CN102295986B - Preparation method of rice bran oil with low acid value - Google Patents
Preparation method of rice bran oil with low acid value Download PDFInfo
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- CN102295986B CN102295986B CN 201110220877 CN201110220877A CN102295986B CN 102295986 B CN102295986 B CN 102295986B CN 201110220877 CN201110220877 CN 201110220877 CN 201110220877 A CN201110220877 A CN 201110220877A CN 102295986 B CN102295986 B CN 102295986B
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Abstract
The invention provides a preparation method of rice bran oil with the low acid value, which comprises the following steps: fresh-keeping the rice bran, extracting the rice bran oil, degumming, de-waxing, decolouring, deacidifying and deodorizing. The invention has the advantages of simple technology and low production cost; since the extracted crude rice bran oil is performed a fresh-keeping treatment, the acid value is relative low. The final finished product rice bran oil treated by the above steps is detected by a method prescribed by GB/T5530-2005, the acid value is between 1.0-3.0 (KOH) (mg/g).
Description
Technical field
The present invention relates to a kind of preparation method of Rice pollard oil, especially relate to a kind of preparation method of low-acid value rice bran oil.
Background technology
Rice pollard oil is the vegetables oil of a kind of nutrition Feng Ying, and it has become another protective foods after sunflower seed oil, Fructus Maydis oil with oil, eats for a long time Rice pollard oil, and the prevention cardiovascular and cerebrovascular diseases is arranged, and the function such as enhance metabolism and anti-ageing.With regard to China's As-Is, it is very large that the rice bran amount is produced in the whole nation per year, because rice bran easily becomes sour rotten, domestic production enterprise disperses in addition, industrial scale is little, is difficult to concentrate carry out the deep processing increment, only is used on a small quantity recovering rice bran oil, most of rice bran only is used as feed and is used in the locality, added value is lower.
The method of refining that CN101781605A discloses a kind of Rice pollard oil on July 21st, 2010, mainly take hair Rice pollard oil (acid number is as 30mg/g) as raw material, through come unstuck, oil foot separation, dewaxing, decolouring, high temperature depickling, deodorization, freezing degreasing, obtain refining rice bran oil, its technological process is relatively complicated, processing condition are had relatively high expectations, and required cost is also higher, and the acid value of the refining rice bran oil that obtains can only reach 3mg/g.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of technique simple, and production cost is low, the preparation method of the low-acid value rice bran oil that quality product is high.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of low-acid value rice bran oil comprises the steps:
(1) keeping rice bran fresh: add the ethylenediamine tetraacetic acid (EDTA) amount that is equivalent to rice bran weight 0.8-1.0% in fresh rice bran, the water that the papoid of 0.08-0.10%, 8-12 are doubly measured stirs;
(2) the hair Rice pollard oil extracts: will adopt extraction to extract Rice pollard oil through rice bran and the water mixture of step (1) Preservation Treatment, extraction temperature be 60～80 ℃, and extraction time is 4-8h;
(3) come unstuck dewaxing: will extract gained hair Rice pollard oil through step (2) and place container with agitator, and stir and be heated to 70 ℃-80 ℃, and process 20-40min under the condition of stirring velocity 60-80r/min, and filter; In the oil of gained, add the same warm water who is equivalent to 3%-5% times of oil weight, speed with 150-250r/min stirs 20-40min, the mass concentration that adds again the 0.8-1.2% that is equivalent to oil-water mixture weight in the oil-water mixture is 6 ± 0.2% calcium chloride solution, and continues to stir 50-70min the 70-80 ℃ of speed with 150-250r/min; Then Slow cooling is to 14-16 ℃, and speed of cooling is 4-6 ℃/h, uses refrigerated centrifuge centrifugal 15-25min under 6000-8000r/min again, must come unstuck, Rice pollard oil dewaxes;
(4) decolouring: will process the gained Rice pollard oil through step (3) and pour in the container with agitator, this Rice pollard oil is heated to after 85-95 ℃ adds the atlapulgite that is equivalent to the heavy 4-6% of oil and the gac of 0.4%-0.6%, absolute pressure be heated under the 3.5-4.5kPa 104-106 ℃ the decolouring 18-22min, use simultaneously magnetic stirrer, filter after the decolouring, remove atlapulgite and gac;
(5) depickling: the Rice pollard oil that will process through step (4) is that 20～30 ℃, stirring velocity are under the condition of 60～80r/min in temperature, heavy quantitatively to add mass concentration be 10%～12% sodium hydroxide solution with acid value according to oil, behind the alkali refining 25-35min, centrifugation; Or the Rice pollard oil that will process through step (4), by the 95%(volume) ethanol and Rice pollard oil volume proportion be that 9-11:1 adds 95% ethanol, at room temperature extracts, and extracted rear separatory, then distillation removes residual solvent;
(6) deodorization: the Rice pollard oil after step (5) depickling is placed a container, under vacuum tightness is 5-7kPa, temperature 200-250 ℃, the condition of stirring velocity 60-80r/min, process 20-30min.
Further, the described extraction of step (2) is soxhlet extraction.
Further, the described extraction of step (2) uses the preferred normal hexane of reagent, Virahol or sherwood oil.
Studies show that, the free fatty acids in the fresh processed rice bran can increase by 5%～7% within one day, stored that the free fatty acids in the rice bran can rise to 70% after one month.Collect the rice bran that is used for extracting mao Rice pollard oil from each millet factory at present, be difficult to kill on the spot ferment fresh-keeping, and Preservation Treatment in addition again after wait concentrating, then spent optimal anti-staling opportunity, acid number has reached 20～30 (KOH) (mg/g), that have even up to 50 (KOH) (mg/g), such raw material can produce serious negative impact to the quality of subsequent handling operation and Rice pollard oil.Therefore, the present invention takes fresh-keeping measure to fresh rice bran.
Technique of the present invention is simple, and production cost is low; The hair Rice pollard oil that extracts since raw material through Preservation Treatment, its acid number is relatively low, the final finished Rice pollard oil after above-mentioned steps is processed is measured with the GB/T5530-2005 prescriptive procedure, acid value 1.0～3.0 (KOH) (mg/g) between.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment.
Embodiment 1
The present embodiment comprises the steps:
(1) keeping rice bran fresh: in fresh rice bran, add the ethylenediamine tetraacetic acid (EDTA) that is equivalent to rice bran weight 0.9%, 0.09% papoid, the water of 10 times of amounts stirs;
(2) Rice pollard oil extracts: will adopt soxhlet extraction to carry oil through the rice bran water mixture of step (1) Preservation Treatment, and use extraction reagent to be sherwood oil, extraction temperature be 70 ℃, lixiviate 6h;
(3) come unstuck, dewaxing: will place the 1000mL beaker through the 500g hair Rice pollard oil that step (2) is extracted gained, with the stirring of magnetic force heating stirrer and be heated to 75 ℃, stirring velocity is 70r/min, churning time is 30min, then with the Büchner funnel suction filtration that is lined with common filter paper; Be equivalent to oily 5% the same warm water that weighs in the oil of suction filtration processing, adding, speed with 200r/min stirs 30min, the mass concentration that adds again oil-water mixture 1% in the oil-water mixture is 6% calcium chloride solution, and continue to stir 1h 75 ℃ of speed with 200r/min, then Slow cooling to 15 ℃, speed of cooling is 5 ℃/h, uses refrigerated centrifuge centrifugal 20min under 7000r/min again, must come unstuck, Rice pollard oil dewaxes;
(4) decolouring: will process the gained Rice pollard oil through step (3) and pour in the round-bottomed flask of 1000mL, with mixture heating up to 90 ℃, add in the oil and be equivalent to oil and weigh 5% atlapulgite and 0.5% gac, under absolute pressure 4.0kPa, be heated to 105 ℃ of decolouring 20min, use simultaneously magnetic stirrer, decolouring is removed atlapulgite and gac by the Büchner funnel suction filtration;
(5) depickling: the Rice pollard oil that will process through step (4) is under the condition of 25 ℃ of temperature, stirring velocity 70 r/min, and heavy quantitatively to add mass concentration with acid value be 11% sodium hydroxide solution according to oil, behind the alkali refining 30min, and centrifugation;
(6) deodorization: the Rice pollard oil after step (5) depickling is processed is placed triangular flask, under the condition of vacuum tightness 5kPa, 250 ℃ of temperature, stirring velocity 70r/min, process 25min.
The present embodiment gained rice finished product oil extracted from rice husks is measured with the GB/T5530-2005 prescriptive procedure, acid value be 2.3 (KOH) (mg/g).
Embodiment 2
The present embodiment comprises the steps:
(1) keeping rice bran fresh: in fresh rice bran, add the ethylenediamine tetraacetic acid (EDTA) that is equivalent to rice bran weight 0.8%, 0.08% papoid, the water of 8 times of amounts stirs;
(2) Rice pollard oil extracts: will adopt soxhlet extraction through the rice bran of step (1) Preservation Treatment, and use reagent to be Virahol, extraction temperature is 80 ℃, lixiviate 4h;
(3) come unstuck, dewaxing: will place the 1000mL beaker through the 500g hair Rice pollard oil that step (2) is extracted gained, with the stirring of magnetic force heating stirrer and be heated to 80 ℃, stirring velocity is 80r/min, churning time is 20min, then with the Büchner funnel suction filtration that is lined with common filter paper; Be equivalent to oily 6% the same warm water that weighs in the oil of suction filtration processing, adding, speed with 250r/min stirs 20min, add again the mass concentration be equivalent to oil-water mixture 1.2% and be 6.2% calcium chloride solution, and continue to stir 50min 80 ℃ of speed with 250r/min, then Slow cooling to 16 ℃, speed of cooling is 6 ℃/h, uses refrigerated centrifuge centrifugal 15min under 8000r/min again, must come unstuck, Rice pollard oil dewaxes;
(4) decolouring: will process the gained Rice pollard oil through step (3) and pour in the round-bottomed flask of 1000mL, with mixture heating up to 95 ℃, add in the oil and be equivalent to oil and weigh 6% atlapulgite and 0.6% gac, under absolute pressure 4.5kPa, be heated to 106 ℃ of decolouring 22min, use simultaneously magnetic stirrer; Decolouring is removed atlapulgite and gac by the Büchner funnel suction filtration;
(5) depickling: the Rice pollard oil that will process through step (4) is that the ratio of 10:1 is added 95% ethanol and extracted in 95% ethanol and Rice pollard oil volume proportion, under 30 ℃ of conditions, through 4 extractions, each extraction time 15min, extracted rear separatory, distillation, desolvation is residual;
(6) deodorization: the Rice pollard oil after step (5) depickling is processed is placed triangular flask, under the condition of vacuum 6.7kPa, 250 ℃ of temperature, stirring velocity 80r/min, process 20min.
The present embodiment gained rice finished product oil extracted from rice husks is measured with the GB/T5530-2005 prescriptive procedure, acid value be 2.6 (KOH) (mg/g).
Embodiment 3
The present embodiment comprises the steps:
(1) keeping rice bran fresh: in fresh rice bran, add the ethylenediamine tetraacetic acid (EDTA) that is equivalent to rice bran weight 1.0%, 0.1% papoid, the water of 12 times of amounts stirs;
(2) Rice pollard oil extracts: will adopt soxhlet extraction to carry oil through the rice bran water mixture of step (1) Preservation Treatment, and use extraction reagent to be ether, extraction temperature be 60 ℃, lixiviate 8h;
(3) come unstuck, dewaxing: will place the 1000mL beaker through the 500g hair Rice pollard oil that step (2) is extracted gained, with the stirring of magnetic force heating stirrer and be heated to 70 ℃, stirring velocity is 60r/min, churning time is 40min, then with the Büchner funnel suction filtration that is lined with common filter paper; In the oil of processing through suction filtration, add oily 4% the same warm water that weighs, speed with 150r/min stirs 40min, the mass concentration that adds again oil-water mixture 0.8% in the oil-water mixture is 5.8% calcium chloride solution, and continue to stir 70min 70 ℃ of speed with 150r/min, then Slow cooling to 14 ℃, speed of cooling is 4 ℃/h, uses refrigerated centrifuge centrifugal 25min under 6000r/min again, must come unstuck, Rice pollard oil dewaxes;
(4) decolouring: will process the gained Rice pollard oil through step (3) and pour in the round-bottomed flask of 1000mL, with mixture heating up to 90 ℃, add in the oil and be equivalent to oil and weigh 4% atlapulgite and 0.4% gac, under absolute pressure 3.5kPa, be heated to 104 ℃ of decolouring 18min, use simultaneously magnetic stirrer, decolouring is removed atlapulgite and gac by the Büchner funnel suction filtration;
(5) depickling: the Rice pollard oil that will process through step (4) is under the temperature room temperature condition, and under the condition of stirring velocity 60r/min, heavy quantitatively to add mass concentration with acid value be 10% sodium hydroxide solution according to oil, behind the alkali refining 25min, and centrifugation;
(6) deodorization: the Rice pollard oil after step (5) depickling is processed is placed triangular flask, under the condition of vacuum tightness 5kPa, 250 ℃ of temperature, stirring velocity 60r/min, process 30min.
The present embodiment gained rice finished product oil extracted from rice husks is measured with the GB/T5530-2005 prescriptive procedure, acid value be 2.8 (KOH) (mg/g).
Claims (3)
1. the preparation method of a low-acid value rice bran oil is characterized in that, comprises the steps:
(1) keeping rice bran fresh: add the ethylenediamine tetraacetic acid (EDTA) that is equivalent to rice bran weight 0.8-1.0% in fresh rice bran, the water that the papoid of 0.08-0.10%, 8-12 are doubly measured stirs;
(2) the hair Rice pollard oil extracts: will adopt extraction to extract Rice pollard oil through rice bran and the water mixture of step (1) Preservation Treatment, extraction temperature be 60～80 ℃, and extraction time is 4-8h;
(3) come unstuck dewaxing: will extract gained hair Rice pollard oil through step (2) and place container with agitator, and stir and be heated to 70 ℃-80 ℃, stirring velocity is 60-80r/min, and churning time is 20-40min, filters; In the oil of gained, add the same warm water who is equivalent to the heavy 3%-5% of oil, speed with 150-250r/min stirs 20-40min, add again the mass concentration that is equivalent to oil-water mixture weight 0.8-1.2% in the oil-water mixture and be 6 ± 0.2% calcium chloride solution, and continue to stir 50-70min the 70-80 ℃ of speed with 150-250r/min; Then Slow cooling is to 14-16 ℃, and speed of cooling is 4-6 ℃/h, uses refrigerated centrifuge centrifugal 15-25min under 6000-8000r/min again, must come unstuck, Rice pollard oil dewaxes;
(4) decolouring: will process the gained Rice pollard oil through step (3) and pour in the container with agitator, this Rice pollard oil is heated to after 85-95 ℃ adds the atlapulgite that is equivalent to the heavy 4-6% of oil and the gac of 0.4%-0.6%, absolute pressure be heated under the 3.5-4.5kPa 104-106 ℃ the decolouring 18-22min, use simultaneously magnetic stirrer, filter after the decolouring, remove atlapulgite and gac;
(5) depickling: the Rice pollard oil that will process through step (4) is that 20～30 ℃, stirring velocity are under the condition of 60～80r/min in temperature, heavy quantitatively to add mass concentration be 10%～12% sodium hydroxide solution with acid value according to oil, behind the alkali refining 25-35min, centrifugation; Or the Rice pollard oil that will process through step (4), by volume mark is that 95% ethanol and Rice pollard oil volume proportion are that 9-11:1 adds 95% ethanol, at room temperature extracts, and has extracted rear separatory, then distillation removes residual solvent;
(6) deodorization: the Rice pollard oil after step (5) depickling is placed a container, under vacuum tightness is 5-7kPa, temperature 200-250 ℃, the condition of stirring velocity 60-80r/min, process 20-30min.
2. the preparation method of described low-acid value rice bran oil according to claim 1, it is characterized in that: step (2), described extraction are soxhlet extraction.
3. the preparation method of described low-acid value rice bran oil according to claim 1 and 2, it is characterized in that: step (2), the reagent that described extraction uses is normal hexane, Virahol or sherwood oil.
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| CN101455242B (en) * | 2008-12-26 | 2011-05-04 | 河南华泰粮油机械工程有限公司 | Rice bran first-level oil refinement production method |
| CN101473873A (en) * | 2009-01-19 | 2009-07-08 | 姚建杉 | Industrial refining production method of rice bran oil and equipment thereof |
| CN101530139A (en) * | 2009-04-17 | 2009-09-16 | 江苏牧羊迈安德食品机械有限公司 | Process for refining rice bran oil by using crude rice bran oil |
| CN101984028B (en) * | 2010-10-29 | 2012-07-04 | 湖南农业大学 | High-oryzanol rice bran oil two-phase extraction de-acidification refining technology |
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