阅读说明：本技术 脱农残羊毛脂的制备方法 (Preparation method of lanolin without pesticide residues ) 是由 姚红枝 于 2021-07-20 设计创作，主要内容包括：本发明属于油脂加工技术领域,具体涉及脱农残羊毛脂的制备方法。本发明羊毛脂与农药残留分子的沸点差,通过高真空分子蒸馏设备,有效的脱除产品中的农药残留,使得产品安全性提高,闪蒸联用三级蒸馏提纯,且温度不同,可将精制羊毛脂中低中高的碳进行分离,如此,使羊毛脂产品中高分子脂肪醇和酸纯度大大提升,脱出水分和去除游离醇和游离酸,使羊毛脂的品质更佳,应用领域更广泛。(The invention belongs to the technical field of grease processing, and particularly relates to a preparation method of lanolin with pesticide residues removed. According to the present invention, the boiling point difference between the lanolin and the pesticide residue molecules is adopted, the pesticide residue in the product is effectively removed through the high vacuum molecular distillation equipment, such that product safety is improved, flash evaporation and three-stage distillation purification are adopted, the temperature is different, low, medium and high carbon in the refined lanolin can be separated, such that the purity of high molecular fatty alcohol and acid in the lanolin product is substantially improved, water is removed, free alcohol and free acid are removed, the quality of the lanolin is better, and the application field is wider.)

1. The preparation method of the lanolin without pesticide residues is characterized by comprising the following steps:

s1, preheating refined lanolin to be in a liquid state through a heat exchanger, and then entering a flash evaporator to obtain a pretreated product;

s2, preheating the pretreated product obtained in the step S1, raising the temperature of the pretreated product, and allowing the preheated product to enter a first-stage molecular distiller for first-stage distillation to obtain a first-stage heavy phase product;

s3, continuously preheating and heating the first-stage heavy phase product in the step S2, and entering a second-stage molecular distiller for secondary distillation to obtain a second-stage heavy phase product;

s4, preheating the first-stage heavy phase product in the step S3 again, raising the temperature, entering a third-stage molecular distiller for third-stage distillation, and collecting a third-stage heavy phase product, namely, the pesticide residue removal lanolin.

2. The method for preparing lanolin with pesticide residue removed according to claim 1, wherein the preheating temperature of the refined lanolin in step S1 is 120-125 ℃.

3. The method for preparing lanolin with pesticide residue removed according to claim 1, wherein in step S2, the temperature for preheating the first-stage heavy phase product is 100-.

4. The method for preparing lanolin with pesticide residue removed according to claim 1, wherein in step S3, the temperature for preheating the pretreatment product is 150-155 ℃, the vacuum degree of the second stage molecular distillation device is 0.01-0.1MPa, the temperature is 150-180 ℃, and the scraper rotation speed is 100-200 rad/min.

5. The method for preparing lanolin with pesticide residue removed according to claim 1, wherein in step S4, the temperature for preheating the second-stage heavy phase product is 180-.

6. The method for preparing lanolin with pesticide residue removed according to claim 1, wherein the third stage molecular distillation device is communicated with the first stage molecular distillation device through a pipeline.

Technical Field

The invention belongs to the technical field of grease processing, and particularly relates to a preparation method of lanolin with pesticide residues removed.

Background

Lanolin is a natural animal grease which is secreted by sheep glands, attached to wool and obtained by recycling waste water through wool washing industry. Lanolin mainly comprises sterols, triterpene alcohols, fatty alcohols and natural lipids (about 94%) formed from approximately equal amounts of fatty acids, and further contains small amounts of free sterols and fatty acids. The crude lanolin recovered from wool washing industry is black brown, has large smell and is easy to rancidity. The refined anhydrous lanolin obtained by refining the crude lanolin is a light yellow paste, is not easy to rancidity, has good emulsifying property, can absorb twice of water, has a melting point of 38-42 ℃, and is mainly used in the cosmetic industry.

However, in the process of sheep breeding, pesticides are often required to be sprayed on wool in order to repel flies and kill lice, so that certain pesticide residues also exist in the generated lanolin, and the lanolin is mainly used in the fields of cosmetics, skin care products and even medical food, and the pesticide residues are likely to cause potential threats and damages to human health. Meanwhile, the refined lanolin also contains water and free fatty acid in excess of proportion, so that the chemical combination between potential surface active groups and structures in the lanolin is tight and difficult to exert, and the lanolin is highly greasy, thereby limiting the application range of the lanolin.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a preparation method of lanolin without pesticide residues, and aims to solve the technical problems that the refined lanolin contains pesticide residues, moisture exceeding the proportion and free fatty acid, so that the chemical bonding between potential surface active groups and structures in the lanolin is tight, the lanolin is difficult to exert, the greasiness is heavy, and the application range of the lanolin is limited.

The invention provides a preparation method of lanolin without pesticide residue, which has the following specific technical scheme:

the preparation method of the lanolin without pesticide residues comprises the following steps:

s1, preheating refined lanolin to be in a liquid state through a heat exchanger, and then entering a flash evaporator to obtain a pretreated product;

s2, preheating the pretreated product obtained in the step S1, raising the temperature of the pretreated product, and allowing the preheated product to enter a first-stage molecular distiller for first-stage distillation to obtain a first-stage heavy phase product;

s3, continuously preheating and heating the first-stage heavy phase product in the step S2, and entering a second-stage molecular distiller for secondary distillation to obtain a second-stage heavy phase product;

s4, preheating the first-stage heavy phase product in the step S3 again, raising the temperature, entering a third-stage molecular distiller for third-stage distillation, and collecting a third-stage heavy phase product, namely, the pesticide residue removal lanolin.

In some embodiments, the temperature at which the refined lanolin is preheated in step S1 is 120-125 ℃.

In some embodiments, in step S2, the temperature for preheating the first-stage heavy phase product is 100-.

In some embodiments, in step S3, the temperature for preheating the pretreated product is 150-.

In some embodiments, in step S4, the temperature for preheating the secondary heavy phase product is 185-.

In certain embodiments, the third stage molecular still is in communication with the first stage molecular still via a conduit.

The invention has the following beneficial effects: according to the present invention, the boiling point difference between the lanolin and the pesticide residue molecules is adopted, the pesticide residue in the product is effectively removed through the high vacuum molecular distillation equipment, such that product safety is improved, flash evaporation and three-stage distillation purification are adopted, the temperature is different, low, medium and high carbon in the refined lanolin can be separated, such that the purity of high molecular fatty alcohol and acid in the lanolin product is substantially improved, water is removed, free alcohol and free acid are removed, the quality of the lanolin is better, and the application field is wider.

Drawings

FIG. 1 is a flow chart of the preparation method of lanolin without pesticide residue provided by the invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings 1 in conjunction with specific embodiments.

Example 1

The preparation method of the lanolin without pesticide residue provided by the embodiment has the following specific technical scheme:

the preparation method of the lanolin without pesticide residues comprises the following steps:

s1, preheating refined lanolin to a liquid state at 120 ℃ through a heat exchanger, and then entering a flash evaporator to obtain a pretreated product;

s2, preheating the pretreated product obtained in the step S1 to 110 ℃, entering a first-stage molecular distiller (with the vacuum degree of 0.01MPa, the temperature of 100 ℃ and the scraper rotation speed of 100rad/min) for first-stage distillation to obtain a first-stage heavy phase product;

s3, continuously preheating the first-stage heavy-phase product in the step S2 to 150 ℃, entering a second-stage molecular distiller (with the vacuum degree of 0.01MPa, the temperature of 150 ℃ and the scraper rotation speed of 100rad/min) for secondary distillation, and obtaining a second-stage heavy-phase product;

s4, preheating the first-stage heavy phase product in the step S3 again to 180 ℃, entering a third-stage molecular distiller (with the vacuum degree of 0.01MPa, the temperature of 180 ℃ and the scraper rotation speed of 100rad/min) for three-stage distillation, and collecting a third-stage heavy phase product, namely, removing pesticide residue lanolin.

Example 2

The preparation method of the lanolin without pesticide residue provided by the embodiment has the following specific technical scheme:

the preparation method of the lanolin without pesticide residues comprises the following steps:

s1, preheating refined lanolin to 125 ℃ liquid state through a heat exchanger, and then entering a flash evaporator to obtain a pretreated product;

s2, preheating the pretreated product obtained in the step S1 to 105 ℃, entering a first-stage molecular distiller (with the vacuum degree of 0.05MPa, the temperature of 150 ℃ and the scraper rotation speed of 200rad/min) for first-stage distillation, and obtaining a first-stage heavy phase product;

s3, continuously preheating the first-stage heavy-phase product in the step S2 to 155 ℃, entering a second-stage molecular distiller (with the vacuum degree of 0.1MPa, the temperature of 180 ℃ and the scraper rotation speed of 200rad/min) for secondary distillation, and obtaining a second-stage heavy-phase product;

s4, preheating the first-stage heavy phase product in the step S3 again to 180-185 ℃, entering a third-stage molecular distiller (with the vacuum degree of 0.1MPa, the temperature of 200 ℃ and the scraper rotation speed of 200rad/min) for three-stage distillation, and collecting a third-stage heavy phase product, namely removing pesticide residue lanolin.

In this embodiment, if the collected lanolin without pesticide residue is detected to be not in accordance with the detection standard, the collected lanolin is refluxed from the third-stage molecular distiller to the first-stage molecular distiller through a pipeline, mixed with refined lanolin to be subjected to pesticide residue removal, and then purified.

Example 3

The preparation method of the lanolin without pesticide residue provided by the embodiment has the following specific technical scheme:

the preparation method of the lanolin without pesticide residues comprises the following steps:

s1, preheating refined lanolin (pesticide residue value is 56.53ppm, pesticide residue value is detected by gel chromatography GPC-solid phase extraction SPE-gas chromatography detection GC method, USP43 and EP10 lanolin detection method) to be in a 122 ℃ liquid state through a heat exchanger, then entering a flash evaporator, removing pesticide residue and part of water in a small molecular organic solvent, and obtaining a pretreated product;

s2, preheating the pretreated product obtained in the step S1 to 103 ℃, entering a first-stage molecular distiller (with the vacuum degree of 0.02MPa, the temperature of 120 ℃ and the scraper rotation speed of 150rad/min) for first-stage distillation, and obtaining a first-stage heavy phase product;

s3, continuously preheating the first-stage heavy-phase product in the step S2 to 152 ℃, entering a second-stage molecular distiller (with the vacuum degree of 0.05MPa, the temperature of 170 ℃ and the scraper rotation speed of 150rad/min) for secondary distillation, and obtaining a second-stage heavy-phase product;

s4, preheating the first-stage heavy phase product in the step S3 again to 183 ℃, entering a third-stage molecular distiller (the vacuum degree is 0.05MPa, the temperature is 190 ℃, the scraper rotation speed is 150rad/min) for three-stage distillation, and collecting a third-stage heavy phase product, namely, the pesticide residue removal lanolin.

In this example, the total pesticide residue of lanolin without pesticide residue in this example was 0.8ppm (the detection method was the same as above).

The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the invention, and the present invention is not limited to the above examples, and those skilled in the art should also be able to make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.