Flash evaporation deodorization method of wool fat

Abstract

The invention discloses a flash evaporation deodorization method for wool fat, and belongs to the technical field of wool fat refining. The method comprises the following steps: S101, dissolving crude wool fat in anhydrous hot ethanol with the volume 4-6 times that of the crude wool fat, feeding the crude wool fat to the inner upper part of vacuum flash evaporation equipment, and spraying the crude wool fat downwards; s102, introducing hot nitrogen into the lower part of the vacuum flash evaporation equipment, wherein the temperature of the hot nitrogen is 95-105 DEG C, and the hot nitrogen is in countercurrent contact with the crude wool fat spraying liquid; and S103, circularly spraying the crude wool fat in the vacuum flash evaporation equipment for a certain time, then conveying the crude wool fat into a first oil-water separator for cooling, and separating ethanol to obtain the wool fat. Exhaust gas of the vacuum flash evaporation equipment is sequentially conveyed to a dynamic wave tower, a condenser, a gas-liquid separator and vacuum equipment; absolute ethyl alcohol is circularly sprayed into the dynamic wave tower, and the temperature of spraying liquid in the dynamic wave tower is 45-50 DEG C. The method provided by the invention can deodorize the wool fat to be tasteless, and also has the advantages of obviously reducing the chromaticity, having higher yield and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of lanolin refining, and particularly relates to a flash deodorization method for lanolin. Background Art

[0002] Lanolin is a mixture of esters, hydrocarbons and lipids secreted by the sebaceous glands of sheep and adhering to the fur. Lanolin and its modified products are widely used in cosmetics, leather, medicine and other industries.

[0003] Crude lanolin is recovered from wool washing wastewater. It is rich in sources, but contains a lot of water, a dark color, a strong odor, and a lot of impurities that affect the quality of lanolin, such as dust, sand, plant debris, inorganic salts of sheep sweat, protein series decomposition products and pigments produced by feces, blood and these oxides, and low ester decomposition products - free fatty acids and free alcohols. Therefore, crude lanolin cannot be directly used in industries such as cosmetics and needs to be refined. Lanolin is usually refined by deacidification, decolorization, deodorization and / or chromatography. Deodorization commonly uses steam deodorization or vacuum deodorization.

[0004] For example, the patent with application number CN202110816593.9 adopts vacuum deodorization for deodorization. For example, the patent with publication number CN87100677A also adopts vacuum deodorization for deodorization.

[0005] Compared with ordinary oils, lanolin has a more complex composition and is difficult to deodorize. It is difficult to deodorize lanolin to a level that is odorless using existing technologies. Summary of the invention

[0006] In order to solve the above problems, the embodiment of the present invention provides a flash deodorization method for lanolin, which utilizes the characteristics that lanolin is insoluble in low-temperature ethanol but soluble in hot ethanol, ethanol itself is volatile, and ethanol is easy to distill. The technical solution is as follows: See also Figure 2 The embodiment of the present invention provides a flash deodorization method for lanolin, the method comprising: S101: Dissolve the crude lanolin in 4-6 times the volume of anhydrous hot ethanol, and then send it to the upper part of the vacuum flash evaporation equipment and spray it downward.

[0007] S102: Hot nitrogen is introduced into the lower part of the vacuum flash evaporation equipment. The temperature of the hot nitrogen is 95-105°C and it is in countercurrent contact with the crude lanolin spray liquid, which has multiple functions: first, heating the crude lanolin, second, removing odorous substances, and third, evaporating ethanol (there are multiple functions, first, reducing the amount of ethanol, second, removing some impurities, third, facilitating the subsequent recovery of lanolin, and fourth, reducing the amount of liquid carried by lanolin).

[0008] S103: After the crude lanolin is circulated and sprayed in the vacuum flash evaporation equipment for a certain period of time (specifically 2-5 hours), it is sent to the first oil-water separator for cooling (specifically, to below 25°C), and the lanolin is obtained after the ethanol is separated.

[0009] Among them, the exhaust gas of the vacuum flash evaporation equipment is sent to the power wave tower (the pipeline between the vacuum flash evaporation equipment is as short as possible), the condenser, the gas-liquid separator and the vacuum equipment in turn. Anhydrous ethanol is sprayed in the power wave tower in a cycle and the temperature of the spray liquid therein is 45-50°C (by controlling the spraying amount and other means, the temperature cannot be too high to avoid rapid evaporation of ethanol, nor too low to avoid solidification of lanolin). Specifically, the exhaust gas enters the power wave tower from the top and enters the power wave tower downward, the liquid is sprayed upward through the power wave nozzle in the upper or middle part of the power wave tower (to reduce the liquid), the gas contacts the liquid in the countercurrent, the liquid of the power wave tower is sprayed in a cycle, and the gas is discharged from the lower part of the power wave tower. Preferably, an overflow weir is set in the upper part of the power wave tower, and the overflow weir overflows the liquid to the inner wall of the power wave tower to prevent the grease from condensing on the inner wall of the power wave tower. Part of the liquid at the bottom of the power wave tower is sent to the power wave nozzle in the power wave tower, and the other part is sent to the overflow weir. The vacuum degree of the vacuum flash evaporation equipment is -60--30KPa. The spraying volume of the vacuum flash evaporation equipment should ensure that after deodorization, the crude lanolin contains at least one volume of anhydrous ethanol, and the flow rate of hot nitrogen should be greater than 1.0m 3 / h (for the volume of the vacuum flash equipment is 100L).

[0010] The heating reactor is connected with the vacuum flash evaporation equipment to form a circulating spray system. The heating reactor is provided with a stirrer and a first heater, etc. The heating temperature of the heating reactor is 50-60°C, and anhydrous hot ethanol and crude lanolin are added into the heating reactor according to the proportion.

[0011] Among them, the ethanol separated by the first oil-water separator is sent to the heating reactor for reuse after being decolorized and distilled by activated carbon. The decolorization conditions are 30-40°C, the amount of activated carbon used is 3-6% of the weight of lanolin, and the decolorization time is 30-60 minutes. The applicant found that the color of the ethanol separated by the first oil-water separator is darker, and the ethanol recovered by the power wave tower and the condenser is lighter in color (basically colorless). In order to simplify the distillation process of ethanol, the ethanol separated by the first oil-water separator is decolorized to reduce the difficulty of distillation.

[0012] Among them, the liquid output by the vacuum flash evaporation equipment is first filtered (specifically, a pipeline filter, which is filtered while hot) and then sent to the first oil-water separator.

[0013] Among them, after a predetermined time, the spray liquid in the power wave tower is output to the second oil-water separator; in the second oil-water separator, the temperature of the liquid is reduced to below 30°C and the oil in the lower part is separated, and the oil (solidified) is sent to the heating reactor for reuse.

[0014] Furthermore, the condensate (mainly ethanol) separated by the condenser and the liquid phase separated by the gas-liquid separator are sent to the power wave tower (while fresh anhydrous ethanol is added regularly or as needed), and the ethanol separated by the second oil-water separator is distilled and sent to the heating reactor for reuse.

[0015] Furthermore, a defoamer is provided at the top of the vacuum flash equipment to reduce the amount of grease entering subsequent equipment, a second heater is provided at the bottom to prevent the lanolin from solidifying (such as heating to 40-50°C), and the bottom is connected to the heating reactor and the first oil-water separator through a pipeline.

[0016] Specifically, the condensation temperature of the condenser is 0-10°C, and a multi-stage structure can be adopted. The first stage structure uses circulating water for condensation, and the second stage structure can use ice salt water for condensation.

[0017] Specifically, an embodiment of the present invention provides a flash deodorization method for lanolin, the method comprising: S101: Dissolve the crude lanolin in 4-6 times the volume of anhydrous hot ethanol, and then send it to the upper part of the vacuum flash evaporation equipment and spray it downwards. The temperature of the spraying liquid is 50-60°C.

[0018] S102: hot nitrogen is introduced into the lower part of the vacuum flash evaporation equipment, wherein the temperature of the hot nitrogen is 95-105°C and it is in countercurrent contact with the crude lanolin spray liquid, and the vacuum degree of the vacuum flash evaporation equipment is -60--30KPa.

[0019] S103: After the crude lanolin is circulated and sprayed in the vacuum flash evaporation equipment for 2-5 hours, it is sent to the first oil-water separator for cooling, and the lanolin is obtained after the ethanol is separated.

[0020] S104: The ethanol separated by the first oil-water separator is sent to the heating reactor for reuse after being decolorized and distilled by activated carbon. After a predetermined time, the spray liquid in the power wave tower is output to the second oil-water separator; in the second oil-water separator, the temperature of the liquid is reduced to below 30°C and the oil and fat in the lower part are separated, and the oil and fat are sent to the heating reactor for reuse. The condensate separated by the condenser and the liquid phase separated by the gas-liquid separator are sent to the power wave tower, and the ethanol separated by the second oil-water separator is sent to the heating reactor for reuse after being distilled.

[0021] The exhaust gas of the vacuum flash evaporation equipment is sequentially sent to the power wave tower, condenser, gas-liquid separator and vacuum equipment, etc. Anhydrous ethanol is circulated and sprayed in the power wave tower, and the temperature of the spray liquid therein is 45-50°C.

[0022] The technical solution provided by the embodiment of the present invention has the following beneficial effects: (1) Lanolin can be deodorized to no odor; (2) While deodorizing, the color of lanolin can be significantly reduced; for lanolin with low requirements, it can be used directly without decolorization; (3) The power wave tower has three functions: first, to cool the lanolin to facilitate the subsequent condensation process (small condensation temperature difference); second, to recover the lanolin (the recovered lanolin is sent to the heating reactor for reuse), which can increase the lanolin yield to more than 97% (similar to conventional technology); third, to separate the lanolin to prevent the lanolin from condensing on the condenser and pipeline, and to avoid blockage and poor condensation effect. The condenser recovers the ethanol evaporated from the vacuum flash evaporation equipment and the power wave tower. The gas-liquid separator is used to separate the liquid carried by the power wave tower and the condensate of the condenser.

[0023] (4) It can significantly reduce the solid content of lanolin, dissolve the solid content and make it easier to filter; (5) No ethanol is discharged. Compared with lanolin, ethanol is very easy to distill and recycle. Ethanol after simple distillation does not contain the pigments and odorous substances contained in lanolin. Usually only a small amount of ethanol needs to be added, and lanolin usually does not contain ethanol. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a principle block diagram of a flash deodorization system for lanolin provided by an embodiment of the present invention; Figure 2 The present invention provides a flash deodorization method for lanolin. DETAILED DESCRIPTION

[0025] In order to make the objectives, technical solutions and advantages of the present invention more clear, the present invention will be further described in detail below with reference to the accompanying drawings.

[0026] Example 1 Example 1 discloses a flash deodorization method for lanolin, the method comprising: S101: Dissolve 30 kg of crude lanolin (chromaticity 14.7, strong odor, brown color, volume 32 L) in 5 times the volume of anhydrous hot ethanol, and then send it to the upper part of the vacuum flash evaporation equipment and spray it downwards at a spraying temperature of 57°C.

[0027] S102: Hot nitrogen is introduced into the lower part of the vacuum flash evaporation equipment. The temperature of the hot nitrogen is 98°C and it is in countercurrent contact with the crude lanolin spray liquid. The flow rate of the hot nitrogen is 1.5m 3 / h, the vacuum degree of the vacuum flash evaporation equipment is -55Kpa. The exhaust gas of the vacuum flash evaporation equipment is sent to the power wave tower, condenser, gas-liquid separator and vacuum equipment in sequence; anhydrous ethanol is sprayed in the power wave tower in a cycle and the temperature of the spray liquid is 48℃.

[0028] S103: After the crude lanolin is circulated and sprayed in the vacuum flash evaporation equipment for 4 hours, it is filtered and sent to the first oil-water separator for cooling. After separating the ethanol (volume is about 46L), 29.2kg of lanolin is obtained.

[0029] S104: The ethanol separated by the first oil-water separator is decolorized and distilled by activated carbon and then sent to step S101 for reuse. After a predetermined time, the spray liquid in the power wave tower is output to the second oil-water separator; in the second oil-water separator, the temperature of the liquid is reduced to 20°C and the grease in the lower part is separated, and the grease is sent to step S101 for reuse. The condensate separated by the condenser is sent to the power wave tower, and the ethanol separated by the second oil-water separator is distilled and sent to step S101 for reuse.

[0030] The chromaticity of the treated lanolin is 8.8, the color is light yellow, it has no odor and the melting point is 39.2°C.

[0031] Example 2 Example 2 discloses a flash deodorization method for lanolin, the method comprising: S101: Dissolve 30 kg of crude lanolin (chromaticity 14.7, strong odor, brown) in 5.5 volumes of anhydrous hot ethanol, and then send it to the upper part of the vacuum flash evaporation equipment and spray it downwards at a spraying temperature of 55°C.

[0032] S102: Hot nitrogen is introduced into the lower part of the vacuum flash evaporation equipment. The temperature of the hot nitrogen is 100°C and it is in countercurrent contact with the crude lanolin spray liquid. The flow rate of the hot nitrogen is 1.4m 3 / h, the vacuum degree of the vacuum flash evaporation equipment is -45Kpa. The exhaust gas of the vacuum flash evaporation equipment is sent to the power wave tower, condenser, gas-liquid separator and vacuum equipment in sequence; anhydrous ethanol is sprayed in the power wave tower in a cycle and the temperature of the spray liquid is 48℃.

[0033] S103: After the crude lanolin is circulated and sprayed in the vacuum flash evaporation equipment for 4.5 hours, it is filtered and sent to the first oil-water separator for cooling. After separating ethanol (volume is about 51L), 29.0kg of lanolin is obtained.

[0034] S104: The ethanol separated by the first oil-water separator is decolorized and distilled by activated carbon and then sent to step S101 for reuse. After a predetermined time, the spray liquid in the power wave tower is output to the second oil-water separator; in the second oil-water separator, the temperature of the liquid is reduced to 20°C and the grease in the lower part is separated, and the grease is sent to step S101 for reuse. The condensate separated by the condenser is sent to the power wave tower, and the ethanol separated by the second oil-water separator is distilled and sent to step S101 for reuse.

[0035] The chromaticity of the treated lanolin is 8.9, the color is light yellow, odorless, and the melting point is 39.2°C.

[0036] Verification Example The vacuum deodorization conditions are: vacuum deodorization at a vacuum degree of -65 KPa and a temperature of 90°C for 4 hours.

[0037] The conditions for steam deodorization are: 97°C and the amount of steam is 0.2m 3 / kg crude lanolin, deodorize for 4 hours.

[0038] The conditions for nitrogen deodorization are as follows: the crude lanolin is heated to 57°C, sent to a vacuum flash evaporation device, and countercurrently contacted with hot nitrogen at 98°C, with a vacuum degree of -45Kpa.

[0039] The conditions for the ethanol extraction treatment are as follows: dissolving lanolin in 5 times the volume of hot anhydrous ethanol, the extraction temperature is 57°C, stirring for 2 hours, filtering, and then standing for 4 hours and cooling to room temperature to separate the ethanol.

[0040] The conditions of the composite treatment process are as follows: dissolving lanolin in 5 times the volume of hot anhydrous ethanol, the extraction temperature is 57°C, stirring for 2 hours, filtering, standing for 4 hours and cooling to room temperature to separate ethanol; then heating the crude lanolin to 57°C, sending it to a vacuum flash evaporation device, contacting it with 98°C hot nitrogen in countercurrent, and the vacuum degree is -45Kpa.

[0041] Among them, the solid content is the solid content detected when the lanolin is melted, and it is detected after being filtered through a pipeline filter.

[0042] Among them, the color of untreated crude lanolin is 14.7 (APHA color), the solid content is 1-2%, it has a strong odor, and is brown. + means no odor, ++ means a weak odor, +++ means a distinct odor, and ++++ means a strong odor.

[0043] Table 1

[0044] As can be seen from Table 1, the deodorization effect of the method of this patent is better than that of the prior art.

[0045] Comparative Example 1 The process of Comparative Example 1 is basically the same as that of Example 1, except that the exhaust gas of the vacuum flash evaporation equipment in this example is sent to the condenser, the gas-liquid separator and the vacuum equipment in sequence. The chromaticity of the treated lanolin is 8.8, the color is light yellow, odorless, and the melting point is 39.2°C. The yield is 92.5%. It can be seen that nitrogen will take out a large amount of lanolin, resulting in a low yield of lanolin.

[0046] Comparative Example 2 The process of Comparative Example 2 is basically the same as that of Example 1, except that the temperature of the hot nitrogen is 80°C, and the exhaust gas of the vacuum flash evaporation equipment is sent to the condenser, the gas-liquid separator and the vacuum equipment in sequence. The chromaticity of the treated lanolin is 11.5, the color is yellow, there is a faint odor, the melting point is 39.3°C, and the yield is 94.7%. It can be seen that the low temperature of the nitrogen causes the ethanol to be unable to be quickly vaporized, which in turn leads to a high amount of ethanol liquid. At a lower temperature, the decolorization and deodorization effects are not good.

[0047] Comparative Example 3 The process of comparative example 3 is basically the same as that of example 1, except that the spray temperature of the vacuum flash evaporation equipment is 65°C, and the exhaust gas of the vacuum flash evaporation equipment is sent to the condenser, the gas-liquid separator and the vacuum equipment in sequence. After treatment, the first oil-water separator separates 3L of ethanol. The chromaticity of the treated lanolin is 10.3, the color is yellow, there is a faint odor, the melting point is 39.3°C, and the yield is 94.3%. It can be seen that the temperature of the spray liquid is relatively high, and ethanol itself is easy to gasify, resulting in a low ethanol content in the spray liquid in the later stage of processing. Not only does the proportion of lanolin in the exhaust liquid account for a large proportion, but the decolorization and deodorization treatment effects are also poor.

[0048] Comparative Example 4 The process of comparative example 4 is basically the same as that of example 1, except that: 57°C crude lanolin (dissolved in hot ethanol) is directly sprayed in the vacuum flash evaporation equipment without hot nitrogen, and the exhaust gas of the vacuum flash evaporation equipment is sent to the condenser, gas-liquid separator and vacuum equipment in sequence. The chromaticity of the treated lanolin is 12.1, the color is yellow, there is a faint odor, the melting point is 39.3°C, and the yield is 92.3%. Without nitrogen, there are three problems: first, the odorous substances and pigment substances cannot be taken away in time; second, the evaporation speed of ethanol is slow, not only the amount of liquid is large, but also the deodorization and decolorization effects are affected; third, the temperature is low, and the deodorization and decolorization effects are not good. As a result, the deodorization effect is not as good as the vacuum deodorization effect.

[0049] Comparative Example 5 The process of Comparative Example 5 is basically the same as that of Example 1, except that: 65°C crude lanolin (dissolved in hot ethanol) is directly sprayed in the vacuum flash evaporation device (the heating effect is similar to that of hot nitrogen), hot nitrogen is not introduced, and the exhaust gas of the vacuum flash evaporation device is sent to the condenser, gas-liquid separator and vacuum device in sequence. In less than three hours, the ethanol is basically evaporated; the chromaticity of the treated lanolin is 11.5, the color is yellow, there is a faint odor, the melting point is 39.3°C, and the yield is 95.1%. The deodorization effect is similar to that of vacuum deodorization, but the decolorization effect is much worse.

[0050] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A flash deodorization method for lanolin, characterized in that: The method comprises: S101: dissolving crude lanolin in 4-6 times the volume of anhydrous hot ethanol, and then sending it to the upper part of the vacuum flash evaporation equipment and spraying it downward; S102: introducing hot nitrogen gas into the lower part of the vacuum flash evaporation equipment, wherein the hot nitrogen gas has a temperature of 95-105° C. and is in countercurrent contact with the crude lanolin spray liquid; S103: After the crude lanolin is circulated and sprayed in the vacuum flash evaporation device for a certain period of time, it is sent to the first oil-water separator for cooling, and the lanolin is obtained after the ethanol is separated; Among them, the exhaust gas of the vacuum flash evaporation equipment is sent to the power wave tower, condenser, gas-liquid separator and vacuum equipment in sequence; anhydrous ethanol is circulated and sprayed in the power wave tower and the temperature of the spraying liquid is 45-50°C, and the vacuum degree of the vacuum flash evaporation equipment is -60—-30KPa.

2. The flash deodorization method of lanolin according to claim 1, characterized in that: The heating reaction kettle is connected with the vacuum flash evaporation equipment to form a circulating spray system. The heating reaction kettle is provided with a stirrer and a first heater. The heating temperature of the heating reaction kettle is 50-60°C. Anhydrous hot ethanol and crude lanolin are added into the heating reaction kettle according to a proportion.

3. The flash deodorization method of lanolin according to claim 2, characterized in that: The ethanol separated by the first oil-water separator is sent to the heating reactor for reuse after being decolorized and distilled by activated carbon.

4. The flash deodorization method of lanolin according to claim 3, characterized in that: The liquid output from the vacuum flash evaporation device is first filtered and then sent to the first oil-water separator.

5. The flash deodorization method of lanolin according to claim 2, characterized in that: After a predetermined time, the spray liquid in the power wave tower is output to the second oil-water separator; in the second oil-water separator, the temperature of the liquid is reduced to below 30°C and the oil in the lower part is separated, and the oil is sent to the heating reactor for reuse.

6. The flash deodorization method of lanolin according to claim 5, characterized in that: The condensate separated by the condenser is sent to the power wave tower.

7. The flash deodorization method of lanolin according to claim 2, characterized in that: The ethanol separated by the second oil-water separator is distilled and then sent to the heating reactor for reuse.

8. The flash deodorization method of lanolin according to claim 2, characterized in that: The vacuum flash evaporation equipment is provided with a defoamer at the top and a second heater at the bottom to prevent the lanolin from solidifying. The bottom is connected to the heating reactor and the first oil-water separator through a pipeline.

9. The flash deodorization method of lanolin according to claim 1, characterized in that: The condensation temperature of the condenser is 0-10°C.

10. The flash deodorization method of lanolin according to claim 1, characterized in that: The crude lanolin is circulated and sprayed in the vacuum flash evaporation equipment for 2-5 hours.

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