CN113355154B - Refining process of peony seed oil - Google Patents
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- CN113355154B CN113355154B CN202110694294.2A CN202110694294A CN113355154B CN 113355154 B CN113355154 B CN 113355154B CN 202110694294 A CN202110694294 A CN 202110694294A CN 113355154 B CN113355154 B CN 113355154B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
- C11B3/14—Refining fats or fatty oils by distillation with the use of indifferent gases or vapours, e.g. steam
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a refining process of peony seed oil, which relates to the technical field of vegetable oil refining and comprises the following steps: (1) degumming; (2) deacidifying; (3) decoloring; (4) deodorization. The refining of the peony seed oil is completed through four procedures of degumming, deacidification, decoloration and deodorization, the operation is simple, the energy consumption is low, the content of colloidal impurities, the pigment content and the acid value in the finished oil can be obviously reduced, the odor substances in the oil can be removed, the flavor of the finished oil is improved, and the safety of the finished oil is improved.
Description
Technical field:
the invention relates to the technical field of vegetable oil refining, in particular to a refining process of peony seed oil.
The background technology is as follows:
the peony seed oil is the most suitable for human nutrition in the grease discovered so far, and is the most high in nutritive value and the most reasonable in component structure in all edible oils. Peony seed oil contains abundant polyunsaturated fatty acids, which have a nutritional value far exceeding that of olive oil known as "oil for human health". Multiple indexes are higher than other oil types, and are not easy to oxidize and deposit on the vascular wall, the heart coronary artery and other parts of the human body. It is these components that make them play an important role in medicine and nutrition and become ideal edible oils, which are known as "the best edible oils in the world".
The oil refining refers to a series of processes for removing solid impurities, free fatty acids, phospholipids, gum, wax, pigment, and odor contained in vegetable oil. Refining methods generally comprise two main types, namely physical refining and chemical refining, and chemical refining is widely adopted because of the characteristics of wide application range, high and stable quality of refined oil. Chemical refining comprises four steps of degumming, deacidification, decoloration and deodorization, which is commonly called as 'four-step'.
The colloid impurities in the crude oil are mainly phosphorus, so that the quality of the oil is reduced, excessive emulsification between the oil and alkali liquor is promoted in the alkali refining deacidification process, the separation difficulty of the Chinese honeylocust is increased, and the loss of the neutral oil is aggravated. At present, a method of hydration degumming is mainly adopted, and the hydration degumming is a degumming mode that a certain amount of hot water or dilute alkali, saline solution, phosphoric acid and other electrolyte water solutions are added into crude oil at a certain temperature under stirring to coagulate, precipitate and separate the peptized impurities by utilizing the hydrophilization of peptized impurities such as phospholipids and the like. Although the cost of hydration degumming is low, the effect is limited, and the addition of dilute alkali and phosphoric acid can increase the difficulty of wastewater treatment.
The invention comprises the following steps:
the invention aims to solve the technical problem of providing the refining process of the peony seed oil, which not only can effectively reduce the phosphorus content in crude oil, but also is simple and convenient to operate and suitable for batch refining of the crude oil.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
a refining process of peony seed oil comprises the following steps:
(1) Degumming: firstly filtering peony seed crude oil to remove solid particle impurities, then adding calcium gluconate under low-speed stirring, stirring at high speed, adding hot water, stirring at low speed, stopping stirring, standing, and separating to remove water and colloid to obtain degummed oil;
(2) Deacidifying: adding alkali liquor into the degummed oil under high-speed stirring for neutralization, turning to low-speed stirring when soapstock particles appear, stopping stirring, standing, separating an oil layer, and washing the oil layer with water to obtain deacidified oil;
(3) Decoloring: adding active carbon into deacidified oil under high-speed stirring, decolorizing under vacuum, and filtering to obtain a colorless oil;
(4) Deodorizing: pumping the decolorized oil into a deodorizing tower, heating the decolorized oil under vacuum, introducing steam for steam stripping, continuously heating, maintaining the temperature for deodorizing, cooling, and filtering to obtain the final product oil.
The degumming method is different from the prior art in that the calcium gluconate is added first and then the hot water is added, so that the addition of the calcium gluconate can reduce the energy consumption, quicken the flocculation speed, reduce the oil content of the flocculation and optimize the degumming effect.
The addition amount of the calcium gluconate is 0.1-0.5% of the weight of the peony seed crude oil.
The temperature of the hot water is 50-60 ℃, and the addition amount of the hot water is 5-10% of the weight of the peony seed crude oil.
The alkali liquor is sodium hydroxide solution with the mass concentration of 10-20%. The neutralization reaction is utilized to play a deacidification role, and the consumption of alkali liquor is calculated based on the actual acid value of the peony seed oil.
The addition amount of the activated carbon is 1-5% of the weight of the deacidified oil. The pigment in the peony seed oil is efficiently removed by utilizing the strong adsorption effect of the activated carbon.
The vacuum decoloring temperature is 50-60 ℃ and the vacuum degree is 0.01-0.1 MPa. The low-temperature vacuum decolorization is adopted, so that the decolorization time can be shortened, the decolorization temperature can be reduced, and the decolorization effect can be ensured.
The vacuum degree of the heated and dehydrated oil under vacuum is 0.01-0.1 MPa, and the temperature is 120-140 ℃.
The vacuum degree of the steam is 0.01-0.1 MPa.
The temperature of the heat preservation and deodorization is 220-240 ℃.
The rotating speed of the high-speed stirring is 100-300r/min, and the rotating speed of the low-speed stirring is 10-50r/min. The process of degumming, deacidification and decoloration procedures is controlled by adjusting the stirring speed, so that the treatment effect is improved.
The activated carbon belongs to a common decolorizing agent in the field, and when the activated carbon is used for decolorizing the peony seed oil, the decolorizing capacity is limited because the viscosity of the peony seed oil is high. The invention also provides a preparation method of the modified activated carbon, and the prepared modified activated carbon replaces the activated carbon in the technical scheme to be used for decoloring deacidified oil.
The modified activated carbon is prepared from activated carbon and N, N-dimethylformamide, and the preparation method comprises the following steps: adding activated carbon into N, N-dimethylformamide water solution with the volume concentration of 50-80%, carrying out ultrasonic treatment, filtering, drying in a baking oven at 100-120 ℃, transferring into a roasting furnace, and roasting in an inert atmosphere at 400-500 ℃ to obtain the modified activated carbon.
The mass ratio of the active carbon to the N, N-dimethylformamide aqueous solution is 1:5-10.
The specific surface area and the pore diameter of the activated carbon are increased by modifying the activated carbon with N, N-dimethylformamide, so that the adsorption activity of the activated carbon is improved.
The beneficial effects of the invention are as follows:
(1) According to the invention, the peony seed crude oil is not heated in the degumming procedure, and hot water is adopted instead of boiling water, so that the heating energy consumption can be greatly reduced; meanwhile, in order to ensure the degumming effect, calcium gluconate is used as a degumming auxiliary agent, and the colloid impurities in the peony seed crude oil are efficiently removed by the hydration degumming principle, so that the phosphorus content is reduced.
(2) The refining of the peony seed oil is completed through four procedures of degumming, deacidification, decoloration and deodorization, the operation is simple, the energy consumption is low, the content of colloidal impurities, the pigment content and the acid value in the finished oil can be obviously reduced, the odor substances in the oil can be removed, the flavor of the finished oil is improved, and the safety of the finished oil is improved.
The specific embodiment is as follows:
the invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
(1) Degumming: filtering 10kg of peony seed crude oil, removing solid particle impurities, adding calcium gluconate accounting for 0.4% of the weight of the peony seed crude oil under low-speed stirring at 30r/min, stirring at 150r/min for 30min, adding hot water accounting for 5% of the weight of the peony seed crude oil at 60 ℃, stirring at 30r/min for 2h, stopping stirring, standing for 5h, and separating to remove water and colloid to obtain degummed oil.
(2) Deacidifying: adding 1kg of alkali liquor with the mass concentration of 20% into the degummed oil under high-speed stirring at 150r/min for neutralization, turning to low-speed stirring at 50r/min when nigre particles appear, stopping stirring, standing for 3h, separating an oil layer, and washing the oil layer with water to obtain the deacidified oil.
(3) Decoloring: adding 3% of active carbon by weight of deacidified oil into deacidified oil under high-speed stirring at 200r/min, vacuum decolorizing for 5h at 60deg.C under vacuum degree of 0.07MPa, and filtering to obtain colorless oil.
(4) Deodorizing: pumping the decolorized oil into a deodorizing tower, heating the decolorized oil under vacuum at a vacuum degree of 0.08MPa and a temperature of 140 ℃, introducing steam with a vacuum degree of 0.05MPa for steam stripping for 0.5h, continuously heating to 230 ℃, preserving heat and deodorizing for 1h, cooling, and filtering to obtain the finished oil.
Example 2
(1) Degumming: filtering 10kg of peony seed crude oil, removing solid particle impurities, adding calcium gluconate accounting for 0.5% of the weight of the peony seed crude oil under 40r/min low-speed stirring, stirring at 250r/min high speed for 30min, adding hot water accounting for 10% of the weight of the peony seed crude oil at 60 ℃, stirring at 40r/min low speed for 2h, stopping stirring, standing for 5h, and separating to remove water and colloid to obtain degummed oil.
(2) Deacidifying: adding 1kg of alkali liquor with the mass concentration of 20% into the degummed oil under high-speed stirring at 200r/min for neutralization, turning to low-speed stirring at 30r/min when nigre particles appear, stopping stirring, standing for 3h, separating an oil layer, and washing the oil layer with water to obtain the deacidified oil.
(3) Decoloring: adding activated carbon accounting for 4% of the deacidified oil by weight into the deacidified oil under high-speed stirring at 250r/min, decolorizing under vacuum for 5h at 60 ℃ and under vacuum degree of 0.05MPa, and filtering to obtain the deacidified oil.
(4) Deodorizing: pumping the decolorized oil into a deodorizing tower, heating the decolorized oil under vacuum at a vacuum degree of 0.08MPa and a temperature of 120 ℃, introducing steam with a vacuum degree of 0.05MPa for steam stripping for 1h, continuously heating to 230 ℃, preserving heat and deodorizing for 0.5h, cooling, and filtering to obtain the finished oil.
Example 3
(1) Degumming: filtering 10kg of peony seed crude oil, removing solid particle impurities, adding calcium gluconate accounting for 0.5% of the weight of the peony seed crude oil under low-speed stirring at 50r/min, stirring at high speed at 200r/min for 30min, adding hot water accounting for 8% of the weight of the peony seed crude oil at 60 ℃, stirring at low speed at 40r/min for 2h, stopping stirring, standing for 5h, and separating to remove water and colloid to obtain degummed oil.
(2) Deacidifying: adding 1kg of alkali liquor with the mass concentration of 20% into the degummed oil under high-speed stirring at 200r/min for neutralization, turning to low-speed stirring at 40r/min when nigre particles appear, stopping stirring, standing for 3h, separating an oil layer, and washing the oil layer with water to obtain the deacidified oil.
(3) Decoloring: adding activated carbon accounting for 5% of the deacidified oil by weight into the deacidified oil under high-speed stirring at 200r/min, decolorizing under vacuum for 5h at 60 ℃ and under vacuum degree of 0.08MPa, and filtering to obtain the deacidified oil.
(4) Deodorizing: pumping the decolorized oil into a deodorizing tower, heating the decolorized oil under vacuum at 130 ℃ and 0.08MPa, steam at 0.05MPa is introduced to strip for 1h, heating to 230 ℃, preserving heat and deodorizing for 1h, cooling, and filtering to obtain the final product oil.
Example 4
Example 4 differs from example 1 in that the activated carbon was replaced with an equivalent amount of modified activated carbon, which was prepared as follows:
adding 10g of active carbon into 55g of N, N-dimethylformamide water solution with the volume concentration of 65%, carrying out ultrasonic treatment for 3h, filtering, drying in a baking oven at 110 ℃ to constant weight, transferring into a baking furnace, and baking in an argon atmosphere at 500 ℃ for 5h to obtain the modified active carbon.
Comparative example 1
Comparative example 1 differs from example 1 in that the calcium gluconate is replaced by an equivalent amount of citric acid.
Comparative example 2
Comparative example 2 differs from example 1 in that no calcium gluconate was added.
The phosphorus content of the finished oils of example 1, example 2, example 3, comparative example 1, comparative example 2 were measured according to the first method of GB 5009.87-2016 determination of phosphorus in food safety national standard food, and the results are shown in Table 1.
TABLE 1
Project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
Phosphorus content mg/kg | 6.5 | 5.8 | 5.2 | 10.4 | 15.7 |
From the data in table 1, it can be seen that the addition of calcium gluconate can enhance the degumming effect.
The peony seed crude oil was scanned for full wavelength using a UV-1900i type UV-vis spectrophotometer to determine the maximum absorption wavelength, and absorbance before and after refining of examples 1, 2, 3, and 4 was measured at this wavelength, and the decolorization ratio was calculated, and the results are shown in table 2.
Decoloration ratio= (A) 0 -A 1 )/A 0 ×100%;
A 0 Absorbance before refining; a is that 1 The absorbance before refining.
TABLE 2
Project | Example 1 | Example 2 | Example 3 | Example 4 |
Decoloring rate% | 91.2 | 92.8 | 94.3 | 97.5 |
As can be seen from the data in table 2, the use of modified activated carbon can enhance the decolorizing effect.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The refining process of the peony seed oil is characterized by comprising the following steps of:
(1) Degumming: firstly filtering peony seed crude oil to remove solid particle impurities, then adding calcium gluconate under low-speed stirring, stirring at high speed, adding hot water, stirring at low speed, stopping stirring, standing, and separating to remove water and colloid to obtain degummed oil;
(2) Deacidifying: adding alkali liquor into the degummed oil under high-speed stirring for neutralization, turning to low-speed stirring when soapstock particles appear, stopping stirring, standing, separating an oil layer, and washing the oil layer with water to obtain deacidified oil;
(3) Decoloring: adding modified activated carbon into deacidified oil under high-speed stirring, decolorizing under vacuum, and filtering to obtain a colorless oil;
(4) Deodorizing: pumping the decolorized oil into a deodorizing tower, heating the decolorized oil under vacuum, introducing steam for steam stripping, continuously heating, preserving heat and deodorizing, cooling, and filtering to obtain the final product oil;
the modified activated carbon is prepared from activated carbon and N, N-dimethylformamide, and the preparation method comprises the following steps: adding activated carbon into an N, N-dimethylformamide water solution with the volume concentration of 50-80%, carrying out ultrasonic treatment, filtering, drying in a baking oven at 100-120 ℃, transferring into a roasting furnace, and roasting in an inert atmosphere at 400-500 ℃ to obtain modified activated carbon;
the mass ratio of the active carbon to the N, N-dimethylformamide aqueous solution is 1:5-10.
2. The refining process of peony seed oil according to claim 1, wherein: the addition amount of the calcium gluconate is 0.1-0.5% of the weight of the peony seed crude oil.
3. The refining process of peony seed oil according to claim 1, wherein: the temperature of the hot water is 50-60 ℃, and the addition amount of the hot water is 5-10% of the weight of the peony seed crude oil.
4. The refining process of peony seed oil according to claim 1, wherein: the alkali liquor is sodium hydroxide solution with the mass concentration of 10-20%.
5. The refining process of peony seed oil according to claim 1, wherein: the addition amount of the modified activated carbon is 1-5% of the weight of the deacidified oil.
6. The refining process of peony seed oil according to claim 1, wherein: the vacuum decoloring temperature is 50-60 ℃, and the vacuum degree is 0.01-0.1 MPa.
7. The refining process of peony seed oil according to claim 1, wherein: the vacuum degree of the heated and dehydrated oil under vacuum is 0.01-0.1 MPa, and the temperature is 120-140 ℃.
8. The refining process of peony seed oil according to claim 1, wherein: the temperature of the heat preservation and deodorization is 220-240 ℃.
9. The refining process of peony seed oil according to claim 1, wherein: the rotating speed of the high-speed stirring is 100-300r/min, and the rotating speed of the low-speed stirring is 10-50r/min.
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RU79889U1 (en) * | 2008-06-20 | 2009-01-20 | Государственное образовательное учреждение высшего профессионального образования "Ульяновский государственный технический университет" | DEVICE FOR CLEANING OIL PRODUCTS FROM SERAORGANIC IMPURITIES |
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