CN111303993A - Application of novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances - Google Patents
Application of novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances Download PDFInfo
- Publication number
- CN111303993A CN111303993A CN202010201030.4A CN202010201030A CN111303993A CN 111303993 A CN111303993 A CN 111303993A CN 202010201030 A CN202010201030 A CN 202010201030A CN 111303993 A CN111303993 A CN 111303993A
- Authority
- CN
- China
- Prior art keywords
- oil
- silicon dioxide
- edible oil
- content
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
-
- 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
-
- 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
- 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
Abstract
The invention discloses application of a novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances, and particularly discloses a treatment method of edible oil, which comprises the following steps: mixing the degummed oil with silicon dioxide, removing water and filtering to obtain a crude edible oil product; wherein the water content of the silicon dioxide is 35-43%, the average particle size is 15-26 μm, and the water content is the percentage of the mass of water in the silicon dioxide in the total mass of the silicon dioxide and the water. According to the invention, silica is adopted to carry out adsorption treatment on the degummed oil, so that impurities, namely risk substances, in the edible oil are efficiently removed, the step of washing in a degummed section can be omitted, the energy consumption is reduced, the consumption of a decolorizing agent in a decolorizing process can be reduced, the stability of the treated edible oil is improved, and the earthy taste is weakened.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to application of a novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances.
Background
The crude oil obtained by squeezing or leaching contains a large amount of impurities, which not only affects the edible value and safe storage of the oil, but also brings difficulty to deep processing. The common crude oil needs to be subjected to degumming, deacidification, decoloration, deodorization, dewaxing and other processes to obtain the required finished oil.
Wherein, after acid washing (for example, adding phosphoric acid with the mass concentration of 0.05-0.1%) and alkali washing (for example, adding sodium hydroxide with the mass concentration of 7-12%) (the soap content is about 350ppm), hot water and phosphoric acid (for example, acidic hot water with the mass concentration of 5-8%, the adding amount is usually 3-10% of the oil weight) are added to remove residual soap after degumming, and the degumming process is mainly used for removing phospholipid and soap of the crude oil and usually needs to be matched with a water washing process to remove residual soap.
The main functions of the decolorizing section are to remove pigments in the grease, remove colloid substances such as trace metals, soaps, phospholipids and the like and some odor substances, and remove risk substances such as polycyclic aromatic hydrocarbons, pesticide residues and the like. At present, the common decolorization method in industry is an adsorption decolorization method, namely, an adsorbent is used for adsorbing pigments and other impurities in oil under certain conditions, and the common adsorbent is activated clay, activated carbon, attapulgite and the like.
The existing decoloring process generally comprises the steps of heating the degummed oil to 105-115 ℃, adding a certain amount of activated clay for adsorption, and filtering the degummed oil through a filter after adsorbing for a period of time to obtain the decolored oil. However, this process has certain drawbacks: (1) the amount of the activated clay used for removing impurities and other risk substances during decoloring is larger; moreover, generally, the influence of clay on the oil and fat components, such as the formation of conjugated polyene, is increased by using clay in an increased amount to form conjugated double bonds; (2) because the addition amount of the activated clay is large and the adsorption capacity of the activated clay to pigments is strong, the decolorized oil is light in color and almost colorless, which is contrary to the moderate refining advocated by the nation; (3) the adsorbent dosage is large, the filter cake volume is large, and the oil loss is large; (4) because the activated clay has earthy smell, the decolored oil has heavier earthy smell, the burden of the subsequent deodorization working section is increased, and the cost is increased to a certain extent.
Disclosure of Invention
The invention aims to overcome the defects that the quality of oil is reduced and the oil consumption is high due to the fact that the consumption of a decoloring agent is high in an edible oil decoloring process in the prior art, and provides the application of a novel environment-friendly adsorbent in efficiently adsorbing plant oil risk substances. The silica can effectively remove the risk substances, trace metals, soaps, phospholipids and other colloids in the edible oil, simultaneously can save the step of washing in a degumming section, reduces the energy consumption, meets the requirements of national standards on the edible oil, also improves the stability of the edible oil and reduces the production cost.
The invention solves the technical problems through the following technical scheme.
The invention provides a method for treating edible oil, which comprises the following steps: mixing the degummed oil with silicon dioxide, removing water and filtering to obtain a crude edible oil product; wherein the water content of the silicon dioxide is 35-43%, the average particle size is 15-26 μm, and the water content is the percentage of the mass of water in the silicon dioxide in the total mass of the silicon dioxide and the water.
In the present invention, the silica is in the form of a solid, amorphous porous silica, SiO in dry matter2The purity of the product is more than 99%, and the product has strong adsorption capacity on impurities (such as phosphorus, soap, iron, copper, calcium, magnesium and the like) and risk substances (such as benzopyrene, aflatoxin and the like). The adsorption principle is as follows: the surface polarity of the silicon dioxide has strong affinity to polar pollutants, when the oil is heated, the silicon dioxide adsorbs impurities in the oil, after the oil is adsorbed for a period of time, the silicon dioxide is subjected to vacuum drying, at the moment, the water in the silicon dioxide is evaporated, and SiO2Reduced particle size and polarityContaminants are trapped in the voids and the dried down particles are filtered off through a filter precoated with diatomaceous earth.
In the present invention, the silica preferably has a water content of 35% to 40%, for example 35%, 38% or 40%.
In the present invention, the average particle size of the silica is preferably 16 to 23 μm, for example 16 μm, 18 μm, 20 μm or 23 μm.
In the present invention, the pore surface area of the silica may be a pore surface area conventional in the art, and is preferably 700-1000m2G, e.g. 800m2/g、900m2In g or 1000m2/g。
In the present invention, the pore volume of the silica may be that conventionally used in the art, and is preferably 1.8 to 2.2mL/g, for example 2.0mL/g or 2.2 mL/g.
In the present invention, the silica may have a permeability as conventional in the art, preferably 0.09 to 0.13darcy, for example 0.10darcy, 0.11darcy or 0.12 darcy.
In the treatment method, the degummed oil can be obtained by a degummed oil obtained by a conventional degummed process in the field of crude oil, and the degummed process can comprise acid washing and alkali washing steps, wherein the acid washing conditions and operation can be conditions and operation conventional in the field. The agent used in the acid washing may be an inorganic acid, further phosphoric acid, for example, an aqueous phosphoric acid solution having a mass concentration of 0.05 to 0.1%. The conditions and operations of the alkaline washing may be those conventional in the art. The agent used in the alkaline washing may be an inorganic base, further sodium hydroxide, for example, an aqueous solution of sodium hydroxide with a mass concentration of 7-12%.
The degummed oil is degummed oil with or without a water washing step, and preferably the degummed oil without the water washing step. The invention can effectively adsorb soap by treating the silicon dioxide, thereby saving the water washing step after degumming in the traditional process (namely, the crude oil can be directly added with the silicon dioxide for treatment after the steps of acid washing and alkali washing), thereby saving a water washing centrifugal machine, reducing environmental pollution, saving the gold sewage treatment and protecting the environment.
In the processing method, the degummed oil can be vegetable oil degummed oil, such as sunflower seed degummed oil.
In the treatment method, the mass ratio of the silica to the degummed oil can be the mass ratio which is conventional in the field, and is preferably (0.08-0.13):100, such as 0.08: 100. 0.1: 100 or 0.12: 100, the amount of silica used in the present invention is small.
In the treatment process, the temperature of the mixing may be a temperature conventional in the art, preferably 75-85 ℃, for example 75 ℃.
In the treatment method, the mixing mode can be a conventional mode in the field, such as stirring. The stirring speed may be a speed conventional in the art, preferably 80 to 160r/min, such as 80r/min, 100r/min or 140 r/min. The stirring time may be a time conventional in the art, preferably 15-30min, for example 15min or 20 min. The preferable conditions are favorable for better adsorption of impurities and risk substances.
In the treatment process, the temperature at which water is removed may be a temperature conventional in the art, preferably 90 to 95 ℃, for example 90 ℃, which facilitates the removal of water from the silica.
In the treatment process, the vacuum for water removal may be conventional in the art, and is preferably 50 to 100mbar, such as 50mbar, 80mbar or 100 mbar.
In the treatment process, the time for removing water may be a time conventional in the art, and is preferably 2 to 4 hours, such as 2 hours, 2.5 hours, or 3 hours.
In the treatment method, the filtration conditions and operations may be those conventional in the art. For example, the filtration is performed by a filter, preferably, the filter is precoated with a diatomite coating for assisting the filtration of silica, and the amount of diatomite in the diatomite coating is preferably 1.5-2.0kg/m2For example 1.5kg/m2、1.8kg/m2。
Preferably, the treatment method further comprises the following decolorization methods: and mixing the crude edible oil with activated clay and filtering to obtain decolored oil.
Impurities and risk substances in the crude edible oil treated by the silicon dioxide are removed, and then activated clay is added to only adsorb pigments in the crude edible oil, and the addition amount of the activated clay is greatly reduced because other substances are adsorbed. Meanwhile, the volume of the filter cake treated by the silicon dioxide is greatly reduced, and the oil consumption is correspondingly reduced. In addition, the stability of the decolored oil treated by combining the silicon dioxide and the activated clay is improved compared with that of the decolored oil treated by singly using the activated clay.
In the decoloring method, the mass ratio of the crude edible oil to the activated clay can be 100: (0.01-0.05), for example 100: 0.05. according to the invention, the silica is used for treating the degummed oil, so that the consumption of activated clay can be obviously reduced, the earthy smell is weakened, and the energy consumption is reduced for the subsequent deodorization working section.
In the decolorization method, the temperature of the mixing can be a temperature conventional in the art, preferably 100-120 ℃, for example 105 ℃.
In the decoloring method, the mixing may be performed in a manner conventional in the art, such as stirring. The stirring speed may be as conventional in the art, preferably 80-120r/min, e.g. 100 r/min. The stirring time may be a time conventional in the art, preferably 15-30min, e.g. 20 min. The above preferred conditions favor better adsorption of the pigment by the activated clay.
In the decoloring method, the conditions and operation of the filtration may be those conventional in the art, for example, the filtration may be performed by a filter.
The treatment process may also include dewaxing and deodorisation steps.
The dewaxing conditions and operations may be those conventional in the art, and crystallization is preferred. The crystallization can be performed by cooling and then growing crystals. The temperature of the growing crystal can be 4-6 ℃, for example 4 ℃. The time for growing the crystal can be 48-72h, such as 48h, 60h or 72 h.
Wherein, the conditions and operations of deodorization can be the conventional conditions and operations in the field. The temperature of the deodorization is preferably 220-250 ℃, such as 220 ℃, 230 ℃ or 250 ℃; the vacuum level of the deodorization is preferably 10-90mbar, such as 20mbar or 50 mbar; the deodorization time is preferably 40-80min, such as 60 min.
In the invention, the phosphorus content of the 'crude oil' is 150-ppm, the soap content is 800-1200ppm, the Fe content is 2.0-4.0ppm, the Cu content is 0.2-1.0ppm, the Ca content is 1.0-2.0ppm, the Mg content is 1.0-2.0ppm, the benzopyrene content is 5-10ppb and the aflatoxin B1 content is 5-10 ppb.
In the invention, the content of phosphorus in the degummed oil is 12-25ppm, the content of soap is 300-400ppm, the content of Fe is 2.0-4.0ppm, the content of Cu is 0.2-1.0ppm, the content of Ca is 1.0-2.0ppm, the content of Mg is 1.0-2.0ppm, the content of benzopyrene is 5-10ppb, and the content of aflatoxin B1 is 3-10 ppb.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the silica is adopted to carry out adsorption treatment on the degummed oil, so that the step of washing in a degummed section can be omitted while impurities, namely risk substances, in the edible oil are efficiently removed, the energy consumption is reduced, the using amount of a decolorizing agent in a decolorizing process can also be reduced, the stability of the treated edible oil is improved, and the earthy taste is weakened.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The degummed oil in the following examples is prepared by a conventional degumming process, and specifically comprises the following steps: 5000g of crude oil of different batches is heated to 80 ℃, phosphoric acid aqueous solution with the mass concentration of 0.08 percent (the adding amount of the phosphoric acid aqueous solution is 0.08 percent of the weight of the crude oil) is added and stirred for 30min at 100r/min, then sodium hydroxide aqueous solution with the mass concentration of 7 percent (the adding amount of the sodium hydroxide aqueous solution is 0.06 percent of the weight of the oil) is added and stirred for 30min at 100r/min, and the degummed oil is obtained, and the parameters of the obtained degummed oil are shown in each example and each comparative example.
Activated clay in the following examples was purchased from Xuyi Hengxin Clay Tech, Inc., lot No. 20181225.
The detection method of each index in the following examples is as follows:
1. method for detecting impurities
(1) Phosphorus: the third method in the determination of phosphorus in GB5009.87-2016 food products: inductively coupled plasma emission spectrometry (see GB5009.268 determination of multiple elements in food P5-P8)
(2) Soap: GB/T5533-2008 plant oil soap content determination method
(3) Iron: the first method in the determination of iron in GB5009.90-2016 food products: flame atomic absorption spectrometry (P1-P4)
(4) Copper: the first method in the determination of copper in GB 5009.13-2017 food: graphite oven atomic absorption spectrometry (P1-P4)
(5) Calcium: the first method for measuring magnesium in GB5009.92-2016 food comprises: flame atomic absorption spectrometry (P1-P4)
(6) Magnesium: the first method in the determination of magnesium in GB5009.241-2017 food is as follows: flame atomic absorption spectrometry (P1-P4)
2. Method for detecting risk substance
(1) Aflatoxin B1: determination of aflatoxins of B and G groups in GB5009.22-2016 food by second method high performance liquid chromatography-pre-column derivatization (P7-P11)
(2) Benzopyrene: determination of benzo (a) pyrene in GB5009.27-2016 food
3. Color detection method
GB/T22460-
4. Method for detecting induction period
An experimental instrument: oxitest grease oxidation analyzer
The experimental method comprises the following steps: cleaning the sample plate and the sample chamber without any grease; accurately weighing 5.0000g of grease in a sample tray, heating (the temperature is set to 90 ℃) after a cover is covered, and introducing oxygen (the oxygen is set to 6bar) when the temperature reaches; when the temperature and the oxygen reach set values, closing an oxygen valve, and allowing the sample in the sample chamber to react under the conditions; and judging the induction period of the grease according to the pressure of oxygen in the sample chamber, wherein the grease is not oxidized at first, the pressure of the oxygen in the grease is maintained at 6bar all the time, the grease is oxidized after a certain time, the pressure of the oxygen is reduced sharply, and the time corresponding to the inflection point is the induction period of the grease.
5. Method for detecting peroxide value
Second method for determining peroxide value in GB5009.227-2016 food products: potentiometric titration (P4-P6).
The parameters of the silicas used in the following examples 1-3 and comparative example 2 are shown in Table 1;
TABLE 1
Example 1
The method for treating the edible oil comprises the following steps:
(1) heating sunflower seed degummed oil (5000g) to 75 ℃, adding silicon dioxide with the mass of 0.08% of the degummed oil, and mixing at the stirring speed of 80r/min for 15 min;
(2) mixing the degummed oil and silicon dioxide, heating the oil to 90 ℃, and drying for 3 hours under the condition that the vacuum degree is 50mbar to completely evaporate the water in the silicon dioxide;
(3) precoating 1.5kg of diatomite on the filtering area of each square meter of the filtering machine, and then filtering the oil treated in the step (2); obtaining crude edible oil (4950g), the detection results of which are shown in Table 2;
(4) then heating the oil to 105 ℃, adding activated clay accounting for 0.05 percent of the oil by mass for decolorization, stirring at 100r/min, mixing for 20min, and filtering to obtain decolorized oil (4875 g); the detection results are shown in table 3;
(5) cooling the obtained decolored oil through a crystallizing tank, cooling to 4 ℃ for crystal growing, wherein the crystal growing time is 72 hours, and obtaining dewaxed oil;
(6) heating the dewaxed oil to 220 deg.C, deodorizing at vacuum degree of 20mbar for 60min, performing multiple heat exchange between hot oil and cold oil, and cooling with cold water to < 35 deg.C to obtain the final product oil (4812.5g), which was detected as shown in Table 4.
TABLE 2
TABLE 3
TABLE 4
| Item | Example 1 (Process according to the invention) |
| Colour(s) | Light yellow to orange yellow |
| Induction period/h | 11h |
| Peroxide number/mmol/kg | 0.1 |
| Yield/% | 96.25 |
Example 2
The method for treating the edible oil comprises the following steps:
(1) heating sunflower seed degummed oil (5000g) to 75 ℃, adding silicon dioxide with the mass of 0.10% of the degummed oil, and mixing at the stirring speed of 100r/min for 20 min;
(2) mixing the degummed oil and the silicon dioxide, heating the oil to 90 ℃, and drying for 2.5 hours under the condition that the vacuum degree is 80mbar to completely evaporate the water in the silicon dioxide;
(3) precoating 1.8kg of diatomite on the filtering area of each square meter of the filtering machine, and then filtering the oil treated in the step (2); crude edible oil (4937.5g) was obtained, and the results are shown in Table 5;
(4) then heating the oil to 105 ℃, adding activated clay accounting for 0.05 percent of the oil by mass for decolorization, stirring at 100r/min, mixing for 20min, and filtering to obtain decolorized oil (4875 g); the results are shown in Table 6;
(5) cooling the obtained decolorized oil through a crystallizing tank until the temperature is reduced to 4 ℃ for crystal growing, wherein the crystal growing time is 60 hours;
(6) heating the dewaxed oil to 230 deg.C, deodorizing at vacuum degree of 20mbar for 60min, performing multiple heat exchange between hot oil and cold oil, and cooling with cold water to < 35 deg.C to obtain the final product oil (4800g), which is detected as shown in Table 7.
TABLE 5
TABLE 6
| Index (I) | Color (Red and yellow) |
| Degumming oil (before silicon dioxide treatment) | R＝2.9Y＞70 |
| Crude edible oil (after silicon dioxide treatment and before activated clay treatment) | R＝2.8Y＞70 |
| Decolorizing oil (after activated clay treatment) | R＝1.2Y＝16 |
TABLE 7
| Item | Example 2 (Process according to the invention) |
| Colour(s) | Light yellow to orange yellow |
| Induction period/h | 11.5h |
| Peroxide number/mmol/kg | 0.12 |
| Yield/% | 96 |
Example 3
The method for treating the edible oil comprises the following steps:
(1) heating sunflower seed degummed oil (5000g) to 75 ℃, adding silicon dioxide with the mass of 0.12% of that of the degummed oil, and mixing at the stirring speed of 140r/min for 15 min;
(2) mixing the degummed oil and the silicon dioxide, heating the oil to 90 ℃, and drying for 2 hours under the condition that the vacuum degree is 100mbar to completely evaporate the water in the silicon dioxide;
(3) precoating 1.5kg of diatomite on the filtering area of each square meter of the filtering machine, and then filtering the oil treated in the step (2); crude edible oil (4962.5g) was obtained, and the results are shown in Table 8;
(4) then heating the oil to 105 ℃, adding activated clay accounting for 0.05 percent of the oil by mass for decolorization, stirring at 100r/min, mixing for 20min, and filtering to obtain decolorized oil (4850 g); the results are shown in Table 9;
(5) cooling the obtained decolorized oil through a crystallizing tank until the temperature is reduced to 4 ℃ for crystal growing, wherein the crystal growing time is 48 hours;
(6) heating the dewaxed oil to 250 deg.C, deodorizing at a vacuum of 50mbar for 60min, and cooling to < 35 deg.C with cold water after multiple heat exchanges between hot oil and cold oil to obtain a finished oil (4825g), which was tested as shown in Table 10.
TABLE 8
TABLE 9
| Index (I) | Color (Red and yellow) |
| Degumming oil (before silicon dioxide treatment) | R＝3.0Y＞70 |
| Crude edible oil (after silicon dioxide treatment and before activated clay treatment) | R＝2.8Y＞70 |
| Decolorizing oil (after activated clay treatment) | R＝1.3Y＝15 |
Watch 10
| Item | Example 3 (Process according to the invention) |
| Colour(s) | Light yellow to orange yellow |
| Induction period/h | 11h |
| Peroxide number/mmol/kg | 0.15 |
| Yield/% | 96.5 |
Comparative example 1
The method for treating the edible oil of the comparative example comprises the following steps:
(1) heating oleum Helianthi (5000g) to 105 deg.C, adding activated clay 1.0% of the weight of the degummed oil, decolorizing at stirring speed of 200r/min, mixing for 40min, and filtering to obtain decolorized oil (4800g), with detection results shown in Table 11;
(2) cooling the obtained decolorized oil through a crystallizing tank until the temperature is reduced to 4 ℃ for crystal growing, wherein the crystal growing time is 72 hours;
(3) heating the dewaxed oil (4775g) to 220 deg.C, performing deodorization experiment under vacuum degree of 20mbar, wherein deodorization reaction time is 60min, performing multiple heat exchange between hot oil and cold oil, and cooling with cold water to less than 35 deg.C to obtain finished oil (4750g), and the detection results are shown in Table 12.
TABLE 11
TABLE 12
| Item | COMPARATIVE EXAMPLE 1 (PRIOR ART) |
| Colour(s) | Light yellow |
| Induction period/h | 10h |
| Peroxide number/mmol/kg | 0.5 |
| Yield/% | 95 |
The test takes sunflower seed oil as an example, the prior process is compared with the process of the invention, and the results show that the process of the invention can reduce the soap content in the degummed oil to 0 after being treated by silicon dioxide without a water washing step; however, the prior art cannot remove the residual soap by only using activated clay for decolorization without a water washing step. Meanwhile, the oil obtained by the process of the invention has the advantages of dark color, enhanced oxidation stability (longer induction period and lower peroxide value), small filter cake volume, higher yield, effective reduction of oil consumption and reduction of required comprehensive cost.
Comparative example 2
The method for treating the edible oil of the comparative example comprises the following steps:
(1) heating sunflower seed degummed oil (5000g) to 75 ℃, adding silicon dioxide with the mass of 0.08% of the degummed oil, and mixing at the stirring speed of 80r/min for 15 min;
(2) mixing the degummed oil and silicon dioxide, heating the oil to 90 ℃, and drying for 3 hours under the condition that the vacuum degree is 50mbar to completely evaporate the water in the silicon dioxide;
(3) precoating 1.5kg of diatomite on the filtering area of each square meter of the filtering machine, and then filtering the oil treated in the step (2); crude edible oil (4950g) was obtained, and the results are shown in Table 13;
(4) then heating the oil to 105 ℃, adding activated clay accounting for 0.05 percent of the oil by mass for decolorization, stirring at 100r/min, mixing for 20min, and filtering to obtain decolorized oil (4875 g); the results are shown in Table 14;
(5) cooling the obtained decolorized oil through a crystallizing tank until the temperature is reduced to 4 ℃ for crystal growing, wherein the crystal growing time is 72 hours;
(6) heating the dewaxed oil to 220 deg.C, deodorizing at vacuum degree of 20mbar for 60min, performing multiple heat exchange between hot oil and cold oil, and cooling with cold water to < 35 deg.C to obtain the final product oil (4800g), which is detected as shown in Table 15.
Watch 13
TABLE 14
Watch 15
| Item | Comparative example 2 (Process according to the invention) |
| Colour(s) | Light yellow to orange yellow |
| Induction period/h | 10h |
| Peroxide number/mmol/kg | 0.3 |
| Yield/% | 96.0 |
Comparative examples 3 to 4
This comparative example treated an edible oil using the same conditions, procedures and parameters as in example 2, except that the parameters of the silica used were different. The results of the measurements before and after the silica treatment (silica mixing, water removal and filtration) are shown in table 16;
TABLE 16
From the above results, it can be seen that the water content of silica affects the adsorption capacity, and the too low water content has a poor adsorption effect, especially affects the adsorption of soap, and the too high water content causes the inability to form particles, which is difficult to apply. Meanwhile, the particle size of the silicon dioxide can also influence the adsorption effect, and the proper particle size (15-26 mu m) is favorable for the reaction with the degummed oil, so that the adsorption effect is good; the mixing of silica and degummed oil is not facilitated due to the excessively large particle size, and the feeding step in production is influenced due to the increase of density when the particle size is excessively small.
Claims (10)
1. The processing method of the edible oil is characterized by comprising the following steps: mixing the degummed oil with silicon dioxide, removing water and filtering to obtain a crude edible oil product; wherein the water content of the silicon dioxide is 35-43%, the average particle size is 15-26 μm, and the water content is the percentage of the mass of water in the silicon dioxide in the total mass of the silicon dioxide and the water.
2. The method of treating edible oil according to claim 1, wherein the silica has a moisture content of 35% to 40%;
and/or the average particle size of the silicon dioxide is 16-23 μm;
and/or the surface area of the pores of the silicon dioxide is 700-1000m2/g；
And/or the pore volume of the silicon dioxide is 1.8-2.2 mL/g;
and/or the permeability of the silicon dioxide is 0.09-0.13 darcy.
3. The method of treating edible oil according to claim 2, wherein the silica has a moisture content of 35%, 38% or 40%;
and/or the average particle size of the silicon dioxide is 16 μm, 18 μm, 20 μm or 23 μm;
and/or the silica has a pore surface area of 800m2/g、900m2In g or 1000m2/g；
And/or the pore volume of the silicon dioxide is 2.0mL/g or 2.2 mL/g;
and/or the silica has a permeability of 0.10darcy, 0.11darcy, or 0.12 darcy.
4. The method of treating an edible oil according to claim 1, wherein the degummed oil is a degummed oil that does not comprise a water washing step;
and/or the degummed oil is vegetable oil degummed oil;
and/or the degumming oil has the phosphorus content of 12-25ppm, the soap content of 300-400ppm, the Fe content of 2.0-4.0ppm, the Cu content of 0.2-1.0ppm, the Ca content of 1.0-2.0ppm, the Mg content of 1.0-2.0ppm, the benzopyrene content of 5-10ppb and the aflatoxin B1 content of 3-10 ppb;
and/or in the treatment method, the mass ratio of the silicon dioxide to the degummed oil is (0.08-0.13): 100;
and/or, in the treatment method, the temperature of the mixing is 75-85 ℃;
and/or in the treatment method, the mixing mode is stirring, and the stirring speed is 80-160 r/min; the stirring time is 15-30 min;
and/or in the treatment method, the temperature for removing water is 90-95 ℃;
and/or in the treatment method, the vacuum degree for water removal is 50-100 mbar;
and/or in the treatment method, the time for removing water is 2-4 h;
and/or in the treatment method, the filtration is carried out by a filter, and the filter is precoated with a diatomite coating.
5. The method of claim 4, wherein the degummed oil is sunflower seed degummed oil;
and/or in the treatment method, the mass ratio of the silicon dioxide to the degummed oil is 0.08: 100. 0.1: 100 or 0.12: 100, respectively;
and/or, in the treatment method, the temperature of the mixing is 75 ℃;
and/or in the treatment method, the mixing mode is stirring, the stirring speed is 80r/min, 100r/min or 140r/min, and the stirring time is 15min or 20 min;
and/or in the treatment method, the temperature for removing water is 90 ℃;
and/or in the treatment method, the vacuum degree for water removal is 50mbar, 80mbar or 100 mbar;
and/or in the treatment method, the time for removing water is 2h, 2.5h or 3 h;
and/or in the treatment method, the filtration is carried out by a filter, the filter is precoated with a diatomite coating, and the dosage of the diatomite in the diatomite coating is 1.5-2.0kg/m2。
6. The method for treating edible oil according to any one of claims 1 to 5, wherein the method further comprises the following decolorization method: and mixing the crude edible oil with activated clay and filtering to obtain decolored oil.
7. The method for treating edible oil according to claim 6, wherein in the decoloring method, the mass ratio of the crude edible oil to the activated clay is 100: (0.01-0.05);
and/or, in the decoloring method, the mixing temperature is 100-120 ℃;
and/or in the decoloring method, the mixing mode is stirring, the stirring speed is 80-120r/min, and the stirring time is 15-30 min;
and/or in the decoloring method, the filtration is carried out by a filter.
8. The method for treating edible oil according to claim 7, wherein in the decoloring method, the mass ratio of the crude edible oil to the activated clay is 100: 0.05;
and/or, in the decoloring method, the temperature of the mixing is 105 ℃;
and/or in the decoloring method, the mixing mode is stirring, the stirring speed is 100r/min, and the stirring time is 20 min.
9. The method of claim 6, further comprising dewaxing and deodorizing steps.
10. The method for treating edible oil according to claim 9, wherein the dewaxing employs a temperature-reduced crystal growth, the temperature of the crystal growth is 4-6 ℃, and the time of the crystal growth is 48-72 h;
and/or the temperature of deodorization is 220-250 ℃;
and/or the vacuum degree of deodorization is 10-90 mbar;
and/or the deodorization time is 40-80 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010201030.4A CN111303993A (en) | 2020-03-20 | 2020-03-20 | Application of novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010201030.4A CN111303993A (en) | 2020-03-20 | 2020-03-20 | Application of novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111303993A true CN111303993A (en) | 2020-06-19 |
Family
ID=71155608
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010201030.4A Pending CN111303993A (en) | 2020-03-20 | 2020-03-20 | Application of novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111303993A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748409A (en) * | 2020-07-24 | 2020-10-09 | 湖北葛店人福药用辅料有限责任公司 | Vegetable oil and refining method thereof |
| CN116875379A (en) * | 2023-05-31 | 2023-10-13 | 山东三聚生物能源有限公司 | Method and system for demetallizing biological raw oil |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85107676A (en) * | 1984-12-07 | 1986-06-10 | 格雷斯公司 | The soft silica method for refining of glyceride oil |
| CN1152333A (en) * | 1994-07-13 | 1997-06-18 | 亨凯尔公司 | Process for removal of dissolved metallic catalyst from ester products |
| JP2001097712A (en) * | 1999-09-30 | 2001-04-10 | Tokuyama Corp | Method for producing minute and globular silica |
| CN102821842A (en) * | 2010-03-24 | 2012-12-12 | 赢创德固赛有限公司 | Coarse support silica particles |
| CN110548480A (en) * | 2019-10-14 | 2019-12-10 | 广汉市迈德乐食品有限公司 | Degumming adsorbent for hot pot beef tallow and application thereof |
-
2020
- 2020-03-20 CN CN202010201030.4A patent/CN111303993A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85107676A (en) * | 1984-12-07 | 1986-06-10 | 格雷斯公司 | The soft silica method for refining of glyceride oil |
| CN1152333A (en) * | 1994-07-13 | 1997-06-18 | 亨凯尔公司 | Process for removal of dissolved metallic catalyst from ester products |
| JP2001097712A (en) * | 1999-09-30 | 2001-04-10 | Tokuyama Corp | Method for producing minute and globular silica |
| CN102821842A (en) * | 2010-03-24 | 2012-12-12 | 赢创德固赛有限公司 | Coarse support silica particles |
| CN110548480A (en) * | 2019-10-14 | 2019-12-10 | 广汉市迈德乐食品有限公司 | Degumming adsorbent for hot pot beef tallow and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 马苏德: "TriSyl二氧化硅+滤饼+白土去除食用油脂中杂质和色素", 《中国油脂》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748409A (en) * | 2020-07-24 | 2020-10-09 | 湖北葛店人福药用辅料有限责任公司 | Vegetable oil and refining method thereof |
| CN111748409B (en) * | 2020-07-24 | 2023-06-20 | 湖北葛店人福药用辅料有限责任公司 | Vegetable oil and refining method thereof |
| CN116875379A (en) * | 2023-05-31 | 2023-10-13 | 山东三聚生物能源有限公司 | Method and system for demetallizing biological raw oil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0234221B2 (en) | Method for refining glyceride oils using acid-treated amorphous silica | |
| Gerçel et al. | Removal of disperse dye from aqueous solution by novel adsorbent prepared from biomass plant material | |
| EP0185182B1 (en) | Method for refining glyceride oils using amorphous silica | |
| TWI229007B (en) | Process and composition for removing trace contaminants from glyceride oils | |
| TW212141B (en) | ||
| CN111303993A (en) | Application of novel environment-friendly adsorbent in efficient adsorption of plant oil risk substances | |
| CN102994224B (en) | Water-free de-soaping and pre-decolorization refining method for grease | |
| Boukerroui et al. | Regeneration and reuse waste from an edible oil refinery | |
| CA1298853C (en) | Method for treating caustic refined glyceride oils for removal of soaps and phospholipids | |
| CN109182609B (en) | Bentonite method sugarcane juice sulfur-free clarification process | |
| CN113563970A (en) | Production process for reducing amount of oil smoke of refined edible vegetable oil | |
| CN104891588B (en) | A kind of modified molecular screen, its preparation method and the application in water process | |
| CN114682238B (en) | Regeneration method of waste clay | |
| CN111518616A (en) | Refining method of camellia seed oil | |
| CN113318701A (en) | Removing aflatoxin B in soil-pressed peanut oil1Adsorbent and preparation method thereof | |
| TW201532668A (en) | Treated waste products, methods of preparing them and using the same | |
| US5264597A (en) | Process for refining glyceride oil using precipitated silica | |
| CN104845734B (en) | The absorption decoloring method of one vegetable oil | |
| CN108423859B (en) | Printing and dyeing wastewater treatment method for cationic dye | |
| CA1163228A (en) | Method for refining oils and fats | |
| CN103710144B (en) | Preparation method of low-methoxyaniline value soybean oil | |
| CN113789220A (en) | Oil tea oil refining method | |
| AU628084B2 (en) | Process for refining glyceride oil | |
| CN112156759A (en) | Method for decolorizing rapeseed oil by using composite bentonite | |
| CN113444569A (en) | Method for refining waste animal and vegetable oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200619 |
|
| WD01 | Invention patent application deemed withdrawn after publication |