阅读说明：本技术 粗羊毛脂的精制工艺 (Refining process of crude lanolin ) 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,具体涉及粗羊毛脂的精制工艺。本发明提供的粗羊毛脂的精制工艺,通过熔化、酸化、脱色、真空除臭、乳化和沉淀步骤实现对出羊毛脂进行处理,获得精制后的羊毛脂,用硫酸钠替代磷酸,如此使剧烈的酸化反应变得缓慢,从而利于下一步反应,并且含硫的污水相比于含磷污水更容易处理,减少了环境污染,节约污水处理成本。(The invention belongs to the technical field of grease processing, and particularly relates to a refining process of crude lanolin. The refining process of the crude lanolin, provided by the invention, realizes treatment of the lanolin through the steps of melting, acidification, decoloration, vacuum deodorization, emulsification and precipitation to obtain the refined lanolin, and uses sodium sulfate to replace phosphoric acid, so that the violent acidification reaction is slowed, the next reaction is facilitated, and compared with phosphorus-containing sewage, the sulfur-containing sewage is easier to treat, the environmental pollution is reduced, and the sewage treatment cost is saved.)

1. The refining process of the crude lanolin is characterized by comprising the following steps:

s1, introducing the crude lanolin into an oven for melting to obtain a molten product;

s2, introducing the molten product obtained in the step S1 into a reaction kettle, and adding a sodium sulfate solution for acidification reaction to obtain an acidified product;

s3, adding hydrogen peroxide into the acidified product obtained in the step S2, stirring and decoloring to obtain a decolored product;

s4, performing vacuum deodorization treatment on the decolored product in the step S3 to obtain a deodorized product;

s5, adding an isopropanol solution into the deodorization product obtained in the step S4 for layering and impurity removal, and collecting a grease layer, namely a layering product;

s6, adding sodium hydroxide into the layered product in the step S5, precipitating, and collecting supernatant, namely refined lanolin.

2. The refining process of crude lanolin according to claim 1, wherein in step S1, the oven temperature is 50-70 ℃.

3. The refining process of crude lanolin according to claim 1, wherein in step S2, the concentration of said sodium sulfate solution is 80-90%, the mass ratio of said molten product to said sodium sulfate solution is 500:1, and the reaction temperature in said reaction kettle is 50-70 ℃.

4. The refining process of crude lanolin according to claim 1, wherein in step S3, said hydrogen peroxide is 4-6% of the weight of said crude lanolin, said stirring time is 30-50min, and said stirring temperature is 55-65 ℃.

5. The refining process of crude lanolin according to claim 1, wherein in step S4, said vacuum deodorization comprises the steps of: heating the reaction kettle to 90 deg.C, deodorizing under the vacuum degree of 480mmHg for 4-6 hours.

6. The refining process of crude lanolin according to claim 1, wherein in step S5, the concentration of said isopropyl alcohol solution is 25-30%, and 0.25L of isopropyl alcohol solution is added per 1kg of molten product.

7. The refining process of crude lanolin according to claim 1, wherein in step S5, after adding isopropanol solution, 80-90% sodium thiosulfate solution is added, and the mass ratio of said molten product to said sodium thiosulfate solution is 500: 1.

8. The refining process of crude lanolin according to claim 1, wherein in step S6, the mass ratio of said sodium hydroxide to said melted product is 1:80-100, and the time of said precipitation is 4-6 hours.

9. The refining process of crude lanolin according to claim 1, wherein 0.017% BHT antioxidant is added to the refined lanolin.

Technical Field

The invention belongs to the technical field of grease processing, and particularly relates to a refining process of crude lanolin.

Background

Lanolin is a mixture of esters, hydrocarbons and lipids secreted from sebaceous glands and adhering to the skin. Lanolin is not an ester, does not have a structure of glycerin, and is an ester of lanolin alcohol and lanolin fatty acid. Lanolin is a precious raw material, has strong water absorption, no irritation and stable emulsifying property, and can be modified in various ways due to the abundant active groups. Lanolin and its modified products are widely used in the industries of cosmetics, leather, medicine, etc.

Crude lanolin is recovered from wool washing waste water, has abundant sources, contains more water, has dark color and large smell, contains more impurities which influence the quality of lanolin, such as dust, sandy soil, plant sundries, inorganic salts of sheep sweat components, protein series decomposition products generated from excrement, blood and oxides, pigments and the like, and decomposition products of low ester components, namely free fatty acid and free alcohol. Therefore, crude lanolin cannot be directly applied to cosmetics and other industries, so purification of crude lanolin is required to remove impurities. The refined lanolin has stable chemical property, is not easy to rancidity and breed bacteria, has light color and can be widely applied to the cosmetic industry.

In the existing refining process of lanolin, phosphoric acid is used as an acidifying agent, so that a large amount of phosphorus-containing sewage is discharged, the environmental pollution is caused, the reaction is severe, the subsequent process is not facilitated, and the refining effect is influenced.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a refining process of crude lanolin, aiming at solving the technical problems that phosphoric acid is used as an acidifying agent in the prior refining process of the lanolin, so that a large amount of phosphorus-containing sewage is discharged, the environment is polluted, the reaction is severe, the subsequent process is not facilitated, and the refining effect is influenced.

The invention provides a refining process of crude lanolin, which has the following specific technical scheme:

the refining process of crude lanolin includes the following steps:

s1, introducing the crude lanolin into an oven for melting to obtain a molten product;

s2, introducing the molten product obtained in the step S1 into a reaction kettle, and adding a sodium sulfate solution for acidification reaction to obtain an acidified product;

s3, adding hydrogen peroxide into the acidified product obtained in the step S2, stirring and decoloring to obtain a decolored product;

s4, performing vacuum deodorization treatment on the decolored product in the step S3 to obtain a deodorized product;

s5, adding an isopropanol solution into the deodorization product obtained in the step S4 for layering and impurity removal, and collecting a grease layer, namely a layering product;

s6, adding sodium hydroxide into the layered product in the step S5, precipitating, and collecting supernatant, namely refined lanolin.

In certain embodiments, in step S1, the oven temperature is 50-70 ℃.

In certain embodiments, in step S2, the concentration of the sodium sulfate solution is 80 to 90%, the mass ratio of the molten product to the sodium sulfate solution is 500:1, and the reaction temperature in the reaction kettle is 50 to 70 ℃.

In some embodiments, in step S3, the hydrogen peroxide is 4-6% by weight of the crude lanolin, the stirring time is 30-50min, and the stirring temperature is 55-65 ℃.

In certain embodiments, in step S4, the vacuum deodorization comprises the steps of: heating the reaction kettle to 90 deg.C, deodorizing under the vacuum degree of 480mmHg for 4-6 hours.

In certain embodiments, the concentration of the isopropanol solution in step S5 is 25-30%, and 0.25L of the isopropanol solution is added per 1kg of the molten product.

In certain embodiments, in step S5, after the addition of the isopropanol solution, an additional 80-90% sodium thiosulfate solution is added, and the mass ratio of the molten product to the sodium thiosulfate solution is 500: 1.

In certain embodiments, in step S6, the mass ratio of the sodium hydroxide to the molten product is 1:80 to 100, and the precipitation time is 4 to 6 hours.

In certain embodiments, 0.017% BHT antioxidant is added to the refined lanolin.

The invention has the following beneficial effects: the refining process of the crude lanolin, provided by the invention, realizes treatment of the lanolin through the steps of melting, acidification, decoloration, vacuum deodorization, emulsification and precipitation to obtain the refined lanolin, and uses sodium sulfate to replace phosphoric acid, so that the violent acidification reaction is slowed, the next reaction is facilitated, and compared with phosphorus-containing sewage, the sulfur-containing sewage is easier to treat, the environmental pollution is reduced, and the sewage treatment cost is saved.

Drawings

FIG. 1 is a flow chart of a refining process of crude lanolin provided by the present invention;

FIG. 2 is a schematic view of the layered material in step S5 in example 3 of the present 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 1-2 in conjunction with specific embodiments.

Example 1

The refining process of crude lanolin provided by this example has the following specific technical scheme:

the refining process of crude lanolin includes the following steps:

s1, introducing the crude lanolin into an oven to melt, wherein the temperature of the oven is 50-70 ℃, and obtaining a molten product.

S2, introducing the molten product obtained in the step S1 into a reaction kettle (the temperature is set to be 50-70 ℃) and adding a sodium sulfate solution with the concentration of 80-90% to carry out acidification reaction, wherein the mass ratio of the sodium sulfate solution to the molten product is 1:500, and obtaining an acidified product.

S3, adding hydrogen peroxide into the acidified product obtained in the step S2, stirring (at 55-65 ℃ for 30-50min), and decolorizing, wherein the addition amount of hydrogen peroxide is 4-6% of the mass of the crude lanolin obtained in the step S1, so as to obtain the decolorized product.

S4, performing vacuum deodorization treatment on the decolorized product in the step S3, wherein the vacuum deodorization comprises the following steps: heating the reaction kettle to 90 ℃, and deodorizing for 4-6 hours under the condition that the vacuum degree is 480mmHg to obtain a deodorizing product.

S5, adding 25-30% isopropanol solution into the deodorization product in the step S4 for layering and impurity removal, adding 0.25L of isopropanol solution into each 1kg of melting product, then adding 80-90% of sodium thiosulfate solution, wherein the mass ratio of the melting product to the sodium thiosulfate solution is 500:1, and collecting a grease layer, namely a layering product.

S6, adding sodium hydroxide into the layered product in the step S5, wherein the mass ratio of the sodium hydroxide to the molten product is 1:80-100, precipitating for 4-6 hours, and collecting supernatant, namely refined lanolin.

Example 2

The refining process of crude lanolin provided by this example has the following specific technical scheme:

the refining process of crude lanolin includes the following steps:

s1, introducing the crude lanolin into an oven to melt, wherein the temperature of the oven is 50-70 ℃, and obtaining a molten product.

S2, introducing the molten product obtained in the step S1 into a reaction kettle (the temperature is set to be 50-70 ℃) and adding a sodium sulfate solution with the concentration of 80-90% to carry out acidification reaction, wherein the mass ratio of the sodium sulfate solution to the molten product is 1:500, and obtaining an acidified product.

S3, adding hydrogen peroxide into the acidified product obtained in the step S2, stirring (at 55-65 ℃ for 30-50min), and decolorizing, wherein the addition amount of hydrogen peroxide is 4-6% of the mass of the crude lanolin obtained in the step S1, so as to obtain the decolorized product.

S4, performing vacuum deodorization treatment on the decolorized product in the step S3, wherein the vacuum deodorization comprises the following steps: heating the reaction kettle to 90 ℃, and deodorizing for 4-6 hours under the condition that the vacuum degree is 480mmHg to obtain a deodorizing product.

S5, adding 25-30% isopropanol solution into the deodorization product in the step S4 for layering and impurity removal, adding 0.25L of isopropanol solution into each 1kg of melting product, then adding 80-90% of sodium thiosulfate solution, wherein the mass ratio of the melting product to the sodium thiosulfate solution is 500:1, and collecting a grease layer, namely a layering product.

S6, adding sodium hydroxide into the layered product in the step S5, wherein the mass ratio of the sodium hydroxide to the molten product is 1:80-100, precipitating for 4-6 hours, and collecting supernatant, namely refined lanolin.

Example 3

The refining process of crude lanolin provided by this example has the following specific technical scheme:

the refining process of crude lanolin includes the following steps:

s1, introducing the crude lanolin into an oven for melting, wherein the temperature of the oven is 60 ℃, and obtaining a molten product. The crude lanolin in a molten state can be put into a reaction kettle for subsequent operation.

S2, introducing the molten product obtained in the step S1 into a reaction kettle (the temperature is set to be 60 ℃) and adding a sodium sulfate solution with the concentration of 85% to carry out acidification reaction, wherein the mass ratio of the sodium sulfate solution to the molten product is 1:500, and obtaining an acidified product. Sodium sulfate is added to prevent the subsequent hydrogen peroxide from reacting too fast, and the reaction speed of the hydrogen peroxide is adjusted.

And S3, adding hydrogen peroxide into the acidified product obtained in the step S2, stirring (the temperature is 60 ℃ and the time is 45min), and decoloring, wherein the addition amount of the hydrogen peroxide is 4-6% of the mass of the crude lanolin obtained in the step S1, so that a decolored product is obtained. The hydrogen peroxide and impurities in the lanolin form peroxides, and the hydrogen peroxide is also used for bleaching.

S4, performing vacuum deodorization treatment on the decolorized product in the step S3, wherein the vacuum deodorization comprises the following steps: heating the reaction kettle to 90 ℃, and deodorizing for 5 hours under the condition that the vacuum degree is 480mmHg to obtain a deodorizing product. This step removes the off-flavor from the crude lanolin.

S5, adding 28% isopropanol solution into the deodorization product in the step S4 for layering and impurity removal, adding 0.25L of isopropanol solution into each 1kg of melting product, then adding 85% sodium thiosulfate solution, wherein the mass ratio of the melting product to the sodium thiosulfate solution is 500:1, and collecting a grease layer, namely a layering product. The isopropyl alcohol is used to reduce the emulsification of the surfactant in the reactor liquid, and is effective to remove impurities from the oil again, separating the impurities from the oil layer. As shown in fig. 2, the layering is divided into three layers, namely a grease layer, a saponification layer and a water + impurity layer from top to bottom, the water + impurity layer is discharged firstly, and the discharging time is less than 30 min; discharging the saponified layer for less than 30 min. The last remaining grease layer was collected.

S6, adding sodium hydroxide into the layered product in the step S5, wherein the mass ratio of the sodium hydroxide to the molten product is 1:90, precipitating for 5 hours, and collecting supernatant, namely refined lanolin. Sodium hydroxide is used to neutralize free fatty acids in crude lanolin.

0.017% of BHT antioxidant is added into refined lanolin, so as to prevent air from entering the lanolin, and oxidize the surface of the lanolin to degrade the lanolin.

The lanolin obtained in the embodiment is a light yellow paste, the Hunter whiteness is 94.56%, the odor is pure and free of grease odor, the bacteria detection is qualified, and no skin irritation response is detected.

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.