WO2016127827A1 - Method for extracting maize germ oil assisted by steam explosion and ethanol - Google Patents

Method for extracting maize germ oil assisted by steam explosion and ethanol Download PDF

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Publication number
WO2016127827A1
WO2016127827A1 PCT/CN2016/072733 CN2016072733W WO2016127827A1 WO 2016127827 A1 WO2016127827 A1 WO 2016127827A1 CN 2016072733 W CN2016072733 W CN 2016072733W WO 2016127827 A1 WO2016127827 A1 WO 2016127827A1
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WIPO (PCT)
Prior art keywords
corn germ
oil
steam explosion
pulverized
soaked
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PCT/CN2016/072733
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French (fr)
Chinese (zh)
Inventor
杨瑞金
倪双双
张益奇
李鹏飞
张文斌
赵伟
华霄
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江南大学
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Publication of WO2016127827A1 publication Critical patent/WO2016127827A1/en

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting

Definitions

  • the invention relates to a method for steam explosion and ethanol assisted extraction of corn germ oil, and belongs to the technical field of fine processing of agricultural and sideline products.
  • Corn germ is a by-product of the alcohol industry and the corn starch industry. China's annual output is around 1.4 million tons.
  • the corn germ contains 35 to 57% fat, 17 to 28% crude protein, 7 to 16% ash, 1.5 to 5.5% starch, and 7.0% cellulose.
  • At present, about 300,000 tons of corn germ is used in China for oil production every year, and the production of corn germ oil is nearly 120,000 tons.
  • the content of unsaturated fatty acids in corn germ oil accounts for more than 80%, of which oleic acid is above 60%, and the VE content ranks first in vegetable oil. Long-term consumption is beneficial to the human body and is known as “nutritious healthy oil”.
  • corn germ oil production methods include a press method, a solvent extraction method, and a pre-press-solvent extraction method.
  • the pressing method squeezes the corn oil from the corn germ by means of mechanical external force, and has the advantages of simple process, less supporting equipment and good oil quality; the disadvantage is that the mechanical power consumption is large, and the residual oil of the cake after pressing is high.
  • the protein in the cake is highly denatured and cannot be used as a good plant protein resource.
  • Solvent extraction method using liquid-liquid extraction principle using an organic solvent (such as hexane) capable of dissolving corn germ oil, extracting the oil in the corn germ, the advantage is that the amount of residual oil in the cake is low, and it is easy to achieve large Automated production of scale.
  • the disadvantages are that most of the solvents used for leaching are flammable and explosive, and have certain toxicity, and the production safety is poor; the leached hair oil contains more non-oil substances, darker color and poor quality.
  • the pre-press-solvent extraction method is a combination method, which solves the disadvantages of the pressing method and the solvent extraction method to a certain extent, but fundamentally, this is a method of treating the symptoms and not treating the pressing, failing to truly solve the pressing. The resulting waste of protein resources and environmental pollution caused by organic solvent extraction.
  • the invention adopts the steam explosion technology to replace the heat treatment process for a long time, and uses the aqueous ethanol solution as the oil extraction medium and the demulsifier instead of the traditional water enzymatic method. .
  • the object of the present invention is to provide a method for steam explosion and ethanol assisted extraction of corn germ oil, which solves the traditional oil extraction method or low extraction rate of free oil or serious environmental pollution, high residual oil content in slag phase, waste of high quality protein resources, enzyme Problems such as large dosage and high cost.
  • the dried corn germ 1 is soaked in a low concentration citric acid solution according to a certain ratio of material to liquid, filtered and drained to discard the filtrate, and the soaked corn germ 2 is collected.
  • Corn germ 2 soaked with a low concentration of citric acid solution is subjected to steam explosion treatment.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried in a blast drying oven, and is pulverized by a pulverizer to a volume average particle diameter (MV) of 30 to 80 ⁇ m to obtain an oil extracting material I.
  • MV volume average particle diameter
  • the raw material I obtained in the step C is stirred uniformly at a certain temperature by using an aqueous solution of ethanol, and the oil is extracted after the alkali is adjusted. After the reaction is finished, the mixture is centrifuged to obtain an incompatible three-phase free oil, an aqueous phase and a slag phase. Free corn germ oil, weighed.
  • the corn germ is a by-product of the wet production of starch and is currently marketed.
  • the concentration of citric acid in step A is 0.01 to 0.1 M, and the ratio of material to liquid is 1:1 to 1:5 (w/v, Kg/L), and immersed for 0.5 to 3 hours.
  • the corn germ is immersed in step A and then filtered using a polyester gauze having a mesh size of 100 to 250.
  • the moisture content of the wet corn germ obtained after soaking in step A is 60% to 70%.
  • the steam explosion pressure in step B is 0.5 to 1.8 MPa ⁇ 0.1 MPa, and the time is set to 15 to 120 s.
  • the steam explosion chamber is 5L, and the corn germ is about 1.5Kg after each soaking, and the treatment is 15-120s.
  • the drying temperature in the step C is 50 to 70 ° C, so that the moisture content of the material after drying is 2% to 4% (wet basis).
  • the powder is pre-pulverized to an average particle diameter of 100 to 200 ⁇ m; and then finely pulverized by a roller compactor to make the average particle diameter of the material 30 to 80 ⁇ m.
  • the reaction temperature in the step D is 50 to 80 ° C, and the ratio of material to liquid is 1:4 to 1:8 (w/v), The concentration of the aqueous alcohol solution is 15 to 35% (v/v), the alkali is adjusted to pH 8.0 to 10.0, and the reaction time is 0.5 to 3 hours.
  • the invention has the beneficial effects that the steam blasting technology of the invention uses the fiber mechanism and the oil-protein composite structure of the corn germ to change and separate at the moment of pressure release, so that the internal structure is loose, and the dissolution of the oil in the cell is promoted, so that the free oil is extracted.
  • the oil rate has increased significantly.
  • the invention adopts the ethanol solution as the extraction medium, eliminates the use of the enzyme, greatly shortens the oil-making cycle, and the enzyme is expensive, and the use of the low-concentration ethanol aqueous solution largely saves the cost; the ethanol recovery condition is simple and does not pollute the environment. It can be recycled after recycling.
  • the method of the invention has the advantages of high oil extraction rate, low cost and good quality, and solves the problems of low extraction rate, high cost and long cycle of corn germ oil when extracted by traditional water enzymatic method.
  • the steam explosion equipment is a common steam explosion machine in the new food processing equipment.
  • the steam explosion machine sold by the Zhengdao Heavy Machinery Factory of Hebi City, China is sold under the trade name QBS200B steam explosion process test bench.
  • the blast drying equipment is an electric heating constant temperature blast drying box sold by Shanghai Senxin Experimental Instrument Co., Ltd. of China under the trade name DGG-9070A.
  • the pulverizing equipment is a pulverizer commonly used in the field of food processing technology, which can meet the requirements of different pulverization fineness. For example, Zhejiang Wenling Linda Machinery Co., Ltd.
  • Free oil yield free oil / oil content in the raw material ⁇ 100%
  • the dried corn germ is not subjected to any pretreatment, and only is subjected to crushing treatment, and is pulverized by a Chinese medicine pulverizer to a volume average particle diameter of about 184 ⁇ m, and then pulverized by a roller compactor to a volume average particle diameter of about 35 ⁇ m to obtain an oil-removing raw material.
  • the oil extraction raw material was heated at 60 ° C, the ratio of solid to liquid was 1:7 (w/v), the concentration of the aqueous ethanol solution was 30% (v/v), and the pH of the system was adjusted to 9.0.
  • the reaction time was 2 h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
  • the free oil extraction rate is only 77.83%, and the fat content of the slag phase accounts for 13.57% of the total oil.
  • the dried corn germ is not soaked in a low concentration citric acid solution, and the dry material is directly subjected to steam explosion treatment to set its steam explosion.
  • the pressure is 1.3 MPa ⁇ 0.1 MPa and the dwell time is 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ after steam explosion is dried in a blast drying oven at 50 ° C; it is pulverized to a volume average particle diameter of about 170 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 41 ⁇ m to obtain oil extraction. raw material.
  • the obtained raw materials were oiled at 60 ° C at a ratio of material to liquid of 1:7 (w/v), aqueous ethanol solution of 30% (v/v), and adjusted to pH 9.0, and the reaction time was 2 h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
  • the free oil extraction rate increased to 86.71%, and the slag phase fat content accounted for 5.22% of the total oil.
  • the dried corn germ 1 was soaked in a 0.1 M citric acid solution for 3 hours according to the ratio of material to liquid (w/v), drained and discarded, and the soaked corn germ 2 was collected.
  • the corn germs immersed in citric acid were subjected to steam explosion treatment, and the steam explosion pressure was set to 0.5 MPa ⁇ 0.1 MPa, and the dwell time was 120 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 140 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 38 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 140 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 38 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to oil extraction at a temperature ratio of 1:4 (w/v) at a ratio of a liquid to liquid of 35% (v/v) at a temperature of 60 ° C, and the pH of the system is adjusted to 10.0. 3h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
  • the free oil extraction rate was 87.36%, and the fat content of the slag phase was 6.41% of the total oil.
  • the dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2 hours according to the ratio of material to liquid 1: 2, and then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ⁇ 0.1 MPa, and the dwell time was 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 70 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 145 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 35 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 145 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 35 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to a liquid-to-liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v), and the pH of the system is adjusted to 9.0 at 60 ° C for the reaction time. 1.5h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
  • the free oil extraction rate was 90.32%, and the fat content of the slag phase was only 4.51% of the total oil.
  • the dried corn germ 1 was soaked in a 0.1 M citric acid solution for 0.5 h according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ⁇ 0.1 MPa, and the dwell time was 15 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 65 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 162 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 40 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 162 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 40 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to oil concentration at a ratio of a liquid to liquid ratio of 1:8 (w/v), an aqueous ethanol solution of 20% (v/v), and a system pH of 8.0 at 80 ° C for a reaction time. 3h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
  • the free oil extraction rate was 88.93%, and the fat content of the slag phase accounted for only 5.32% of the total oil.
  • the dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2 hours according to the ratio of material to liquid 1: 2, and then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ⁇ 0.1 MPa, and the dwell time was 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 171 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 36 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 171 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 36 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to a liquid-to-liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v), and the pH of the system is adjusted to 9.0 at 60 ° C for the reaction time. 2h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
  • the dried corn germ 1 was soaked in a 0.01 M citric acid solution for 2 hours according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 immersed in citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ⁇ 0.1 MPa, and the dwell time was 60 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 152 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 40 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 152 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 40 ⁇ m.
  • the raw material (I) obtained in the step (3) is at a ratio of a feed liquid to a ratio of 1:7 (w/v) at a solution ratio of 30% (v/v), and an aqueous ethanol solution concentration of 30% (v/v).
  • the system was adjusted to pH 9.0 for oil extraction, and the reaction time was 2.5 h. After centrifugation at 5000 rpm for 15 min, the incompatible three phases - free oil, water phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
  • the free oil extraction rate was 87.91%, and the fat content of the slag phase only accounted for 6.38% of the total oil.
  • the dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2 hours according to the ratio of material to liquid 1: 2, and then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ⁇ 0.1 MPa, and the dwell time was 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 170 ⁇ m using a Chinese medicine pulverizer, and is no longer crushed by a rolling mill to obtain an oil extracting material (I).
  • the raw material (I) obtained in the step (3) is subjected to a liquid-to-liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v), and the pH of the system is adjusted to 9.0 at 60 ° C for the reaction time. 2.5h. After centrifugation at 5000 rpm for 15 min, the incompatible three phases - free oil, water phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
  • the free oil extraction rate was 80.18%, and the fat content of the slag phase accounted for only 15.92% of the total oil.
  • the dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2.5 h according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ⁇ 0.1 MPa, and the dwell time was 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 168 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 72 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 168 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 72 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to oil concentration at a ratio of a liquid to liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 35% (v/v), and a system pH of 9.5 at 50 ° C for a reaction time. 0.5h. After centrifugation at 5000 rpm for 15 min, the incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
  • the free oil extraction rate was 88.55%, and the fat content of the slag phase was 7.01% of the total oil.
  • Dry corn germ 1 was soaked in a 0.1 M citric acid solution for 2.5 h according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ⁇ 0.1 MPa, and the dwell time was 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 164 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 33 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 164 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 33 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to oil concentration at a ratio of a liquid to liquid ratio of 1:7 (w/v), an aqueous ethanol solution of 15% (v/v), and a system pH of 9.5 at 60 ° C for a reaction time. 3h. After centrifugation at 5000 rpm for 15 min, the incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
  • the free oil extraction rate was 82.15%
  • the fat content of the slag phase was 7.01% of the total oil
  • the fat content in the emulsion was 9.23% of the total oil.
  • the dried corn germ 1 was soaked in a 0.1 M citric acid solution for 2 hours according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
  • the corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ⁇ 0.1 MPa, and the dwell time was 30 s.
  • the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
  • the corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 170 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 36 ⁇ m.
  • Oil raw material (I) is pulverized to a volume average particle diameter of about 170 ⁇ m using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 36 ⁇ m.
  • the raw material (I) obtained in the step (3) is subjected to oil extraction at a ratio of a liquid to liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v) at 61 ° C, and a pH of 9.0. 2h. After centrifugation at 5000 rpm for 15 min, an incompatible three-phase, free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was obtained.
  • the peroxide value of the hair oil was determined to be only 0.81 mmol/kg, and the vitamin E content was as high as 105.49 mg/100 g.

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  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
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Abstract

According to a method for extracting maize germ oil assisted by steam explosion and ethanol, after using a low-concentration citric acid solution for immersing, steam explosion processing is used, so that the thermal processing time is greatly shortened; and an ethanol-water solution is used as an oil extracting medium and a demulsifier is used to substitute plenty of enzymes used in the traditional aqueous enzymatic method, so that the production costs are reduced and the quality of the product is improved.

Description

一种汽爆及乙醇辅助提取玉米胚芽油的方法Method for steam explosion and ethanol assisted extraction of corn germ oil 技术领域Technical field
本发明涉及一种汽爆及乙醇辅助提取玉米胚芽油的方法，属于农副产品精细加工技术领域。The invention relates to a method for steam explosion and ethanol assisted extraction of corn germ oil, and belongs to the technical field of fine processing of agricultural and sideline products.
背景技术Background technique
玉米胚芽为酒精工业和玉米淀粉工业的副产物，中国的年产量在140万t左右。玉米胚芽含有35～57％的油脂、17～28％的粗蛋白、7～16％的灰分、1.5～5.5％淀粉和7.0％左右的纤维素。目前，中国大约每年大约有30万吨玉米胚芽用于制油，玉米胚芽油的产量近12万t。玉米胚芽油的不饱和脂肪酸含量占80％以上，其中油酸在60％以上，VE含量居植物油首位，长期食用对人体大有裨益，有“营养健康油”之称。Corn germ is a by-product of the alcohol industry and the corn starch industry. China's annual output is around 1.4 million tons. The corn germ contains 35 to 57% fat, 17 to 28% crude protein, 7 to 16% ash, 1.5 to 5.5% starch, and 7.0% cellulose. At present, about 300,000 tons of corn germ is used in China for oil production every year, and the production of corn germ oil is nearly 120,000 tons. The content of unsaturated fatty acids in corn germ oil accounts for more than 80%, of which oleic acid is above 60%, and the VE content ranks first in vegetable oil. Long-term consumption is beneficial to the human body and is known as “nutritious healthy oil”.
目前玉米胚芽油的生产方法有压榨法、溶剂浸提法和预榨-溶剂浸提法。压榨法借助机械外力，将玉米油从玉米胚芽中挤压出来，其优点是：工艺简单，配套设备少，油品质好；其缺点是：机械动力消耗大，压榨后的饼残油量高，饼粕中的蛋白质变性严重，无法作为优质的植物蛋白资源加以利用。溶剂浸提法应用液液萃取原理，选用某种能够溶解玉米胚芽油的有机溶剂(如己烷)，将玉米胚芽中的油脂萃取出来，其优点是：饼粕残油量低，容易实现大规模的自动化生产。其缺点是：浸提所用溶剂绝大多数易燃易爆，且具有一定的毒性，生产的安全性较差；浸出的毛油中所含非油物质较多，色泽较深，质量较差。预榨-溶剂浸提法是一种结合方法，在一定程度上解决了压榨法和溶剂浸提法的缺点，但是从根本上讲，这是一种治标不治本的方法，未能真正解决压榨造成的蛋白资源浪费以及有机溶剂浸提造成的环境污染。At present, corn germ oil production methods include a press method, a solvent extraction method, and a pre-press-solvent extraction method. The pressing method squeezes the corn oil from the corn germ by means of mechanical external force, and has the advantages of simple process, less supporting equipment and good oil quality; the disadvantage is that the mechanical power consumption is large, and the residual oil of the cake after pressing is high. The protein in the cake is highly denatured and cannot be used as a good plant protein resource. Solvent extraction method using liquid-liquid extraction principle, using an organic solvent (such as hexane) capable of dissolving corn germ oil, extracting the oil in the corn germ, the advantage is that the amount of residual oil in the cake is low, and it is easy to achieve large Automated production of scale. The disadvantages are that most of the solvents used for leaching are flammable and explosive, and have certain toxicity, and the production safety is poor; the leached hair oil contains more non-oil substances, darker color and poor quality. The pre-press-solvent extraction method is a combination method, which solves the disadvantages of the pressing method and the solvent extraction method to a certain extent, but fundamentally, this is a method of treating the symptoms and not treating the pressing, failing to truly solve the pressing. The resulting waste of protein resources and environmental pollution caused by organic solvent extraction.
为了综合利用油脂和蛋白资源、解决有机溶剂的使用问题，水酶(剂)法提油应运而生。但水酶法提取工艺均存在生产周期冗长、使用酶量大、成本高昂等不利于进行大规模工业化生产的致命因素，仅能在学术研究上起到一定的示范作用。进入资源、能源越来越匮乏的21世纪，我们所追求的走一条绿色、环保、节能、高效的生产、发展之路，科研的目的亦是如此。In order to comprehensively utilize oil and protein resources and solve the problem of the use of organic solvents, the water enzyme (agent) method came into being. However, the water enzymatic extraction process has the fatal factors that are not conducive to large-scale industrial production, such as long production cycle, large amount of enzymes, and high cost. It can only play a certain role in academic research. In the 21st century, where resources and energy are becoming scarcer, we are pursuing a green, environmentally friendly, energy-saving and efficient production and development path, as well as the purpose of scientific research.
为了解决上述水酶法生产玉米胚芽油的问题，结合玉米胚芽特性，本发明采用蒸汽爆破技术取代较长时间的热处理过程，以及采用乙醇水溶液作为提油介质及破乳剂代替传统水酶法提油。In order to solve the problem of the above-mentioned water enzymatic production of corn germ oil, combined with the characteristics of corn germ, the invention adopts the steam explosion technology to replace the heat treatment process for a long time, and uses the aqueous ethanol solution as the oil extraction medium and the demulsifier instead of the traditional water enzymatic method. .
发明内容 Summary of the invention
本发明的目的是提供一种汽爆及乙醇辅助提取玉米胚芽油的方法，解决传统提油方法或游离油提取率低或环境污染严重、渣相中残油量高、优质蛋白质资源浪费、酶用量大、成本高昂等问题。The object of the present invention is to provide a method for steam explosion and ethanol assisted extraction of corn germ oil, which solves the traditional oil extraction method or low extraction rate of free oil or serious environmental pollution, high residual oil content in slag phase, waste of high quality protein resources, enzyme Problems such as large dosage and high cost.
本发明技术方案主要包括以下步骤：The technical solution of the present invention mainly includes the following steps:
A、预处理干玉米胚芽1A. Pretreatment of dried corn germ 1
将干玉米胚芽1按照一定料液比，采用低浓度柠檬酸溶液进行浸泡后，过滤沥干弃去过滤液，收集浸泡后的玉米胚芽2。The dried corn germ 1 is soaked in a low concentration citric acid solution according to a certain ratio of material to liquid, filtered and drained to discard the filtrate, and the soaked corn germ 2 is collected.
B、蒸汽爆破处理浸泡后玉米胚芽2B. Steam blasting treatment of corn germ after soaking 2
将使用低浓度柠檬酸溶液浸泡过的玉米胚芽2进行蒸汽爆破处理。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。Corn germ 2 soaked with a low concentration of citric acid solution is subjected to steam explosion treatment. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
C、干燥汽爆后玉米胚芽3及粉碎C, corn germ 3 after drying steam explosion and smash
汽爆后的玉米胚芽3采用鼓风干燥箱烘干，使用粉碎机将其粉碎至体积平均粒径(MV)30～80μm，得到提油原料Ⅰ。The corn germ 3 after steam explosion is dried in a blast drying oven, and is pulverized by a pulverizer to a volume average particle diameter (MV) of 30 to 80 μm to obtain an oil extracting material I.
D、乙醇水溶液提取玉米胚芽油D. Extraction of corn germ oil from aqueous ethanol solution
将步骤C得到的原料Ⅰ采用乙醇水溶液在一定温度下搅拌均匀，调碱后进行提油，反应结束后离心，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material I obtained in the step C is stirred uniformly at a certain temperature by using an aqueous solution of ethanol, and the oil is extracted after the alkali is adjusted. After the reaction is finished, the mixture is centrifuged to obtain an incompatible three-phase free oil, an aqueous phase and a slag phase. Free corn germ oil, weighed.
在本发明中，所述的玉米胚芽是湿法生产淀粉的副产物，是目前市场上销售的产品。例如山东诸城兴贸玉米开发有限公司的产品。In the present invention, the corn germ is a by-product of the wet production of starch and is currently marketed. For example, the products of Shandong Zhucheng Xingmao Corn Development Co., Ltd.
在本发明的一种实施方式中，步骤A中柠檬酸浓度为0.01～0.1M，以料液比1:1～1:5(w/v，Kg/L)，浸泡0.5～3h。In one embodiment of the present invention, the concentration of citric acid in step A is 0.01 to 0.1 M, and the ratio of material to liquid is 1:1 to 1:5 (w/v, Kg/L), and immersed for 0.5 to 3 hours.
在本发明的一种实施方式中，步骤A中玉米胚芽浸泡后采用目数100～250的涤纶纱布过滤。In one embodiment of the present invention, the corn germ is immersed in step A and then filtered using a polyester gauze having a mesh size of 100 to 250.
在本发明的一种实施方式中，步骤A浸泡沥干后得到的湿玉米胚芽水分含量在60％～70％。In one embodiment of the present invention, the moisture content of the wet corn germ obtained after soaking in step A is 60% to 70%.
在本发明的一种实施方式中，步骤B中蒸汽爆破压力为0.5～1.8MPa±0.1MPa，时间设置为15～120S。汽爆腔体为5L，每次加浸泡后的玉米胚芽1.5Kg左右，处理15-120s。In one embodiment of the present invention, the steam explosion pressure in step B is 0.5 to 1.8 MPa ± 0.1 MPa, and the time is set to 15 to 120 s. The steam explosion chamber is 5L, and the corn germ is about 1.5Kg after each soaking, and the treatment is 15-120s.
在本发明的一种实施方式中，步骤C中烘干温度为50～70℃，使得烘干后物料的水分含量为2％～4％(湿基)。烘干后先预粉碎到平均粒径为100～200μm；再采用碾压机进行精细粉碎，使物料平均粒径30～80μm。In one embodiment of the present invention, the drying temperature in the step C is 50 to 70 ° C, so that the moisture content of the material after drying is 2% to 4% (wet basis). After drying, the powder is pre-pulverized to an average particle diameter of 100 to 200 μm; and then finely pulverized by a roller compactor to make the average particle diameter of the material 30 to 80 μm.
在本发明的一种实施方式中，步骤D中反应温度50～80℃，料液比1:4～1:8(w/v)，乙 醇水溶液的浓度为15～35％(v/v)，调碱至pH 8.0～10.0，反应时间0.5～3h。In one embodiment of the present invention, the reaction temperature in the step D is 50 to 80 ° C, and the ratio of material to liquid is 1:4 to 1:8 (w/v), The concentration of the aqueous alcohol solution is 15 to 35% (v/v), the alkali is adjusted to pH 8.0 to 10.0, and the reaction time is 0.5 to 3 hours.
本发明的有益效果：本发明使用蒸汽爆破技术，使得玉米胚芽的纤维机构、油脂-蛋白复合结构在释压瞬间实现变化和分离，使得内部结构疏松，促进细胞内油脂的溶出，使得游离油提油率明显提高。利用蒸汽爆破技术取代传统水酶法提取玉米胚芽油时长时间的热处理，使得油品的品质更加优良，有效活性成分得以保留，并且减少了生产能耗，节约了成本。本发明采用乙醇溶液作为提取介质，杜绝了酶的使用，大大地缩短了制油周期；且酶价格昂贵，使用低浓度的乙醇水溶液很大程度上节约了成本；乙醇回收条件简单，不污染环境，回收后可循环使用。总而言之，本发明使用方法具有提油率高、成本低、品质好等优点，解决了玉米胚芽油采用传统水酶法提取时提油率低、成本昂贵、周期冗长等问题。The invention has the beneficial effects that the steam blasting technology of the invention uses the fiber mechanism and the oil-protein composite structure of the corn germ to change and separate at the moment of pressure release, so that the internal structure is loose, and the dissolution of the oil in the cell is promoted, so that the free oil is extracted. The oil rate has increased significantly. The use of steam explosion technology to replace the traditional water enzymatic extraction of corn germ oil for a long time heat treatment, so that the quality of the oil is better, the effective active ingredients are retained, and reduce production energy consumption, saving costs. The invention adopts the ethanol solution as the extraction medium, eliminates the use of the enzyme, greatly shortens the oil-making cycle, and the enzyme is expensive, and the use of the low-concentration ethanol aqueous solution largely saves the cost; the ethanol recovery condition is simple and does not pollute the environment. It can be recycled after recycling. In summary, the method of the invention has the advantages of high oil extraction rate, low cost and good quality, and solves the problems of low extraction rate, high cost and long cycle of corn germ oil when extracted by traditional water enzymatic method.
具体实施方式detailed description
蒸汽爆破设备是食品加工新型机械设备中常见的汽爆机，例如由中国鹤壁市正道重机厂以商品名QBS200B汽爆工艺试验台销售的汽爆机。鼓风干燥设备为中国上海森信实验仪器有限公司以商品名DGG-9070A型销售的电热恒温鼓风干燥箱。粉碎设备是在食品加工技术领域里通常使用的粉碎机，可满足不同粉碎细度的要求，例如由浙江温岭市林大机械有限公司以商品名为DFY-500型500克摇摆式高速中药粉碎机和由常州市武进兴业机械设备有限公司以商品名三辊研磨机销售的粉碎机。提油使用的恒温设备、搅拌装置均为目前市场上销售的产品，例如由上海一恒科学仪器有限公司销售的超级恒温循环水浴槽和由上海梅颖浦仪器仪表制造有限公司以商品名84-1磁力搅拌器销售的搅拌装置。离心机是目前市场上销售的产品，例如由上海安亭科学仪器厂以商品名LXJ-IIB大容量低速离心机销售的产品。The steam explosion equipment is a common steam explosion machine in the new food processing equipment. For example, the steam explosion machine sold by the Zhengdao Heavy Machinery Factory of Hebi City, China, is sold under the trade name QBS200B steam explosion process test bench. The blast drying equipment is an electric heating constant temperature blast drying box sold by Shanghai Senxin Experimental Instrument Co., Ltd. of China under the trade name DGG-9070A. The pulverizing equipment is a pulverizer commonly used in the field of food processing technology, which can meet the requirements of different pulverization fineness. For example, Zhejiang Wenling Linda Machinery Co., Ltd. trades the name DFY-500 500g swinging high-speed Chinese medicine pulverizer And the crusher sold by Changzhou Wujin Xingye Machinery Equipment Co., Ltd. under the trade name of three-roll mill. The constant temperature equipment and stirring device used for oil extraction are all products currently on the market, such as the super constant temperature circulating water bath sold by Shanghai Yiheng Scientific Instrument Co., Ltd. and the trade name 84- by Shanghai Meiyingpu Instrument and Meter Manufacturing Co., Ltd. 1 Agitator sold by magnetic stirrer. Centrifuges are currently on the market, such as those sold by Shanghai Anting Scientific Instrument Factory under the trade name LXJ-IIB high-capacity low-speed centrifuge.
粗脂肪测定方法：索氏抽提法Method for determination of crude fat: Soxhlet extraction
游离油得率＝游离油/原料中的含油量×100％Free oil yield = free oil / oil content in the raw material × 100%
实施例1Example 1
将干玉米胚芽不做任何预处理，仅做破碎处理，使用中药粉碎机将其粉碎至体积平均粒径184μm左右，再采用碾压机粉碎至体积平均粒径35μm左右，得到提油原料。The dried corn germ is not subjected to any pretreatment, and only is subjected to crushing treatment, and is pulverized by a Chinese medicine pulverizer to a volume average particle diameter of about 184 μm, and then pulverized by a roller compactor to a volume average particle diameter of about 35 μm to obtain an oil-removing raw material.
将提油原料在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)，调体系pH 9.0进行提油，反应时间2h。反应结束后5000rpm离心15min，得到不相容的四相——游离油、乳状液、水相和渣相，瓢取得到游离玉米胚芽油，称重。The oil extraction raw material was heated at 60 ° C, the ratio of solid to liquid was 1:7 (w/v), the concentration of the aqueous ethanol solution was 30% (v/v), and the pH of the system was adjusted to 9.0. The reaction time was 2 h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
游离油提取率仅为77.83％，其渣相的脂肪含量占总油的13.57％。The free oil extraction rate is only 77.83%, and the fat content of the slag phase accounts for 13.57% of the total oil.
实施例2Example 2
干玉米胚芽不采用低浓度柠檬酸溶液浸泡，干物料直接进行蒸汽爆破处理，设置其汽爆 压力为1.3MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽。The dried corn germ is not soaked in a low concentration citric acid solution, and the dry material is directly subjected to steam explosion treatment to set its steam explosion. The pressure is 1.3 MPa ± 0.1 MPa and the dwell time is 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽采用鼓风干燥箱在50℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径170μm左右，再采用碾压机粉碎至体积平均粒径41μm左右，得到提油原料。The corn germ after steam explosion is dried in a blast drying oven at 50 ° C; it is pulverized to a volume average particle diameter of about 170 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 41 μm to obtain oil extraction. raw material.
将得到的原料在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)，调体系pH 9.0进行提油，反应时间2h。反应结束后5000rpm离心15min，得到不相容的四相——游离油、乳状液、水相和渣相，瓢取得到游离玉米胚芽油，称重。The obtained raw materials were oiled at 60 ° C at a ratio of material to liquid of 1:7 (w/v), aqueous ethanol solution of 30% (v/v), and adjusted to pH 9.0, and the reaction time was 2 h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
游离油提取率增大为86.71％，其渣相的脂肪含量占总油的5.22％。The free oil extraction rate increased to 86.71%, and the slag phase fat content accounted for 5.22% of the total oil.
实施例3Example 3
将干玉米胚芽1按照料液比1:1(w/v)，采用0.1M柠檬酸溶液浸泡3h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.1 M citric acid solution for 3 hours according to the ratio of material to liquid (w/v), drained and discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为0.5MPa±0.1MPa，保压时间为120s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germs immersed in citric acid were subjected to steam explosion treatment, and the steam explosion pressure was set to 0.5 MPa ± 0.1 MPa, and the dwell time was 120 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径140μm左右，再采用碾压机粉碎至体积平均粒径38μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 140 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 38 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在60℃下，按料液比1:4(w/v)，乙醇水溶液浓度35％(v/v)，调体系pH 10.0进行提油，反应时间3h。反应结束后5000rpm离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to oil extraction at a temperature ratio of 1:4 (w/v) at a ratio of a liquid to liquid of 35% (v/v) at a temperature of 60 ° C, and the pH of the system is adjusted to 10.0. 3h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
游离油提取率为87.36％，其渣相的脂肪含量占总油的6.41％。The free oil extraction rate was 87.36%, and the fat content of the slag phase was 6.41% of the total oil.
实施例4Example 4
将干玉米胚芽1按照料液比1:2(w/v)，采用0.05M柠檬酸溶液浸泡2h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2 hours according to the ratio of material to liquid 1: 2, and then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.8MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ± 0.1 MPa, and the dwell time was 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在70℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径145μm左右，再采用碾压机粉碎至体积平均粒径35μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 70 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 145 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 35 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)，调体系pH 9.0进行提油，反应时间1.5h。反应结束后5000rpm离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to a liquid-to-liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v), and the pH of the system is adjusted to 9.0 at 60 ° C for the reaction time. 1.5h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
游离油提取率为90.32％，其渣相的脂肪含量仅占总油的4.51％。 The free oil extraction rate was 90.32%, and the fat content of the slag phase was only 4.51% of the total oil.
实施例5Example 5
将干玉米胚芽1按照料液比1:4(w/v)，采用0.1M柠檬酸溶液浸泡0.5h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.1 M citric acid solution for 0.5 h according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.3MPa±0.1MPa，保压时间为15s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ± 0.1 MPa, and the dwell time was 15 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在65℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径162μm左右，再采用碾压机粉碎至体积平均粒径40μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 65 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 162 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 40 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在80℃下，按料液比1:8(w/v)，乙醇水溶液浓度20％(v/v)，调体系pH 8.0进行提油，反应时间3h。反应结束后5000rpm离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to oil concentration at a ratio of a liquid to liquid ratio of 1:8 (w/v), an aqueous ethanol solution of 20% (v/v), and a system pH of 8.0 at 80 ° C for a reaction time. 3h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
游离油提取率为88.93％，其渣相的脂肪含量仅占总油的5.32％。The free oil extraction rate was 88.93%, and the fat content of the slag phase accounted for only 5.32% of the total oil.
实施例6Example 6
将干玉米胚芽1按照料液比1:2(w/v)，采用0.05M柠檬酸溶液浸泡2h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2 hours according to the ratio of material to liquid 1: 2, and then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.3MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ± 0.1 MPa, and the dwell time was 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径171μm左右，再采用碾压机粉碎至体积平均粒径36μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 171 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 36 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)，调体系pH 9.0进行提油，反应时间2h。反应结束后5000rpm离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to a liquid-to-liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v), and the pH of the system is adjusted to 9.0 at 60 ° C for the reaction time. 2h. After centrifugation at 5000 rpm for 15 min at the end of the reaction, incompatible three phases - free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was taken and weighed.
游离油提取率增大为93.22％，其渣相的脂肪含量仅占总油的3.52％。The free oil extraction rate increased to 93.22%, and the fat content of the slag phase accounted for only 3.52% of the total oil.
实施例7Example 7
将干玉米胚芽1按照料液比1:5(w/v)，采用0.01M柠檬酸溶液浸泡2h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.01 M citric acid solution for 2 hours according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.8MPa±0.1MPa，保压时间为60s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 immersed in citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ± 0.1 MPa, and the dwell time was 60 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径152μm左右，再采用碾压机粉碎至体积平均粒径40μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 152 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 40 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)， 调体系pH 9.0进行提油，反应时间2.5h。反应结束后5000转离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is at a ratio of a feed liquid to a ratio of 1:7 (w/v) at a solution ratio of 30% (v/v), and an aqueous ethanol solution concentration of 30% (v/v). The system was adjusted to pH 9.0 for oil extraction, and the reaction time was 2.5 h. After centrifugation at 5000 rpm for 15 min, the incompatible three phases - free oil, water phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
游离油提取率为87.91％，其渣相的脂肪含量仅占总油的6.38％。The free oil extraction rate was 87.91%, and the fat content of the slag phase only accounted for 6.38% of the total oil.
实施例8Example 8
将干玉米胚芽1按照料液比1:2(w/v)，采用0.05M柠檬酸溶液浸泡2h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2 hours according to the ratio of material to liquid 1: 2, and then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.8MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ± 0.1 MPa, and the dwell time was 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径170μm左右，不再采用碾压机粉碎，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 170 μm using a Chinese medicine pulverizer, and is no longer crushed by a rolling mill to obtain an oil extracting material (I).
将步骤(3)得到的原料(Ⅰ)在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)，调体系pH 9.0进行提油，反应时间2.5h。反应结束后5000转离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to a liquid-to-liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v), and the pH of the system is adjusted to 9.0 at 60 ° C for the reaction time. 2.5h. After centrifugation at 5000 rpm for 15 min, the incompatible three phases - free oil, water phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
游离油提取率为80.18％，其渣相的脂肪含量仅占总油的15.92％。The free oil extraction rate was 80.18%, and the fat content of the slag phase accounted for only 15.92% of the total oil.
实施例9Example 9
将干玉米胚芽1按照料液比1:3(w/v)，采用0.05M柠檬酸溶液浸泡2.5h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.05 M citric acid solution for 2.5 h according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.8MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.8 MPa ± 0.1 MPa, and the dwell time was 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径168μm左右，再采用碾压机粉碎至体积平均粒径72μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 168 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 72 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在50℃下，按料液比1:7(w/v)，乙醇水溶液浓度35％(v/v)，调体系pH 9.5进行提油，反应时间0.5h。反应结束后5000转离心15min，得到不相容的四相——游离油、乳状液、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to oil concentration at a ratio of a liquid to liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 35% (v/v), and a system pH of 9.5 at 50 ° C for a reaction time. 0.5h. After centrifugation at 5000 rpm for 15 min, the incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
游离油提取率为88.55％，其渣相的脂肪含量占总油的7.01％。The free oil extraction rate was 88.55%, and the fat content of the slag phase was 7.01% of the total oil.
实施例10Example 10
将干玉米胚芽1按照料液比1:3(w/v)，采用0.1M柠檬酸溶液浸泡2.5h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。Dry corn germ 1 was soaked in a 0.1 M citric acid solution for 2.5 h according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.3MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。 The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ± 0.1 MPa, and the dwell time was 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径164μm左右，再采用碾压机粉碎至体积平均粒径33μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 164 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 33 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在60℃下，按料液比1:7(w/v)，乙醇水溶液浓度15％(v/v)，调体系pH 9.5进行提油，反应时间3h。反应结束后5000转离心15min，得到不相容的四相——游离油、乳状液、水相和渣相，瓢取得到游离玉米胚芽油，称重。The raw material (I) obtained in the step (3) is subjected to oil concentration at a ratio of a liquid to liquid ratio of 1:7 (w/v), an aqueous ethanol solution of 15% (v/v), and a system pH of 9.5 at 60 ° C for a reaction time. 3h. After centrifugation at 5000 rpm for 15 min, the incompatible four phases - free oil, emulsion, aqueous phase and slag phase were obtained, and the free corn germ oil was obtained and weighed.
游离油提取率为82.15％，其渣相的脂肪含量占总油的7.01％，乳状液中的脂肪含量占总油的9.23％。The free oil extraction rate was 82.15%, the fat content of the slag phase was 7.01% of the total oil, and the fat content in the emulsion was 9.23% of the total oil.
实施例11Example 11
将干玉米胚芽1按照料液比1:2(w/v)，采用0.1M柠檬酸溶液浸泡2h后，沥干弃去滤过液，收集浸泡后的玉米胚芽2。The dried corn germ 1 was soaked in a 0.1 M citric acid solution for 2 hours according to the ratio of material to liquid 1: then drained and the filtrate was discarded, and the soaked corn germ 2 was collected.
将使用柠檬酸浸泡过的玉米胚芽2进行蒸汽爆破处理，设置其汽爆压力为1.3MPa±0.1MPa，保压时间为30s。爆破结束，打开蒸汽爆破机收集仓，收集汽爆后的玉米胚芽3。The corn germ 2 soaked with citric acid was subjected to steam explosion treatment, and the steam explosion pressure was set to 1.3 MPa ± 0.1 MPa, and the dwell time was 30 s. At the end of the blasting, the steam blasting machine is opened to collect the bins, and the corn germs after the steam explosion are collected.
汽爆后的玉米胚芽3采用鼓风干燥箱在60℃下烘干；使用中药粉碎机将其粉碎至体积平均粒径170μm左右，再采用碾压机粉碎至体积平均粒径36μm左右，得到提油原料(Ⅰ)。The corn germ 3 after steam explosion is dried at 60 ° C in a blast drying oven; it is pulverized to a volume average particle diameter of about 170 μm using a Chinese medicine pulverizer, and then pulverized by a roller compactor to a volume average particle diameter of about 36 μm. Oil raw material (I).
将步骤(3)得到的原料(Ⅰ)在61℃下，按料液比1:7(w/v)，乙醇水溶液浓度30％(v/v)，调体系pH 9.0进行提油，反应时间2h。反应结束后5000转离心15min，得到不相容的三相——游离油、水相和渣相，瓢取得到游离玉米胚芽油。测定其毛油的过氧化值仅为0.81mmol/kg，维生素E含量高达105.49mg/100g。The raw material (I) obtained in the step (3) is subjected to oil extraction at a ratio of a liquid to liquid ratio of 1:7 (w/v), an aqueous ethanol solution concentration of 30% (v/v) at 61 ° C, and a pH of 9.0. 2h. After centrifugation at 5000 rpm for 15 min, an incompatible three-phase, free oil, aqueous phase and slag phase were obtained, and the free corn germ oil was obtained. The peroxide value of the hair oil was determined to be only 0.81 mmol/kg, and the vitamin E content was as high as 105.49 mg/100 g.
虽然本发明已以较佳实施例公开如上，但其并非用以限定本发明，任何熟悉此技术的人，在不脱离本发明的精神和范围内，都可做各种的改动与修饰，因此本发明的保护范围应该以权利要求书所界定的为准。 Although the present invention has been disclosed in the above preferred embodiments, the present invention is not limited thereto, and various modifications and changes can be made thereto without departing from the spirit and scope of the invention. The scope of the invention should be determined by the scope of the claims.

Claims (10)

  1. 一种汽爆及乙醇辅助提取玉米胚芽油的方法，其特征在于，将玉米胚芽经蒸汽爆破处理后，烘干粉碎，以乙醇溶液提取玉米胚芽油。A method for extracting corn germ oil by steam explosion and ethanol, characterized in that after the corn germ is subjected to steam explosion treatment, it is dried and pulverized, and the corn germ oil is extracted with an ethanol solution.
  2. 根据权利要求1所述的方法，其特征在于，主要包括以下步骤：将玉米胚芽进行蒸汽爆破处理，爆破结束，收集汽爆后的玉米胚芽；汽爆后的玉米胚芽烘干，使用粉碎机将其粉碎至体积平均粒径30～80μm，得到提油原料；将提油原料采用乙醇水溶液在一定温度下搅拌均匀，调碱后进行提油，反应结束后离心，得到不相容的游离油、水相和渣相，瓢取得到游离玉米胚芽油。The method according to claim 1, comprising the steps of: steam blasting the corn germ, ending the blasting, collecting the corn germ after steam explosion; drying the corn germ after steam explosion, using a pulverizer It is pulverized to a volume average particle diameter of 30 to 80 μm to obtain an oil extraction raw material; the oil extraction raw material is uniformly stirred at a certain temperature by using an aqueous ethanol solution, and the oil is extracted after the alkali adjustment, and the reaction is completed and centrifuged to obtain an incompatible free oil. The aqueous phase and the slag phase are obtained from the free corn germ oil.
  3. 根据权利要求2所述的方法，其特征在于，玉米胚芽在进行蒸汽爆破处理之前，先用低浓度柠檬酸溶液进行浸泡，过滤沥干弃去过滤液。The method of claim 2 wherein the corn germ is soaked with a low concentration of citric acid solution prior to steam explosion treatment, filtered and drained to discard the filtrate.
  4. 根据权利要求3所述的方法，其特征在于，柠檬酸溶液浓度为0.01～0.1M，以料液比1:1～1:5浸泡玉米胚芽0.5～3h。The method according to claim 3, wherein the concentration of the citric acid solution is 0.01 to 0.1 M, and the corn germ is soaked for 0.5 to 3 hours at a ratio of material to liquid of 1:1 to 1:5.
  5. 根据权利要求3所述的方法，其特征在于，玉米胚芽浸泡后采用目数100～250的涤纶纱布过滤。The method according to claim 3, characterized in that the corn germ is soaked and then filtered with a polyester gauze having a mesh size of 100 to 250.
  6. 根据权利要求3所述的方法，其特征在于，浸泡沥干后得到的湿玉米胚芽水分含量在60％～70％。The method according to claim 3, characterized in that the wet corn germ obtained after soaking and draining has a moisture content of 60% to 70%.
  7. 根据权利要求1-6任一所述的方法，其特征在于，蒸汽爆破压力为0.5～1.8MPa±0.1MPa，时间设置为15～120s。The method according to any one of claims 1 to 6, wherein the steam explosion pressure is 0.5 to 1.8 MPa ± 0.1 MPa, and the time is set to 15 to 120 s.
  8. 根据权利要求1-6任一所述的方法，其特征在于，汽爆后的玉米胚芽的烘干温度为50～70℃，烘干后物料的水分含量为2％～4％。The method according to any one of claims 1 to 6, characterized in that the drying temperature of the corn germ after steam explosion is 50 to 70 ° C, and the moisture content of the material after drying is 2% to 4%.
  9. 根据权利要求7所述的方法，其特征在于，玉米胚芽经气爆烘干后，先预粉碎到平均粒径为100～200μm；再采用碾压机进行精细粉碎，使物料平均粒径30～80μm。The method according to claim 7, wherein the corn germ is pre-pulverized to a mean particle size of 100-200 μm after being air-blasted and dried, and then finely pulverized by a roller compactor to make the average particle size of the material 30~. 80μm.
  10. 根据权利要求1所述的方法，其特征在于，乙醇溶液提取玉米胚芽油的温度为50～80℃，pH 8.0～10.0，料液比1:4～1:8，乙醇水溶液的浓度为15～35％，反应时间0.5～3h。 The method according to claim 1, wherein the temperature of the corn germ oil extracted by the ethanol solution is 50-80 ° C, the pH is 8.0 to 10.0, the ratio of material to liquid is 1:4 to 1:8, and the concentration of the aqueous ethanol solution is 15 to 35%, reaction time 0.5 to 3h.
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