CN115193263B - Rotary membrane filtration and purification device, application thereof and camellia oil purification method - Google Patents
Rotary membrane filtration and purification device, application thereof and camellia oil purification method Download PDFInfo
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- CN115193263B CN115193263B CN202210926706.5A CN202210926706A CN115193263B CN 115193263 B CN115193263 B CN 115193263B CN 202210926706 A CN202210926706 A CN 202210926706A CN 115193263 B CN115193263 B CN 115193263B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/16—Rotary, reciprocated or vibrated modules
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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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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/08—Flow guidance means within the module or the apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2315/00—Details relating to the membrane module operation
- B01D2315/02—Rotation or turning
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Abstract
The invention belongs to the technical field of food, and particularly relates to a rotary membrane filtration and purification device, application thereof and a method for purifying camellia oil. The rotary membrane filtering and purifying device provided by the invention is characterized in that the inside of the rotary membrane is provided with the diversion trench, the high-speed operation of the rotary membrane enables the feed liquid to form a certain tangential flow velocity on the surface of the membrane, and the feed liquid is filtered under multiple acting forces such as pressure, gravity, tangential flow velocity and the like. Because the rotary motion of the rotary membrane generates turbulence promotion and a centrifugal effect on materials in the container, high-concentration materials are diffused to the wall of the container, and low-concentration materials are gathered to the middle, so that the rotary membrane has higher pollution resistance, better filtering effect and higher membrane flux, insoluble impurities, colloid, free fatty acid and pigment mixed in the colloid can be effectively removed from the camellia crude oil, degumming, deacidification, decoloration and impurity removal effects to a great extent are achieved, and the purity of the camellia oil is improved.
Description
Technical Field
The invention belongs to the technical field of food, and particularly relates to a rotary membrane filtration and purification device, application thereof and a method for purifying camellia oil.
Background
Camellia oil is woody vegetable oil. The camellia oil has rich nutritive value and high dietotherapy effect, wherein the mass fraction of unsaturated fatty acid is more than 90%, and the camellia oil contains various antioxidant components, and has the curative effects of resisting inflammation, tumors and oxidation. At present, the traditional camellia oil refining process is a chemical refining method, and generally comprises the operation procedures of degumming, deacidification, decoloration, deodorization and the like. The traditional processing technology has the defects of loss of natural active nutrient components, complex process, loss of nutrient substances and the like. Therefore, the camellia oil needs to be filtered and purified by adopting a green physical processing technology.
The membrane separation technology has the advantages of high separation efficiency, low energy consumption, environmental protection and the like, and is widely applied to the solid-liquid separation field of food, medicine and the like. The membrane technology has certain application in vegetable oil processing, and the oil refined by the membrane method can achieve the effects of degumming, deacidification and decoloration. At present, the traditional membrane separation generally adopts a filtration mode of a static tubular ceramic membrane, which easily causes the adsorption and deposition of colloidal particles and solute macromolecules on the surface of the membrane or in membrane pores to reduce or block the membrane pore diameter, and has the disadvantages of difficult cleaning and large water consumption. Meanwhile, concentration polarization and membrane pollution phenomena on the membrane surface lead to reduction of membrane permeation flux and deterioration of separation performance.
The low-temperature physical membrane method refining process of the original fragrant tea seed oil disclosed in the invention patent (CN 103215124B, a low-temperature physical membrane method refining process of the original fragrant tea seed oil) and the pressing process of the tea oil seed extracted tea oil disclosed in the invention patent (CN 109897726A, a pressing process of the tea oil seed extracted tea oil) are only filtered by using a tubular ceramic membrane after winterization crystallization, the process is complex, the extraction rate is low, the membrane flux is small, the camellia seeds cannot be fully utilized, and the addition of chemical reagents does not accord with the green food processing concept.
In conclusion, the conventional camellia oil processing technology is mainly a traditional chemical refining method and adopts tubular ceramic membrane filtration treatment, and the methods cannot efficiently retain nutrient substances in the camellia oil and are difficult to fully utilize camellia seeds.
Disclosure of Invention
In view of the above, the present invention provides a rotating membrane filtration and purification device, and a method for purifying camellia oil using the same, wherein the rotating membrane filtration and purification device provided by the present invention can maximally retain nutrients in crude camellia oil, fully utilize camellia seeds, and has the characteristics of low energy consumption, high efficiency and high yield.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a rotary membrane filtration and purification device, which comprises a rotary membrane main body and a concentric cylindrical cover 3; the rotating membrane main body comprises a plurality of rotating membranes 1 and a rotating membrane supporting body 2; the rotary membrane supporting body 2 penetrates through the plurality of rotary membranes 1; the rotary diaphragms 1 are parallelly stacked on the rotary diaphragm support body 2, and the rotary diaphragm main body is positioned in the concentric cylindrical cover 3; the rotary membranes 1 are provided with flow guide grooves 4.
Preferably, the pore diameter of the rotating membrane 1 is independently 0.0005-0.2 μm; the number of the rotary membranes 1 is 12; the diameter of the rotary membrane 1 is 20cm; the membrane flux of the rotating membrane 1 is independently 30-42L/h.m 2 。
The invention also provides application of the rotary membrane filtration and purification device in the technical scheme in the field of camellia oil purification.
The invention also provides a method for filtering and purifying camellia oil, which comprises the following steps:
physically squeezing the camellia seeds, obtaining crude camellia oil;
the camellia oil is obtained by adopting the rotary membrane filtration and purification device of the technical scheme to carry out rotary membrane filtration and purification on the camellia crude oil.
Preferably, the temperature of the rotary membrane filtration purification is 30-60 ℃; the pressure of the rotary membrane for filtration and purification is 0.05-1.5 MPa.
Preferably, the flow rate of the rotary membrane filtration purification is 50-60L/h.
Preferably, the rotating speed of the rotating membrane in the rotating membrane filtration and purification device is 500-1000 r/min.
Preferably, before physically squeezing the camellia seeds, the method further comprises the following steps: sequentially cleaning, drying and screening camellia seeds; the drying temperature is 45-55 ℃; and drying until the water content of the camellia seeds is 10-15%.
Preferably, the mesh number of the sieve used for sieving is 100-150 meshes.
Preferably, the device for physical pressing is a press.
The invention provides a rotary membrane filtration and purification device, which comprises a rotary membrane main body and a concentric cylindrical cover 3; the rotating membrane main body comprises a plurality of rotating membranes 1 and a rotating membrane support body 2; the rotary membrane supporting body 2 penetrates through the rotary membranes 1; the rotary diaphragms 1 are parallelly stacked on the rotary diaphragm support body 2, and the rotary diaphragm main body is positioned in the concentric cylindrical cover 3; the rotary membranes 1 are provided with flow guide grooves 4. The rotary membrane filtration and purification device provided by the invention is characterized in that the inside of the rotary membrane is provided with the diversion trench, in the high-speed operation process of the rotary membrane, the diversion trench enables the feed liquid to form a certain section flow velocity on the surface of the membrane, and the feed liquid is filtered under the action of pressure and the section flow velocity. The rotary membranes are arranged to realize continuous filtration of feed liquid, so that the filter capacity is large, the quality is stable, the filter is not blocked, and the membrane surface is easy to clean. The rotary motion of the rotary membrane generates turbulence promotion and centrifugal action on the materials in the container, so that the high-concentration materials are diffused to the wall of the container, and the low-concentration materials are gathered to the middle. During the filtration and purification process, an open flow passage is formed between the two rotary membranes, and enough space is provided for accommodating high-viscosity oil. Because the high-speed rotation forms turbulent flow to continuously wash the surface of the membrane and remove the pollution on the membrane surface, the solid content of the concentrate can reach more than 80 percent and is not influenced by the solid content of the feed, thereby effectively preventing the pollution and blockage on the membrane surface, ensuring the continuous and stable filtration and leading the rotary membrane to have higher pollution resistance, better filtration effect and higher membrane flux.
Compared with the traditional chemical refining method and the tubular ceramic membrane filtration method, the method for purifying the camellia oil by adopting the rotary membrane filtration and purification device disclosed by the invention effectively combines the principle of a centrifugal machine and a ceramic membrane, is an enhanced membrane separation technology, can effectively remove insoluble impurities, colloids, free fatty acids, pigments and the like which are mixed in crude camellia oil, and achieves the effects of degumming, deacidification, decoloration and impurity removal. In the traditional refining process, chemical additives are adopted to cause chemical residues, so that nutrient substances in the camellia oil are damaged; meanwhile, the traditional process has high operation temperature, many active ingredients are temperature-sensitive substances, and high-temperature treatment causes a great amount of degradation of the active ingredients, so that the nutritional value of the camellia oil is greatly reduced. The rotating film filtration purification of the camellia oil is a non-thermal green physical processing technology, the high-quality camellia oil can be efficiently obtained at low temperature, the nutrient substances in the crude camellia oil are retained to the maximum extent, camellia seeds are fully utilized, and the purity of the camellia oil is improved. The example result shows that the camellia oil obtained by the invention meets the quality index of first-stage pressing camellia seed oil in the national standard (GB/T11765-2018) of camellia seed oil.
In addition, the camellia oil is filtered and purified by using the rotating film, the energy consumption is reduced, the refining process is simplified, chemical reagents such as acid and alkali do not need to be added in the purification process, the camellia oil can run at low temperature without heating, the processing process is green, energy-saving and low in cost, nutrient substances in crude camellia oil are retained to the maximum extent, camellia seeds are fully utilized, high-quality camellia oil with few impurities is obtained, and the processing process is low in energy consumption, high in efficiency and high in yield.
Drawings
FIG. 1 is a schematic view of a rotary membrane filtration purification apparatus used in the present invention, in which 1 is a rotary membrane, 2 is a rotary membrane support, and 3 is a concentric cylindrical housing;
FIG. 2 is a schematic view of a rotary diaphragm used in the present invention, wherein 1 is the rotary diaphragm, and 4 is a guiding groove;
FIG. 3 is a schematic diagram of a method for purifying camellia oil based on a rotating membrane filtration technology.
Detailed Description
As shown in fig. 1 and 2, the present invention provides a rotary membrane filtration purification apparatus comprising a rotary membrane main body and a concentric cylindrical housing 3; the rotating membrane main body comprises a plurality of rotating membranes 1 and a rotating membrane support body 2; the rotary membrane supporting body 2 penetrates through the rotary membranes 1; the rotary diaphragms 1 are parallelly stacked on the rotary diaphragm support body 2, and the rotary diaphragm main body is positioned in the concentric cylindrical cover 3; the rotary membranes 1 are provided with flow guide grooves 4.
Rotation provided by the inventionThe membrane filtration and purification device comprises a rotary membrane main body; the rotating membrane main body comprises a plurality of rotating membranes 1 and a rotating membrane support body 2; the rotary membrane supporting body 2 penetrates through the rotary membranes 1; the rotary diaphragms 1 are parallelly stacked on the rotary diaphragm support body 2; the rotary diaphragms 1 are provided with flow guide grooves 4; the diversion trenches 4 are preferably radial from the center of the rotating membrane 1 to the periphery; the number of the diversion trenches 4 is preferably 12; the width of the diversion trench 4 is preferably 10 mm/lane; the pore diameter of the rotating membrane 1 is independently preferably 0.0005-0.2 μm, and more preferably 0.05-0.14 μm; the number of the rotary membranes 1 is preferably 12; the diameter of the rotating membrane 1 is preferably 20cm; the membrane flux of the rotating membrane 1 is independently preferably 30-42L/h.m 2 More preferably 35 to 40L/h.m 2 (ii) a The rotating membrane 1 is preferably made of a ceramic material sintered at high temperature; the material of the rotary diaphragm support 2 is preferably an inorganic material.
The rotary membrane filtration and purification device provided by the invention comprises a concentric cylindrical cover 3; the rotating membrane body is located inside a concentric cylindrical cage 3; the concentric cylindrical hood 3 is preferably made of glass fiber reinforced plastics.
FIG. 1 is a schematic view of a rotary membrane filtration purification apparatus used in the present invention, and FIG. 2 is a schematic view of a rotary membrane used in the present invention. As can be seen from FIG. 1 and FIG. 2, the center of the rotary membrane filtration and purification device used in the present invention is a rotary membrane support body 2, and a plurality of rotary membranes 1 are stacked in parallel on the rotary membrane support body 2 to form a rotary membrane body, which is located in a concentric cylindrical housing 3.
The invention also provides application of the rotary membrane filtration and purification device in the technical scheme in the field of camellia oil purification.
The invention also provides a method for filtering and purifying camellia oil, which comprises the following steps:
physically squeezing camellia seeds to obtain camellia crude oil;
the camellia oil is obtained by adopting the rotary membrane filtration and purification device of the technical scheme to carry out rotary membrane filtration and purification on the camellia crude oil.
Unless otherwise specified, the present invention does not require any particular source of the raw materials used, and commercially available products known to those skilled in the art may be used.
The camellia seed is physically squeezed to obtain the camellia crude oil.
In the invention, the camellia seeds are preferably fresh and high-quality camellia seeds which are large, full, black-brown in seed shells, free of disease spots and glossy.
In the present invention, before the camellia seeds are physically pressed, the method preferably further comprises: cleaning, drying, screening and shelling camellia seeds in sequence.
In the present invention, the temperature of the drying is preferably 45 to 55 ℃, more preferably 45 to 50 ℃; the camellia seeds are dried until the water content of the camellia seeds is preferably 10-15%, and more preferably 10-12%; the mesh number of the screen used for the screening is preferably 100 to 150 meshes, and more preferably 120 meshes. The cleaning process is not particularly limited, and the camellia seeds are cleaned by adopting the well-known cleaning process in the field; the peeling process is not particularly limited in the present invention, and a peeling process well known in the art may be used.
In the present invention, the apparatus for physical pressing is preferably a press; the physical pressing process is not particularly limited in the present invention, and a physical pressing process well known in the art may be used.
After the camellia oil is obtained, the camellia oil is obtained by adopting the rotary membrane filtration and purification device of the technical scheme to carry out rotary membrane filtration and purification on the camellia oil.
In the invention, the temperature of the rotary membrane filtration purification is preferably 30-60 ℃, and more preferably 45 ℃; the pressure of the rotary membrane filtration purification is preferably 0.05-1.5 MPa, and more preferably 1MPa; the flow rate of the rotary membrane filtration purification is preferably 50-60L/h, and more preferably 55L/h; the rotating speed of the rotating membrane in the rotating membrane filtration and purification device is preferably 500-1000 r/min, and more preferably 750r/min.
FIG. 3 is a schematic view of the method for purifying camellia oil based on the rotary membrane filtration technology provided by the present invention. As shown in figure 3, the camellia oil product is obtained by drying, sieving and squeezing raw camellia seeds to obtain crude camellia oil, and then filtering and purifying the crude camellia oil through a rotating film.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
Cleaning camellia seeds, drying at 50 ℃ for 2h to keep the water content of the dried camellia seeds at 10%, then sieving with a 100-mesh sieve, peeling, and putting into a squeezer for physical squeezing to obtain crude camellia oil; putting the camellia crude oil into a rotary membrane filtration and purification device for filtration and purification, wherein 12 flow guide grooves with the width of 10 mm/channel are formed in the rotary membrane, the aperture of the rotary membrane is 0.05 mu m, the number of the rotary membrane is 12, the diameter of the rotary membrane is 20cm, and the rotating speed of the rotary membrane is 500r/min; filtering and purifying crude oleum Camelliae Japonicae at 30 deg.C and pressure of 0.05MPa and flow rate of 50L/h with membrane flux of 35L/h.m 2 And finally obtaining the camellia oil.
Example 2
Cleaning camellia seeds, drying at 45 ℃ for 2.5h to keep the water content of the dried camellia seeds at 12%, then sieving with a 120-mesh sieve, peeling, and putting into a squeezer for physical squeezing to obtain crude camellia oil; putting the camellia crude oil into a rotary membrane filtration and purification device for filtration and purification, wherein 12 diversion trenches with the width of 10 mm/channel are arranged on the rotary membrane, the aperture of the rotary membrane is 0.1 mu m, the number of the rotary membrane is 12, the diameter of the rotary membrane is 20cm, and the rotating speed is 750r/min; filtering and purifying crude camellia oil at 45 deg.C under 1MPa and flow rate of 55L/h, with membrane flux of 42L/h.m 2 And finally obtaining the camellia oil.
Example 3
Cleaning camellia seeds, drying at 55 ℃ for 3h to keep the water content of the dried camellia seeds at 15%, then sieving with a 150-mesh sieve, peeling, and putting into a squeezer for physical squeezing to obtain crude camellia oil; putting the camellia crude oil into a rotary membrane filtration and purification device for filtration and purification, wherein 12 diversion trenches with the width of 10 mm/channel are arranged on the rotary membrane, the aperture of the rotary membrane is 0.14 mu m, the number of the rotary membrane is 12, the diameter of the rotary membrane is 20cm, and the rotating speed is 1000r/min; filtering and purifying crude camellia oil at 60 deg.C under 1.5MPa and flow rate of 60L/hThe membrane flux is 30L/h.m 2 And finally obtaining the camellia oil.
Comparative example 1
The traditional chemical refining method comprises the following steps: cleaning camellia seeds, drying at 60 ℃ for 4h to keep the water content of the camellia seeds at 10%, then peeling the dried camellia seeds, and sending the camellia seeds into a squeezer for squeezing. Carrying out high-temperature hydration degumming, heating camellia oil to 70 ℃, adding 3% of same-temperature water, stirring for 1h at the speed of 100r/min, and standing for 4h. Then, low-temperature alkali refining is used, the mass fraction of NaOH alkali liquor is 14%, the volume ratio of camellia oil to NaOH solution is 1, stirring is carried out at 70r/min, the temperature of the oil is raised to 80 ℃, the water consumption is controlled to be 10% of the mass of the oil, and stirring is carried out continuously in the washing process; sucking oil into a decoloring tank by vacuum, adding 1-3% of activated clay and 3-5% of activated carbon, heating to 95 ℃ for dehydration, drying by a vacuum drier, and feeding the dried oil into a drying tower for decoloring for 20min at a vacuum degree of 9kPa; sucking the decolorized oil into a deodorization pot, heating to 150 ℃, turning over steam, continuously heating to 240 ℃, and turning off a heating system for cooling after 2 hours; feeding deodorized oil into a freezing crystallization tank with gas, winterizing, stopping circulation of refrigerant in jacket when oil temperature is below 3 deg.C to reduce oil temperature to 0 deg.C, maintaining for 24 hr, and filtering to obtain camellia oil.
Comparative example 2
Tubular ceramic membrane filtration method: cleaning camellia seeds, drying at 50 ℃ for 3h to keep the water content of the camellia seeds at 10%, sieving with a 80-mesh sieve, peeling, and putting into a squeezer for physical squeezing to obtain crude camellia oil;
pumping the crude camellia oil into a degumming tank by using a pump, adding a flocculating agent (weak acid and inorganic salt with the mass ratio of 1; adding perlite and activated carbon in a mass ratio of 3.
Comparative example 3
The traditional chemical refining method comprises the following steps: cleaning camellia seeds, and drying at 55 deg.C for 5h to keep the water content of camellia seeds at 12%; then husking dried camellia seeds, and delivering into a squeezer for squeezing. Performing high-temperature hydration degumming, heating camellia oil to 80 deg.C, adding 4% of same-temperature water, stirring at 120r/min for 1.5 hr, and standing for 6 hr. Then, low-temperature alkali refining is used, the mass fraction of NaOH alkali liquor is 18%, the volume ratio of camellia oil to NaOH solution is 2; sucking oil into a decoloring tank by vacuum, adding 1-3% of activated clay and 3-5% of activated carbon, heating to 100 ℃ for dehydration, drying by a vacuum drier, and feeding the dried oil into a drying tower for decoloring for 25min with the vacuum degree of 10kPa; sucking the decolorized oil into a deodorization pot, heating to 150 ℃, turning over steam, continuously heating to 230 ℃, and turning off a heating system for cooling after 2 hours; feeding deodorized oil into a freezing crystallization tank with gas, performing winterization treatment, stopping circulation of refrigerant in jacket to reduce oil temperature to 0 deg.C when oil temperature is below 3 deg.C, maintaining for 12 hr, and filtering to obtain oleum Camelliae Japonicae.
Comparative example 4
Tubular ceramic membrane filtration method: cleaning camellia seeds, drying at 55 ℃ for 4h to keep the water content of the camellia seeds at 12%, sieving with a 100-mesh sieve, peeling, and putting into a squeezer for physical squeezing to obtain crude camellia oil;
pumping the crude camellia oil into a degumming tank by using a pump, adding a flocculating agent (weak acid and inorganic salt with the mass ratio of 1; adding perlite and activated carbon in a mass ratio of 6. Filtering with 0.8 μm ceramic membrane at 50 deg.C under 0.2MPa and flow rate of 2L/h, adding potassium hydroxide into dewaxed crude oil, stirring, standing for settling, collecting supernatant, adding filter aid, and filtering to obtain camellia oil.
Comparative example 5
The traditional chemical refining method comprises the following steps: cleaning camellia seeds, and drying at 50 deg.C for 6h to keep the water content of camellia seeds at 15%; then husking dried camellia seeds, and delivering into a squeezer for squeezing. And (3) carrying out high-temperature hydration degumming, heating the camellia oil to 90 ℃, adding 5% of same-temperature water, stirring for 2h at a speed of 140r/min, and standing for 8h. Then, low-temperature alkali refining is used, the mass fraction of NaOH alkali liquor is 24%, the volume ratio of camellia oil to NaOH solution is 3, stirring is carried out at the speed of 90r/min, the oil temperature is increased to 85 ℃, the water consumption is controlled to be 15% of the oil mass, and stirring is carried out continuously in the washing process; sucking oil into a decoloring tank by vacuum, adding 1-3% of activated clay and 3-5% of activated carbon, heating to 105 ℃ for dehydration, drying by a vacuum drier, and feeding the dried oil into a drying tower for decoloring for 30min with the vacuum degree of 8kPa; sucking the decolorized oil into a deodorization pot, heating to 150 ℃, turning over steam, continuously heating to 250 ℃, and turning off a heating system for cooling after 2 hours; feeding deodorized oil into a freezing crystallization tank with gas, performing winterization treatment, stopping circulation of refrigerant in jacket to reduce oil temperature to 0 deg.C when oil temperature is below 3 deg.C, maintaining for 48 hr, and filtering to obtain oleum Camelliae Japonicae.
Comparative example 6
Tubular ceramic membrane filtration method: cleaning camellia seeds, drying at 60 ℃ for 5h to keep the water content of the camellia seeds at 15%, sieving with a 120-mesh sieve, peeling, and putting into a squeezer for physical squeezing to obtain crude camellia oil;
pumping the camellia crude oil into a degumming tank by using a pump, adding a flocculating agent (weak acid and inorganic salt with the mass ratio of 1; adding perlite and activated carbon in a mass ratio of 9. Filtering with ceramic membrane with membrane diameter of 1.2 μm at 40 deg.C under 0.1MPa and flow rate of 2.5L/h, adding potassium hydroxide into dewaxed crude oil, stirring, standing for settling, collecting supernatant, adding filter aid, and filtering to obtain camellia oil.
Performance test
The color, moisture content, volatile matter, insoluble impurities, phospholipid content, acid value and peroxide value of the camellia oil obtained in the examples 1 to 3 and the comparative examples 1 to 6 are measured by the following specific measuring method: the color is measured according to the method for measuring the color of luvibond of animal and vegetable fat in the national standard GB/T22460-2008, the water content and the volatile content are measured according to the method for measuring the water content and the volatile content of the animal and vegetable fat in the national standard GB 5009.236-2016, the insoluble impurities are measured according to the method for measuring the insoluble impurities of the animal and vegetable fat in the national standard GB/T15688-2008, the phospholipid content is measured according to the method for measuring the phospholipid content in the national standard GB/T5537-2008, the acid value is measured according to the method for measuring the acid value in food in the national standard GB 5009.229-2016, and the peroxide value is measured according to the method for measuring the peroxide value in the food in the national standard GB 5009.227-2016.
TABLE 1 results of quality test of camellia oil obtained in examples 1 to 3 and comparative examples 1 to 6
As can be seen from Table 1, the camellia oil obtained in example 1 meets the quality index of the first-stage oil camellia oil pressed in the national standard (GB/T11765-2018) of oil camellia oil.
The color of the camellia oil obtained by the rotary membrane filtration in example 1 is reduced compared with that obtained by the tubular ceramic membrane filtration in comparative example 2 and the traditional chemical refining method in comparative example 1, and the red value is reduced by 25% compared with that obtained by the traditional chemical refining method. The contents of water and volatile matters in the camellia oil filtered by the rotary membrane are 0.04%, and are respectively reduced by 43% and 60% compared with the content (0.07%) filtered by a tubular ceramic membrane and the content (0.10%) filtered by a traditional chemical refining method. The insoluble impurities in the camellia oil filtered by the rotary membrane are 0.02 percent, and are respectively reduced by 50 percent compared with the filtration content (0.04 percent) of the tubular ceramic membrane and 60 percent compared with the filtration content (0.05 percent) of the traditional chemical refining method, which indicates that the removing effect of the camellia oil filtered by the rotary membrane on trace water, volatile matters and insoluble impurities in the grease is better. In addition, the phospholipid content (20.45 mg/g) of the camellia oil filtered by the rotary membrane is reduced by 37% compared with the phospholipid content (32.28 mg/g) filtered by the tubular ceramic membrane, and the phospholipid content (49.32 mg/g) of the camellia oil filtered by the traditional chemical refining method is reduced by 59%, which shows that the camellia oil filtered by the rotary membrane has higher removal rate of the phospholipid in the oil and better degumming effect. The acid value (0.78 mg/g) and the peroxide value (0.18 g/100 g) of the camellia oil filtered by the rotary membrane are reduced compared with the acid value (0.88 mg/g) and the peroxide value (0.21 g/100 g) of the tubular ceramic membrane filter and the acid value (0.92 mg/g) and the peroxide value (0.23 g/100 g) of the camellia oil filtered by the traditional chemical refining method, and the fact that the camellia oil filtered by the rotary membrane shows better deacidification effect and oxidation resistance is shown. According to the results, the quality of the camellia oil obtained by the rotary membrane filtration is higher than that of the camellia oil obtained by the tubular ceramic membrane filtration and the traditional chemical refining.
As can be seen from Table 1, the camellia oil obtained in example 2 meets the quality index of the first-stage oil camellia oil pressed in the national standard (GB/T11765-2018) of oil camellia oil.
The color of the camellia oil filtered by the rotating film in example 2 is reduced compared with that of the camellia oil filtered by the tubular ceramic film in comparative example 4 and the traditional chemical refining method in comparative example 3, and the red value is reduced by 32% compared with that of the traditional chemical refining method. The contents of water and volatile matters in the camellia oil filtered by the rotary membrane are 0.03 percent, and are respectively reduced by 50 percent compared with the content (0.06 percent) of the camellia oil filtered by the tubular ceramic membrane and 63 percent compared with the content (0.08 percent) of the camellia oil filtered by the traditional chemical refining method. The insoluble impurities in the camellia oil filtered by the rotary membrane are 0.01%, and are respectively reduced by 67% compared with the filtration content (0.03%) of the tubular ceramic membrane and 75% compared with the content (0.04%) of the camellia oil filtered by the traditional chemical refining method, which indicates that the camellia oil filtered by the rotary membrane has a better removal effect on trace water, volatile matters and insoluble impurities contained in the oil. In addition, the phospholipid content (18.32 mg/g) of the camellia oil filtered by the rotary membrane is reduced by 40% compared with the phospholipid content (30.46 mg/g) filtered by the tubular ceramic membrane, and the phospholipid content (46.35 mg/g) of the camellia oil filtered by the traditional chemical refining method is reduced by 60%, which shows that the camellia oil filtered by the rotary membrane has higher removal rate of the phospholipid in the oil and better degumming effect. The acid value (0.65 mg/g) and the peroxide value (0.16 g/100 g) of the camellia oil filtered by the rotary membrane are reduced compared with the acid value (0.76 mg/g) and the peroxide value (0.20 g/100 g) of the tubular ceramic membrane filter and the acid value (0.83 mg/g) and the peroxide value (0.22 g/100 g) of the camellia oil filtered by the traditional chemical refining method, which shows that the camellia oil filtered by the rotary membrane has better deacidification effect and oxidation resistance. According to the results, the quality of the camellia oil obtained by the rotary membrane filtration is higher than that of the camellia oil obtained by the tubular ceramic membrane filtration and the traditional chemical refining.
As can be seen from Table 1, the camellia oil obtained in example 3 meets the quality index of the first-grade pressed camellia oil in the national standard (GB/T11765-2018) of camellia oil.
The color of the camellia oil filtered by the rotating film in example 3 is reduced compared with that of the camellia oil filtered by the tubular ceramic film in comparative example 6 and the traditional chemical refining method in comparative example 5, and the red value is reduced by 20% compared with that of the traditional chemical refining method. The content of water and volatile matters in the camellia oil filtered by the rotary membrane is 0.05%, which is respectively reduced by 29% compared with the content (0.07%) of the tubular ceramic membrane and 44% compared with the content (0.09%) of the camellia oil filtered by the traditional chemical refining method. The insoluble impurities in the camellia oil filtered by the rotary membrane are 0.02%, and are respectively reduced by 33% compared with the filtration content (0.03%) of the tubular ceramic membrane and 50% compared with the content (0.04%) of the camellia oil filtered by the traditional chemical refining method, which indicates that the camellia oil filtered by the rotary membrane has a better removal effect on trace water, volatile matters and insoluble impurities contained in the oil. In addition, the phospholipid content (21.66 mg/g) of the camellia oil filtered by the rotary membrane is reduced by 39% compared with that (35.29 mg/g) of the camellia oil filtered by the tubular ceramic membrane, and the phospholipid content (53.71 mg/g) of the camellia oil filtered by the traditional chemical refining method is reduced by 60%, which shows that the camellia oil filtered by the rotary membrane has higher removal rate of the phospholipid in the oil and better degumming effect. The acid value (0.81 mg/g) and the peroxide value (0.19 g/100 g) of the camellia oil filtered by the rotary membrane are reduced compared with the acid value (0.92 mg/g) and the peroxide value (0.23 g/100 g) of the tubular ceramic membrane filter and the acid value (0.95 mg/g) and the peroxide value (0.24 g/100 g) of the traditional chemical refining, which shows that the camellia oil filtered by the rotary membrane has better deacidification effect and oxidation resistance. According to the results, the quality of the camellia oil obtained by filtering through the rotary membrane filtering and purifying device is higher than that of the camellia oil obtained by filtering through the tubular ceramic membrane and through traditional chemical refining.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (4)
1. The method for filtering and purifying camellia oil is characterized by comprising the following steps of:
physically squeezing camellia seeds to obtain crude camellia oil;
performing rotary membrane filtration and purification on the camellia crude oil by adopting a rotary membrane filtration and purification device to obtain camellia oil;
the rotary membrane filtration and purification device comprises a rotary membrane main body and a concentric cylindrical cover (3); the rotating membrane main body comprises a plurality of rotating membranes (1) and a rotating membrane support body (2); the rotary membrane supporting body (2) penetrates through the rotary membranes (1); the rotary membranes (1) are parallelly stacked on the rotary membrane supporting body (2), and the rotary membrane main body is positioned in the concentric cylindrical cover (3); the rotary diaphragms (1) are provided with flow guide grooves (4); the aperture of the rotary membrane (1) is 0.0005 to 0.2 mu m independently; the number of the rotary membranes (1) is 12; the diameter of the rotary membrane (1) is 20cm; the membrane flux of the rotating membrane (1) is independent from 30 to 42L/h.m 2 (ii) a The rotary membrane (1) is made of a ceramic material sintered at high temperature;
the temperature of the rotary membrane filtration purification is 30 to 60 ℃; the pressure of the rotary membrane for filtration and purification is 0.05 to 1.5 MPa; the flow rate of the rotary membrane filtration and purification is 50 to 60L/h; the rotating speed of a rotating membrane in the rotating membrane filtering and purifying device is 500 to 1000r/min.
2. The method according to claim 1, wherein prior to physically pressing the camellia seeds, further comprising: sequentially cleaning, drying and screening camellia seeds; the drying temperature is 45 to 55 ℃; and drying until the water content of the camellia seeds is 10-15%.
3. The method as claimed in claim 2, wherein the mesh size of the screen used for screening is 100 to 150 mesh.
4. The method of claim 1, wherein the apparatus used for physical pressing is a press.
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