CN110642826A - Method for extracting vitamin E from tea oil deodorized distillate by using molecular distillation technology - Google Patents
Method for extracting vitamin E from tea oil deodorized distillate by using molecular distillation technology Download PDFInfo
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Abstract
The invention discloses a method for extracting vitamin E from deodorized distillate of tea oil by using a molecular distillation technology, which comprises the following steps of (1) esterification pretreatment; (2) primary molecular distillation; (3) secondary molecular distillation; (4) and (3) three-stage molecular distillation. The invention optimizes the molecular distillation experimental conditions by an orthogonal experimental method. Experiments show that when the evaporation temperature is 200 ℃, the feeding rate is 4mL/min, and the rotating speed of a film scraper is 150rpm, the purity of the product vitamin E reaches the highest value, namely 0.93%. The high performance liquid chromatography is used for analyzing the components of the raw materials, and a method for analyzing the content of tocopherol from the raw materials to the product is established. The high performance liquid chromatography is used for analyzing the content of the tocopherol, the raw materials do not need to be pretreated, the operation is simple and easy, and the accuracy is high.
Description
Technical Field
The invention belongs to the technical field of vitamin E extraction from tea oil deodorized distillate, and particularly relates to a method for extracting vitamin E from tea oil deodorized distillate by a molecular distillation technology.
Background
The oil tea seed oil can reach consumers only by refining procedures of degumming, deacidification, decoloration, deodorization and the likeAnd (5) eating requirements. The oil and fat is deodorized to produce deodorized distillate with free fatty acid, glyceride, natural vitamin E, sterol ester and oxidation product as main components, and the most developed natural vitamin E is. Natural vitamin E is a mixture of four tocopherols and four tocotrienols, and is classified into alpha-, beta-, gamma-, delta-tocopherols and alpha-, beta-, gamma-, delta-tocotrienols according to the difference of the number of positions methylated on the benzene ring. Vitamin E has various physiological function activities, and can be widely applied to industries such as cosmetics, medicines, foods and the like. The camellia seed oil contains abundant vitamin E, however, after crude oil is refined, the loss of nutrient substances such as the vitamin E is found to be large, the quality of the camellia oil is directly reduced, and most of the loss of the camellia oil is remained in soapstock and deodorized distillate. The byproducts in the tea oil processing process are comprehensively utilized, active substances in the tea oil are extracted, waste materials are changed into valuable materials, and the tea oil processing method has important research and economic values. At present, the domestic method for preparing natural high-content vitamin E by using grease as a raw material mainly comprises a supercritical extraction method (SFE), a molecular distillation Method (MD) and the like. Supercritical CO2The extraction (SCDE) has the advantages of strong extraction capability, no toxicity, safety, wide sources, easy removal from products and the like, and is a green extraction technology which is developed rapidly in recent years. But the deodorized distillate has high content of nonvolatile components and coloring matter substances, these nonvolatile components are mainly unsaturated fatty acids and are liable to undergo autooxidation, and further the coloring matter also affects the storage of the essential oil, so that the quality of the supercritical extract deteriorates rapidly and the storage period is short. Molecular distillation techniques rely on the difference in the mean free path of movement of the molecules of a mixture to separate them at temperatures well below their boiling points. Therefore, the molecular distillation technology is particularly suitable for separating high boiling point, heat sensitivity and easy oxide systems. The method is intended to adopt a multistage molecular distillation technology to extract natural vitamin E in the deodorized distillate of the tea oil so as to provide a theoretical basis for industrial production, carry out waste utilization and make a contribution to environmental protection.
Disclosure of Invention
The invention aims to provide a method for extracting high-purity vitamin E from tea oil deodorizer distillate. The method takes the deodorized distillate of the tea oil as a raw material, adopts cation exchange resin to catalyze esterification reaction, and then carries out tertiary molecular distillation on the esterification product to gradually remove fatty acid and a small amount of other impurities.
The invention solves the technical problems through the following technical scheme,
a method for extracting vitamin E from deodorized distillate of tea oil by molecular distillation comprises,
(1) esterification pretreatment: according to the weight ratio of alcohol oil of 1: 1.4-1.8 adding a tea oil deodorized distillate raw material into ethanol, then adding a catalyst accounting for 10-30% of the weight of the mixed solution and a molecular sieve accounting for 15-25% of the weight of the mixed solution, stirring and reacting at 50-70 ℃ for 4.5-6.5 hours, and washing a reaction product to obtain a mixture taking vitamin E and fatty acid ethyl ester as main components;
(2) primary molecular distillation: performing primary molecular distillation on 500g of molecular distillation raw material obtained by pretreatment in the step (1), wherein the preheating temperature is 40-70 ℃; under the conditions that the system pressure is 0.1Pa, the heating wall surface temperature is 80-100 ℃, and the scraper rotating speed is 80-110 rpm, the heavy phase of a primary molecular distillation product is obtained by entering the molecular distillation device at a feeding rate of 5-7 mL/min, and light phase components with low boiling points such as aldehyde, ketone, carbohydrate and the like are mainly removed;
(3) secondary molecular distillation: carrying out secondary molecular distillation on a heavy phase obtained from the primary molecular distillation product, wherein the preheating temperature is 75-95 ℃; under the conditions that the system pressure is 0.1Pa, the heating wall surface temperature is 120-150 ℃, and the scraper plate rotating speed is 90-110 rpm, the mixture enters a molecular distillation device at a feeding rate of 3-5 mL/min to obtain a secondary molecular distillation product; collecting heavy phase components in the process, and removing light phase components with low boiling points such as rich fatty acid ethyl ester;
(4) three-stage molecular distillation: subjecting the heavy phase obtained from the second molecular distillation product to a third molecular distillation to separate vitamin E and triglyceride; under the condition that the system pressure is 0.1Pa, the heating wall surface temperature is 160-240 ℃, and the film scraping rotating speed is 100-200 rpm, the mixture enters a molecular distillation device at a feeding rate of 2-4 mL/min, vitamin E in a light phase is collected, and the content of the vitamin E in a product is used as a detection index.
As a preferred technical solution, in the step (1), the catalyst is preferably a south-opening 001 x 7 type cation exchange resin; the molecular sieve is used as a water absorbent, and the molecular sieve is a spherical 5A type molecular sieve.
As a preferable technical scheme, in the step (1), the weight ratio of ethanol to the tea oil deodorized distillate is preferably 1: 1.5, the mass fraction of the catalyst is 20%, the reaction temperature is 50 ℃, the reaction time is 6 hours, and the esterification rate of the deodorized distillate of the tea oil reaches 96.2%.
As a preferable technical scheme, after the step (1), the mixture obtained in the step (1) is subjected to ultrasonic treatment and then low-temperature freezing recrystallization, and the molecular distillation raw material is further purified by filtering to remove crystals.
As an optimal technical scheme, in the step (2), the optimal technological parameters are that the preheating temperature is 55-65 ℃, the system pressure is 0.1Pa, the heating wall surface temperature is 80-95 ℃, the scraper rotating speed is 95-110 rpm, and the feeding rate is 5.5-7 mL/min.
As a preferred technical scheme, in the step (2), the process parameters are preferably that the preheating temperature is 85 ℃, the system pressure is 0.1Pa, the heating wall surface temperature is 90 ℃, the scraper rotating speed is 100rpm, and the feeding rate is 6 mL/min. .
As a preferred technical scheme, in the step (3), the process parameters are preferably that the preheating temperature is 90 ℃, the system pressure is 0.1Pa, the heating wall surface temperature is 135 ℃, the scraper rotating speed is 100rpm, and the feeding rate is 4 mL/min.
As a preferable technical scheme, before the steps (2), (3) and (4) and before the molecular distillation is started, the tightness of each exhaust valve is checked, and the cold trap is ensured to be filled with liquid nitrogen so as to better ensure the vacuum degree and protect an oil diffusion pump.
As a preferred technical scheme, in the step (4), the technological parameters are preferably that the temperature of the heating wall surface is 200 ℃, the film scraping rotating speed is 150rpm, the feeding speed is 4mL/min, the heavy phase is triglyceride, and the light phase is vitamin E.
The molecular distillation experimental conditions were optimized by orthogonal experimental method. Experiments show that when the evaporation temperature is 200 ℃, the feeding rate is 4mL/min, and the rotating speed of a film scraper is 150rpm, the purity of the product vitamin E reaches the highest value, namely 0.93%. The high performance liquid chromatography is used for analyzing the components of the raw materials, and a method for analyzing the content of tocopherol from the raw materials to the product is established. The high performance liquid chromatography is used for analyzing the content of the tocopherol, the raw materials do not need to be pretreated, the operation is simple and easy, and the accuracy is high.
Drawings
FIG. 1 is a vitamin E standard HPLC chromatogram of an embodiment of the present invention.
Detailed Description
The invention is explained in further detail below with reference to the figures and examples.
The embodiment of the invention selects the following instruments:
molecular distillation apparatus of KDL5 type, UIC, Germany;
HY-8(A) type oscillator;
model TDL-40B desk high capacity centrifuge;
german sykam liquid chromatograph;
shanghai Yangrong Biochemical Instrument plant RE52CS-1 rotary evaporator;
DHG-9076A electric heating constant temperature air drying oven of Shanghai essence macro experimental facility Limited;
KQ-2200 ultrasonic cleaner of ultrasonic apparatus Limited of Kunshan city;
sadoris scientific instruments, Beijing, Inc. ALB-224 analytical balance, etc.
The embodiment of the invention selects the following reagents:
dry hydrogen strong acid cation exchange resin;
the ether, the ethanol, the potassium hydroxide and the anhydrous sodium sulfate are analytically pure;
chromatographic grade methanol;
a molecular sieve;
alpha-tocopherol, beta-tocopherol standards;
the distillate for deodorizing tea oil is provided by Wanshan tea-oil tea Co., Ltd.
Example 1 esterification pretreatment
An esterification pretreatment method for extracting vitamin E from deodorized distillate of tea oil by molecular distillation technology comprises the steps of,
(1) esterification pretreatment: the fatty acid is converted into fatty acid ethyl ester, so that the boiling point difference and the solubility of the vitamin E and the free fatty acid can be enlarged, a better raw material is provided for the next separation, the purity of the product is improved, the quality of the product is improved, and the storage period is prolonged. When the tea oil deodorized distillate is subjected to esterification pretreatment, the alcohol oil weight ratio is 1: adding a tea oil deodorized distillate raw material into ethanol according to a material-to-liquid ratio of 1.4-1.8, then adding a catalyst accounting for 10-30% of the weight of the mixed solution and a molecular sieve accounting for 15-25% of the weight of the mixed solution, stirring and reacting for 4.5-6.5 hours at 50-70 ℃, and washing a reaction product, thereby obtaining a mixture with vitamin E and fatty acid ethyl ester as main components; the catalyst is selected from Nankai 001 x 7 type cation exchange resin; the molecular sieve is a spherical 5A type molecular sieve;
(2) and (2) carrying out ultrasonic treatment on the mixture obtained in the step (1), then carrying out low-temperature freezing recrystallization, and filtering to remove crystals, thereby further purifying the molecular distillation raw material.
The reaction conversion, defined as the ratio of the number of moles of hydroxyl groups converted to the number of moles of total hydroxyl groups in the deodorized distillate, can be calculated from the change in the acid value of the reactants. 3-4 g of the reaction mixture was taken out, dissolved in 50ml (v: v ═ 1: 1) of a mixture of anhydrous ethanol and anhydrous ether, and subjected to acid-base titration with 0.1mol/L of a potassium hydroxide standard solution, and the acid value and the esterification rate were calculated.
According to the steps, the weight ratio of ethanol to the tea oil deodorized distillate is 1: 1.5, the mass fraction of the catalyst is 20%, the mass fraction of the molecular sieve is 20%, the reaction temperature is 50 ℃, the reaction time is 6 hours, and the esterification rate of the deodorized distillate of the tea oil reaches 96.2%.
In the step, the raw materials are pretreated by esterification of ethyl, and the method has the following main advantages: 1. the molecular size is small, the steric hindrance is small, the activity is high, and the esterification reaction is easier to carry out; 2. the source is wide, the price is relatively low, and the cost is low; 3. does not form an azeotrope with water, is easy to recover and reduces the production cost; 4. the reaction condition is mild, and industrialization is easy to realize; 5. methanol and other substances harmful to human bodies are not introduced, and the product can be used in the field of food and medicine.
In addition, cation exchange resin is used as a catalyst in the esterification reaction, and the method has the following advantages: 1. after the reaction is finished, the post-treatment is easy; 2. the paint has no acid and alkali and basically has no corrosion to equipment; 3. can be recycled.
Example 2 analysis of esterification reaction results
The method of example 1 is used for carrying out esterification pretreatment on the deodorized distillate of the camellia oleosa seed oil, so that the acid value of the deodorized distillate of the camellia oleosa seed oil is reduced to be below 3mgKOH/g, most fatty acids are converted into fatty acid ethyl esters, and a better raw material is provided for the next molecular distillation.
Aiming at the oil-tea camellia seed oil deodorized distillate system, the adopted strong-acid cation exchange resin has higher activity from the esterification result, and is an ideal esterification catalyst.
Suitable operating conditions for the esterification reaction are: adopting a molecular sieve as a water absorbent, wherein the mass ratio of ethanol to deodorized distillate is 1: 1.4-1.8 percent, 10-30 percent of acidic resin catalyst, 15-25 percent of molecular sieve, 50-70 ℃ of reaction temperature, 4.5-6.5 hours of reaction time and 96.2 percent of esterification rate.
Because of adopting milder reaction conditions, the recovery rate of the tocopherol is higher in the esterification process. The calculation process is shown in table 1.
TABLE 1 equilibrium of vitamin E during esterification
m1-total amount of tocopherols in the esterification product; m is2-total amount of tocopherols in the starting material;
and then, washing and filtering the acidic resin catalyst and the molecular sieve by using a hot ethanol solution, so that adsorbed ethyl ester can be removed, the resin can be effectively recovered, and the acidic resin catalyst and the molecular sieve can be reused for 3-4 times.
In order to further remove the sterol, the sterol can be recrystallized after ultrasonic treatment, and the obtained sterol crystals are removed by suction filtration, so that the burden of molecular distillation operation is further reduced.
Example 3 molecular distillation treatment
A method for extracting vitamin E from deodorized distillate of tea oil by molecular distillation comprises,
(1) primary molecular distillation: preheating 500g of the raw material obtained by the treatment in the embodiment 1 at the preheating temperature of 40-70 ℃; under the system pressure of 0.1Pa, the heavy phase of a primary molecular distillation product is obtained by observing that the heavy phase enters a molecular distillation device at different heating wall surface temperatures of 80-100 ℃, different scraper rotating speeds of 80-110 rpm and different feeding rates of 5-7 mL/min, and the heavy phase is mainly removed from light phase components with lower boiling points, such as aldehyde, ketone, carbohydrate and the like;
the influence of the temperature of a heating wall surface of molecular distillation, the rotating speed of a scraper and the feeding speed on the separation of fatty acid ethyl ester in a mixture taking vitamin E and fatty acid ethyl ester as main components is inspected in the primary molecular distillation process, and the content of the vitamin E in a product is used as a detection index;
in the first-stage molecular distillation, the second-stage molecular distillation and the third-stage molecular distillation, before starting the molecular distillation, the tightness of each exhaust valve is required to be noticed, and the cold trap is ensured to be filled with liquid nitrogen so as to better ensure the vacuum degree and protect an oil diffusion pump;
(2) secondary molecular distillation: carrying out secondary molecular distillation on a heavy phase obtained from the primary molecular distillation product, wherein the preheating temperature is 75-95 ℃; under the condition that the system pressure is 0.1Pa, the mixture enters a molecular distillation device at different heating wall surface temperatures of 120-150 ℃, different scraper rotating speeds of 90-110 rpm and different feeding rates of 3-5 mL/min to obtain a secondary molecular distillation product; collecting heavy phase components in the process, and removing light phase components with low boiling points such as rich fatty acid ethyl ester;
the influence of the preheating temperature, the heating wall surface temperature, the scraper rotating speed and the feeding speed of the molecular distillation on the separation of fatty acid ethyl ester in a mixture taking vitamin E and fatty acid ethyl ester as main components is inspected in the secondary molecular distillation process;
(3) three-stage molecular distillation: carrying out third molecular distillation on the heavy phase obtained by the secondary molecular distillation to separate vitamin E and triglyceride, and observing that the heavy phase enters a molecular distillation device at different heating wall surface temperatures of 160-240 ℃, different wiped film rotating speeds of 100-200 rpm and different feeding rates of 2-4 mL/min to obtain a third-stage molecular distillation product; collecting vitamin E in the light phase by taking the content of the vitamin E in the product as a detection index;
in this process, the influence of the temperature of the heating wall of the molecular distillation, the rotational speed of the scraper and the feed rate on the separation of glycerides from a mixture based on vitamin E and triglycerides was examined.
Example 4
The high performance liquid chromatography method for measuring the content of the vitamin E comprises the following steps,
(1) preparation of standard solution of alpha-tocopherol: accurately weighing 100mg of alpha-tocopherol standard substance, putting the alpha-tocopherol standard substance into a 100ml volumetric flask, and diluting the alpha-tocopherol standard substance to a scale value by using an ethanol solution to prepare a standard solution with the concentration of 1 mg/ml;
taking out a certain amount of standard solution of 1mg/ml by using a sampler, and diluting the standard solution by using ethanol to prepare tocopherol standard solutions with the concentrations of 10 mu g/ml, 20 mu g/ml, 30 mu g/ml, 40 mu g/ml and 50 mu g/ml respectively;
(2) preparation of a solution to be tested: taking the sample obtained at the end of the separation and extraction process in the embodiment 2 as an example, weighing about 1.0g of the sample obtained at the end of the separation and extraction process in the embodiment 2, putting the sample into a 25ml volumetric flask, diluting the sample to a scale with ethanol, preparing a solution to be detected, and putting the solution into a refrigerator;
(3) HPLC analysis: chromatographic conditions ODSC18Chromatography column (4.6 mm. times.250 mm, 5 μm); mobile phase: methanol-water solution (98: 2); the detection wavelength is 300 nm; the flow rate is 1 mL/min; the column temperature was 30 ℃.
And (4) taking the concentration of the standard sample as an abscissa and taking a response peak value corresponding to the corresponding concentration as an ordinate to make a graph to obtain a standard curve of the peak value relative to the concentration.
Performing liquid phase analysis on the liquid to be detected under the same condition, and substituting the response peak into a standard curve Sα＝aCαAnd b, obtaining the concentration of the sample to be detected, wherein the calculation formula is as follows:
xliquid to be tested＝xα+xβ+γ+xd；
Si-a response peak;
Cα-alpha-tocopherol solution concentration (mg/mL ethanol);
xi-mass percent concentration of tocopherol homologues;
v-volume of prepared assay sample solution (mL);
m-sample weight (g);
a. b-constant.
Example 5 Experimental study of Primary and Secondary molecular distillation
The product of the esterification pretreatment of example 1 was subjected to concentration of tocopherol by three molecular distillations, wherein the first two molecular distillations were mainly to distill off aldehydes, ketones, carbohydrates, fatty acid methyl esters, fatty acid ethyl esters and the like having lower boiling points than tocopherol, while monoglycerides having boiling points close to that of tocopherol were not easily separated.
According to literature reports, the closer the preheating temperature is to the temperature of the heating wall surface, the better the mass transfer and heat transfer effects are, and the better the separation effect is. In the experimental implementation process, the preheating temperature of the primary molecular distillation and the secondary molecular distillation is 75-95 ℃, and preferably not more than 80 ℃.
The content of alpha-VE in the heavy phase product obtained by two times of molecular distillation is increased from 0.0072 percent of the raw material to 0.0366 percent.
Example 6 three-stage molecular distillation experiment condition optimization
And on the basis of the secondary molecular distillation, increasing the temperature of the heating wall surface, and carrying out tertiary molecular distillation on the heavy phase obtained by the secondary molecular distillation to separate the vitamin E and the triglyceride. By using L9(34) And an orthogonal table, wherein an orthogonal test is established by taking the evaporation temperature, the feeding rate and the film scraping rotating speed as 3 factors, and the vitamin E content of the obtained light component is measured. The factor levels are shown in Table 2.
TABLE 2 orthogonal factor horizon
TABLE 3 results of orthogonal experiments in molecular distillation experiments
The results of the three-stage molecular distillation orthogonal test are shown in Table 3. As can be seen from Table 3, RA＞Rc＞RBThe main and secondary sequences of the influence of the A, B, C factors on the extraction rate are A > C > B; the optimum extraction conditions are A2B2C2I.e., an evaporation temperature of 200 ℃, a feed rate of 4mL/min, and a wiped film rotation speed of 150 rpm.
The content of vitamin E in the molecular distillation product reaches 0.93 percent by a verification test under the condition.
EXAMPLE 7 vitamin E assay
It can be found from experiments that natural vitamin E obtained from the deodorized distillate of tea oil is mainly α -tocopherol having the highest activity, and thus the content of vitamin E is measured using α -tocopherol as a standard sample.
(1) Investigation of linear relationships
Under the HPLC condition of example 4, 20 μ L of 5 kinds of solubility control solutions were injected, and the chromatographic peak area was recorded;
the peak area of the control is set as the ordinate (Y), the mass concentration of the control is set as the abscissa (X), and a standard curve equation is established, so that the regression equation Y is 149003 · X-30209, and r is 0.9995, and the linear relation is good.
(2) Sample content determination and repeatability experiments
The same sample is accurately weighed to total 5 parts, after extraction is carried out under the optimal extraction condition, 5 parts of test solution is prepared according to the method described in the embodiment 4, the measured average value of the vitamin content is 0.927%, and the RSD is 1.1%, which shows that the method has good repeatability.
(3) Stability test
The peak areas of chlorogenic acid are respectively determined for 0, 2, 4, 8 and 24 hours after the preparation of the same test solution. The result RSD was 1.2%, indicating that the sample had good stability over 24 h.
Tests show that the content of alpha-VE in the raw materials can be improved by nearly 13 times by carrying out three-stage molecular distillation on the pretreated deodorized distillate of the tea oil, so that the natural vitamin E mainly containing natural alpha-VE is obtained.
The dry hydrogen strong acid cation exchange resin adopted by the invention has higher activity and is an ideal esterification catalyst.
Suitable operating conditions for the esterification reaction of the present invention are: a molecular sieve is adopted as a water absorbent, and the mass ratio of ethanol to deodorized distillate of tea oil is 1: 1.5, the mass fraction of the catalyst is 20%, the reaction temperature is 50 ℃, the reaction time is 6 hours, and the esterification rate reaches 96.2%.
Due to the adoption of mild reaction conditions, the recovery rate of the tocopherol in the esterification process is high, impurities can be effectively distinguished from target products, and the method is economical in cost. And then, carrying out three times of molecular distillation on the esterified product to gradually remove fatty acid and a small amount of other impurities. Wherein, the third-stage distillation adopts an orthogonal test method to optimize the experimental conditions, and when the evaporation temperature is 200 ℃, the feeding rate is 4mL/min, and the film scraping rotating speed is 150rpm, the purity of the vitamin E reaches the highest and is 0.93 percent.
In addition, the high performance liquid chromatography is adopted to analyze the components of the raw materials, and an analysis method from the raw materials to the tocopherol content of the product is established. The tocopherol content is analyzed by high performance liquid chromatography, the raw materials do not need to be pretreated, the operation is simple and easy, and the accuracy is high. Although the total content of vitamin E in the raw materials of the tea oil deodorized distillate is not high, the alpha-VE content with the highest physiological activity is very high, and the tea oil deodorized distillate has very high comprehensive application value.
Claims (9)
1. A method for extracting vitamin E from deodorized distillate of tea oil by molecular distillation comprises,
(1) esterification pretreatment: according to the weight ratio of alcohol oil of 1: 1.4-1.8 adding a tea oil deodorized distillate raw material into ethanol, then adding a catalyst accounting for 10-30% of the weight of the mixed solution and a molecular sieve accounting for 15-25% of the weight of the mixed solution, stirring and reacting at 50-70 ℃ for 4.5-6.5 hours, and washing a reaction product to obtain a mixture taking vitamin E and fatty acid ethyl ester as main components;
(2) primary molecular distillation: performing primary molecular distillation on 500g of molecular distillation raw material obtained by pretreatment in the step (1), wherein the preheating temperature is 40-70 ℃; under the conditions that the system pressure is 0.1Pa, the heating wall surface temperature is 80-100 ℃, and the scraper rotating speed is 80-110 rpm, the heavy phase of a primary molecular distillation product is obtained by entering the molecular distillation device at a feeding rate of 5-7 mL/min, and light phase components with low boiling points such as aldehyde, ketone, carbohydrate and the like are mainly removed;
(3) secondary molecular distillation: carrying out secondary molecular distillation on a heavy phase obtained from the primary molecular distillation product, wherein the preheating temperature is 75-95 ℃; under the conditions that the system pressure is 0.1Pa, the heating wall surface temperature is 120-150 ℃, and the scraper plate rotating speed is 90-110 rpm, the mixture enters a molecular distillation device at a feeding rate of 3-5 mL/min to obtain a secondary molecular distillation product; collecting heavy phase components in the process, and removing light phase components with low boiling points such as rich fatty acid ethyl ester;
(4) three-stage molecular distillation: subjecting the heavy phase obtained from the second molecular distillation product to a third molecular distillation to separate vitamin E and triglyceride; under the condition that the system pressure is 0.1Pa, the heating wall surface temperature is 160-240 ℃, and the film scraping rotating speed is 100-200 rpm, the mixture enters a molecular distillation device at a feeding rate of 2-4 mL/min, vitamin E in a light phase is collected, and the content of the vitamin E in a product is used as a detection index.
2. The method for extracting vitamin E from the tea oil deodorizer distillate using molecular distillation as claimed in claim 1, wherein in step (1), the catalyst is preferably cation exchange resin of south opening 001 x 7 type; the molecular sieve is used as a water absorbent, and the molecular sieve is a spherical 5A type molecular sieve.
3. The method for extracting vitamin E from the deodorized distillate of tea oil using molecular distillation as claimed in claim 1, wherein the weight ratio of ethanol to deodorized distillate of tea oil in step (1) is 1: 1.5, the mass fraction of the catalyst is 20%, the reaction temperature is 50 ℃, the reaction time is 6 hours, and the esterification rate of the deodorized distillate of the tea oil reaches 96.2%.
4. The method for extracting vitamin E from a tea oil deodorizer distillate using a molecular distillation technique as claimed in claim 1, wherein after the step (1), the mixture obtained in the step (1) is subjected to ultrasonic treatment and then to low-temperature freezing recrystallization, and the molecular distillation raw material is further purified by filtering to remove crystals.
5. The method for extracting vitamin E from tea oil deodorizer distillate by using molecular distillation technology as claimed in claim 1, wherein in step (2), the process parameters are preheating temperature 55-65 ℃, system pressure 0.1Pa, heating wall temperature 80-95 ℃, scraper rotation speed 95-110 rpm, and feeding rate 5.5-7 mL/min.
6. The method for extracting vitamin E from tea oil deodorizer distillate by molecular distillation as claimed in claim 1, wherein in step (2), the process parameters are preheating temperature 85 deg.C, system pressure 0.1Pa, heating wall temperature 90 deg.C, scraper rotation speed 100rpm, and feed rate 6 mL/min.
7. The method for extracting vitamin E from tea oil deodorizer distillate by molecular distillation as claimed in claim 1, wherein in step (3), the process parameters are preheating temperature of 90 deg.C, system pressure of 0.1Pa, heating wall temperature of 135 deg.C, scraper rotation speed of 100rpm, and feed rate of 4 mL/min.
8. The method for extracting vitamin E from the deodorized distillate of tea oil by molecular distillation as claimed in claim 1, wherein in step (4), the process parameters are that the temperature of the heating wall surface is 200 ℃, the rotating speed of the wiped film is 150rpm, the feeding rate is 4mL/min, the heavy phase is triglyceride, and the light phase is vitamin E.
9. The method for extracting vitamin E from deodorized distillate of tea oil by molecular distillation as claimed in claim 1, wherein in steps (2), (3) and (4), before starting molecular distillation, the tightness of each vent valve is checked, and the cold trap is filled with liquid nitrogen to better ensure vacuum degree and protect oil diffusion pump.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209964A (en) * | 2020-10-20 | 2021-01-12 | 浙江万盛股份有限公司 | Preparation method of TCPP (trichloropropylphosphate) flame retardant |
| CN112941126A (en) * | 2021-04-01 | 2021-06-11 | 福建省格兰尼生物工程股份有限公司 | Method for extracting soybean vitamin E from non-soybean deodorized distillate |
| CN115475400A (en) * | 2022-09-30 | 2022-12-16 | 湘南学院 | Method for removing polycyclic aromatic hydrocarbon in tea oil by molecular distillation |
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2019
- 2019-09-05 CN CN201910836437.1A patent/CN110642826A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 李娟: "脱臭馏出物中提取天然维生素E的工艺研究", 《天津大学硕士学位论文》 * |
| 陈焱等: "油茶籽油脱臭馏出物维生素E的分子蒸馏工艺研究", 《江西农业大学学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209964A (en) * | 2020-10-20 | 2021-01-12 | 浙江万盛股份有限公司 | Preparation method of TCPP (trichloropropylphosphate) flame retardant |
| CN112209964B (en) * | 2020-10-20 | 2023-04-07 | 浙江万盛股份有限公司 | Preparation method of TCPP (trichloropropylphosphate) flame retardant |
| CN112941126A (en) * | 2021-04-01 | 2021-06-11 | 福建省格兰尼生物工程股份有限公司 | Method for extracting soybean vitamin E from non-soybean deodorized distillate |
| CN115475400A (en) * | 2022-09-30 | 2022-12-16 | 湘南学院 | Method for removing polycyclic aromatic hydrocarbon in tea oil by molecular distillation |
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