CN102827686B - High-pressure steam emulsion breaking method for aqueous enzymatic extraction of soybean oil - Google Patents
High-pressure steam emulsion breaking method for aqueous enzymatic extraction of soybean oil Download PDFInfo
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- 239000000839 emulsion Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- 235000012424 soybean oil Nutrition 0.000 title claims abstract description 14
- 239000003549 soybean oil Substances 0.000 title claims abstract description 14
- 238000000605 extraction Methods 0.000 title claims abstract description 12
- 230000002255 enzymatic effect Effects 0.000 title claims abstract description 10
- 239000003921 oil Substances 0.000 claims abstract description 11
- 235000019198 oils Nutrition 0.000 claims abstract description 11
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- 244000068988 Glycine max Species 0.000 claims abstract description 7
- 235000010469 Glycine max Nutrition 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
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- 239000008267 milk Substances 0.000 claims description 13
- 210000004080 milk Anatomy 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 abstract description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 abstract description 2
- 239000008158 vegetable oil Substances 0.000 abstract description 2
- 239000000413 hydrolysate Substances 0.000 abstract 2
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- 108091005658 Basic proteases Proteins 0.000 abstract 1
- 108010009736 Protein Hydrolysates Proteins 0.000 abstract 1
- 238000002203 pretreatment Methods 0.000 abstract 1
- 235000019871 vegetable fat Nutrition 0.000 abstract 1
- 230000004044 response Effects 0.000 description 23
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- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 description 1
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Abstract
The invention discloses a high-pressure steam emulsion breaking method for the aqueous enzymatic extraction of soybean oil, and belongs to a vegetable oil and fat extraction technology. The method comprises the following steps of: (1) performing extruding-expansion pre-treatment on crushed soybeans to obtain expanded materials, mixing the expanded materials and water to obtain a mixed solution, adding alkaline proteases into the mixed solution for enzymolysis, and performing centrifugal separation to obtain free oil, emulsion, hydrolysate and residues after the enzymolysis; (2) preheating theemulsion and the hydrolysate, which are obtained in the step (1), and introducing high-pressure heating steam into the preheated emulsion and the preheated hydrolysate for emulsion breaking; and (3) performing centrifugal separation to obtain the soybean oil after the emulsion breaking. Process equipment required by the method is simple, and the method is convenient to operate, high in emulsion breaking rate and short in emulsion breaking time.
Description
Technical field
The invention belongs to the extraction processing technology of Vegetable oil lipoprotein, relate generally to a kind of method of aqueous enzymatic extraction soybean oil high pressure steam breakdown of emulsion.
Background technology
Breakdown of emulsion is the ten minutes critical step in the aqueous enzymatic extraction soybean oil, and breakdown of emulsion is more thorough, and the rate of recovery of grease is more high.The quality of breakdown of emulsion directly has influence on the economic worth of whole technology.
The method of breakdown of emulsion is divided into chemical demulsification and physics breakdown of emulsion.Adding emulsion splitter is chemical method.Centrifugal, change temperature, apply electrostatic field, adopt coalescing agent etc. to belong to physical method.The original intention of exploring aqueous enzymatic method technology be in the grease leaching process with an organic solvent with the poisonous and harmful chemical reagent for this reason, easily select physical method as the breakdown of emulsion means.Hanmoungjai (2001) adopts proteolytic enzyme to act on rice bran, and to the emulsion layer method breakdown of emulsion that boils that obtains, oil only is 79% and 68% with the recovery of protein rate.Aparna (2002) adopts 18000g ultra-high speed centrifugation breakdown of emulsion, and oily yield has improved 40% than contrast, but this centrifugation apparatus can't be applied to scale operation.Moura etc. (2008) adopt proteolytic enzyme in conjunction with the method breakdown of emulsion of pH adjusting or Phospholipid hydrolase enzymolysis, the grease of 70%-80% in the recyclable milk sap in soybean aqueous enzymatic method oil-producing technique.Carry in the oil at the soybean aqueous enzymatic method, Wu (2009) explores the mode breakdown of emulsion of enzymolysis and regulation system pH, Jung (2009) further reclaims the free oil condition to the endo-protease breakdown of emulsion and has carried out optimizing research, in the hope of contributing for the development that advances this environmentally friendly oil extracting process of aqueous enzymatic method.In addition, the foreign scholar adopts organic solvent directly to extract oil in the milk sap under study for action mostly, with the oily effect that from the oil plant cell, discharges behind the investigation enzymolysis, and the research that further breaks through from technological layer does not appear in the newspapers, and, problems such as existing demulsification technology exists the breakdown of emulsion time long, and demulsification efficiency is low.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned the deficiencies in the prior art, and a kind of method of aqueous enzymatic extraction soybean oil high pressure steam breakdown of emulsion is provided, and reaches the purpose of simplifying demulsification technology, improving demulsification efficiency.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of method of aqueous enzymatic extraction soybean oil high pressure steam breakdown of emulsion, this method may further comprise the steps: the soybean after (1) will pulverize adopts expelling-expansion pretreatment to obtain expanded material, expanded material mixed with water obtain mixed solution, add Sumizyme MP in the mixed solution and carry out enzymolysis, centrifugation obtains free oil, milk sap, hydrolyzed solution and residue behind the enzymolysis; (2) milk sap that step (1) is obtained and hydrolyzed solution are preheating to 80 ℃, and breakdown of emulsion is carried out in milk sap and the heating steam of hydrolyzed solution feeding high pressure after preheating, and described vapor pressure is 14-22Mpa, and vapor temperature is 80-120 ℃, steam treatment time 6-14s; (3) centrifugation 15min both must soybean oil under 8000r/min behind the breakdown of emulsion.
Described steam breakdown of emulsion preferred parameter is: vapor pressure is 19.6Mpa, and vapor temperature is 116 ℃, steam treatment time 12s.
Present method adopts high pressure steam to carry out breakdown of emulsion, high pressure steam acts on protein in milk sap and the hydrolyzed solution, lymphatic temperament etc., make them that sex change take place, thereby make and originally separate out in milk sap and hydrolyzed solution with the grease of protein emulsifying, and then make grease be released, have the advantages that required processing unit is simple, the breakdown of emulsion time is short, demulsification efficiency is high.
Description of drawings
Fig. 1 is overall process route map of the present invention;
Fig. 2 is that vapor pressure is to the figure that influences of demulsification efficiency;
Fig. 3 is that vapor temperature is to the figure that influences of demulsification efficiency;
Fig. 4 is that the steam treatment time is to the figure that influences of demulsification efficiency;
Fig. 5 is vapor pressure and vapor temperature interaction response surface figure;
Fig. 6 is vapor pressure and steam treatment time interaction response surface figure;
Fig. 7 is vapor temperature and steam treatment time interaction response surface figure.
Specific embodiments
Below in conjunction with accompanying drawing the specific embodiment of the invention is described in detail.
A kind of method of aqueous enzymatic extraction soybean oil high pressure steam breakdown of emulsion, this method may further comprise the steps: the soybean after (1) will pulverize adopts expelling-expansion pretreatment to obtain expanded material, expanded material mixed with water obtain mixed solution, add Sumizyme MP in the mixed solution and carry out enzymolysis, centrifugation obtains free oil, milk sap, hydrolyzed solution and residue behind the enzymolysis; (2) milk sap that step (1) is obtained and hydrolyzed solution are preheating to 80 ℃, and breakdown of emulsion is carried out in milk sap and the heating steam of hydrolyzed solution feeding high pressure after preheating, and described vapor pressure is 14-22Mpa, and vapor temperature is 80-120 ℃, steam treatment time 6-14s; (3) centrifugation 15min both must soybean oil under 8000r/min behind the breakdown of emulsion.
Described steam breakdown of emulsion preferred parameter is: vapor pressure is 19.6Mpa, and vapor temperature is 116 ℃, steam treatment time 12s.
Embodiment high pressure steam demulsification technology optimized parameter shaker test
1 materials and methods
1.1 test raw material
| Soybean | Heilungkiang Academy of Agricultural Sciences cultivates cultivates farming 42, and wherein protein content is 41.6%, and fat content is 21.3%, and water ratio is 10.6%, ash content 4.3%. |
| Alcalase alkaline endo proteolytic enzyme | Novo company (1.2 * 10 5U/mL) |
2.1.2 test apparatus and equipment
| Instrument | Manufacturer |
| CX-500 type Ultrasonic Cleaners | Beijing medical facilities two factories |
| Electronic analytical balance | Mettler-Toledo Instrument (Shanghai) Co., Ltd. |
| Beater disintegrating machine | China Tianjin Tai Site Instr Ltd. |
| LDZ5-2 type table-type low-speed whizzer | Anting Scientific Instrument Factory, Shanghai |
| Electric-heated thermostatic water bath | Yuyao City east electric instrument factory |
| The TGL-16G high speed tabletop centrifuge | Anting Scientific Instrument Factory, Shanghai |
| Accurate electric blender | Jintan City, Jiangsu Province high honour instrument |
| Soxhlet extractor | Tianjin Glass Instrument Factory |
| The electric heating constant temperature air dry oven | Shanghai Yiheng Scientific Instruments Co., Ltd |
1.2 test method
1.2.1 the composition measurement of beans
The mensuration of moisture: according to GB/T14489.1-2008
The mensuration of crude fat: according to GB/T5512-2008
1.2.2 calculation formula
2 results and discussion
2.1 high pressure steam demulsification technology list factor condition is to the influence of demulsification efficiency
2.1.1 vapor pressure is to the influence of demulsification efficiency
Vapor temperature is 100 ℃, and the steam treatment time is 10s, investigates vapor pressure to the influence of demulsification efficiency, the results are shown in Figure 2.By Fig. 2 result as can be seen vapor pressure obviously increase greater than the 8Mpa demulsification efficiency, but when vapor pressure during greater than 18Mpa, demulsification efficiency begins to descend, so vapor pressure is selected 14-22Mpa in the response surface test design below.
2.2.2 vapor temperature is to the influence of demulsification efficiency
Vapor pressure is 18Mpa, and the steam treatment time is 10s, investigates vapor temperature to the influence of demulsification efficiency, the results are shown in Figure 3.By Fig. 3 result as can be seen near vapor temperature demulsification efficiency 100 ℃ have higher value to occur because consider interaction, so vapor temperature is chosen in 80-120 ℃ in the response surface test design below.
2.2.3 the steam treatment time is to the influence of demulsification efficiency
Be 18Mpa at vapor pressure, vapor temperature is 100 ℃, investigates the steam treatment time to the influence of demulsification efficiency, the results are shown in Figure 4.By Fig. 4 result as can be seen when the steam treatment time during greater than 10s demulsification efficiency obviously reduce, so steam treatment selection of time 6-14s in the response surface test design below.
2.3 the response surface optimum experimental reaction conditions of high pressure steam demulsification technology
2.3.1 empirical factor level code table
On the basis of single factor research, choosing vapor pressure, vapor temperature, steam treatment time 3 factors is independent variable(s), is response value with the demulsification efficiency, according to the center combination principle of design, and the experiment of design response surface analysis, its level of factor coding schedule sees Table 3-1.
Table 3-1 level of factor coding schedule
2.3.2 response surface experimental establishment and experimental result
This experimental applications response surface optimized method carries out process optimization.With x
1, x
2, x
3, be independent variable(s), be response value Y with the demulsification efficiency, response surface experimental program and the results are shown in Table 3-2.Experiment 1-14 is factorial experiment, and 15-20 is 5 center tests, in order to the estimating experiment error.
Table 3-2 response surface experimental program and experimental result
2.3.3 response surface interpretation
Carry out data analysis by statistical analysis software SAS9.1, it is as follows to set up quadratic response face regression model:
Y=88.426+3.47x 1 + 5.15x 2 -2.704x 1 2 -1.013x 1 x 2 + 2.048x 1 x 3 -2.364x 2 2 + 2.75x 2 x 3 -1.871x 3 2 Regression analysis and The results of analysis of variance see Table 3-3 alternately mutually significant response surface analysis see Fig. 5-Fig. 7.
Table 3-3 returns and The results of analysis of variance
| Variable | Degree of freedom | Sum of squares | All square | The F value | Pr>F |
| x 1 | 1 | 164.4093 | 164.4093 | 124.1032 | 0.0001 |
| x 2 | 1 | 362.6727 | 362.6727 | 273.761 | 0.0001 |
| x 3 | 1 | 30.04443 | 30.04443 | 22.67883 | 0.000766 |
| x 1 2 | 1 | 105.3784 | 105.3784 | 79.54414 | 0.0001 |
| x 1 x 2 | 1 | 8.20125 | 8.20125 | 6.190657 | 0.032094 |
| x 1 x 3 | 1 | 33.53805 | 33.53805 | 25.31597 | 0.000513 |
| x 2 2 | 1 | 80.5851 | 80.5851 | 60.82911 | 0.0001 |
| x 2 x 3 | 1 | 60.5 | 60.5 | 45.66801 | 0.0001 |
| x 3 2 | 1 | 50.47513 | 50.47513 | 38.10081 | 0.000105 |
| |
9 | 858.0234 | 95.33594 | 71.96368 | 0.0001 |
| |
10 | 13.24779 | 1.324779 | ? | ? |
| Lose and intend | 5 | 2.082385 | 0.416477 | 0.186503 | 0.955466 |
| Summation | 19 | 871.2712 | ? | ? | ? |
Annotate: by analysis, the relative coefficient (R of total regression
2) be 98.48%, the coefficient of determination (R
2Adj) be 97.11%
By showing 3-3 as can be known, the linear relationship between equation dependent variable and the independent variable(s) is obvious, and this model returns significantly (p＜0.0001), and it is not remarkable to lose the plan item, and this model R
2=98.48%, R
2 Adj=97.11%, illustrate that this model and experimental fit are good, linear relationship is remarkable between independent variable(s) and the response value, and the theory that can be used for this reaction is inferred.Can obtain the factor contributions rate by the F check is:
x 2 x 1 x 3 , i.e. vapor temperature〉and vapor pressure〉the steam treatment time.
Application responds face optimizing analytical procedure is analyzed regression model, and seeking the optimal response result is 19.6Mpa for vapor pressure, and vapor temperature is 116 ℃, and the steam treatment time is 12s, and response surface has optimum value 93.41 ± 1.48%.
2.4 confirmatory experiment and simultaneous test
Under the top condition that the response surface analysis method is tried to achieve, namely vapor pressure is 19.6Mpa, and vapor temperature is 116 ℃, and the steam treatment time is 12s, carries out 3 parallel laboratory tests, and the mean value of 3 parallel laboratory tests of demulsification efficiency is 94.27%.The demulsification efficiency predictor is 93.41 ± 1.48%.Experimental value and regression equation predictor that response value is described are coincide good.
3 experiment conclusion
Utilize the response surface analysis method that high pressure steam demulsification technology parameter is optimized.Having set up corresponding mathematical model is that later pilot scale and suitability for industrialized production provided fundamental basis, and to have obtained optimum vapor pressure be 19.6Mpa, and vapor temperature is 116 ℃, and the steam treatment time is 12s.Through the checking with simultaneous test as can be known under optimum high pressure steam demulsification technology condition demulsification efficiency can reach about 93.41%.
Claims (2)
1. the method for an aqueous enzymatic extraction soybean oil high pressure steam breakdown of emulsion, this method may further comprise the steps: the soybean after (1) will pulverize adopts expelling-expansion pretreatment to obtain expanded material, expanded material mixed with water obtain mixed solution, add Sumizyme MP in the mixed solution and carry out enzymolysis, centrifugation obtains free oil, milk sap, hydrolyzed solution and residue behind the enzymolysis; It is characterized in that: (2) are preheating to 80 ℃ with milk sap and the hydrolyzed solution that step (1) obtains, breakdown of emulsion is carried out in milk sap and the heating steam of hydrolyzed solution feeding high pressure after preheating, described vapor pressure is 14-22Mpa, and vapor temperature is 80-120 ℃, steam treatment time 6-14s; (3) behind the breakdown of emulsion under 8000r/min centrifugation 15min namely get soybean oil.
2. the method for a kind of aqueous enzymatic extraction soybean oil high pressure steam breakdown of emulsion according to claim 1, it is characterized in that described steam breakdown of emulsion preferred parameter is: vapor pressure is 19.6Mpa, and vapor temperature is 116 ℃, steam treatment time 12s.
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| CN105331439A (en) * | 2015-11-26 | 2016-02-17 | 东北农业大学 | Method for extracting soybean blend oil and compound protein by using aqueous enzymatic method |
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