CN111471511A - Preparation method of safflower camellia seed oil - Google Patents

Preparation method of safflower camellia seed oil Download PDF

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CN111471511A
CN111471511A CN202010180899.5A CN202010180899A CN111471511A CN 111471511 A CN111471511 A CN 111471511A CN 202010180899 A CN202010180899 A CN 202010180899A CN 111471511 A CN111471511 A CN 111471511A
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camellia seed
camellia
oil
safflower
slurry
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杨胜利
刘兴泉
孟祥河
何浙华
余琳
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Zhejiang University of Technology ZJUT
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/06Production of fats or fatty oils from raw materials by pressing
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/16Refining fats or fatty oils by mechanical means

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Mechanical Engineering (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)

Abstract

The invention discloses a preparation method of safflower camellia seed oil, which comprises the steps of adding water into camellia seeds, crushing the camellia seeds, adding a demulsifier for pulping, then carrying out ultrasonic and microwave treatment, and squeezing to extract camellia seed oil, wherein the oil yield of the oil product is more than 28%, the peroxide value is lower than 3.6mmo L/kg, and the acid value is lower than 0.4 mgKOH/g.

Description

Preparation method of safflower camellia seed oil
(I) technical field
The invention relates to the technical field of biology, in particular to a preparation method of safflower camellia oil.
(II) background of the invention
The unsaturated fatty acid in the safflower camellia seed is up to 93%, and all indexes meet or exceed the first-grade edible oil standard of the squeezed camellia seed oil. And has no bitter taste, can be squeezed and eaten instantly, and has fragrant and mellow smell. The safflower camellia oil mainly contains unsaturated oleic acid and linoleic acid, does not contain linolenic acid, has rich antioxidant substances, and is stable in grease and not easy to oxidize. Wherein the oleic acid content is 74-87%, not only can supply a large amount of heat energy required by human body, but also can regulate the concentration ratio of high-density lipoprotein and low-density lipoprotein cholesterol in human plasma, and has a certain effect on softening blood vessels. However, oleic acid synthesized by the human body cannot meet the requirement and needs to be taken from food, so that the edible oil with higher oleic acid content is beneficial to health. The linoleic acid is necessary for human body, and the linoleic acid can not be synthesized by human body, and is harmful to human body when being eaten excessively. The safflower camellia oil contains oleic acid and linoleic acid in a proportion close to the proportion required by human bodies, is similar to breast milk, and is not possessed by other vegetable oils. The safflower and camellia contains various active substances besides unsaturated fatty acid. For example, the content of squalene is between 120-280mg/kg, and the content of natural vitamin E is 10-20 times of that of olive oil. In view of rich resources and excellent nutritional composition, the safflower camellia seeds are hopeful to be one of high-quality edible vegetable oil resources in the future in China.
At present, vegetable oils in the market are various in variety, but the camellia oil is processed late, and quality problems such as nutrient loss, poor flavor, high acidity and the like are caused due to improper processing method.
Disclosure of the invention
The invention provides the advantages of an ultrasonic wave and microwave pretreatment method, and overcomes the defects of high quality and low cost of the traditional squeezing method which are difficult to fuse.
The invention adopts the following technical scheme:
the invention provides a preparation method of safflower camellia oil, which comprises the following steps:
(1) pretreatment of safflower camellia seeds: mixing the safflower camellia seed kernels with water, and crushing by a wet method to obtain safflower camellia seed kernel slurry;
(2) tempering: adding a demulsifier into the slurry of the safflower and camellia seed kernels, and stirring for 30-60 minutes at the temperature of 25-30 ℃ and at the speed of 20-30 r/min to obtain the slurry after tempering; the demulsifier is one of sodium carbonate, sodium chloride or magnesium chloride;
(3) ultrasonic pretreatment: treating the modified slurry for 20-40 minutes under the conditions of power of 400-;
(4) microwave wave pretreatment: performing microwave treatment on the camellia seed residue obtained in the step (3) for 2-4 minutes under the conditions that the power density is 4-8w/g and the vacuum degree is 0.03-0.06MPa to obtain microwave pretreatment residue;
(5) squeezing: squeezing the microwave pretreated residue at 20-25 deg.C under 20-60MPa for 1.5-2.0 hr (preferably squeezing in a squeezer at 20-25 deg.C, slowly increasing pressure, keeping pressure at 20-60MPa for 20-30 min for 1.5-2.0 hr to obtain juice;
(6) and (3) filtering: filtering the juice in the step (2) by using 100-mesh filter cloth with 300 meshes under 0.3-0.5MPa (preferably using a plate and frame filter) to obtain filtrate;
(7) decanting: naturally settling and separating the filtrate obtained in the step (6) at 16-20 ℃ (preferably adopting a decanting barrel, wherein the decanting time is 4-6 hours), obtaining an upper oil phase and a lower water phase after oil and water are separated, and taking the upper oil phase;
(8) centrifugal separation: centrifuging the lower aqueous phase in the step (7) (preferably at 4000-;
(9) vacuum filtration: combining the oil phase in the step (7) and the oil phase in the step (8), and filtering under vacuum (preferably at the temperature of 16-20 ℃ and the vacuum degree of-0.085-0.095 MPa), and taking the filtrate to obtain the safflower camellia seed oil.
Further, the camellia seed kernel in the step (1) is prepared by peeling and underwear-removing camellia seeds, and the camellia seeds are selected from the camellia seeds of high mountain red produced in Chunan county of Zhejiang province.
Furthermore, the volume of the water used in the step (1) is 4-8 m L/g, preferably 6, based on the weight of the safflower camellia seed kernel, and the wet crushing refers to crushing the camellia seed in an aqueous phase state.
Further, the mass addition amount of the demulsifier in the step (2) is 0.2-0.4% of the weight of the safflower mountain tea seed pulp.
Further, the step (3) is carried out under the conditions of 450W of power, 20kHz of frequency and 25 ℃ for 30 minutes.
Further, the microwave power density in the step (4) is preferably 6 w/g.
Further, the squeezing temperature of the step (5) is 20 ℃, the pressure is slowly increased, the pressure reaches the maximum value of 50MPa within 25 minutes, and the pressure holding time is 1.5 hours.
Further, 200-mesh filter cloth is selected in the step (6), and the filtering pressure is 0.3-0.5 MPa.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the oil yield of the oil pressing method product is more than 28%, the peroxide value is lower than 3.6mmo L/kg, and the acid value is lower than 0.4 mgKOH/g.
(2) The method has the advantages of simple process, simple used equipment, easily obtained and safe reagents, low production cost and easy realization of industrialization.
(IV) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
in the invention, if not specifically indicated, all equipment, reagents and raw materials can be purchased from the market or are commonly used in the industry, and the used methods are conventional methods in the field if no special description is provided.
The camellia seed of the alpine safflower is camellia oleifera (Camellia Chi.) of Camellia of Theaceae, and is selected from camellia seeds of alpine safflower produced in Chunan county of Zhejiang province.
Example 1
(1) The camellia seed pretreatment comprises the steps of selecting alpine camellia seed, peeling off the skin, removing underwear and obtaining camellia seed kernel, taking 2kg of camellia seed kernel, adding 8L water, and crushing by a wet method to prepare 10kg of camellia seed kernel slurry;
(2) tempering: adding 200g (0.2% of the mass of the camellia seed kernel pulp) of sodium carbonate into 10kg of camellia seed kernel pulp, and stirring for 30 minutes at 25 ℃ under the condition of 20 revolutions per minute to obtain 10.02kg of modified pulp;
(3) ultrasonic pretreatment: putting 10.02kg of the modified slurry into ultrasonic waves, treating for 20 minutes at 20 ℃, controlling the power to be 400W and the frequency to be 20kHz to obtain 10.02kg of ultrasonic pretreated slurry, centrifugally separating water at 4000 rpm, and drying at 40 ℃ to obtain 2.4kg of camellia seed residues;
(4) microwave wave pretreatment: 2.4kg of camellia seed residue after ultrasonic pretreatment is put into microwave for treatment for 2 minutes, the power density is 4w/g, the vacuum degree is 0.03MPa, and 2kg of microwave pretreatment residue is obtained;
(5) squeezing: 2kg of microwave pretreatment slag is put into a squeezer to be squeezed, the squeezing temperature is 20 ℃, the pressure is slowly increased, the pressure reaches the maximum value of 20MPa within 20 minutes, and the pressure holding time is 1.5 hours, so that 0.87kg of juice is obtained;
(6) and (3) filtering: filtering the squeezed juice with a plate-frame filter, selecting 100-mesh filter cloth, and filtering under 0.3MPa to obtain filtrate;
(7) decanting: putting the filtrate in a decanting barrel, and naturally settling and separating oil and water at 16 deg.C for 4 hr. After the oil and water are separated, taking 0.57kg of upper oil phase;
(8) centrifugal separation: centrifuging the decanted lower water phase at 4000 rpm for 15 min, and collecting the upper oil phase 0.04 kg;
(9) vacuum filtration: and (4) mixing the oil phase obtained after the decantation in the step (7) and the oil phase obtained by the centrifugation in the step (8) together, and performing vacuum filtration at the temperature of 16 ℃ and the vacuum degree of-0.085 MPa to obtain 0.54kg of the alpine safflower camellia seed oil.
The camellia oil prepared in this example had an oil yield of 27.1%, a peroxide value of 3.82mmo L/kg, and an acid value of 0.41 mgKOH/g.
And (3) oil yield determination:
Figure BDA0002412492130000041
in formula (1):
M0the mass of the safflower mountain tea seed kernel is g;
M1is the mass of camellia oil, g.
Measurement of acid value:
weighing 3g of sample (accurate to 0.0002g) in an erlenmeyer flask, adding 50m L neutral ethanol, heating and dissolving on a water bath, then placing to room temperature, adding 1 drop of phenolphthalein indicator, and dropping to reddish with 0.05 mol/L of potassium hydroxide standard solution until the color does not fade for 10 s.
Acid value X1(mgKOH/g) calculated according to formula (2):
Figure BDA0002412492130000042
in the formula (2), c is the concentration of a potassium hydroxide standard solution, mol/L;
v-sample consumption Potassium hydroxide Standard solution volume, m L;
56.1-the mass of potassium hydroxide equivalent to 1.00 ml of standard solution of potassium hydroxide [ c (KOH) ═ 1.000 mol/L ], mg;
m is the sample mass, g.
Determination of peroxide number:
accurately weighing 5g of uniformly mixed oil sample, adding the uniformly mixed oil sample into a 250m L iodine measuring flask, adding 10m L trichloromethane, dissolving the sample, adding 15m L acetic acid and 1m L saturated potassium iodide solution, quickly covering a bottle stopper, shaking the solution uniformly for 1min, keeping the solution in dark for 3min, taking out the solution, adding 75m L water, taking a starch solution as an indicator, titrating the precipitated iodine by using a sodium thiosulfate standard solution, and shaking forcefully in the titration process to simultaneously perform a blank test.
Figure BDA0002412492130000051
In formula (3): v1Volume of sodium thiosulfate standard solution consumed by the sample, m L;
V0volume of sodium thiosulfate standard solution consumed for the blank test, m L;
c-concentration of standard solution of sodium thiosulfate, mol/L;
m-mass of sample, g.
Example 2
(1) Pretreating Camellia seed by selecting Camellia seed, peeling, removing underwear to obtain 2kg seed kernel, adding 10L, and wet crushing to obtain 12kg seed kernel slurry;
(2) tempering: adding 36g (0.3% of the weight of the camellia seed kernel pulp) of sodium chloride into 12kg of camellia seed kernel pulp, stirring for 40 minutes at 28 ℃ and 25 r/min to obtain 12.036kg of modified pulp;
(3) ultrasonic pretreatment: 12.036kg of the modified serous fluid is put into ultrasonic waves, the treated serous fluid is processed for 30 minutes at 25 ℃, the power is 450W, the frequency is 25kHz, 12.036kg of ultrasonic pre-treated serous fluid is obtained, water is centrifugally separated at 5000 r/min, and 2.4kg of camellia seed dregs are obtained after drying at 50 ℃;
(4) microwave wave pretreatment: 2.4kg of the ultrasonic pretreatment material slag is put into microwaves for treatment for 3 minutes, the power density is 6w/g, the vacuum degree is 0.05MPa, and 1.98kg of the microwave pretreatment material slag is obtained;
(5) squeezing: 1.98kg of the material residue after microwave pretreatment is put into a squeezer to be squeezed, the squeezing temperature is 22 ℃, the pressure is slowly increased, the pressure reaches the maximum value of 40MPa within 25 minutes, and the pressure holding time is 1.8 hours, so that 0.89kg of juice is obtained;
(6) and (3) filtering: filtering the squeezed juice with a plate-and-frame filter, selecting 200-mesh filter cloth, and filtering under 0.5MPa to obtain filtrate;
(7) decanting: putting the filtrate in a decanting barrel, and naturally settling and separating oil and water at 18 deg.C for 5 hr. After the oil and water are separated, taking 0.61kg of upper oil phase;
(8) centrifugal separation: centrifuging the decanted lower water phase at 4500 rpm for 20 min, and collecting upper oil phase 0.03 kg;
(9) vacuum filtration: and (4) mixing the oil phase obtained after the decantation in the step (7) and the oil phase obtained by the centrifugation in the step (8) together, and performing vacuum filtration at the temperature of 18 ℃ and the vacuum degree of-0.090 MPa to obtain 0.57kg of the alpine safflower camellia seed oil.
The camellia oil prepared in this example, tested by the method of example 1, had an oil yield of 28.4%, a peroxide value of 3.35mmo L/kg, and an acid value of 0.36 mgKOH/g.
Example 3
(1) The camellia seed pretreatment comprises selecting camellia seed from Gaoshan, peeling, and removing underwear to obtain camellia seed kernel, adding 16L into 2kg camellia seed kernel, and wet crushing to obtain 18kg camellia seed kernel slurry;
(2) tempering: adding 72g (0.4% of the mass of the camellia seed kernel pulp) of magnesium chloride into 18kg of camellia seed kernel pulp, and stirring for 60 minutes at 30 ℃ at 30 r/min to obtain 18.072kg of modified pulp;
(3) ultrasonic pretreatment: 18.072kg of the modified serous fluid is put into ultrasonic waves to be processed for 40 minutes at 30 ℃, the power is 500W, the frequency is 30kHz, 18.072kg of ultrasonic pre-processed serous fluid is obtained, water is centrifugally separated at 5000 r/min, and 2.4kg of camellia seed dregs are obtained after drying at 60 ℃;
(4) microwave wave pretreatment: 2.4kg of the ultrasonic pretreatment material slag is put into microwaves for treatment for 4 minutes, the power density is 8w/g, the vacuum degree is 0.06MPa, and 1.96kg of the microwave pretreatment material slag is obtained;
(5) squeezing: 1.96kg of the material slag after microwave pretreatment is put into a squeezer to be squeezed, the squeezing temperature is 25 ℃, the pressure is slowly increased, the pressure reaches the maximum value of 60MPa within 30 minutes, and the pressure holding time is 2.0 hours, so that 0.91kg of juice is obtained;
(6) and (3) filtering: filtering the squeezed juice with a plate-frame filter, selecting 300-mesh filter cloth, and filtering under the filtering pressure of 0.5MPa to obtain filtrate;
(7) decanting: putting the filtrate in a decanting barrel, and naturally settling and separating oil and water at 20 deg.C for 6 hr. After the oil and water are separated, taking 0.58g of upper oil phase;
(8) centrifugal separation: centrifuging the decanted lower water phase at 5000 rpm for 25 min, and collecting upper oil phase 0.04 g;
(9) vacuum filtration: and (4) mixing the oil phase obtained after the decantation in the step (7) and the oil phase obtained by the centrifugation in the step (8) together, and performing vacuum filtration at the temperature of 20 ℃ and the vacuum degree of-0.095 MPa to obtain 0.55g of the alpine safflower camellia seed oil.
The camellia oil prepared in this example, tested by the method of example 1, had an oil yield of 27.6%, a peroxide value of 3.57mmo L/kg, and an acid value of 0.39 mgKOH/g.

Claims (8)

1. A preparation method of safflower camellia oil is characterized by comprising the following steps:
(1) pretreatment of safflower camellia seeds: mixing the safflower camellia seed kernels with water, and crushing by a wet method to obtain safflower camellia seed kernel slurry;
(2) tempering: adding a demulsifier into the slurry of the safflower and camellia seed kernels, and stirring for 30-60 minutes at the temperature of 25-30 ℃ and at the speed of 20-30 r/min to obtain the slurry after tempering; the demulsifier is one of sodium carbonate, sodium chloride or magnesium chloride;
(3) ultrasonic pretreatment: treating the modified slurry for 20-40 minutes under the conditions of power of 400-500W, frequency of 20-30kHz and 20-30 ℃ to obtain ultrasonic pretreatment slurry, centrifuging, precipitating and drying to obtain camellia seed residue;
(4) microwave wave pretreatment: performing microwave treatment on the camellia seed residue obtained in the step (3) for 2-4 minutes under the conditions that the power density is 4-8w/g and the vacuum degree is 0.03-0.06MPa to obtain microwave pretreatment residue;
(5) squeezing: squeezing the microwave pretreated residue at 20-25 deg.C under 20-60MPa for 1.5-2.0 hr to obtain juice;
(6) and (3) filtering: filtering the juice in the step (5) by using 100-mesh 300-mesh filter cloth under 0.3-0.5MPa to obtain filtrate;
(7) decanting: naturally settling and separating the filtrate obtained in the step (6) at 16-20 ℃, obtaining an upper oil phase and a lower water phase after oil and water are separated, and taking the upper oil phase;
(8) centrifugal separation: centrifuging the lower-layer water phase in the step (7) and taking the upper-layer oil phase;
(9) vacuum filtration: and (4) combining the oil phase obtained in the step (7) and the oil phase obtained in the step (8), and performing vacuum filtration to obtain filtrate, thus obtaining the safflower camellia seed oil.
2. A method according to claim 1, wherein the water is used in an amount of 4-8 m L/g (by volume based on the weight of the camellia seed kernel) in step (1).
3. The method of claim 1, wherein the demulsifier of step (2) is added in an amount of 0.2-0.4% by weight based on the weight of the slurry of the seeds of camellia sinensis var.
4. The method according to claim 1, wherein the step (3) is carried out at a power of 450W and a frequency of 20kHz at 25 ℃ for 30 minutes.
5. The method of claim 1, wherein the microwave power density of step (4) is 6 w/g.
6. The method of claim 1, wherein the pressing temperature in step (5) is 20 ℃, the pressure is slowly increased, the pressure reaches a maximum of 50MPa for 25 minutes, and the pressure holding time is 1.5 hours.
7. The method of claim 1, wherein step (6) employs 200 mesh filter cloth.
8. The method of claim 1, wherein the vacuum filtration conditions of step (9) are: the temperature is 16-20 ℃, and the vacuum degree is-0.085 to-0.095 MPa.
CN202010180899.5A 2020-03-16 2020-03-16 Preparation method of safflower camellia seed oil Pending CN111471511A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105886107A (en) * 2014-12-19 2016-08-24 贵州省黎平县黔香园油脂有限公司 Strong-flavor camellia oil cold-pressing process
CN109423353A (en) * 2017-08-22 2019-03-05 湖南宏健茶油生物科技有限公司 A kind of method of cold pressing and physical method refining camellia seed oil
CN109593598A (en) * 2019-01-14 2019-04-09 湖南泥头山油茶开发有限公司 A kind of processing technology of camellia oil

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105886107A (en) * 2014-12-19 2016-08-24 贵州省黎平县黔香园油脂有限公司 Strong-flavor camellia oil cold-pressing process
CN109423353A (en) * 2017-08-22 2019-03-05 湖南宏健茶油生物科技有限公司 A kind of method of cold pressing and physical method refining camellia seed oil
CN109593598A (en) * 2019-01-14 2019-04-09 湖南泥头山油茶开发有限公司 A kind of processing technology of camellia oil

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Application publication date: 20200731