CN116376631A - Preparation process of camellia oil for cosmetics - Google Patents

Preparation process of camellia oil for cosmetics Download PDF

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CN116376631A
CN116376631A CN202310325529.XA CN202310325529A CN116376631A CN 116376631 A CN116376631 A CN 116376631A CN 202310325529 A CN202310325529 A CN 202310325529A CN 116376631 A CN116376631 A CN 116376631A
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oil
camellia
alkali
amount
cosmetics
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周飞
程巧鸳
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Zhejiang Shancharun Biotechnology Co ltd
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Zhejiang Shancharun Biotechnology Co ltd
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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
    • C11B1/06Production 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
    • 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
    • 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
    • C11B3/02Refining fats or fatty oils by chemical reaction
    • C11B3/06Refining fats or fatty oils by chemical reaction with bases
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Cosmetics (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention discloses a preparation process of camellia oil for cosmetics, and belongs to the technical field of camellia oil preparation. The preparation process comprises a squeezing production process and a refining production process, wherein the squeezing production process comprises the following steps of: crushing camellia seeds, removing shells to obtain a pressed material; rolling the pressed material, and further steaming and frying to obtain a material blank; mechanically squeezing the embryo, and further filtering to obtain camellia crude oil; the refining production process comprises the following steps: and (3) performing alkali refining, water washing, decoloring, filtering, deodorizing, cooling and freezing on the camellia crude oil obtained in the step (S1) to obtain the camellia oil for cosmetics. The camellia oil obtained by the preparation process disclosed by the invention has excellent performance and can be used for preparing cosmetics.

Description

Preparation process of camellia oil for cosmetics
Technical Field
The invention belongs to the technical field of camellia oil preparation, and particularly relates to a preparation process of camellia oil for cosmetics.
Background
Tea-oil Camellia (Camellia Oleifera Abe.) is a evergreen, long-life oil woody plant of the genus Camellia (Camellia) of the family Camellia (Theaceae). The fruit of the camellia oleifera contains 2-3 seeds with the diameter of 2-3 cm, the seed kernel accounts for 60-75% of the whole seeds, and the oil content of the seed kernel is very high and can reach 40-60% by mass. China is the country with the most widely distributed camellia plants, and is also the largest camellia oil production base in the world. The camellia oil is obtained by squeezing or leaching camellia seeds, and is clear and transparent, light yellow in color and fragrant in smell. The camellia oil is also called tea oil, tea seed oil and tea seed oil, and is a nutritional oil with excellent curative effect and health care performance.
The camellia oil is rich in unsaturated fatty acid, and becomes one of the base vegetable oils for cosmetics due to the characteristics of natural and mild nature, strong permeability, difficult oxidative deterioration, safety and the like. Developed countries or regions in the world develop skin-beautifying oil, hair-beautifying oil, body-care oil and other products which take camellia oil as raw materials, and are popular in the international market.
At present, the camellia oil products are plentiful and the cosmetic-grade camellia oil products are few.
Disclosure of Invention
In order to solve at least one of the technical problems, the invention adopts the following technical scheme:
the invention provides a preparation process of camellia oil for cosmetics, which comprises a squeezing production process and a refining production process, and comprises the following steps:
s1, squeezing production technology: crushing camellia seeds, removing shells to obtain a pressed material; rolling the pressed material, and further steaming and frying to obtain a material blank; mechanically squeezing the embryo, and further filtering to obtain camellia crude oil;
s2, refining production technology: alkali refining, washing, decolorizing, filtering, deodorizing, cooling and freezing the camellia crude oil obtained in the step S1 to obtain camellia oil for cosmetics,
wherein, in the alkali refining process, the Baume degree of the alkali liquor is determined according to the value of the wool oleic acid, and when the value of the wool oleic acid is more than 6, the Baume degree of the alkali liquor is selected to be 16-18; when the value of the linoleic acid is less than or equal to 6, the Baume degree of the alkali liquor is selected to be 14-16.
Further, in the step S1, the shell content in the pressed material is 10-15%, so that the following benefits are achieved:
(1) Mutual friction is increased during blank rolling, so that paste is avoided, and a loosening effect is achieved;
(2) When steaming and frying, the material has the effects of ventilation and heat transfer, so that the material is easy to steam thoroughly;
(3) Can act as capillary pores during oil extraction by squeezing.
In some embodiments of the present invention, step S2 specifically includes:
s21, alkali refining: heating the camellia crude oil under stirring at 20-30 rpm, and stopping heating when the oil temperature reaches 30 ℃; adjusting the stirring speed to 50-70 rpm, adding alkali liquor, and continuously stirring for 10-30 minutes; then the stirring speed is adjusted to 20-30 r/min, when the soapstock is separated from the oil, the stirring is stopped, the precipitation is carried out for 6-10 hours, and the soapstock is discharged;
s22, washing: heating the oil temperature to 80-85 ℃, and washing the oil with hot water with the temperature 5 ℃ higher than the oil temperature;
s23, decoloring: heating the oil temperature to 105 ℃, vacuumizing to-0.098 Mpa, adding a decoloring agent, keeping the oil temperature to 105 ℃, and reacting for 15-20 minutes;
s24, filtering: filtering the decolorized tea oil by using a plate-frame filter;
s25, deodorizing and cooling: heating tea oil under vacuum degree of-0.098 Mpa, when the oil temperature reaches 100 ℃, opening a steam valve of a deodorization pot to enable steam water mist in the deodorization pot to be in a spray umbrella shape, when the oil temperature reaches 110 ℃, opening the steam valve to enable the steam mist to evaporate, sucking odor in the oil along with vacuum, when the oil temperature reaches 235-245 ℃, keeping for 2-3 hours, and then cooling by utilizing water;
s26, freezing: and (3) cooling the oil to 4-5 ℃ for crystallization and crystal growth for more than 48 hours, and filtering to obtain camellia oil finished product oil.
In some embodiments of the invention, in step S21, the lye amount comprises a theoretical amount of alkali and a super amount of alkali, said theoretical amount of alkali being obtained using the following table:
Figure SMS_1
Figure SMS_2
wherein, the acid value refers to the acid value which needs to be reduced, and the number before the decimal point and the number after the decimal point are respectively checked on the table to obtain theoretical alkali amount and then added; the amount of super base is determined using the following table:
Figure SMS_3
further, when the amount of the super alkali is determined, the solid alkali is selected to account for 0.25% of the weight of the oil.
The alkali liquor dosage determined by the method can be used for deacidifying crude oil better and protecting the performance of camellia oil.
In some embodiments of the invention, after adding the alkali liquor, when the stirring speed is adjusted to 20-30 r/min, the tea oil is heated, the heating speed is 1 ℃ per minute, and the oil temperature is increased to 35-45 ℃. If the temperature is too high, such as 2 ℃/min, or if the temperature is too high, such as raising the temperature to 60 ℃, the performance of the resulting camellia oil will be affected.
In some embodiments of the invention, hot brine at the same oil temperature is added during the temperature rising process when the soapstock is separated from the oil, and the amount of hot brine added is not less than the amount of alkali liquor.
1. In some embodiments of the invention, in step S22, the water washing process is repeated 4 times, and salt is added to the hot water during the 1 st to 3 rd water washing, wherein the salt is used in an amount of 3 to 5% of the total amount of crude oil.
In some embodiments of the present invention, in step S23, the decoloring agent is clay and activated carbon, the clay is added in an amount of 7 to 15% by weight of the tea oil, and the activated carbon is added in an amount of 0.2 to 1.0% by weight of the tea oil.
In some embodiments of the invention, in step S25, the deodorized oil is used to exchange heat with the oil to be deodorized in the next batch. Therefore, the deodorized oil and the oil to be deodorized are subjected to heat exchange, so that on one hand, the deodorized oil can be cooled, and on the other hand, the deodorized oil can be quickly warmed, and energy and time are saved.
The beneficial effects of the invention are that
Compared with the prior art, the invention has the following beneficial effects:
1. the invention controls the shell content to be 10-15% in the material pressing process, and has the following advantages: mutual friction is increased during blank rolling, so that paste is avoided, and a loosening effect is achieved; when steaming and frying, the material has the effects of ventilation and heat transfer, so that the material is easy to steam thoroughly; can act as capillary pores during oil extraction by squeezing.
2. The alkali liquor dosage determined by the method can be used for deacidifying crude oil better and protecting the performance of camellia oil.
3. The invention ensures the high performance of the obtained camellia oil by adjusting parameters in the heating process after alkali refining, such as heating speed and temperature range, timely and proper addition of salt and the like, so that the camellia oil can be used for cosmetic production.
4. The present invention utilizes the heat exchange between the deodorized oil and the oil to be deodorized in the next batch. Therefore, the deodorized oil and the oil to be deodorized are subjected to heat exchange, so that on one hand, the deodorized oil can be cooled, and on the other hand, the deodorized oil can be quickly warmed, and energy and time are saved.
Drawings
Figure 1 shows a schematic representation of the press process flow of the present invention.
Figure 2 shows a schematic diagram of the refining process flow of the present invention.
Detailed Description
Unless otherwise indicated, implied from the context, or common denominator in the art, all parts and percentages in the present application are based on weight and the test and characterization methods used are synchronized with the filing date of the present application. Where applicable, the disclosure of any patent, patent application, or publication referred to in this application is incorporated by reference in its entirety, and the equivalent patents to those cited are incorporated by reference, particularly as they relate to the definitions of terms in the art. If the definition of a particular term disclosed in the prior art does not conform to any definition provided in this application, the definition of that term provided in this application controls.
Numerical ranges in this application are approximations, so that it may include the numerical values outside of the range unless otherwise indicated. The numerical range includes all values from the lower value to the upper value that increase by 1 unit, provided that there is a spacing of at least 2 units between any lower value and any higher value. For ranges containing values less than 1 or containing fractions greater than 1 (e.g., 1.1,1.5, etc.), then 1 unit is suitably considered to be 0.0001,0.001,0.01, or 0.1. For a range containing units of less than 10 (e.g., 1 to 5), 1 unit is generally considered to be 0.1. These are merely specific examples of what is intended to be provided, and all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be expressly stated in this application.
The terms "comprises," "comprising," "including," and their derivatives do not exclude the presence of any other component, step or procedure, and are not related to whether or not such other component, step or procedure is disclosed in the present application. For the avoidance of any doubt, all use of the terms "comprising," "including," or "having" herein, unless expressly stated otherwise, may include any additional additive, adjuvant, or compound. Rather, the term "consisting essentially of … …" excludes any other component, step or process from the scope of any of the terms recited below, as those out of necessity for operability. The term "consisting of … …" does not include any components, steps or processes not specifically described or listed. The term "or" refers to the listed individual members or any combination thereof unless explicitly stated otherwise.
In order to make the technical problems, technical schemes and beneficial effects solved by the invention more clear, the invention is further described in detail below with reference to the embodiments.
Examples
The following examples are presented herein to demonstrate preferred embodiments of the present invention. It will be appreciated by those skilled in the art that the techniques disclosed in the examples which follow represent techniques discovered by the inventor to function in the practice of the invention, and thus can be considered to constitute preferred modes for its practice. Those of skill in the art should, in light of the present disclosure, appreciate that many changes can be made in the specific embodiments which are disclosed and still obtain a like or similar result without departing from the spirit or scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, the disclosure of which is incorporated herein by reference as is commonly understood by reference.
Those skilled in the art will recognize, or be able to ascertain using no more than routine experimentation, many equivalents to the specific embodiments of the invention described herein. Such equivalents are intended to be encompassed by the claims.
The experimental methods in the following examples are conventional methods unless otherwise specified. The instruments used in the following examples are laboratory conventional instruments unless otherwise specified; the test materials used in the examples described below, unless otherwise specified, were purchased from conventional chemical reagent stores.
Example 1
1. Squeezing production process
As shown in fig. 1, the crude oil is obtained after tea seed acceptance, crushing, embryo rolling, steaming, squeezing and filtering. The method comprises the following specific steps:
1. tea seed acceptance
The camellia seeds are required to be yellow and bright in color, free of mildew, free of impurities and free of pollution, and have relatively crisp sounds (the seed shells are completely separated) by hand shaking.
2. Crushing and rolling the embryo
Tea oil seeds are husked by a husking machine.
The requirements of husking and kernel-shell separation are as follows: the shell breaking rate is high, no seeds leak, and the powder amount is less than 5%; the shell content in the kernel is between 5 and 10 percent, and a 10-mesh/inch inspection sieve is used for inspection (the aperture is 2 mm); the kernel content in the shell is not more than 0.5%, if the whole seeds are removed, the seeds are counted after the shell is removed. When the shell and kernel are separated, the proportion of the shell and kernel is controlled, and the camellia seed raw material for one-time squeezing and oil extraction is controlled to contain 12 percent of residual shell, so that the camellia seed oil has the following advantages:
(1) Mutual friction is increased during blank rolling, so that the blank is prevented from being pasty, and a loosening effect is achieved;
(2) When steaming and frying, the material has the effects of ventilation and heat transfer, so that the material is easy to steam thoroughly;
(3) Can act as capillary pores during oil extraction by squeezing.
3. Steaming and frying
The steaming and frying conditions are as follows: and (5) exhausting air from the top of the steamer for 10-15 min.
The steaming and frying effect is mainly as follows:
(1) The grease is more fully prepared;
(2) The power consumption for oil extraction is reduced;
(3) The material adjusting blank structure is suitable for the squeezing requirement;
(4) Is convenient for preparing grease with better quality.
The surface of the steamed material embryo is Gu Huangse, and the inside and outside are uniformly cooked.
4. Squeezing
And squeezing the blank by using a novel full-automatic hydraulic oil press.
Necessary conditions for oil extraction by pressing:
(1) The pressure of the hydraulic press is regulated to 60Mpa;
(2) The squeezing time is as long as possible (more than or equal to 50min, but not more than 80 min) within a certain limit.
Squeezing to obtain camellia seed crude oil.
5. Filtration
If the camellia seed crude oil has better quality, the camellia seed crude oil can be filtered by adopting two parallel filtering net type pipeline filters only by simple filtering treatment to remove cake scraps. However, for camellia seed crude oil with more impurities, the camellia seed crude oil needs to be pretreated by a plate-and-frame filter press, namely insoluble mechanical impurities in the crude oil are separated as much as possible.
One operation period of the plate-and-frame filter press consists of four stages of assembling, filtering, unloading and cleaning filter cloth. In operation, filtration is stopped when the pressure of the filtered oil phase reaches 0.35 Mpa. And then compressed air is introduced to blow out residual grease in filter residues as much as possible, then a filter plate compactor is loosened, filter residues on the filter plates are removed, filter cloth is cleaned, and finally the filter cloth is recombined and production is continued.
The optimal temperature for filtering camellia seed oil is 35-40 ℃, and the filtered oil sludge can be mixed into oil for re-squeezing so as to recover grease.
4200kg of checked camellia seeds are pressed by the method to obtain 1200kg of crude oil, and the crude oil rate reaches 28.57%.
2. Refining production process
As shown in figure 2, the refining production process comprises alkali refining, water washing, decolorizing, filtering, deodorizing, freezing and degreasing (freezing) and the like, and finally filling. The detailed steps are as follows:
1. alkali refining
Opening an oil inlet valve of the alkali refining pot, pumping the oil into the alkali refining pot, starting slow stirring (20-30 r/min), then opening a steam valve of the alkali refining pot to heat, closing the steam valve when the oil temperature in the alkali refining pot reaches 30 ℃, changing the alkali refining pot into fast stirring (50-70 r/min), and starting to add alkali liquor into the oil of the alkali refining pot.
(1) Preparation of lye
The Baume degree (Biee) of the alkali liquor is measured by using a Baume meter, and the Baume degree is between 12 and 18, and the Baume degree is determined according to the acid value required to be reduced by the crude oil: when the valence of the linoleic acid is 6 to 7, the Baume degree used is 18. This choice is not a conventional choice, but the best results obtained through repeated experiments by the inventors.
Pumping the prepared alkali liquor from the alkali dissolving and preparing pool into an alkali liquor box for standby.
(2) Dosage of lye
The dosage of the alkali liquor is calculated according to the acid value and weight of the crude oil and the acid value and theoretical alkali which are achieved by the required finished oil and the excessive alkali.
For 1200kg crude oil obtained by the above 1 squeeze, the crude oil acid value is 6.7, the acid value of the finished oil is required to be below 0.6, and the alkali liquor consumption is calculated as follows:
theoretical amount of base (kg/t):
looking up "theoretical amount of base (kg) required per t of crude oil" in table 1, the actual reduction in acid number was 6.7-0.6=6.1, with baume selected to be 16. The table lookup shows that the theoretical alkali dosage corresponding to the acid value of 6.0 and the Baume degree of 16 is 38.58kg/t, the theoretical alkali dosage corresponding to the acid value of 0.1 and the Baume degree of 16 is 0.64kg/t. Thus, the theoretical base amount is 38.58kg/t+0.64 kg/t=39.22 kg/t.
Super base amount (kg/t):
the solid alkali is 0.1-0.3% of crude oil, and is obtained by looking up the required super alkali amount (kg) of each t of crude oil in table 2 according to 0.25% and looking up the table: super base = 25.50kg/t.
The actual alkali liquor dosage is as follows: (theoretical base+excess base) × Mao Youliang (t) = (39.22+22.50) kg/t×1.2t= 74.06kg.
TABLE 1 theoretical amount of alkali (kg) required per t crude oil
Figure SMS_4
TABLE 2 super alkali amount (kg) required per t crude oil
Figure SMS_5
Opening an alkali liquor box valve, slowly putting the prepared alkali liquor into crude oil in an alkali refining pot, wherein the alkali liquor can not be put too fast or too slow, after 5-10 minutes, according to the capacity of the alkali liquor box and the alkali addition amount, the alkali liquor is added, closing the alkali liquor putting valve of the alkali liquor box, rapidly stirring for 20 minutes, uniformly stirring the alkali liquor and the crude oil, and then regulating the stirring to be slow (20-30 r/min).
Heating: when the slow stirring is started, a steam valve of the alkali refining pot is started, heating is started, the heating speed is controlled at 1 ℃/min (the heating speed is controlled by the steam valve), and the oil temperature is increased to 40 ℃. In the heating process, when soapstock and oil are obviously separated, hot brine with the same oil temperature is added and sprayed into an alkali refining pot, the added hot brine amount is not less than the added alkali solution amount, the salt amount is 3-5 per mill of the crude oil amount, after the hot brine is added, a stirring button of the alkali refining pot is closed, stirring is stopped, and precipitation is carried out for 8 hours.
Placing soapstock: and (3) after crude oil in the alkali refining pot is precipitated for 8 hours, the crude oil is filled in a bottom discharge port of the alkali refining pot by a plastic barrel, and a valve at the bottom of the alkali refining pot is opened. When the mixture is discharged, the water-oil mixture is firstly discharged, the mixture is poured into an oil separating tank, so that water and oil are separated, the oil which floats on the surface after separation is recovered and reused, when the mixture is discharged, the soapstock which is colloid is discharged, the soapstock is poured into a soapstock big box, and when the mixture of the soapstock and the oil is discharged, a valve at the bottom of the alkali refining pot is closed.
2. Washing with water
Checking the water-washing pot, closing the emptying valve on the water-washing pot and all valves at the bottom of the water-washing pot, pressing down the hydraulic jet pump, starting the vacuum pump, and then slowly opening the water-washing pot vacuum valve. When the vacuum gauge on the water-washing pot rises, the oil in the alkali refining pot is sucked into the water-washing pot by utilizing vacuum. After the oil in the alkali refining pot is completely sucked, the oil inlet valve is closed, and the vacuum pump and the water washing pot vacuum valve are closed at the same time. Opening the emptying valve of the water-washing pot, starting slow stirring, and opening the steam valve of the water-washing pot, starting steam discharge and heating.
When the temperature is raised, hot water which is ready for washing is prepared in the hot water blending tank, a water inlet valve of the hot water blending tank is opened, the water tank is placed into the water level of 80%, a water inlet valve is closed, a steam valve of the hot water blending tank is opened, and the temperature of the water in the hot water blending tank is raised. When the water temperature is raised to 90 ℃, the steam inlet valve of the hot water tank is closed for standby.
When the temperature of the oil in the water-washing pot is raised to be 5 ℃ lower than the temperature of the hot water in the water tank (85 ℃), the steam inlet valve of the water-washing pot is closed, water draining and water washing are started, and the hot water in the hot water tank is put into the water-washing pot.
Adding water: the water adding amount is 15% of the weight of the crude oil, the scale is calculated according to the capacity of the hot water tank and the water adding amount, after water is added, the hot water valve is closed, and meanwhile, the stirring is switched into rapid stirring. After stirring for 15 minutes, the stirring was stopped and the oil of the water-wash pot was allowed to settle for 1 hour. After 1 hour, the valve at the bottom of the water-washing pot is opened, water and soapstock at the bottom of the water-washing pot are discharged, and the valve at the bottom of the water-washing pot is immediately closed until oil comes out.
The water washing process is repeated for 4 times, salt is added in the 1 st to 3 rd times of water washing, the dosage is 3 to 5 per mill of the crude oil, the salt is put into a hot water tank, and the 4 th time of water washing is performed.
3. Decoloring (decoloring)
After the oil in the water-washing pot is sucked into the decolorizing pot, stirring is started, then the heat conduction oil valve of the decolorizing pot is opened to start heating, when the oil temperature is raised to 105 ℃, the heat conduction oil valve is closed, a vacuum table is observed, when the vacuum table reaches-0.098 Mpa, the decolorizing agent, namely clay and activated carbon, is started to be added, wherein the addition amount of clay is 10% of the weight of the oil, and the addition amount of activated carbon is 0.8% of the weight of the oil.
After adding the decoloring agent, keeping the oil temperature at 105 ℃ and reacting for 15-20 minutes. Then cooling the oil temperature in the decoloring pot to 65-80 ℃ by using cooling water.
4. Filtration
After the filter cloth on the filter frame and the preparation work of filtering are placed, an oil drain valve of the decoloring pot is opened, and a valve between a pipeline of a filter pump and the filter is opened. And (3) starting the decoloring oil pump, namely starting filtering, and adjusting the stirring regulator of the decoloring pot to be stirred slowly in the filtering process so as to prevent clay precipitation and filtering while stirring. The filtered oil which is not very clear is discharged into a dirty oil tank, and the oil is discharged into the clean oil tank after the fresh oil comes out. And after the oil is normal, opening an oil inlet valve of the decoloring pot, opening a dirty oil pump, and sucking the dirty oil in the dirty oil tank into the decoloring pot for re-filtering.
During filtration, the pressure gauge on the filter is kept at 0.20MPa and not more than 0.25MPa.
5. Deodorization method
And (3) enabling the oil to be deodorized to enter the deodorizing pot through a group of coils in the heat exchange pot, closing an emptying valve of the deodorizing pot, and then starting a water vapor vacuum pump to suck the oil in the clean oil tank into the deodorizing pot. The vacuum gauge is always kept at about-0.098 Mpa, and when the oil temperature reaches 100deg.C, the steam valve of the deodorizing pan is opened to make the steam water mist in the deodorizing pan in spray umbrella shape. When the oil temperature reaches above 110 ℃, the steam valve is opened, so that the water mist can be evaporated, and the odor in the oil can be sucked away along with the vacuum. When the oil temperature reached 240 ℃, it was maintained for 3 hours.
6. Cooling
And (3) cooling the oil in the deodorizing pot in a heat exchange pot, and closing an oil outlet valve at the bottom of the deodorizing pot after the oil is emptied, so that the oil is cooled in the heat exchange pot. When the oil is put into the heat exchange pot, the valve of the heat exchange pot can be opened to allow water to enter the heat exchange pot for cooling, and the water flows out of the heat exchange pot through the coil pipe of the heat exchange pot. When the oil in the deodorizing pot is completely put into the heat exchange pot, the oil outlet valve at the bottom of the deodorizing pot is immediately closed, and the oil inlet and deodorizing operation of the next pot of oil are repeatedly started, so that the oil in the clean oil tank flows into the deodorizing pot through the coil pipe on the heat exchange pot, on one hand, cold oil can pass through the heat exchange pot, the oil temperature in the heat exchange pot is reduced, and on the other hand, the oil flowing into the deodorizing pot is quickly heated, and the energy and time are saved.
7. Freeze-thawing
The grease is subjected to alkali refining, water washing, decolorization and deodorization, and is pumped into a crystallization tank by an oil pump. After one pot of oil is filled, the oil pump is closed, the oil inlet valve is closed, the stirring of the crystallization tank is started, the circulating cooling water pump of the refrigerating unit is started, all valves (the crystallization tank needing to be frozen) of the brine circulation of the refrigerating unit are opened, the brine circulation pump and the refrigerating unit are started for cooling, when the isothermal temperature reaches 4 ℃, the stirring is stopped for crystallization and crystal growth, and when the oil temperature is risen to about 6 ℃, the refrigerating unit is started again for cooling (the refrigerating unit and the stirring are simultaneously started and closed, depending on the state of the crystallization and crystal growth of the oil and fat). The oil temperature was kept at about 5 ℃. The time for crystallizing and growing is not less than 48 hours.
And after the crystallization and crystal growing time is finished, an oil outlet valve at the bottom of the crystallization tank is opened, standing filtration is carried out under the dead weight pressure, the flow rate of an oil outlet nozzle is large when filtration is started, the oil flows into the turbid oil disc firstly, and the oil in the turbid oil disc is returned into the crystallization tank by an oil pump. And after the oil outlet flow of the oil nozzle is obviously reduced, the oil is treated as normal filtration, and the filtered oil flows into a finished oil tank. When the oil nozzle is basically incapable of discharging oil, the oil outlet valve is closed, the filter plate is loosened, the oil flowing out from the oil nozzle and the filter plate is placed in the turbid oil disc, the oil in the turbid oil disc is returned to other crystallization tanks by the oil pump, the filter paper is taken out, the oil attached to the filter paper is placed on the oil receiving disc, and the oil is naturally discharged.
8. Storage of
And filling the filtered finished oil into a storage tank for later use.
Example 2
Camellia oil was prepared using the method of example 1, except that the baume calculation of the lye was determined using the method disclosed in chinese invention patent CN106350208A, as shown in table 3:
TABLE 3 selection of acid value of camellia oil and Baume degree of lye
Figure SMS_6
Figure SMS_7
The crude oil has an acid value of 6.7, and the acid value is reduced by 6.7-0.6=6.1, so that the baume degree of the alkali liquor is 18.
Theoretical base (kg/t):
looking up the "kg table of theoretical alkali liquor required per t of crude oil" in Table 1, it is found that the theoretical alkali dosage corresponding to acid value of 6.0 and Baume degree of 18 is 33.96kg/t, and the theoretical alkali dosage corresponding to acid value of 0.1 and Baume degree of 18 is 0.57kg/t. Thus, the theoretical base amount is 33.96kg/t+0.57 kg/t= 34.53kg/t.
Super base amount (kg/t):
the amount of crude oil is 0.1 to 0.3 percent, and the total amount of the crude oil is obtained by looking up a table of the required super alkali amount kg per t of crude oil in table 2 according to 0.25 percent: super base = 19.80kg/t.
The actual alkali liquor dosage is as follows: (theoretical base+excess base) × Mao Youliang (t) = (34.53+19.80) kg/t×1.2t=54.33 kg.
Example 3
The camellia oil was prepared using the method of example 1, with the same 18 baume selection, except that the theoretical alkali content was calculated according to the calculation formula disclosed in the literature "Chen Linjie, ma Cheng Jin, huang Qun, ma mingyou, huang Changsong. Study on tea seed oil refining. Chinese oil crop theory, 2008,30 (2): 235-238." to give the theoretical alkali content as: 47.04kg.
The dosage of the super alkali is 0.25 percent of the weight of the crude oil, and 27.01kg of the super alkali is obtained.
The actual alkali liquor dosage is: 47.04 kg+27.01kg=74.05 kg.
Example 4
The camellia oil was prepared by the method of example 1, except that during alkali refining in the refining process, the temperature raising rate was controlled at 2 c/min after alkali addition, and the oil temperature was raised to 45 c.
Example 5
The camellia oil was prepared by the method of example 1, except that the temperature raising rate was controlled at 1 c/min and the oil temperature was raised to 60 c after alkali addition during alkali refining in the refining process.
Example 6
The camellia oil was prepared using the method of example 1, except that during the alkali refining process, there was no step of adding hot brine when the temperature was raised after the alkali placement.
Example 7
Camellia oil was prepared using the method of example 1, except that during the decolorization of the refining process, the decolorization was performed at normal atmospheric pressure.
The crude camellia oil and the finished camellia oil obtained in examples 1 to 7 were measured for acid value, and the peroxide value of the finished camellia oil was measured. Wherein, the acid value is measured according to GB 5009.229-2016 (determination of acid value in food safety national Standard food), and the peroxide value is measured according to GB 5009.227-2016 (determination of peroxide value in food safety national Standard food). The results are shown in Table 4:
TABLE 4 acid value and peroxide value of camellia oil prepared by each method
Figure SMS_8
Further, the finished camellia oil obtained in examples 1 to 7 was examined for color, transparency (20 ℃), insoluble impurity content and vitamin E content according to GB/T5009.37-2003, GB/T5525-2008, GB/T15688-2008 and GB 5009.82-2016, respectively, and the results are shown in Table 5:
table 5 color and luster properties of camellia oil prepared by each method
Figure SMS_9
From this, it can be seen that the camellia oil prepared by the method of example 1 has optimal properties and can be applied to the preparation of cosmetics.
Example 8
Crude camellia oil was prepared by the method of example 1, except that the shell content in the pressed material was controlled to be 8%.4200kg of checked camellia seeds are subjected to 960kg of crude oil, and the crude oil rate is 22.86%.
Example 9
Crude camellia oil was prepared by the method of example 1, except that the shell content in the pressed material was controlled to be 18%.4200kg of checked camellia seeds obtain 935kg of crude oil with the crude oil rate of 22.26%.
All documents mentioned in this application are incorporated by reference as if each were individually incorporated by reference. Further, it will be appreciated that various changes and modifications may be made by those skilled in the art after reading the above teachings, and such equivalents are intended to fall within the scope of the claims appended hereto.

Claims (10)

1. The preparation process of the camellia oil for cosmetics comprises a squeezing production process and a refining production process, and is characterized by comprising the following steps:
s1, squeezing production technology: crushing camellia seeds, removing shells to obtain a pressed material; rolling the pressed material, and further steaming and frying to obtain a material blank; mechanically squeezing the embryo, and further filtering to obtain camellia crude oil;
s2, refining production technology: alkali refining, washing, decolorizing, filtering, deodorizing, cooling and freezing the camellia crude oil obtained in the step S1 to obtain camellia oil for cosmetics,
wherein, in the alkali refining process, the Baume degree of the alkali liquor is determined according to the value of the wool oleic acid, and when the value of the wool oleic acid is more than 6, the Baume degree of the alkali liquor is selected to be 16-18; when the value of the linoleic acid is less than or equal to 6, the Baume degree of the alkali liquor is selected to be 14-16.
2. The process for preparing camellia oil for cosmetics according to claim 1, wherein in step S1, the shell content in the pressed material is 10-15%.
3. The process for preparing camellia oil for cosmetics according to claim 1, wherein step S2 specifically comprises:
s21, alkali refining: heating the camellia crude oil under stirring at 20-30 rpm, and stopping heating when the oil temperature reaches 30 ℃; adjusting the stirring speed to 50-70 rpm, adding alkali liquor, and continuously stirring for 10-30 minutes; then the stirring speed is adjusted to 20-30 r/min, when the soapstock is separated from the oil, the stirring is stopped, the precipitation is carried out for 6-10 hours, and the soapstock is discharged;
s22, washing: heating the oil temperature to 80-85 ℃, and washing the oil with hot water with the temperature 5 ℃ higher than the oil temperature;
s23, decoloring: heating the oil temperature to 105 ℃, vacuumizing to-0.098 Mpa, adding a decoloring agent, keeping the oil temperature to 105 ℃, and reacting for 15-20 minutes;
s24, filtering: filtering the decolorized tea oil by using a plate-frame filter;
s25, deodorizing and cooling: heating tea oil under vacuum degree of-0.098 Mpa, when the oil temperature reaches 100 ℃, opening a steam valve of a deodorization pot to enable steam water mist in the deodorization pot to be in a spray umbrella shape, when the oil temperature reaches 110 ℃, opening the steam valve to enable the steam mist to evaporate, sucking odor in the oil along with vacuum, when the oil temperature reaches 235-245 ℃, keeping for 2-3 hours, and then cooling by utilizing water;
s26, freezing: and (3) cooling the oil to 4-5 ℃ for crystallization and crystal growth for more than 48 hours, and filtering to obtain camellia oil finished product oil.
4. A process for preparing camellia oil for cosmetics according to claim 3, wherein in step S21, the alkali solution amount comprises a theoretical alkali amount and an super alkali amount, and the theoretical alkali amount is obtained by using the following table:
Figure FDA0004153104950000021
wherein, the acid value refers to the acid value which needs to be reduced, and the number before the decimal point and the number after the decimal point are respectively checked on the table to obtain theoretical alkali amount and then added; the amount of super base is determined using the following table:
Figure FDA0004153104950000022
5. a process for preparing camellia oil for cosmetics as claimed in claim 4, wherein the amount of the super alkali is determined to be 0.25% by weight of the oil.
6. The process for preparing camellia oil for cosmetics according to claim 4, wherein the heating of the camellia oil is carried out after the alkali solution is added and the stirring speed is adjusted to 20-30 rpm, the heating speed is 1 ℃/min, and the oil temperature is raised to 35-45 ℃.
7. The process for preparing camellia oil for cosmetics according to claim 6, wherein the hot brine with the same oil temperature is added in the process of heating when the soapstock is separated from the oil, and the amount of the hot brine is not less than the amount of the alkali solution.
8. A process for preparing camellia oil for cosmetics according to claim 3, wherein in step S22, the washing process is repeated 4 times, and salt is added to the hot water at the 1 st to 3 rd washing, wherein the amount of salt is 3 to 5% of the amount of crude oil.
9. The process for preparing camellia oil for cosmetics according to claim 3, wherein in the step S23, the decoloring agent is clay and activated carbon, the clay is added in an amount of 7-15% by weight of the camellia oil, and the activated carbon is added in an amount of 0.2-1.0% by weight of the camellia oil.
10. A process for preparing camellia oil for cosmetics as claimed in claim 3, wherein in step 25, the deodorized oil is heat exchanged with the oil to be deodorized in the next batch.
CN202310325529.XA 2023-03-29 2023-03-29 Preparation process of camellia oil for cosmetics Pending CN116376631A (en)

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