CN102643715B - Method for extracting edible oil by preprocessing ethanol solution in microwave expansion mode - Google Patents

Abstract

The invention relates to a method for extracting edible oil with microwave puffing pretreatment ethanol solution. First, a certain amount of camellia seed kernel oil material or oil tea seed kernel oil material roasted at high temperature is taken, crushed, and then the camellia seed kernel oil material slurry is processed by microwave puffing , take a certain amount of microwave puffed camellia oleifera oil residue for extraction, so that the oil floats up from the oil residue of camellia oleifera seed to form an oil layer, the middle layer is a low-concentration ethanol solution layer, the lower layer is the oil slag layer of camellia oleifera kernel, and finally the upper layer is separated The oil layer gets grease. It can reduce the amount of ethanol, improve the microwave puffing effect of oil, realize the full separation of oil and non-grease substances in oil residue, which is beneficial to improve the oil yield of subsequent processing, and can remove pigment substances in oil residue such as camellia oleifera kernels, It is beneficial to obtain nearly colorless oil and realize rapid separation of oil and non-oil substances. The invention has the characteristics of simple process, low investment and easy industrial production.

Description

Method for extracting edible oil with microwave puffing pretreatment ethanol solution

technical field

The invention belongs to the technical field of deep processing of human food oil, and relates to a method for extracting edible oil with microwave puffing pretreatment ethanol solution.

Background technique

Camellia oleifera seed, also known as camellia seed, is one of the four major woody oil plants in the world. It is mainly distributed in China and is a unique oil resource in our country. Camellia oleifera contains two main useful components, one is tea oil and the other is tea saponin.

Tea seed oil, together with olive oil, is known as the world's two largest woody edible oils, and has been known as the "treasure in oil" since ancient times. It has been confirmed by the China Center for Disease Control that the quality of camellia oil is better than that of western olive oil. Compared with olive oil, high-grade refined tea oil has higher nutrition and health care quality. Olive oil contains 75% to 90% unsaturated fatty acids, while tea oil contains 85% to 97% unsaturated fatty acids, which is the crown of all edible oils.

Present tea oil production enterprises generally adopt pressing, then leaching to extract the tea oil process, and the quality of the tea oil obtained by adopting this process is relatively poor. In order to obtain high-quality camellia oil, patents CN200610031893.1 and CN200810059993.4 used acid protease, cellulase, amylase, etc. to extract tea seed oil with water enzymatic method; patent 200610031452.1 used physical low-temperature cold pressing technology to produce tea seed oil . At present, the oil yield of tea seed oil produced by aqueous enzymatic method, cold pressing method and water substitution method is low, which restricts its application in industry.

Microwave puffing utilizes the heating characteristics of microwaves. When microwave heating is performed, the moisture removal and heat migration directions, heat transfer directions, and vapor pressure migration directions of the materials are all consistent, that is, from the inside of the material to the surface. Because such characteristics are conducive to the generation and accumulation of steam inside the material, the microwave heating speed is fast, the gas temperature inside the material rises sharply, the temperature of the material rises rapidly, the formation rate of the internal steam is higher than the migration rate of the steam, and the material has a vapor pressure gradient. The pressure exceeds the strength of the fibrous tissue structure, the cells rupture, and the oleosomes in the cells rupture (especially in the presence of ethanol, ammonium bicarbonate, sodium bicarbonate and other swelling agents, such as 10% (V/V) ethanol and 2% (W/V) ammonium bicarbonate), so microwave puffing pretreatment of oils such as camellia seed kernels is conducive to improving the oil yield of edible oils such as tea seed oil in the subsequent production.

Contents of the invention

In order to overcome the above-mentioned shortcomings of the prior art, the present invention provides a method for extracting edible oil with microwave pretreated ethanol solution, which has simple process, low investment and is easy to industrialized production .

The technical method adopted by the present invention to solve the technical problems is: a method for extracting edible oil with microwave puffed pretreatment ethanol solution, and its process steps are:

Step 1: Take a certain amount of Camellia oleifera seed oil or Camellia oleifera seed oil that has been roasted at high temperature, crush it, add 0-90% concentration (V/V) ethanol, 0-5% concentration (W/V) Soaking in ammonium bicarbonate or sodium bicarbonate expansion agent to obtain oily residue of camellia oleifera seed, or after ultrasonic treatment, separating the soaking solution to obtain oily residue of camellia oleifera seed;

The second step of microwave expansion treatment of camellia oleifera seed oil slurry: placing the camellia oleifera seed oil slurry obtained above in a certain power vacuum or normal pressure microwave expansion equipment, and processing for a certain period of time to obtain microwave expanded camellia oleifera seed oil residue;

The third step is to take a certain amount of microwave puffed camellia oleifera seed oil residue, add a high-concentration ethanol solution with a concentration of 70-95% (V/V), homogenize it, and heat it in a water bath at 20-90°C for 0.5-3 hours to make the oil The grease and non-grease substances in the residue are fully separated, and the alcohol-soluble substances in the oily residue of camellia oleifera seeds enter the high-concentration ethanol solution with a concentration of 70-95% (V/V). After static stratification, the upper layer is separated. Concentrated ethanol solution, then add high-concentration ethanol solution with a concentration of 70-95% (V/V) to repeat the above operation, repeat the operation 2-3 times, and finally separate the oil residue of the lower layer of camellia seed kernel, in which the oil droplets are distributed on the camellia seed Kernel oil residue, or before adding high-concentration ethanol solution, first add a certain amount of protease, cellulase, pectinase and/or amylase enzyme solution to infiltrate the oil residue for enzymolysis treatment , and then add the above-mentioned high-concentration ethanol solution.

The fourth step is to add water or saturated brine or a low-concentration ethanol solution with a concentration of 10-50% (V/V) to the oil residue of camellia oleifera seed kernels containing high-concentration ethanol solution in the lower layer, so that the ethanol solution in the oil residue of camellia oleifera kernels The final concentration is controlled below 55%, heated in a water bath at 20-90°C for 0.5-3 hours or ultrasonically assisted in a water bath for 0.5-3 hours, so that the oil floats up from the oil residue of camellia oleifera seeds to form an oil layer, with a low-concentration ethanol solution in the middle layer, and the lower layer is the camellia seed kernel oil residue layer;

The fifth step is to separate the upper oil layer, degumming with phospholipase enzymatically, and then filter, or directly filter, and then vacuum dehydration and drying to obtain oil products.

The pulverized particle size of the camellia seed kernel oil residue is 60 mesh to 400 mesh.

The puffing agent adopts ethanol, ammonium bicarbonate, sodium bicarbonate and their compound, the concentration range of ethanol is 0-90% (V/V), and the concentration range of ammonium bicarbonate and sodium bicarbonate is 0-5% ( W/V).

The bulking agent is used in combination with 10%-50% (V/V) low-concentration ethanol solution and 0.5-5% (W/V) ammonium bicarbonate and sodium bicarbonate.

The microwave puffing power is 300-60000W, and the microwave puffing time is 1min-15min.

The concentration of high-concentration ethanol is 70-95% (V/V); the concentration of low-concentration ethanol is 55% (V/V); below; the range of solid-liquid ratio for extraction is 1:3-1:20, and the stirring speed is 1 ～200 rev/min, stirring time 30～180 minutes, temperature controlled in the range of 30～90℃.

The oil plants include camellia oleifera seed, olive, peanut, rapeseed, sunflower seed, sorbifolium, sesame and/or walnut.

The beneficial effects of the present invention are: when ethanol and ammonium bicarbonate or ethanol and sodium bicarbonate are compounded and used, the amount of ethanol can be reduced, the microwave puffing effect of oil can be improved, and the oil yield of subsequent processing can be improved; Using a high-concentration ethanol solution and homogenizing oil residues such as camellia seed kernels can achieve sufficient separation of oil and non-greasy substances in oil residues, which is conducive to improving the oil yield in subsequent processing, and can remove oil residues such as camellia seed kernels The pigment substances in it are beneficial to obtain nearly colorless oil, and high-purity tea saponin and other substances can also be separated from high-concentration ethanol solution; the use of low-concentration ethanol solution is conducive to the floating of oil from oil residue without emulsification layer to realize rapid separation of oil and non-oil substances; extracting oil with ethanol solution after microwave pretreatment of oil belongs to a green and safe production process; the invention has the characteristics of simple process, low investment and easy industrial production.

Description of drawings

Fig. 1 is a block diagram of the process flow of the present invention.

Detailed ways

The present invention will be further described below in conjunction with the accompanying drawings and embodiments.

Referring to Fig. 1, a kind of method for microwave puffing pretreatment ethanol solution leaching edible oil, its process step is:

Step 1: Take a certain amount of Camellia oleifera seed oil or Camellia oleifera seed oil that has been roasted at high temperature, crush it, add 0-90% concentration (V/V) ethanol, 0-5% concentration (W/V) Soaking in ammonium bicarbonate or sodium bicarbonate expansion agent to obtain oily residue of camellia oleifera seed kernel or after ultrasonic treatment, and then separating the soaking solution to obtain oily residue of camellia oleifera seed kernel;

The second step of microwave expansion treatment of camellia oleifera seed oil slurry: placing the camellia oleifera seed oil slurry obtained above in a certain power vacuum or normal pressure microwave expansion equipment, and processing for a certain period of time to obtain microwave expanded camellia oleifera seed oil residue;

The third step is to take a certain amount of microwave puffed camellia oleifera seed oil residue, add a high-concentration ethanol solution with a concentration of 70-95% (V/V), homogenize it, and heat it in a water bath at 20-90°C for 0.5-3 hours to make the oil The grease and non-grease substances in the residue are fully separated, and the alcohol-soluble substances in the oily residue of camellia oleifera seeds enter the high-concentration ethanol solution with a concentration of 70-95% (V/V). After static stratification, the upper layer is separated. Concentrated ethanol solution, then add high-concentration ethanol solution with a concentration of 70-95% (V/V) to repeat the above operation, repeat the operation 2-3 times, and finally separate the oil residue of the lower layer of camellia seed kernel, in which the oil droplets are distributed on the camellia seed Kernel oil residue; before adding high-concentration ethanol solution, add a certain amount of protease, cellulase, pectinase and/or amylase enzyme solution to infiltrate the oil residue for enzymolysis treatment, and then add the above-mentioned high-concentration ethanol solution;

The fourth step is to add water or saturated brine or a low-concentration ethanol solution with a concentration of 10-50% (V/V) to the oil residue of camellia oleifera seed kernels containing high-concentration ethanol solution in the lower layer, so that the ethanol solution in the oil residue of camellia oleifera kernels The final concentration is controlled below 55%, heated in a water bath at 20-90°C for 0.5-3 hours or ultrasonically assisted in a water bath for 0.5-3 hours, so that the oil floats up from the oil residue of camellia oleifera seeds to form an oil layer, with a low-concentration ethanol solution in the middle layer, and the lower layer is the camellia seed kernel oil residue layer;

The fifth step is to separate the upper oil layer, degumming with phospholipase enzymatically, and then filter, or directly filter, and then vacuum dehydration and drying to obtain oil, and the low-concentration ethanol solution can be reused.

The pulverized particle size of the camellia seed kernel oil residue is 60 mesh to 400 mesh.

The puffing agent adopts ethanol, ammonium bicarbonate, sodium bicarbonate and their compound, the concentration range of ethanol is 0-90% (V/V), and the concentration range of ammonium bicarbonate and sodium bicarbonate is 0-5% ( W/V).

The bulking agent is used in combination with 10%-50% (V/V) low-concentration ethanol solution and 0.5-5% (W/V) ammonium bicarbonate and sodium bicarbonate.

The microwave puffing power is 300-60000W, and the microwave puffing time is 1min-15min.

The concentration of high-concentration ethanol is 70-95% (V/V); the concentration of low-concentration ethanol is 55% (V/V); below; the range of solid-liquid ratio for extraction is 1:3-1:20, and the stirring speed is 1 ～200 rev/min, stirring time 30～180 minutes, temperature controlled in the range of 30～90℃.

The oil plants include camellia oleifera seed, olive, peanut, rapeseed, sunflower seed, sorbifolium, sesame and/or walnut.

Example 1: Weigh 10 grams of microwave puffed pretreated Camellia oleifera seed dregs, add 100ml of 90% ethanol solution, homogenate, heat and stir in a water bath at 60°C for 1 hour, pour off the upper 90% ethanol solution, and add again to the lower layer of Camellia oleifera seed dregs 50ml of 90% ethanol solution, heated and stirred in a water bath at 60°C for 1 hour, poured off the 90% ethanol solution in the upper layer, and added 40% ethanol solution to the lower layer of Camellia oleifera seed dregs, so that the final concentration of ethanol in the lower layer of Camellia oleifera seed dregs was about 50%. Heating and stirring in a water bath for 1 hour, standing still, taking the clear oil of the upper layer, can obtain 4.9 grams of Camellia oleifera seed oil.

Example 2: Weigh 10.2 grams of microwave puffed pretreated Camellia oleifera seed dregs, add 100ml of 90% ethanol solution, homogenate, heat and stir in a water bath at 60°C for 1 hour, pour off the upper 90% ethanol solution, and add again to the lower layer of Camellia oleifera seed dregs 50ml of 90% ethanol solution, heated and stirred in a water bath at 60°C for 1 hour, poured off the upper layer of 90% ethanol solution, and added saturated saline to the lower layer of Camellia oleifera seed dregs, so that the final concentration of ethanol in the lower layer of Camellia oleifera seed dregs was about 50%, and placed in a 60°C water bath Heating and stirring for 1 hour, standing still, taking the clear oil in the upper layer, can obtain 5 grams of Camellia oleifera seed oil.

Example 3: Weigh 10.1 grams of microwave puffed pretreated Camellia oleifera seed dregs, add 100ml of 80% ethanol solution, homogenate, heat and stir in a water bath at 50°C for 1 hour, pour off the upper 80% ethanol solution, and add again to the lower layer of Camellia oleifera seed dregs 30ml of 80% ethanol solution, heated and stirred in a water bath at 50°C for 1 hour, poured off the upper 80% ethanol solution, and added 30% ethanol solution to the lower layer of Camellia oleifera seed dregs, so that the final concentration of ethanol in the lower layer of Camellia oleifera seed dregs was about 40%. Heating and stirring in a water bath for 1 hour, standing still, taking the clear oil from the upper layer to obtain 4.7 grams of Camellia oleifera seed oil.

Example 4: Weigh 10.1 grams of microwave puffed pretreated camellia seed dregs, add 15ml of protease enzyme solution with a concentration of 2% (V/V), incubate at 50°C for 1 hour, then add 100ml of 95% ethanol solution, homogenate, 50 Heat and stir in a water bath at ℃ for 1 hour, pour off the 95% ethanol solution in the upper layer, add 30ml of 95% ethanol solution to the camellia oleifera seed residue in the lower layer, heat and stir in a water bath at 50°C for 1 hour, pour off the 95% ethanol solution in the upper layer, Add 40% ethanol solution to make the final concentration of ethanol in the lower layer of Camellia oleifera seed dregs about 50%, heat and stir in a 50°C water bath for 1 hour, let it stand still, take the upper layer of clear oil, and 5.2 grams of Camellia oleifera seed oil can be obtained.

The oil plants in the above embodiments also include camellia oleifera seed, olive oil, peanut, rapeseed, sunflower seed, sorbifolium sorbifolium, sesame and/or walnut.

The present invention can reduce the amount of ethanol used in combination with ethanol and ammonium bicarbonate or ethanol and sodium bicarbonate, improve the microwave puffing effect of oil, and is beneficial to improve the oil yield of subsequent processing; use high-concentration ethanol first Homogenization of solution and oil residues such as camellia oleifera kernels can realize the full separation of oil and non-grease substances in oil residues, which is beneficial to improve the oil yield of subsequent processing, and can remove pigment substances in oil residues such as camellia oleifera kernels, It is beneficial to obtain near-colorless oil, and can also obtain high-purity tea saponin and other substances from high-concentration ethanol solution; the use of low-concentration ethanol solution is conducive to the floating of oil from oil residues without forming an emulsified layer, and realizes the separation of oil and fat. Rapid separation of non-greasy substances; extraction of oil with ethanol solution after microwave pretreatment of oil is a green and safe production process; the invention has the characteristics of simple process, low investment and easy industrial production.

Claims (2)

1. a method for microwave puffing pretreatment ethanol solution leaching edible oil, is characterized in that processing step is: Step 1: Take a certain amount of Camellia oleifera seed oil, crush it , add ethanol with a concentration greater than 0 and not greater than 90% (V/V) and/or alkali with a concentration greater than 0 and not greater than 5% (W/V) Soaking the solution as an expanding agent to obtain the oily residue of camellia oleifera seeds, or after ultrasonic treatment, separating the soaking solution to obtain oily residues of camellia oleifera seeds; wherein the alkali solution is ammonium bicarbonate solution or sodium bicarbonate solution; The second step of microwave puffing treatment of camellia seed kernel oil residue: put the above-mentioned camellia seed kernel oil residue in vacuum or normal pressure microwave puffing equipment with a microwave puffing power of 300-60000W , and the microwave puffing time is 1min-15min to obtain microwave Expanded Camellia oleifera seed oil residue; The third step is to take a certain amount of microwave puffed camellia oleifera seed oil residue, add a high-concentration ethanol solution with a concentration of 70-95% (V/V), homogenize it, and heat it in a water bath at 20-90°C for 0.5-3 hours to make the oil The grease and non-grease substances in the residue are fully separated, and the alcohol-soluble substances in the oily residue of camellia oleifera seeds enter the high-concentration ethanol solution with a concentration of 70-95% (V/V). After static stratification, the upper layer is separated. Concentrated ethanol solution, then add high-concentration ethanol solution with a concentration of 70-95% (V/V) to repeat the above operation, repeat the operation 2-3 times, and finally separate the oil residue of the lower layer of camellia seed kernel, in which the oil droplets are distributed on the camellia seed Kernel oil residue, or before adding high-concentration ethanol solution, first add a certain amount of protease, cellulase, pectinase and/or amylase enzyme solution to infiltrate the oil residue for enzymolysis treatment , and then add the above-mentioned high-concentration ethanol solution; The fourth step is to add water or saturated saline or a low-concentration ethanol solution with a concentration of 10-50% (V/V) to the oil residue of camellia seed kernels containing high-concentration ethanol solution in the lower layer to make the ethanol solution in the oil residue of camellia kernels The final concentration is controlled below 55%, heated in a water bath at 20-90°C for 0.5-3 hours or ultrasonically assisted in a water bath for 0.5-3 hours, so that the oil floats up from the oil residue of camellia oleifera seeds to form an oil layer, with a low-concentration ethanol solution in the middle layer, and the lower layer is the camellia seed kernel oil residue layer; The fifth step is to separate the upper oil layer, degumming with phospholipase enzymatically, and then filter, or directly filter, and then vacuum dehydration and drying to obtain oil products. 2. The method according to claim 1, characterized in that: the bulking agent is one of ethanol or ammonium bicarbonate solution or sodium bicarbonate solution. 3. The method according to claim 1 or 2, characterized in that: the concentration of the low-concentration ethanol solution is 10% to 50% (V/V), and the concentration of ammonium bicarbonate solution and sodium bicarbonate solution is 0.5 to 5% % (W/V). 4. The method for extracting edible oil with microwave puffing pretreatment ethanol solution as claimed in claim 1, characterized in that: olives, peanuts, rapeseeds, sunflower seeds, sorbifoliums, sesame and/or walnuts are used instead of claim Camellia oleifera seed oil in 1. 5. The method as claimed in claim 1, characterized in that: the camellia seed kernel oil material is the camellia seed kernel oil material roasted at high temperature.

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