2) is coated on the inner surface of the cylindrical through hole (3).

5. The method according to claim 4, wherein the membrane layer (2) comprises a transition layer (21) and a separation layer (22); the transition layer (21) is coated on the inner surface of the cylindrical through hole (3); the separation layer (22) is coated on the surface of the transition layer (21).

6. The method according to claim 4 or 5, wherein the transition layer (21) has a thickness of 600 to 900 nm.

7. The method according to claim 4 or 5, characterized in that the thickness of the separation layer (22) is 10-80 nm.

8. The method according to claim 1, wherein the transition layer (21) is an alumina transition layer; the separation layer (22) is a zirconia separation layer.

9. The method according to claim 1, wherein before and after the decolorizing and impurity removing, the volume ratio of the hesperidin alkaline leaching solution to the hesperidin-containing dialysate is 10: 1.

10. a hesperidin extraction method comprises the following steps:

carrying out decoloration and impurity removal on the hesperidin alkaline leaching solution according to the method of any one of claims 1 to 9 to obtain a dialysis solution containing hesperidin;

and carrying out isoelectric point crystallization treatment on the dialysate to obtain the hesperidin.

Technical Field

The invention relates to the technical field of hesperidin production, in particular to a method for decoloring and decontaminating hesperidin alkaline leaching solution.

Background

Hesperidin, also known as nobiletin, is a flavanone glycoside. Hesperidin has effects of maintaining osmotic pressure, enhancing capillary toughness, shortening bleeding time and reducing cholesterol, is clinically used for auxiliary treatment of cardiovascular system diseases, can be used for cultivating various medicines for preventing arteriosclerosis and myocardial infarction, and is one of main raw materials of adult medicine "Maitong". Hesperidin can be used as natural antioxidant in food industry, and can also be used in cosmetic industry.

At present, an alkali extraction and acid precipitation method is mainly used for extracting the hesperidin, the obtained alkali extract is filtered by a 5-micron filter cloth, and due to the fact that the filter cloth has poor interception precision and poor alkali resistance, the filter cloth is often damaged, so that impurities such as suspended matters and the like exist after the hesperidin alkali extract passes through the filter cloth, and the subsequent hesperidin crystallization effect and the system yield are influenced. The crystallization purity of the hesperidin alkaline leaching solution after the filtration of the traditional filter cloth is less than 80 percent, and the added value of the product is lower.

Disclosure of Invention

The invention aims to provide a method for decoloring and impurity removing of hesperidin alkali leaching solution.

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

the invention provides a method for decoloring and decontaminating hesperidin alkaline leaching solution, which comprises the following steps:

carrying out decoloration and impurity removal on the hesperidin alkali leaching solution by adopting a ceramic membrane to obtain a dialysate containing hesperidin; the interception precision of the ceramic membrane is less than or equal to 80 nm; the pressure of the decolorization and impurity removal is more than or equal to 0.2 MPa.

Preferably, the pressure for decoloring and impurity removing is 0.2-0.5 MPa.

Preferably, the temperature for decoloring and impurity removal is 40-50 ℃.

Preferably, the ceramic membrane comprises a cylindrical support 1 and a membrane layer 2; the cylindrical support body is provided with a cylindrical through hole 3 in the length direction; the film layer 2 is coated on the inner surface of the cylindrical through hole 3.

Preferably, the film layer 2 comprises a transition layer 21 and a separation layer 22; the transition layer 21 is coated on the inner surface of the cylindrical through hole 3; the separation layer 22 is coated on the surface of the transition layer 21.

Preferably, the thickness of the transition layer 21 is 600-900 nm.

Preferably, the thickness of the separation layer 22 is 10 to 80 nm.

Preferably, the transition layer 21 is an alumina transition layer; the separation layer 22 is a zirconia separation layer.

Preferably, before and after the decolorization and impurity removal, the volume ratio of the hesperidin alkaline leaching solution to the hesperidin-containing dialysate is 10: 1.

the invention also provides a hesperidin extraction method, which comprises the following steps:

decolorizing and removing impurities from the hesperidin alkaline leaching solution according to the method of the scheme to obtain a dialysis solution containing hesperidin;

and carrying out isoelectric point crystallization treatment on the dialysate to obtain the hesperidin.

The invention provides a method for decoloring and decontaminating hesperidin alkaline leaching solution, which comprises the following steps of decoloring and decontaminating the hesperidin alkaline leaching solution by adopting a ceramic membrane to obtain dialysate containing hesperidin; the interception precision of the ceramic membrane is less than or equal to 80 nm; the pressure of the decolorization and impurity removal is more than or equal to 0.2 MPa. Compared with the traditional filtering means, the content of protein, pigment and pectin in the hesperidin ceramic membrane dialysate obtained by decoloring and removing impurities from the hesperidin alkali leaching solution through the ceramic membrane is reduced, and the light transmittance is improved, so that the purity of a hesperidin product crystallized at a subsequent isoelectric point is improved, the production additional value is increased, and the production cost is reduced. After the hesperidin ceramic membrane dialysate obtained by the method is crystallized, the purity of the hesperidin is more than or equal to 90%, the yield is more than or equal to 90%, and the obtained hesperidin crystallization finished product is white and clean in color.

Drawings

FIG. 1 is a schematic diagram of a ceramic membrane structure, wherein a 1-cylindrical support, a 2-membrane layer, a 3-cylindrical through hole, a 21-transition layer and a 22 separation layer are arranged.

Detailed Description

The invention provides a method for decoloring and decontaminating hesperidin alkaline leaching solution, which comprises the following steps:

carrying out decoloration and impurity removal on the hesperidin alkali leaching solution by adopting a ceramic membrane to obtain a dialysate containing hesperidin; the interception precision of the ceramic membrane is less than or equal to 80 nm; the pressure of the decolorization and impurity removal is more than or equal to 0.2 MPa.

In the invention, the sources of the hesperidin alkaline leaching solution comprise:

leaching the orange peels with alkali liquor, and filtering to obtain an alkaline leaching solution of hesperidin. The leaching parameters are not particularly limited in the invention, and the conventional parameters in the field can be adopted.

In the present invention, the ceramic membrane preferably includes a cylindrical support 1 and a membrane layer 2; the cylindrical support body is provided with a cylindrical through hole 3 in the length direction; the film layer 2 is coated on the inner surface of the cylindrical through hole 3. In the present invention, the cylindrical support 1 serves as a membrane carrier for ensuring the mechanical strength of the ceramic membrane.

In one embodiment of the present invention, the film layer 2 includes a transition layer 21 and a separation layer 22; the transition layer 21 is coated on the inner surface of the cylindrical through hole 3; the separation layer 22 is coated on the surface of the transition layer 21, and the structural schematic diagram is shown in fig. 1.

In the invention, the diameter of the cylindrical support body 1 is preferably 28-32 mm, and more preferably 30 mm; the diameter of the cylindrical through hole is preferably 2-4 mm, and more preferably 3 mm.

In the invention, the thickness of the transition layer 21 is preferably 600-900 nm, and more preferably 800 nm; the thickness of the separation layer 22 is preferably 10-80 nm;

in the present invention; the material of the cylindrical support body is preferably alumina; the transition layer 21 preferably comprises an alumina transition layer; the transition layer 21 is used for increasing the wear resistance of the ceramic membrane and increasing the filtering precision of the membrane core; the separation layer 22 preferably comprises a zirconia separation layer; the separation layer 22 is used for separation. In the present invention, the ceramic membrane is preferably from the same boat crossbar (mansion) fluid technology ltd.

In the invention, the interception precision of the ceramic membrane used for decoloring and impurity removing of the ceramic membrane is preferably 10-80 nm, and more preferably 30-50 nm. According to the invention, the ceramic membrane with proper interception precision is selected to keep impurities such as pigment, protein and the like in the concentrated solution, and other effective components such as hesperidin enter the dialyzate.

In the invention, the pressure for decoloring and impurity removing of the ceramic membrane is preferably 0.2-0.5 MPa, and more preferably 0.3 MPa. The invention ensures that the system has the best system operation stability under the best investment benefit ratio by selecting the proper pressure range.

In the invention, the temperature for decoloring and impurity removal of the ceramic membrane is preferably 40-50 ℃, and more preferably 45 ℃.

Before the ceramic membrane is adopted to carry out decoloration and impurity removal on the hesperidin alkaline leaching solution, the preferable method also comprises the step of carrying out precise filtration on the hesperidin alkaline leaching solution; the precision of the precision filtration is preferably 35-40 mu m; the precise filtration has the function of reducing the turbidity of the hesperidin alkaline leaching solution to zero and preventing the ceramic membrane from being damaged.

In the invention, the content of protein, pigment and pectin in the hesperidin ceramic membrane dialysate obtained by decoloring and removing impurities from the hesperidin alkali leaching solution through the ceramic membrane is reduced, the light transmittance is improved, the purity of the isoelectric crystallization hesperidin product is improved, the production additional value is increased, and the production cost is reduced.

In the invention, before and after the ceramic membrane is decolored and decontaminated, the volume ratio of the hesperidin alkali leaching solution to the hesperidin ceramic membrane dialysate is preferably 10: 1.

in the invention, the ceramic membrane is preferably electrically connected with a computer PLC control system, and the operating pressure, temperature and concentration multiple of membrane filtration are limited within a reasonable range by the computer PLC control system. The operation pressure, temperature and concentration multiple of the filtration can be set, so that the energy consumption of the ceramic membrane can be saved, and the cost is reduced.

The invention also provides a hesperidin extraction method, which comprises the following steps: decolorizing and removing impurities from the hesperidin alkaline leaching solution according to the method of the scheme to obtain a dialysis solution containing hesperidin; and carrying out isoelectric point crystallization treatment on the dialysate to obtain the hesperidin.

In the present invention, the isoelectric point crystallization comprises the steps of: adjusting the pH value of the dialysate to 8.2-8.5, standing until hesperidin crystals are separated out, performing microfiltration by using filter cloth, collecting the hesperidin crystals, and drying the hesperidin crystals to obtain the hesperidin.

In the invention, the reagent for adjusting the pH value of the hesperidin ceramic membrane dialysate is preferably hydrochloric acid; the standing time is preferably 1-3 h, and more preferably 2 h; the pore diameter of the filter cloth is preferably 5 μm; the drying mode is preferably drying.

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.

Example 1

1) Collecting hesperidin alkaline leaching solution from a certain biotechnology limited company in Sichuan in the production process by an alkaline leaching method. The hesperidin content in the hesperidin alkaline leaching solution is 0.5%, and the hesperidin purity is 73%.

2) Precisely filtering the hesperidin alkali leaching solution obtained in the step 1) (the precision is 35 mu m), pressurizing to 0.3MPa, and performing ceramic membrane decoloring and impurity removal, wherein the ceramic membrane is from same-boat vertical and horizontal (Xiamen) fluid technology limited company, the operating temperature of the ceramic membrane decoloring and impurity removal is 43 ℃, and the operation is carried out until the ratio of the volume of a feed liquid to the volume of a final concentrated solution is 1: and 8, obtaining a ceramic membrane concentrated solution and a hesperidin ceramic membrane dialysate.

3) The obtained hesperidin ceramic membrane dialysate is further subjected to isoelectric point crystallization treatment, wherein the purity of the hesperidin obtained by the isoelectric point crystallization treatment is 92%, and the content of the hesperidin is 0.5%. According to the base number of 600 tons of hesperidin alkaline leaching liquid per day, 3 tons of finished hesperidin with the purity of 92 percent are produced per day, and the additional value of the production is increased by 5.

Example 2

1) Collecting hesperidin alkaline leaching solution from a certain biotechnology limited company in Yunnan in the production process by an alkaline solution leaching method. The hesperidin content in the hesperidin alkaline leaching solution is 0.6%, and the hesperidin purity is 71%.

2) Precisely filtering the hesperidin alkali leaching solution obtained in the step 1) (the precision is 40 mu m), pressurizing to 0.6MPa, and performing ceramic membrane decoloring and impurity removal, wherein the ceramic membrane is from same-boat vertical and horizontal (Xiamen) fluid technology limited company, the operating temperature of the ceramic membrane decoloring and impurity removal is 48 ℃, and the operation is carried out until the ratio of the volume of the feeding solution to the volume of the final concentrated solution is 1: and 9, obtaining a ceramic membrane concentrated solution and a hesperidin ceramic membrane dialysate.

3) The obtained hesperidin ceramic membrane dialysate is further subjected to isoelectric point crystallization treatment, the purity of the hesperidin obtained by the isoelectric point crystallization treatment reaches 91%, and the content of the hesperidin is 0.6%. According to the base number of 700 tons of hesperidin alkaline leaching liquid material liquid every day, 4 tons of finished hesperidin products with 91% purity are obtained every day, and the additional value of the production is increased by 7 ten thousand yuan in a conversion manner.

Example 3

1) Collecting hesperidin alkaline leaching solution from a certain biotechnology limited company in the production process by an alkaline leaching method. The hesperidin content in the hesperidin alkaline leaching solution is 0.5%, and the hesperidin purity is 75%.

2) Precisely filtering the hesperidin alkali leaching solution obtained in the step 1) (the precision is 40 mu m), pressurizing to 0.6MPa by using a booster pump, decoloring and impurity-removing a ceramic membrane, wherein the ceramic membrane is from a same-boat vertical and horizontal (Xiamen) fluid technology company Limited, the operating temperature of the ceramic membrane decoloring and impurity-removing is 50 ℃, and the operation is carried out until the ratio of the volume of a feeding solution to the volume of a final concentrated solution is 1: and (10) obtaining a ceramic membrane concentrated solution and a hesperidin ceramic membrane dialysate.

3) The obtained hesperidin ceramic membrane dialysate is further subjected to isoelectric point crystallization treatment, the purity of the hesperidin obtained by the isoelectric point crystallization treatment reaches 95%, and the content of the hesperidin is 0.5%. According to the base number of 400 tons of hesperidin alkaline leaching liquid material liquid per day, 2 tons of finished hesperidin with the purity of 93 percent are obtained per day, and the additional value of the production is increased by 3 ten thousand yuan in a conversion manner.

Comparative example

The decolorizing and impurity removing effects of the ceramic membrane and the 5 μm filter cloth on the hesperidin alkali leaching solution are compared, and the method refers to example 1. The results are shown in Table 1.

TABLE 1 comparison of the decolorizing and impurity-removing effects of ceramic membranes and 5 μm filter cloth on hesperidin alkaline leaching solution

As can be seen from Table 1, compared with the traditional method in which 5 μm filter cloth is adopted to filter and remove impurities from the hesperidin alkali leaching solution, the method has the advantages that the ceramic membrane is adopted to achieve better decolorizing and impurity removing effects on the hesperidin alkali leaching solution, the hesperidin purity is higher, and the content of impurities such as neotype glycoside, hesperetin, pectin and the like is lower.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.