CN108559620B - Production method of torreya grandis refined oil - Google Patents
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings or cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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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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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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- 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
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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- 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
- C11B3/16—Refining fats or fatty oils by mechanical means
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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
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
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Abstract
The invention belongs to the technical field of oil refining. The invention discloses a production method of torreya grandis refined oil, which comprises two processes of crude oil extraction and refining, wherein the refining comprises the process steps of degumming, deacidification, decoloration, winterization and the like. The invention provides a special process for refining and processing Chinese torreya oil, aiming at the problem that the Chinese torreya oil production does not have a special production process technology. The refining technology provided by the invention has the advantages of simple refining process, clear process parameters and strong operability; the quality index of the refined oil meets the national edible oil standard, and the fatty acid keeps the original ecology; the refined oil retains the inherent taste, smell and flavor of the Chinese torreya oil; no crystallization, ribbon, granular crystallization or trace cloud-like precipitation occurs in the storage process of the refined oil, and the commodity performance is good; the oil yield of refining is high, and the refining cost is low.
Description
Technical Field
The invention relates to the technical field of oil refining, in particular to a production method of torreya grandis refined oil.
Background
Torreya is a gymnosperm of Taxaceae (Taxaceae) genus Torreya, and is evergreen arbour. Chinese has 3 varieties and 2 varieties of torreya: the first variety is Torreya grandis (Torreya grandis fort. ex lindl.) distributed in zhejiang, anhui, fujian and jiang; the second variety is Torreya grandis (Torreya fargesii) distributed in the areas of Qinbai mountain, Zhibaxing and Emei; the third variety is Torreya jackii (Torreya jackii) distributed in Zhejiang, Fujian and Jiangxi; the first of the 2 varieties is Torreya fargesii var. yunnanensis distributed in Yunnan (and Burma), and the second variety is Torreya delongensis distributed in Tuchang, Zhejiang. The Chinese Torreya seeds are mainly edible by artificial planting or harvesting, namely Chinese Torreya (Torreya grandis fort. var. Merrillii), are varieties (strains) artificially bred from Chinese Torreya trees, are propagated into nursery stocks through grafting propagation or cutting propagation and then popularized and planted, are mainly concentrated in 10 provinces such as Zhejiang, Su, Wan, Jiang and the like in the south of Yangtze river basin, and are concentrated in city counties such as Zhuge, Zhongzhou, Dongyang and the like in the Huishan area of Zhejiang province.
The oil content of Chinese torreya kernels is up to 50%, the content of linoleic acid and oleic acid in fatty acid components of oil is highest, and next, the contents of sciadonic acid and palmitic acid are highest. Compared with other woody plant oil, the high linoleic acid and the high pinic acid are characteristic indexes of the high nutritional function of the Chinese torreya oil, and the pinic acid is unique to the Chinese torreya oil. The Chinese torreya seed crude oil obtained by squeezing or leaching contains more impurities, has too deep color, has higher content of some solid impurities such as saponin, and has certain astringent taste when being directly eaten. Meanwhile, if the seeds are improperly stored, the undesirable substances such as aflatoxin and the like can be generated, so that many indexes of the Chinese torreya seed crude oil do not meet the national edible oil standard. Therefore, the torreya grandis seed crude oil cannot be directly used as a commodity, and needs to be refined and processed to produce refined oil. However, the fatty acid components, active substance components and physical properties of different woody plant oils are greatly different, so that the corresponding processing technology needs to be studied with pertinence.
There is no complete processing technology for refining Chinese torreya oil in production. At present, the extraction technology of Chinese torreya oil is researched more, such as cold pressing technology, supercritical extraction and the like. But the torreya grandis oil refining technology is rarely reported, and few reports are only limited to the research of a single factor in a laboratory, and no production application exists. Some enterprises try to refine and produce the Chinese torreya oil, the process is basically applied to the high-temperature refining production process of the traditional herb oil such as rapeseed oil, and the like, and the process parameters do not accord with the specific physical characteristics and the nutritional chemical characteristics of the Chinese torreya oil. The biggest problem exists in that the raw fatty acid components of the Chinese torreya oil and the special flavor, taste and smell of the Chinese torreya oil are difficult to be reserved, and the risk of generating undesirable substances such as trans-fatty acid and the like is high although the undesirable substances in the crude oil can be removed after refining processing, so that the product quality meets the relevant national standards of edible oil. Leading to the loss or damage of a plurality of precious natural active beneficial components and the flavor substances of the Chinese torreya, obviously reducing the content of active nutrient substances and almost becoming pure oil.
Disclosure of Invention
In order to solve the problems, the invention provides a production method of Chinese torreya refined oil, which can realize the refining of Chinese torreya oil and can maintain active nutrient substances and special smell of Chinese torreya oil to the maximum extent.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a production method of torreya grandis refined oil comprises the following steps:
firstly, crude oil extraction: squeezing Chinese torreya seeds, and then performing pressure filtration at normal temperature to obtain Chinese torreya crude oil;
secondly, refining:
a) degumming: mixing the crude oil and water according to the weight ratio of 10: 0.7-1.3, stirring for 10-20 minutes at 35-85 ℃, standing for 2.5-3.5 hours, and removing lower-layer impurities and water by using a settling separation method to obtain the degummed oil;
b) deacidifying: mixing the degummed oil with a sodium hydroxide solution, and performing deacidification treatment at 45-95 ℃ to obtain deacidified oil;
c) and (3) decoloring: adding deacidified oil into a decolorizing kettle, heating to 70-80 ℃, adding activated clay accounting for 2% of the weight of the deacidified oil, uniformly stirring, heating to 85-150 ℃, carrying out decolorizing reaction for 1-1.5 hours under the pressure of-0.06-0.08 MPa, cooling to 55-65 ℃, filtering while hot and naturally cooling to room temperature to obtain decolorized oil;
d) winterization: adding the decolored oil into a winterization tank, cooling to 18-22 ℃, controlling the stirring speed at 20-22 rpm, growing crystals at constant temperature for 36-60 hours, performing first filter pressing at the pressure of 0.1-0.4 MPa after crystal precipitates appear to remove the crystal precipitates and waxiness, then injecting the first filter pressing product into another winterization tank, cooling to 6-8 ℃ within 5 minutes, stirring at the speed of 10-12 rpm, continuing winterization for 10-14 hours after constant temperature, and finally performing second filter pressing at the pressure of 0.1-0.5 MPa to remove the crystal precipitates and the waxiness to obtain the torreya grandis refined oil.
Preferably, the torreya grandis crude oil is prepared by squeezing torreya grandis seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature, wherein the content of impurities in the torreya grandis crude oil is less than 0.25 wt%.
Preferably, the torreya grandis seeds are sun-dried torreya grandis seeds.
Preferably, the treatment temperature after mixing is 35-45 ℃ and the temperature of water is 35-45 ℃ during degumming in the step two a).
Preferably, in the deacidification treatment in the step two b), the weight of the sodium hydroxide in the sodium hydroxide solution is 1/10-2/10 of the weight of the degummed oil.
Preferably, the deacidification treatment in the step two b) is carried out at 48-52 ℃.
Preferably, in the step two c), activated clay is added and uniformly stirred, and then the mixture is heated to 85-95 ℃.
Preferably, in the step two c), the decoloration reaction is carried out, and then the product is cooled to 55-65 ℃ at a cooling rate of 1-3 ℃/h.
Preferably, in the step two d), the destaining oil is added into a winterization tank and cooled to 18-22 ℃ at a cooling rate of 1.5-2.5 ℃/h.
Therefore, the invention has the following beneficial effects: aiming at the current situation that no special production process technology exists in the production of Chinese torreya oil, a set of special process for refining and processing Chinese torreya oil is provided. The refining technology provided by the invention has the advantages of simple refining process, clear process parameters and strong operability; the quality index of the refined oil meets the national edible oil standard, and the fatty acid keeps the original ecology; the refined oil retains the inherent taste, smell and flavor of the Chinese torreya oil; no crystallization, ribbon, granular crystallization or trace cloud precipitation occurs in the storage process of the refined oil; the oil yield of refining is high, and the refining cost is low.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. 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.
In the present invention, all the equipments and materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
A production method of torreya grandis refined oil comprises the following steps:
firstly, crude oil extraction: squeezing the sun-dried Chinese torreya seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature to obtain Chinese torreya crude oil, wherein the content of impurities in the Chinese torreya crude oil is less than 0.25 wt%;
secondly, refining:
a) degumming: mixing the crude oil with water at the temperature of 35 ℃ according to the weight ratio of 10: 0.7, stirring for 10 minutes at 35 ℃, standing for 2.5 hours, and removing lower-layer impurities and water by a settling separation method to prepare the degummed oil;
b) deacidifying: mixing the degummed oil with a sodium hydroxide solution, and performing deacidification treatment at 45 ℃ to obtain deacidified oil; the weight of the sodium hydroxide in the added sodium hydroxide solution is 1/10-2/10 of the weight of the degummed oil;
c) and (3) decoloring: adding the deacidified oil into a decoloring kettle, heating to 70 ℃, adding activated clay accounting for 2 percent of the weight of the deacidified oil, uniformly stirring, heating to 85 ℃, decoloring under the pressure of-0.06 MPa for 1 hour, cooling to 55 ℃ at the cooling rate of 1 ℃/h, filtering while hot, and naturally cooling to room temperature to obtain the decolored oil;
d) winterization: adding the destaining oil into a winterization tank, cooling to 18 ℃ at a cooling rate of 1.5 ℃/h, controlling the stirring rate at 20rpm, growing crystals at a constant temperature for 36 hours, performing first pressure filtration at a pressure of 0.1MPa after crystal precipitates appear to remove the crystal precipitates and waxes, then injecting the first pressure filtration product into another winterization tank, cooling to 6 ℃ within 5 minutes, stirring at a rotating speed of 10rpm, continuing winterization for 10 hours after the constant temperature is maintained, and finally performing second pressure filtration at a pressure of 0.1MPa to remove the crystal precipitates and the waxes to obtain the torreya grandis refined oil.
Example 2
A production method of torreya grandis refined oil comprises the following steps:
firstly, crude oil extraction: squeezing the sun-dried Chinese torreya seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature to obtain Chinese torreya crude oil, wherein the content of impurities in the Chinese torreya crude oil is less than 0.25 wt%;
secondly, refining:
a) degumming: mixing the crude oil with water at the temperature of 90 ℃ according to the weight ratio of 10: 1.3 stirring for 20 minutes at 90 ℃ after mixing, then standing for 3.5 hours, and removing lower-layer impurities and water by a settling separation method to prepare the degummed oil;
b) deacidifying: mixing the degummed oil with sodium hydroxide according to a solution, and performing deacidification treatment at 90 ℃ to obtain deacidified oil; the weight of the sodium hydroxide in the added sodium hydroxide solution is 2/10 of the weight of the degummed oil;
c) and (3) decoloring: adding the deacidified oil into a decoloring kettle, heating to 80 ℃, adding activated clay accounting for 2 percent of the weight of the deacidified oil, uniformly stirring, heating to 150 ℃, decoloring and reacting for 1.5 hours under the pressure of 0.08MPa, cooling to 65 ℃ at the cooling rate of 3 ℃/h, filtering while hot, and naturally cooling to room temperature to obtain the decolored oil;
d) winterization: adding the destaining oil into a winterization tank, cooling to 22 ℃ at a cooling rate of 2.5 ℃/h, controlling the stirring rate at 22rpm, growing crystals at a constant temperature for 60 hours, performing first pressure filtration at a pressure of 0.4MPa after crystal precipitates appear to remove the crystal precipitates and waxes, then injecting the first pressure filtration product into another winterization tank, cooling to 8 ℃ within 5 minutes, stirring at a rotating speed of 12rpm, continuing winterization for 14 hours after the constant temperature is maintained, and finally performing second pressure filtration at a pressure of 0.5MPa to remove the crystal precipitates and the waxes to obtain the torreya grandis refined oil.
Example 3
A production method of torreya grandis refined oil comprises the following steps:
firstly, crude oil extraction: squeezing the sun-dried Chinese torreya seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature to obtain Chinese torreya crude oil, wherein the content of impurities in the Chinese torreya crude oil is less than 0.25 wt%;
secondly, refining:
a) degumming: mixing the crude oil with water at the temperature of 40 ℃ according to the weight ratio of 10: 1 stirring for 15 minutes at 40 ℃ after mixing, standing for 3 hours, and removing lower-layer impurities and water by a settling separation method to prepare the degummed oil;
b) deacidifying: mixing the degummed oil with sodium hydroxide according to a solution, and performing deacidification treatment at 50 ℃ to obtain deacidified oil; the weight of the sodium hydroxide in the added sodium hydroxide solution is 3/20 of the weight of the degummed oil;
c) and (3) decoloring: adding the deacidified oil into a decoloring kettle, heating to 75 ℃, adding activated clay accounting for 2 percent of the weight of the deacidified oil, uniformly stirring, heating to 90 ℃, decoloring under the pressure of-0.04 MPa for 1.2 hours, cooling to 60 ℃ at the cooling rate of 2 ℃/h, filtering while hot, and naturally cooling to room temperature to obtain the decolored oil;
d) winterization: adding the decolored oil into a winterization tank, cooling to 20 ℃ at a cooling rate of 2 ℃/h, controlling the stirring rate at 21rpm, growing crystals at a constant temperature for 48 hours, performing first filter pressing at a pressure of 0.25MPa after crystal precipitates appear to remove the crystal precipitates and waxiness, then injecting the first filter pressing product into another winterization tank, cooling to 7 ℃ within 5 minutes, stirring at a rotating speed of 11rpm, continuing winterization for 12 hours after the temperature is constant, and finally performing second filter pressing at a pressure of 0.3MPa to remove the crystal precipitates and the waxiness to obtain the torreya grandis refined oil.
Example 4
A production method of torreya grandis refined oil comprises the following steps:
firstly, crude oil extraction: squeezing the sun-dried Chinese torreya seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature to obtain Chinese torreya crude oil, wherein the content of impurities in the Chinese torreya crude oil is less than 0.25 wt%;
secondly, refining:
a) degumming: mixing the crude oil with water at the temperature of 45 ℃ according to the weight ratio of 10: 1 stirring for 15 minutes at 45 ℃ after mixing, standing for 3.0 hours, and removing lower-layer impurities and water by using a settling separation method to prepare the degummed oil;
b) deacidifying: mixing the degummed oil with a sodium hydroxide solution, and performing deacidification treatment at 55 ℃ to obtain deacidified oil; the weight of the sodium hydroxide in the added sodium hydroxide solution is 3/20 of the weight of the degummed oil;
c) and (3) decoloring: adding deacidified oil into a decolorizing kettle, heating to 75 ℃, adding activated clay accounting for 2 percent of the weight of the deacidified oil, stirring uniformly, heating to 95 ℃, decolorizing under the pressure of 0.02MPa for 1.2 hours, cooling to 60 ℃ at the cooling rate of 2 ℃/h, filtering while hot, and naturally cooling to room temperature to obtain decolorized oil;
d) winterization: adding the destaining oil into a winterization tank, cooling to 20 ℃ at a cooling rate of 2.0 ℃/h, controlling the stirring rate at 21rpm, growing crystals at a constant temperature for 40 hours, performing first pressure filtration at a pressure of 0.25MPa after crystal precipitates appear to remove the crystal precipitates and waxes, then injecting the first pressure filtration product into another winterization tank, cooling to 7 ℃ within 5 minutes, stirring at a rotating speed of 11rpm, continuing winterization for 12 hours after the constant temperature is maintained, and finally performing second pressure filtration at a pressure of 0.3MPa to remove the crystal precipitates and the waxes to obtain the torreya grandis refined oil.
Example 5
A production method of torreya grandis refined oil comprises the following steps:
firstly, crude oil extraction: squeezing the sun-dried Chinese torreya seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature to obtain Chinese torreya crude oil, wherein the content of impurities in the Chinese torreya crude oil is less than 0.25 wt%;
secondly, refining:
a) degumming: mixing the crude oil with water at the temperature of 60 ℃ according to the weight ratio of 10: 1 stirring for 15 minutes at 60 ℃ after mixing, standing for 3.0 hours, and removing lower-layer impurities and water by using a settling separation method to prepare the degummed oil;
b) deacidifying: mixing the degummed oil with a sodium hydroxide solution, and performing deacidification treatment at 70 ℃ to obtain deacidified oil; the weight of the sodium hydroxide in the added sodium hydroxide solution is 3/20 of the weight of the degummed oil;
c) and (3) decoloring: adding deacidified oil into a decolorizing kettle, heating to 75 ℃, adding activated clay accounting for 2 percent of the weight of the deacidified oil, stirring uniformly, heating to 120 ℃, decolorizing under the pressure of 0.04MPa for 1.2 hours, cooling to 60 ℃ at the cooling rate of 2 ℃/h, filtering while hot, and naturally cooling to room temperature to obtain decolorized oil;
d) winterization: adding the destaining oil into a winterization tank, cooling to 20 ℃ at a cooling rate of 2.0 ℃/h, controlling the stirring rate at 21rpm, growing crystals at a constant temperature for 56 hours, performing first pressure filtration at a pressure of 0.25MPa after crystal precipitates appear to remove the crystal precipitates and waxes, then injecting the first pressure filtration product into another winterization tank, cooling to 7 ℃ within 5 minutes, stirring at a rotating speed of 11rpm, continuing winterization for 12 hours after the constant temperature is maintained, and finally performing second pressure filtration at a pressure of 0.3MPa to remove the crystal precipitates and the waxes to obtain the torreya grandis refined oil.
Test example 1: preparation of Chinese torreya oil crude oil
The method comprises the steps of drying and frying 2 types of seeds of the Chinese torreya which grows in the current year to obtain raw seeds, and frying according to the method for producing the dried Chinese torreya fruits. Mechanically shelling 2 Chinese torreya seeds to obtain kernels, and squeezing the 2 seed kernel raw materials to prepare oil, wherein the water content of the kernels is 8-10% during squeezing. The pressed oil was tested for 2 important indices (acid value, peroxide value) and fatty acid composition of 2 crude oils obtained by pressing.
The results show that the pressed oil yield of the raw material seeds obtained by the sun-drying and stir-frying methods is higher, and the two methods have no obvious difference (Table 1). The fatty acid content did not change significantly between the 2 pressed oils, but the general trend was that the saturated fatty acids increased and the unsaturated fatty acid content changed irregularly (table 2), probably because the retention of saturated fatty acids in the pressed residue was reduced by high temperature frying. The acid value of the fried raw material seed pressed oil is obviously higher than that of the dried Chinese torreya raw material seed pressed oil, which shows that the oil and fat property of the fried Chinese torreya oil is changed and the content of free fatty acid is increased. After the pressed oil is stored for 60 days, the acid value and the peroxide value of the dried torreya grandis raw material seed pressed oil are not obviously improved; the acid value of the stir-fried raw material seed pressed oil is not obviously improved, but the peroxide value is obviously increased. It is shown that the antioxidant substances of the roasted torreya grandis seed oil may be affected, shortening the storage period (table 1).
TABLE 1 characteristics of pressed oils of different torreya grandis kernel raw materials
TABLE 2 relative amounts of the respective components of fatty acids of fats and oils
Test example 2: degumming of Chinese torreya oil
Taking 12 parts of the dried Chinese torreya seed squeezed crude oil samples (each 100g), dividing the samples into 4 groups, and 3 samples in each group. The 4 groups of samples were heated to 20 deg.C, 40 deg.C, 60 deg.C or 80 deg.C, respectively. After treatment at different temperatures, 12mL of hot water is added into each sample, the mixture is stirred for 15 minutes for hydration degumming, the mixture is kept stand for 3 hours after reaction, and then filtration is carried out to obtain filtrate such as phospholipid and the like, and the filtrate is weighed. Calculating the degumming rate: degumming rate (%) (phospholipid content of crude oil-phospholipid content of degummed oil)/phospholipid content of crude oil.
Determining and analyzing the influence of degumming temperature on the physicochemical indexes of degummed oil:
the degumming procedure is to carry out hydration degumming to remove the colloid-soluble impurities by utilizing the hydrophilic characteristic of the phospholipid. Table 3 shows that the content of phospholipids in the torreya grandis crude oil is low, most of the phospholipids in the crude oil are removed in the hot water degumming process, and the degumming rate increases with the increase of the degumming temperature. The degumming rate at 20 ℃ is 44.7 percent, which shows that the content of phospholipid in the degummed oil is still higher, and the stability of the grease and the refining effect of the subsequent process are influenced. The degumming rates of the three temperatures of 40 ℃, 60 ℃ and 80 ℃ are all more than 90 percent, and statistical analysis shows that no significant difference exists among the 3 temperatures, but the degumming rates are all significantly higher than 30 ℃ degumming oil (P is less than 0.05), and the corresponding product requirements are met. The acid value, iodine value, peroxide value and other basic quality indexes of the degummed oil at 3 temperatures have no significant difference (Table 3). Therefore, degumming at 40 ℃ is the preferred temperature.
TABLE 3 influence of degumming temperature on degumming effect and physicochemical index of Chinese torreya oil
Note: in color, Y: yellow, R: red (same below).
Test example 3: deacidification of torreya grandis oil
A sodium hydroxide solution was added to 100g of the degummed oil sample, and the amount of alkali added was calculated by a conventional method. Adding alkali, shaking, heating to 30 deg.C, and standing for 30 min. The mixture was washed by adding 15mL of hot water to each of 3 samples, heating to 30 deg.C, 50 deg.C, 70 deg.C and 90 deg.C, and washing with stirring. The mixture was centrifuged by a centrifuge to remove the precipitate. Calculating the deacidification rate: deacidification rate (%) (acid value of crude oil-acid value of deacidified oil)/acid value of crude oil. Deacidification test the deacidified oil obtained at the optimum deacidification temperature was used for the next procedure test.
The influence of deacidification temperature on deacidification oil physical and chemical indexes is measured and analyzed:
the deacidification process is a process of removing free fatty acid from the grease to convert the free fatty acid into soapstock which is insoluble in oil. As can be seen from Table 4, most of the free fatty acids in the degummed oil were removed during the deacidification in the alkaline refining, and the deacidification rate increased with the increase of the deacidification temperature. The deacidification rate at 30 ℃ is 60.0 percent, the acid value of the deacidified oil is 1.01, and the stability and the storage time of the grease are influenced due to the high acid value. The deacidification rates of the three temperatures of 50 ℃, 70 ℃ and 90 ℃ are more than 98%, statistical analysis shows that no significant difference exists among the 3 temperatures, but the deacidification rates are significantly lower than 30 ℃ (P is less than 0.05), the acid value is below 0.04, and the corresponding product requirements are met; there was no significant difference in other basic quality indicators such as relative density, refractive index, peroxide number, etc. of the 3-temperature degummed oils (table 4). Therefore, 50 ℃ deacidified oil is selected to enter the next refining process.
TABLE 4 influence of deacidification temperature on deacidification effect and physicochemical index of Chinese torreya oil
Test example 4: decolorization of torreya grandis oil
Firstly, 100g of deacidified oil sample is heated to 40 ℃, 2g of activated clay is added into each sample, and each group of 3 samples are heated to 60 ℃, 90 ℃, 120 ℃ and 150 ℃ respectively, and are continuously and gently stirred for 1 h. After cooling to 50 ℃ and suction filtration of the mixture, an oil sample was taken and absorbance was measured at 520 nm. Calculating the decolorization rate: the decolorization ratio (%) (absorbance before decolorization-absorbance after decolorization)/absorbance before decolorization. Decolorization test the decolorized oil obtained at the optimum decolorization temperature is used in the next process test.
Determining and analyzing the influence of the decoloring temperature on physicochemical indexes of the decolored oil:
the decolorization process is a process for removing pigment substances in the oil, and as can be seen from table 5-1, most of the oil pigment can be removed at four decolorization temperatures, and the color of the decolorized oil is obviously lighter than that of the deacidified oil. After decolorization, the peroxide value of the oil and fat is significantly reduced, but the acid value is increased. The decolorization rate at 60 ℃ is 54.5%, the color of the grease is still dark, and the peroxide value is 1.98 and is slightly higher. The decolorization rates of the three temperatures of 90 ℃, 120 ℃ and 150 ℃ are all over 80 percent, and statistical analysis shows that no significant difference exists among the 3 temperatures, but the decolorization rates are all significantly higher than 60 ℃ (P is less than 0.05); the peroxide value of 3 temperatures is significantly lower than 60 ℃ de-colorizing oil due to the increased temperature, which increases the ability of the de-colorizing agent to adsorb peroxide. However, the higher the temperature, the higher the acid value rise and the more the saponificate runs off. The relative density, the refractive index and other basic quality indexes of the 3-temperature decolored oil are not obviously different. As can be seen from Table 5-2, the deacidified oil still retained a certain astringent taste of the torreya grandis oil, but the decolored oil had no astringent taste. The decolorized oil at 60 ℃ and 90 ℃ still retains the inherent taste and smell of the Chinese torreya oil.
The main physicochemical indexes of the decolored oil at three temperatures of 5-1, 5-2, 90 ℃, 120 ℃ and 150 ℃ in the comprehensive table already meet the national standards of related edible oil and also meet the national standards of representative woody edible oil camellia oil (GB 11765-2003). But only 90 ℃ destaining oil keeps the inherent taste and smell of the Chinese torreya oil, so the 90 ℃ destaining oil is selected to enter the next refining procedure.
TABLE 5-1 Effect of decolorizing temperature on decolorizing Effect and physicochemical indices of Torreya grandis oil
TABLE 5-2 Effect of decolorizing temperature on deodorizing Effect and physicochemical indices of Torreya grandis oil
| Sample(s) | Taste of the product | Smell(s) |
| Deacidified oil | Slightly astringent taste | Has heavy odor |
| 60℃ | Has the inherent taste of Chinese torreya oil | Has the inherent smell of Chinese torreya oil |
| 90℃ | Has the inherent taste of Chinese torreya oil | Has the inherent smell of Chinese torreya oil |
| 120℃ | Has no peculiar smell | Has no peculiar smell |
| 150℃ | Has no peculiar smell | Has no peculiar smell |
Test example 5: deodorization of torreya grandis oil
100g of decolorized oil samples are stored in a stainless steel container, each 3 samples are respectively placed in a deodorizer modified by a vertical pressure steam sterilizer, the temperature is firstly heated to 85 ℃, then the vacuum is pumped to 500Pa, the temperature is continuously heated to 80 ℃, 120 ℃, 160 ℃ and 200 ℃, the temperature is kept for 2 hours, and then the temperature is cooled and reduced to normal temperature and normal pressure under vacuum. Deodorization test the deodorized oil obtained at the optimum deodorization temperature was used for the next process test.
Determining and analyzing the influence of the deodorization temperature on the physicochemical indexes of the deodorization oil:
the deodorization step is a process of removing unpleasant odor and unpleasant taste in the decolorized oil, and it can be seen from table 6 that after the deodorization of torreya grandis oil, the peroxide value of the oil is further reduced, but the color is increased. Other basic quality indexes such as acid value, relative density, refractive index and the like have no significant difference. The deodorized oil at 80 ℃ and 120 ℃ both retains the inherent taste of the Chinese torreya oil and reflects the unique quality of the Chinese torreya oil. Deodorizing at 160 deg.C and 200 deg.C to lose original flavor and smell of torreya grandis oil. Considering that all indexes of the decolored oil reach the national standards of related edible oil, and the cost of high-temperature deodorization, the torreya grandis oil refining does not need a high-temperature refining process.
TABLE 6 influence of deodorization temperature on deodorization effect and physicochemical index of Torreya grandis oil
Test example 6: dewaxing of torreya grandis oil
Winterization (dewaxing): the destaining oil obtained in the experimental example 4 and the destaining oil obtained in the experimental example 5 (120 ℃) are respectively stored in a stainless steel container and are slowly cooled to 20 +/-2 ℃, the freezing rate is controlled to be 2 +/-0.5 ℃/h, the stirring speed is controlled to be 20-22r/min, the crystallization is continuously carried out for 48 +/-12 h after the constant temperature, crystalline precipitates appear, the first pressure filtration is carried out at the moment, a plate-and-frame filter press is adopted, the filtration pressure is 0.25 +/-0.15 MPa, solid lipid crystals and wax are removed, and the filtered substances are dried and weighed. Injecting the first filter pressing into another winterization tank, rapidly cooling the grease by using a heat exchanger, cooling to 7 +/-1 ℃ within 5 minutes, generating sheet crystalline wax, controlling the stirring speed to be 10-12r/min, keeping the winterization for about 12 hours after constant temperature, carrying out second filter pressing at the moment, removing solid grease crystals and wax, drying and weighing the filtered substances, wherein the filtering pressure is 0.30 +/-0.2 MPa. The above 2 dewaxing tests were repeated 3 times. Dewaxing to obtain the torreya grandis oil product.
As a dewaxing process control group 1, 3 parts of 100g decolored oil (90 ℃) samples are respectively stored in stainless steel containers, placed in water bath pots for cooling, respectively cooled to 4 ℃, and kept stand for 48 hours. The filtrate was collected by low temperature filtration, dried and weighed.
As a dewaxing process control group 2, 3 samples of 100g of deodorized oil (120 ℃) were respectively stored in stainless steel containers, placed in water bath pots for cooling, respectively cooled to 4 ℃, and kept stand for 48 hours. The filtrate was collected by low temperature filtration, dried and weighed.
Calculating the dewaxing rate: dewaxing ratio (%). percent weight of filtrate/weight of oil before filtration. And filtering to obtain the finished oil.
Determining and analyzing the influence of the dewaxing process on the physical and chemical indexes of the dewaxed oil:
the dewaxing process is a process of separating out high-melting-point wax and high-melting-point grease in oil at low temperature, and the lower the temperature in a certain range, the higher the dewaxing rate.
The de-waxing oil used as a material was dewaxed, and as seen from table 7-1, the temperature-staged dewaxing process was favorable to the precipitation of various wax substances, and the dewaxing rate was significantly higher than that of the one-time temperature-decreasing dewaxing process (comparative 1). The reason is that the sectional type dewaxing process separates out wax substances with different properties at different temperature periods by different temperature periods and controlling different cooling rates. Meanwhile, compared with the control, the temperature sectional type dewaxing process can further reduce the acid value and the peroxide value (shown in a table 7-1) and make up for the influence caused by the non-deodorization procedure. Furthermore, the staged dewaxing process can retain the inherent taste, smell and flavor of the Chinese torreya oil to a greater extent, and the dewaxed oil has no peculiar smell (Table 7-3).
When the deodorized oil is used as a material for dewaxing, as shown in Table 7-2, the temperature-staged dewaxing process is also beneficial to the precipitation of various wax substances, and the dewaxing rate is higher than that of the one-time temperature-reducing dewaxing process (control 2), but no significant difference exists in the statistical level. Likewise, the temperature-staged dewaxing process further reduced the acid number and peroxide number (tables 7-2) as compared to control 2, but again at a statistically insignificant level. The deodorized oil only has the inherent taste of the Chinese torreya oil slightly and has no inherent taste of the Chinese torreya oil after the sectional dewaxing process (Table 7-4). The physical and chemical properties of 2 kinds of oil after dewaxing of the decolored oil and the deodorized oil are integrated, and the dewaxed oil has no obvious difference. The only difference is taste and smell, and the de-waxing by de-coloring oil can keep certain inherent taste and smell of Chinese torreya oil. Therefore, it is considered that the torreya grandis refining does not require a deodorization step.
TABLE 7-1 influence of dewaxing temperature on dewaxing effect and physicochemical index of destained oil
TABLE 7-2 influence of dewaxing temperature on dewaxing effect and physicochemical index of deodorized oil
TABLE 7-3 flavor and odor after de-oiling and dewaxing
| Sample(s) | Taste of the product | Smell(s) |
| Decolouring oil | Has the inherent taste of Chinese torreya oil and slight peculiar smell | Has the inherent smell of Chinese torreya oil |
| New process | Has the inherent taste of Chinese torreya oil and no peculiar smell | Has the inherent smell of Chinese torreya oil |
| Control group 1 | Slightly peculiar smell of Chinese torreya oil | Slightly peculiar smell of Chinese torreya oil |
TABLE 7-4 flavor and smell of deodorized oil after dewaxing
| Sample(s) | Taste of the product | Smell(s) |
| Deodorized oil | Slightly peculiar flavor of Chinese torreya oil | Has little inherent smell of Chinese torreya oil |
| New process | Slightly peculiar flavor of Chinese torreya oil and no peculiar smell | Has little inherent smell of Chinese torreya oil |
| Control group 2 | Slightly has the inherent taste of the Chinese torreya oil and has no peculiar smell | Has no inherent smell of Chinese torreya oil |
Test example 7: verification of new process combination
In order to verify the refining effect of the refining temperature in each process, the optimum temperature combination obtained by the temperature test of different processes in each example and the traditional edible oil refining temperature are subjected to a laboratory refining comparison test, and the main process parameters are shown in table 8.
The detection on the obtained refined oil (Table 9) shows that the invention group is the same as the traditional refining method, the physicochemical indexes of the refined Chinese torreya oil all completely conform to the national standards of edible vegetable oil such as GB 2716-. Meanwhile, the heavy metal content (total arsenic and lead), pesticide residue (dimethoate and fenthion) and other undesirable substances (aflatoxin B1, benzo (alpha) pyrene, BHA and BHT) of the refined Chinese torreya oil are not detected. However, the flavor and taste inherent to the torreya grandis oil were not found in the refined oils of the conventional refining methods, while the flavor and taste inherent to the torreya grandis oil remained in the refined oils of the group of the present invention (table 8).
TABLE 8 Process parameter differences for the two refining methods
TABLE 9 physicochemical Properties of refined oils of the refining technique of the present invention and the conventional technique
Note: ND means not detected.
The fatty acid component of the torreya grandis oil of the refining technology of the invention is as follows:
the detection of the obtained refined oil shows that (table 10), the ratio of main fatty acid components to crude oil of the torreya grandis refined oil produced by the refining technology and the traditional refining technology has certain change, the change trend is that the content of saturated fatty acid is reduced, the content of unsaturated fatty acid is increased, but no significant difference exists in statistical analysis (P >0.05), and the influence of the refining temperature on the content of single fatty acid component of torreya grandis oil is small. The total amount of Saturated Fatty Acid (SFA), unsaturated fatty acid (USFA), monounsaturated fatty acid (NUSFA) and polyunsaturated fatty acid (MUSFA) is calculated, so that the SFA content, the NUSFA content and the NUSFA content of the refined oil obtained by crude oil and 2 refining techniques have no character difference, the MUSFA content of the refined oil has no remarkable difference with the crude oil, the 'original ecology' of the fatty acid component of the grease is kept, but the MUSFA content of the traditional refined oil is remarkably higher than that of the crude oil and the refined oil of the invention (P is less than 0.05).
TABLE 10 Effect of combination temperature factory pilot plant on fatty acid composition of refined oils
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (5)
1. A production method of torreya grandis refined oil is characterized by comprising the following steps:
firstly, crude oil extraction: squeezing the sun-dried Chinese torreya seeds at a low temperature of less than 80 ℃ and carrying out secondary filter pressing at normal temperature to obtain Chinese torreya crude oil;
secondly, refining:
a) degumming: mixing the crude oil and water according to the weight ratio of 10: 0.7-1.3, stirring for 10-20 minutes at 40-45 ℃, standing for 2.5-3.5 hours, and removing lower-layer impurities and water by using a settling separation method to obtain the degummed oil; during degumming, the temperature of water is 40-45 ℃;
b) deacidifying: mixing the degummed oil with a sodium hydroxide solution, and performing deacidification treatment at 45-90 ℃ to obtain deacidified oil; the weight of the sodium hydroxide in the added sodium hydroxide solution is 1/10-2/10 of the weight of the degummed oil;
c) and (3) decoloring: adding deacidified oil into a decoloring kettle, heating to 70-80 ℃, adding activated clay accounting for 2% of the weight of the deacidified oil, uniformly stirring, heating to 85-95 ℃, decoloring under the pressure of-0.06-0.08 MPa for 1-1.5 hours, cooling to 55-65 ℃, filtering while hot, and naturally cooling to room temperature to obtain the decolored oil;
d) winterization: adding the decolored oil into a winterization tank, cooling to 18-22 ℃, controlling the stirring speed at 20-22 rpm, growing crystals at constant temperature for 36-60 hours, performing first filter pressing at the pressure of 0.1-0.4 MPa after crystal precipitates appear to remove the crystal precipitates and waxiness, then injecting the first filter pressing product into another winterization tank, cooling to 6-8 ℃ within 5 minutes, stirring at the speed of 10-12 rpm, continuing winterization for 10-14 hours after constant temperature, and finally performing second filter pressing at the pressure of 0.1-0.5 MPa to remove the crystal precipitates and the waxiness to obtain the torreya grandis refined oil.
2. The production method of torreya grandis refined oil according to claim 1, wherein the production method comprises the following steps: the content of impurities in the torreya grandis crude oil is less than 0.25 wt%.
3. The production method of torreya grandis refined oil according to claim 1, wherein the production method comprises the following steps:
and the deacidification treatment in the second step b) is carried out at 48-52 ℃.
4. The production method of torreya grandis refined oil according to claim 1, wherein the production method comprises the following steps:
in the second step c), cooling to 55-65 ℃ at a cooling rate of 1-3 ℃/h after the decolorization reaction.
5. The production method of torreya grandis refined oil according to claim 1, wherein the production method comprises the following steps:
in the second step d), adding the destaining oil into a winterization tank and cooling to 18-22 ℃ at a cooling rate of 1.5-2.5 ℃/h.
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