CN101485366A - Method for refining vegetable seed crude oil using immobilized phospholipase A1 - Google Patents
Method for refining vegetable seed crude oil using immobilized phospholipase A1 Download PDFInfo
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- CN101485366A CN101485366A CNA2009100713987A CN200910071398A CN101485366A CN 101485366 A CN101485366 A CN 101485366A CN A2009100713987 A CNA2009100713987 A CN A2009100713987A CN 200910071398 A CN200910071398 A CN 200910071398A CN 101485366 A CN101485366 A CN 101485366A
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Abstract
The invention provides a method for refining rape seed crude oil by immobilized phosphatidase A1, and relates to the method for refining the rape seed crude oil. The problems of inactivation of enzyme caused by an uneasily controlled enzyme reaction condition during production and high cost of phosphatidase in enzyme process degumming can be solved by selecting the immobilized phosphatidase A1 for degumming. The method for refining the rape seed crude oil by the immobilized phosphatidase A1 is realized by the following steps: 1, preparing a reaction solution; 2, preparing a mixed solution; 3, preparing granulated immobilized enzyme; 4, pretreating the rape seed crude oil; 5, adding the immobilized enzyme into the oil; and 6, stirring and centrifugating to realize the refined rape seed crude oil by the immobilized phosphatidase A1. The rape seed crude oil is subjected to the degumming treatment by the method to improve degumming efficiency. Compared with the prior method, the method improves the degumming efficiency by 5 to 30 percent and the economic benefit by 1 to 3 percent.
Description
Technical field:
The present invention relates to a kind of method of rapeseed oil being carried out refining.
Background technology:
Coming unstuck is a important step in the rapeseed oil refining process, is the necessary condition that guarantees that physical refining carries out smoothly, most important to improving refining yield and oil quality.Colloid removes not thorough, has both influenced the deep processing of oil product and the stability of oil product, also influences the cooking consumption of oil product.The main purpose of coming unstuck is the phosphatide that removes in the oil, and phosphatide divides hydrated phospholipid and nonhydratable phosphatide, in degumming tech, hydrated phospholipid can be removed by the method for simple hydration degum, nonhydratable phosphatide has obvious hydrophobic, difficulty combines with water in hydration degum, removes comparatively difficulty.Because the factor of rapeseed maturity period climatic influences and rapeseed maturity, and reason such as technological operation control in the production and processing, often make to have more nonhydratable phosphatide in mao vegetable seed, traditional aquation technology can't be removed, and this has just influenced the quality of product oil.
Development through decades, particularly physical refining successful implementation, people have released multiple Degumming method, as utilize that traditional hydration degum, simple acid system come unstuck, Special comes unstuck and enzyme method for degumming etc., the enzyme method for degumming is a new and high technology of oil and fat refining, and this technology has huge using value aspect economic benefit that improves oil prodution industry and the environmental-protecting performance.The enzyme method for degumming can drop to phosphorus content in the oil below the 10mg/kg, but the existence of free phosphorus lipase costs an arm and a leg, and is difficult for reclaiming problems such as catalyzing hydrolysis condition harshness.
Summary of the invention
The present invention is wayward and cause the high problem of phosphatidase cost in enzyme deactivation and the enzymatic degumming in order to solve in the actual production enzyme reaction condition, and has proposed to use immobilized phospholipase A
1The refining vegetable seed crude oil.Use immobilized phospholipase A
1The refining vegetable seed crude oil is realized by following steps: one, 1.0～15g sodium alginate is dissolved in 50～500g distilled water standby, with 5～50mL phospholipase A
1Join 50～500mL, pH value and be among 5 the HAc-NaAc or citric acid solution, it is standby to obtain enzyme liquid; Two, be that 0.5～3: 1 ratio is mixed with sodium alginate soln and enzyme liquid with volume ratio, obtain mixed liquor; Three, 1.0～15g shitosan is dissolved in 2～10% acetums of 50～500g, joins the CaCl of 0.05～0.2mol/L of preparation 100～1000mL again
2In the solution, mixed liquor is dropwise joined CaCl
2In the mixed solution, form circular granular, particle left standstill under 30～50 ℃ condition, dry after 40～60 minutes, the graininess immobilised enzymes is standby; Four, get the vegetable seed crude oil hydrated phospholipid in hydration degum method removal vegetable seed crude oil earlier, the citric acid solution that add mass concentration then and be 40～50% in treated vegetable seed crude oil, quality is vegetable seed crude oil 0.1～2% also stirred 5～30 minutes with 500～1500 rev/mins speed, added mass concentration again and be 4% NaOH solution in treated vegetable seed crude oil and constantly stir until the pH of vegetable seed crude oil value to stop to add NaOH solution between 4.0～6.0; Five, in the vegetable seed crude oil of adjusting the pH value, be incorporated as 0.05～0.5% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 45～60 ℃ of conditions; Six, the vegetable seed crude oil that the adds immobilised enzymes speed with 40～100r/min was stirred 2～12 hours, then to the vegetable seed crude oil that adds immobilised enzymes centrifugal 1～5 minute with the speed of 6000～8000r/min, remove the impurity in the heavy phase, promptly realize with immobilized phospholipase refining vegetable seed crude oil.
Phospholipase A in the method for refining vegetable seed crude oil of the present invention after the immobilization
1Hear resistance be improved, can in the pH of broad scope, keep higher activity, the sensitiveness of reaction environment is reduced, make easier control of operating condition and enforcement.Phospholipase A after the immobilization
1But more than the successive reaction 25h, can also recycle and reuse, improved the efficient of coming unstuck, improved 5～30% than existing method, reduce production costs, cost has reduced by 20～40% than existing method, but the high long-time continuous of the present invention's stability is operated, the retentive activity height, up to 50～80%, the present invention can carry out the large-scale industry operation.
The specific embodiment
The specific embodiment one: use immobilized phospholipase A in the present embodiment
1The refining vegetable seed crude oil is realized by following steps: one, 1.0～15g sodium alginate is dissolved in 50～500g distilled water standby, with 5～50mL phospholipase A
1Join 50～500mL, pH value and be among 5 the HAc-NaAc or citric acid solution, it is standby to obtain enzyme liquid; Two, be that the ratio of 0.5～3:1 is mixed with sodium alginate soln and enzyme liquid with volume ratio, obtain mixed liquor; Three, 1.0～15g shitosan is dissolved in 2～10% acetums of 50～500g, joins the CaCl of 0.05～0.2mol/L of preparation 100～1000mL again
2In the solution, mixed liquor is dropwise joined CaCl
2In the mixed solution, form circular granular, particle left standstill under 30～50 ℃ condition, dry after 40～60 minutes, the graininess immobilised enzymes is standby; Four, get the vegetable seed crude oil hydrated phospholipid in hydration degum method removal vegetable seed crude oil earlier, the citric acid solution that add mass concentration then and be 40～50% in treated vegetable seed crude oil, quality is vegetable seed crude oil 0.1～2% also stirred 5～30 minutes with 500～1500 rev/mins speed, added mass concentration again and be 4% NaOH solution in treated vegetable seed crude oil and constantly stir until the pH of vegetable seed crude oil value to stop to add NaOH solution between 4.0～6.0; Five, in the vegetable seed crude oil of adjusting the pH value, be incorporated as 0.1～0.5% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 45～60 ℃ of conditions; Six, the vegetable seed crude oil that the adds immobilised enzymes speed with 40～100r/min was stirred 2～12 hours, then to the vegetable seed crude oil that adds immobilised enzymes centrifugal 1～5 minute with the speed of 6000～8000r/min, remove the impurity in the heavy phase, promptly realize with immobilized phospholipase refining vegetable seed crude oil.
After carrying out vegetable seed crude oil refining treatment with present embodiment, the phosphorus content of vegetable seed crude oil is at 10～20mg/kg, and phosphorus content has reduced more than 80% when not coming unstuck, and after measured, the enzyme activity of graininess immobilised enzymes is between 50～80% in the present embodiment.
The specific embodiment two: the difference of the present embodiment and the specific embodiment one is to be dissolved in 80～400g distilled water 2～12g sodium alginate standby in the step 1.Other step is identical with the specific embodiment one.
The specific embodiment three: the difference of the present embodiment and the specific embodiment one is in the step 1 10～40mL phospholipase A
1Join 100～400mL, pH value and be among 5 the HAc-NaAc or citric acid solution.Other step is identical with the specific embodiment one.
The specific embodiment four: the difference of the present embodiment and the specific embodiment one is in the step 1 20～30mL phospholipase A
1Join 200～300mL, pH value and be among 5 the HAc-NaAc or citric acid solution.Other step is identical with the specific embodiment one.
The specific embodiment five: the difference of the present embodiment and the specific embodiment one is in the step 1 the 25mL phospholipase A
1Join 250mL, pH value and be among 5 the HAc-NaAc or citric acid solution.Other step is identical with the specific embodiment one.
The specific embodiment six: it is standby that the difference of the present embodiment and the specific embodiment one is that 2～12g shitosan in the step 3 is dissolved in 4～8% acetums of 80～400g.Other step is identical with the specific embodiment one.
The specific embodiment seven: the difference of the present embodiment and the specific embodiment one is to prepare in the step 3 CaCl of 0.08～0.12mol/L of 200～800mL
2Solution.Other step is identical with the specific embodiment one.
The specific embodiment eight: the difference of the present embodiment and the specific embodiment one is to prepare in the step 3 CaCl of 0.09～0.11mol/L of 300～700mL
2Solution.Other step is identical with the specific embodiment one.
The specific embodiment nine: the difference of the present embodiment and the specific embodiment one is the CaCl of the 0.1mol/L of preparation 600mL in the step 3
2Solution.Other step is identical with the specific embodiment one.
The specific embodiment ten: the difference of the present embodiment and the specific embodiment one is in the step 4 to add mass concentration is 41～49%, quality is vegetable seed crude oil 0.5～1.8% citric acid solution and stirred 8～16 minutes with 600～1400 rev/mins speed in treated vegetable seed crude oil.Other step is identical with the specific embodiment one.
The specific embodiment 11: the difference of the present embodiment and the specific embodiment one is in the step 4 to add mass concentration is 42～48%, quality is vegetable seed crude oil 1～1.6% citric acid solution and stirred 10～14 minutes with 700～1200 rev/mins speed in treated vegetable seed crude oil.Other step is identical with the specific embodiment one.
The specific embodiment 12: the difference of the present embodiment and the specific embodiment one is in the step 4 to add mass concentration is 45%, quality is vegetable seed crude oil 1.5% citric acid solution and stirred 12 minutes with 1000 rev/mins speed in treated vegetable seed crude oil.Other step is identical with the specific embodiment one.
The specific embodiment 13: the difference of the present embodiment and the specific embodiment one is in the step 4 to add mass concentration in treated vegetable seed crude oil is 4% NaOH solution and constantly stirs stop to add NaOH solution when the pH of vegetable seed crude oil value is between 4.5～5.8.Other step is identical with the specific embodiment one.
The specific embodiment 14: the difference of the present embodiment and the specific embodiment one is in the step 5 to be incorporated as 0.15～0.45% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 50～58 ℃ of conditions in the vegetable seed crude oil of adjusting the pH value.Other step is identical with the specific embodiment one.
The specific embodiment 15: the difference of the present embodiment and the specific embodiment one is in the step 5 to be incorporated as 0.25% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 54～56 ℃ of conditions in the vegetable seed crude oil of adjusting the pH value.Other step is identical with the specific embodiment one.
The specific embodiment 16: the difference of the present embodiment and the specific embodiment one is in the step 5 to be incorporated as 0.25% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 55 ℃ of conditions in the vegetable seed crude oil of adjusting the pH value.Other step is identical with the specific embodiment one.
The specific embodiment 17: the difference of the present embodiment and the specific embodiment one is in the step 6 vegetable seed crude oil that the adds immobilised enzymes speed with 50～90r/min was stirred 4～10 hours.Other step is identical with the specific embodiment one.
The specific embodiment 18: the difference of the present embodiment and the specific embodiment one is in the step 6 the vegetable seed crude oil that adds immobilised enzymes with the speed of 6200～7800r/min centrifugal 1～5 minute.Other step is identical with the specific embodiment one.
Claims (10)
1, a kind of immobilized phospholipase A that uses
1The method of refining vegetable seed crude oil is characterized in that realizing by following steps with immobilized phospholipase refining vegetable seed crude oil: one, 1.0～15g sodium alginate is dissolved in 50～500g distilled water standby, with 5～50mL phospholipase A
1Join 50～500mL, pH value and be among 5 the HAc-NaAc or citric acid solution, it is standby to obtain enzyme liquid; Two, be that 0.5～3: 1 ratio is mixed with sodium alginate soln and enzyme liquid with volume ratio, obtain mixed liquor; Three, 1.0～15g shitosan is dissolved in 2～10% acetums of 50～500g, joins the CaCl of 0.05～0.2mol/L of preparation 100～1000mL again
2In the solution, mixed liquor is dropwise joined CaCl
2In the mixed solution, form circular granular, particle left standstill under 30～50 ℃ condition, dry after 40～60 minutes, the graininess immobilised enzymes is standby; Four, get the vegetable seed crude oil hydrated phospholipid in hydration degum method removal vegetable seed crude oil earlier, the citric acid solution that add mass concentration then and be 40～50% in treated vegetable seed crude oil, quality is vegetable seed crude oil 0.1～2% also stirred 5～20 minutes with 500～1500 rev/mins speed, added mass concentration again and be 4% NaOH solution in treated vegetable seed crude oil and constantly stir to stop to add NaOH solution when the pH of vegetable seed crude oil value is between 4.0～6.0; Five, in the vegetable seed crude oil of adjusting the pH value, be incorporated as 0.05～0.5% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 45～60 ℃ of conditions; Six, the vegetable seed crude oil that the adds immobilised enzymes speed with 40～100r/min was stirred 2～12 hours, then to the vegetable seed crude oil that adds immobilised enzymes centrifugal 1～5 minute with the speed of 6000～8000r/min, remove the impurity in the heavy phase, promptly realize with immobilized phospholipase refining vegetable seed crude oil.
2, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that being dissolved in 80～400g distilled water 2～12g sodium alginate standby in the step 1.
3, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in the step 1 10～40mL phospholipase A
1Join 100～400mL, pH value and be among 5 the HAc-NaAc or citric acid solution.
4, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in the step 3 2～12g shitosan being dissolved in 4～8% acetums of 80～400g standby.
5, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that preparing in the step 3 CaCl of 0.08～0.12mol/L of 200～800mL
2Solution.
6, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in treated vegetable seed crude oil, adding in the step 4 mass concentration and be 41～49% citric acid solution and stirred 8～16 minutes with 600～1400 rev/mins speed.
7, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in treated vegetable seed crude oil, adding in the step 4 mass concentration and be 4% NaOH solution and constantly stir and between 4.5～5.8, stop to add NaOH solution until the pH of vegetable seed crude oil value.
8, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in the step 5 in the vegetable seed crude oil of adjusting the pH value, being incorporated as 0.15～0.45% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 50～58 ℃ of conditions.
9, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in the step 5 in the vegetable seed crude oil of adjusting the pH value, being incorporated as 0.2～0.3% immobilised enzymes of the vegetable seed quality of crude oil of adjusting the pH value under 54～56 ℃ of conditions.
10, according to claim 1 with immobilized phospholipase refining vegetable seed crude oil, it is characterized in that in the step 6 vegetable seed crude oil that the adds immobilised enzymes speed with 50～90r/min was stirred 4～10 hours, and with the speed of 6200～7800r/min centrifugal 1.5～4 minutes.
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| CNA2009100713987A CN101485366A (en) | 2009-02-12 | 2009-02-12 | Method for refining vegetable seed crude oil using immobilized phospholipase A1 |
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| CNA2009100713987A CN101485366A (en) | 2009-02-12 | 2009-02-12 | Method for refining vegetable seed crude oil using immobilized phospholipase A1 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102010025764A1 (en) | 2010-07-01 | 2012-01-05 | Süd-Chemie AG | Phospholipase-support complex |
| CN102367396A (en) * | 2011-08-16 | 2012-03-07 | 哈尔滨工业大学 | Method of immobilizing phospholipase A1 by oxidation of sodium periodate for degumming of soybean crude oil |
| CN102399628A (en) * | 2011-09-20 | 2012-04-04 | 东北农业大学 | Method for degumming crude soybean oil by immobilized phosphatidase membrane |
| CN102399627A (en) * | 2011-09-26 | 2012-04-04 | 华南理工大学 | Improved vegetable oil enzymatic degumming method |
| CN102504946A (en) * | 2011-11-04 | 2012-06-20 | 福建春辉生物工程有限公司 | Method for refining camellia seed crude oil beneficial to individuals with hypertension, hyperglycemia, hyperlipidemia |
| CN102533439A (en) * | 2011-10-28 | 2012-07-04 | 东北农业大学 | Detachable oil continuous degumming membrane reactor |
| CN102559378A (en) * | 2010-11-10 | 2012-07-11 | 东北农业大学 | Method for refining raw oil by using magnetic immobilized phospholipase A1 |
| CN102776066A (en) * | 2012-07-24 | 2012-11-14 | 东北农业大学 | Degumming method through immobilized phospholipase A2 |
| CN102796721A (en) * | 2012-05-17 | 2012-11-28 | 东北农业大学 | Method for immobilizing phospholipase A2 by using sodium alginate-chitosan |
| CN102807917A (en) * | 2012-07-18 | 2012-12-05 | 东北农业大学 | Method for degumming by using immobilized phospholipase C |
| CN103352064A (en) * | 2013-06-25 | 2013-10-16 | 天津大学 | Method for preparing corn protein active peptide by using composite carrier immobilized double enzymes |
| CN104593145A (en) * | 2015-01-21 | 2015-05-06 | 东北农业大学 | Method for degumming crude soybean oil by combined application of immobilized phospholipase C and immobilized phospholipase A1 |
| CN112430501A (en) * | 2020-12-18 | 2021-03-02 | 江西省粮油科学技术研究所 | Degumming method of cornus wisoniana raw oil |
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2009
- 2009-02-12 CN CNA2009100713987A patent/CN101485366A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012001153A1 (en) | 2010-07-01 | 2012-01-05 | Süd-Chemie AG | Phospholipase-carrier complex |
| DE102010025764A1 (en) | 2010-07-01 | 2012-01-05 | Süd-Chemie AG | Phospholipase-support complex |
| CN102559378A (en) * | 2010-11-10 | 2012-07-11 | 东北农业大学 | Method for refining raw oil by using magnetic immobilized phospholipase A1 |
| CN102559378B (en) * | 2010-11-10 | 2013-10-23 | 东北农业大学 | Method for refining raw oil by using magnetic immobilized phospholipase A1 |
| CN102367396A (en) * | 2011-08-16 | 2012-03-07 | 哈尔滨工业大学 | Method of immobilizing phospholipase A1 by oxidation of sodium periodate for degumming of soybean crude oil |
| CN102367396B (en) * | 2011-08-16 | 2013-03-13 | 哈尔滨工业大学 | Method of immobilizing phospholipase A1 by oxidation of sodium periodate for degumming of soybean crude oil |
| CN102399628A (en) * | 2011-09-20 | 2012-04-04 | 东北农业大学 | Method for degumming crude soybean oil by immobilized phosphatidase membrane |
| CN102399627A (en) * | 2011-09-26 | 2012-04-04 | 华南理工大学 | Improved vegetable oil enzymatic degumming method |
| CN102399627B (en) * | 2011-09-26 | 2012-09-05 | 华南理工大学 | Improved vegetable oil enzymatic degumming method |
| CN102533439A (en) * | 2011-10-28 | 2012-07-04 | 东北农业大学 | Detachable oil continuous degumming membrane reactor |
| CN102533439B (en) * | 2011-10-28 | 2013-12-11 | 东北农业大学 | Detachable oil continuous degumming membrane reactor |
| CN102504946B (en) * | 2011-11-04 | 2013-09-04 | 福建春辉生物工程有限公司 | Method for refining camellia seed crude oil beneficial to individuals with hypertension, hyperglycemia, hyperlipidemia |
| CN102504946A (en) * | 2011-11-04 | 2012-06-20 | 福建春辉生物工程有限公司 | Method for refining camellia seed crude oil beneficial to individuals with hypertension, hyperglycemia, hyperlipidemia |
| CN102796721A (en) * | 2012-05-17 | 2012-11-28 | 东北农业大学 | Method for immobilizing phospholipase A2 by using sodium alginate-chitosan |
| CN102807917A (en) * | 2012-07-18 | 2012-12-05 | 东北农业大学 | Method for degumming by using immobilized phospholipase C |
| CN102776066A (en) * | 2012-07-24 | 2012-11-14 | 东北农业大学 | Degumming method through immobilized phospholipase A2 |
| CN103352064A (en) * | 2013-06-25 | 2013-10-16 | 天津大学 | Method for preparing corn protein active peptide by using composite carrier immobilized double enzymes |
| CN104593145A (en) * | 2015-01-21 | 2015-05-06 | 东北农业大学 | Method for degumming crude soybean oil by combined application of immobilized phospholipase C and immobilized phospholipase A1 |
| CN112430501A (en) * | 2020-12-18 | 2021-03-02 | 江西省粮油科学技术研究所 | Degumming method of cornus wisoniana raw oil |
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Open date: 20090722 |