CN105238552A - Preparation method of rice bran crude oil with low acid value and low phosphorus content - Google Patents
Preparation method of rice bran crude oil with low acid value and low phosphorus content Download PDFInfo
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- CN105238552A CN105238552A CN201510691426.0A CN201510691426A CN105238552A CN 105238552 A CN105238552 A CN 105238552A CN 201510691426 A CN201510691426 A CN 201510691426A CN 105238552 A CN105238552 A CN 105238552A
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Abstract
The invention discloses a preparation method of rice bran crude oil with a low acid value and low phosphorus content, and belongs to the field of food processing. The method comprises the following steps that rice bran heated through medium-short wave infrared is stabilized, deacidification and dephosphorization are conducted on stabilized rice bran extracted through ethyl alcohol, and the rice bran crude oil is extracted. According to the preparation method of the rice bran crude oil with the low acid value and the low phosphorus content, the technology is simple, the production cost is low, and the prepared rice bran crude oil has the advantages of being low in acid value and phosphorus content, light in color and luster and the like. Determination is conducted through a GB/T5530-2005 method, and the acid value of the rice bran crude oil ranges from 0.5 KOH mg/g to 4 KOH mg/g; determination is conducted through a GB/T5537-2008 method, and the phosphorus content of the rice bran crude oil ranges from 50 ppm to 130 ppm.
Description
Technical field
The present invention relates to the preparation method of a kind of low acid number and low phosphorus content Rice bran crude oil, belong to food processing field.
Background technology
Rice pollard oil is the grease utilizing paddy processing gained byproduct rice bran to prepare, China's paddy annual output 200000000 tons, and machining obtains 2,000 ten thousand tons, byproduct rice bran, can produce Rice pollard oil 3,000,000 tons.Rice pollard oil is nutritious, a kind of desirable edible vegetable oil, its lipid acid composition is comparatively balanced, oleic acid and linolic acid ratio are about 1:1.1, and containing abundant tens kinds of natural bioactive ingredients such as vitamin-E, compound lipid, phosphatide, tocotrienols, squalene, plant sterol, thiaminogen, unsaturated fatty acid content, up to more than 80%, has become another the protective foods oil after sunflower seed oil, Fructus Maydis oil.Long-term edible rice bran oil, has prevention cardiovascular and cerebrovascular diseases, and the function such as enhance metabolism.
During paddy processing, rice bran leaves parent and contacts with oxygen, and rice bran is containing active very strong lipase, under the effect of lipolytic enzyme, the free fatty acids of Rice bran crude oil rises rapidly, and Rice bran crude oil free fatty acid content reaches 10% ~ 15%, and some is even up to 15% ~ 30%; Secondly, the Rice bran crude oil phosphorus content of extract by solvents is at about 300ppm, and glue dopant species is many, complicated components, mainly hydrated phospholipid and non-hydratable phospholipid, is difficult to clean removing.Refining Degumming Procedures is the origin or beginning operation of whole refining process, and the quality of degumming effect determines the effect of the decolouring of postorder, deodorization, depickling and winterization, directly affects outward appearance and the grade judgement of final finished oil.
At present, oil and fat refining deacidifying process mainly adopts chemical alkali refining method and physical refining method, and these two kinds of methods are all not suitable for the depickling of peracid value rice bran oil.Chemistry alkali refining method is large for oil and fat refining loss, and general acid number is the grease of 20mgKOH/g, and after alkali refining, oily loss reaches 55%, and needs repeatedly alkali refining for the Rice pollard oil of high acid value, causes the loss of the nutritive ingredients such as more than 95% thiaminogen.In addition, alkali refining produces a large amount of waste water, contaminate environment.The physical refining method of Rice pollard oil adopts distillation depickling method, namely saturation steam stripping removing free fatty acids is passed into, although the effect of stripping depickling is very good, but this method requires strict to grease pre-treatment, the Rice pollard oil that free fatty acid content is higher needs repeatedly to carry out High Temperature High Pressure distillation process, and consume a large amount of heat energy, electric energy, production cost is high, vitamin-E is lost in free fatty acids, causes nutrient loss.Grease at high temperature, can produce the insalubrious material such as trans fatty acid and propylene chlorohydrin, and after edible, Developing restraint is grown.
Esterification deacidification method utilizes enzyme catalyst to add glycerol method to carry out reduction grease, but the method esterification temperature is high, after adding catalyzer, can produce a sweet ester, DAG, make grease sex change, be not suitable for making edible oil.Use relevant enzyme is expensive, and production cost is high, cannot carry out scale operation.
The extracting method of current Rice bran crude oil has solvent extration, sub sigmaritical extraction method etc., and the crude oil that these methods are extracted has the shortcomings such as acid value is high, color and luster is dark, impurity is many.
Summary of the invention
In order to overcome above problem, the present invention adopts two step solvent extrations, first uses alcohol extraction rice bran depickling dephosphorization, then extracts Rice bran crude oil by n-hexane extraction method.Alcohol extraction not only can reach the object of depickling, can also remove other impurity, greatly reduces Rice bran crude oil later stage refinement step, saves Financial cost.
The object of the present invention is to provide a kind of low cost, high-level efficiency, and be applicable to the low acid number of suitability for industrialized production and the preparation method of low phosphorus content Rice bran crude oil.
Described method first carries out stabilization treatment to rice bran, then adopts alcohol extraction to carry out depickling dephosphorization to rice bran, then from the rice bran after depickling dephosphorization treatment, extracting Rice bran crude oil.
In one embodiment of the invention, described stabilization treatment adopts medium short wave Infrared Heating stabilization, and wherein equilibrium temperature is 60 ~ 80 DEG C, and steady time is 15 ~ 60min, and material thickness is 3 ~ 8mm.
In one embodiment of the invention, described depickling dephosphorization is in the rice bran after stabilization, adds alcoholic solution and carries out lixiviate, and extracting times is 1 ~ 2 time, and extraction temperature is 0 ~ 40 DEG C, and solid-liquid ratio is 1:3 ~ 1:5, and extraction time is 30 ~ 90min.
In one embodiment of the invention, the ethanol that the alcohol that described alcohol extraction uses is volume fraction is 94-96%.
In one embodiment of the invention, described extraction Rice bran crude oil adopts restricted-access media Rice bran crude oil, and extraction solvent is normal hexane.
In one embodiment of the invention, described extraction Rice bran crude oil adopts normal hexane lixiviate 1 ~ 3 time, and solid-liquid ratio is 1:3 ~ 1:5, and extraction temperature is normal temperature, and extraction time is 1 ~ 3h.
In one embodiment of the invention, described method, specifically comprises the steps:
(1) rice bran stabilization: fresh rice bran is through medium short wave Infrared Heating stabilization, and stable condition is temperature 60 ~ 80 DEG C, and steady time is 15 ~ 60min, and material thickness is 3 ~ 8mm;
(2) rice bran extraction depickling dephosphorization: the rice bran through step (1) stabilizing treatment is mixed with the ethanol of volume fraction 95%, adopt extraction depickling dephosphorization, extracting times is 1 ~ 2 time, extraction temperature is 0 ~ 40 DEG C, solid-liquid ratio is 1:3 ~ 1:5, and extraction time is 30 ~ 90min;
(3) Rice bran crude oil extracts: the raw rice bran after step (2) depickling dephosphorization is at room temperature evaporated and removed residual ethanol, and adopt restricted-access media Rice bran crude oil, extraction solvent is normal hexane; Extracting times is 1 ~ 3 time, and solid-liquid ratio is 1:3 ~ 1:5, and extraction temperature is normal temperature, and extraction time is 1 ~ 3h; Vacuum filtration, vacuum revolves steaming, centrifugal, namely obtains Rice bran crude oil.
Beneficial effect of the present invention:
(1) at present collect from each meter of factory the rice bran being used for extracting Rice bran crude oil, adopt the process of extruding puffing stabilising method more, temperature is close to 120 DEG C, and rice bran quality is destroyed serious, causes the Rice bran crude oil color and luster that extracts dark, is unfavorable for that refining is decoloured.The medium short wave infra-red stabilization rice bran temperature that the present invention adopts is low, destroys little to rice bran quality, and the Rice bran crude oil quality of extraction is better, and the speed of becoming sour of controlled raw rice bran processed.The crude oil of conventional normal hexane extraction, later stage refining procedures include come unstuck, dewax, depickling, the step such as decolouring and deodorization, and the Rice bran crude oil later stage refining that the inventive method obtains only needs to decolour, and greatly reduces refining cost.
(2) present invention process is simple, and production cost is low; The Rice bran crude oil extracted have passed through stabilization treatment due to raw material, its acid number is relatively low, the Rice bran crude oil GB/T5530-2005 prescriptive procedure obtained through above-mentioned steps process measures, and Rice bran crude oil acid value is between 0.5 ~ 4 (KOH) (mg/g); Measure with GB/T5537-2008 prescriptive procedure, phosphorus content is between 50 ~ 130ppm; Thiaminogen content is between 1.8% ~ 2.0%, and tocopherol content, between 880 ~ 900ppm, remains a large amount of nutritive substances.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1
Rice bran crude oil is prepared by following steps:
(1) rice bran stabilization: thin layer fresh rice bran being paved into thickness 5mm, is placed in medium short wave infrared drying oven, and setting equilibrium temperature is 80 DEG C, and heat-up time is 60min.
(2) rice bran extraction depickling dephosphorization: solvent extraction method will be adopted through the rice bran of step (1) stabilization treatment, use Extraction solvent to be 95% (volume) ethanol, extracting times is 1 time, and solid-liquid ratio is 1:3, extraction temperature is 0 DEG C, and extraction time is 30min.
(3) Rice bran crude oil extracts: the dry rice bran 200g after step (2) depickling dephosphorization is placed in 2000mL beaker, extraction temperature is room temperature, solid-liquid ratio is 1:3, extraction time is 2h, extracting times is 2 times, reaction mixture carries out vacuum filtration, and filtrate is carried out vacuum and revolved steaming, centrifugally obtains Rice bran crude oil.
The present embodiment gained Rice bran crude oil GB/T5530-2005 prescriptive procedure measures, and acid value is 2.7 (KOH) (mg/g); Measure with GB/T5537-2008 prescriptive procedure, phosphorus content is 126ppm; Rice bran crude oil extraction yield be 82% (to omit alcohol steep step, crude oil that direct normal hexane extraction obtains for 100%); Thiaminogen component content is 1.9% (the crude oil two-story valley dimension cellulose content that omission alcohol steep step, direct normal hexane extraction obtain is 2.7%); Tocopherol content is 899ppm (in the crude oil that omission alcohol steep step, direct normal hexane extraction obtain, tocopherol content is 1145ppm); Adopt method of the present invention, destroy little to rice bran quality, a large amount of thiaminogen and tocopherol can be retained.
Embodiment 2
Rice bran crude oil is prepared by following steps:
(1) rice bran stabilization: thin layer fresh rice bran being paved into thickness 8mm, is placed in medium short wave infrared drying oven, and setting equilibrium temperature is 80 DEG C, and heat-up time is 60min.
(2) rice bran extraction depickling dephosphorization: solvent extraction method will be adopted through the rice bran of step (1) stabilization treatment, using and extracting reagent is 94% (volume) ethanol, and extracting times is 1 time, and solid-liquid ratio is 1:4, extraction temperature is 40 DEG C, and extraction time is 1h.
(3) Rice bran crude oil extracts: the dry rice bran 200g after step (2) depickling dephosphorization is placed in 2000mL beaker, extraction temperature is room temperature, solid-liquid ratio is 1:3, extraction time is 2h, extracting times is 2 times, reaction mixture carries out vacuum filtration, and filtrate is carried out vacuum and revolved steaming, centrifugally obtains Rice bran crude oil.
The present embodiment gained Rice bran crude oil GB/T5530-2005 prescriptive procedure measures, and acid value is 2.2 (KOH) (mg/g); Measure with GB/T5537-2008 prescriptive procedure, phosphorus content is 68ppm; Rice bran crude oil extraction yield is 80%; Thiaminogen component content is 1.88%; Tocopherol content is 898ppm, remains a large amount of thiaminogen and tocopherol.
Embodiment 3
Rice bran crude oil is prepared by following steps:
(1) rice bran stabilization: thin layer fresh rice bran being paved into thickness 3mm, is placed in medium short wave infrared drying oven, and setting equilibrium temperature is 60 DEG C, and heat-up time is 30min.
(2) rice bran extraction depickling dephosphorization: solvent extraction method will be adopted through the rice bran of step (1) stabilization treatment, using and extracting reagent is 96% (volume) ethanol, and extracting times is 2 times, and solid-liquid ratio is 1:5, extraction temperature is 0 DEG C, and extraction time is 1.5h.
(3) Rice bran crude oil extracts: the dry rice bran 200g after step (2) depickling dephosphorization is placed in 2000mL beaker, extraction temperature is room temperature, solid-liquid ratio is 1:3, extraction time is 2h, extracting times is 2 times, reaction mixture carries out vacuum filtration, and filtrate is carried out vacuum and revolved steaming, centrifugally obtains Rice bran crude oil.
The present embodiment gained Rice bran crude oil GB/T5530-2005 prescriptive procedure measures, and acid value is 1.8 (KOH) (mg/g); Measure with GB/T5537-2008 prescriptive procedure, phosphorus content is 62ppm; Rice bran crude oil extraction yield is 79.2%; Thiaminogen component content is 1.88%; Tocopherol content is 893ppm, remains a large amount of thiaminogen and tocopherol.
Embodiment 4
Rice bran crude oil is prepared by following steps:
(1) rice bran stabilization: thin layer fresh rice bran being paved into thickness 4mm, is placed in medium short wave infrared drying oven, and setting equilibrium temperature is 75 DEG C, and heat-up time is 15min.
(2) rice bran extraction depickling dephosphorization: solvent extraction method will be adopted through the rice bran of step (1) stabilization treatment, using and extracting reagent is 95% (volume) ethanol, and extracting times is 1 time, and solid-liquid ratio is 1:4, extraction temperature is 20 DEG C, and extraction time is 1h.
(3) Rice bran crude oil extracts: the dry rice bran 200g after step (2) depickling dephosphorization is placed in 2000mL beaker, extraction temperature is room temperature, solid-liquid ratio is 1:4, extraction time is 1h, extracting times is 3 times, reaction mixture carries out vacuum filtration, and filtrate is carried out vacuum and revolved steaming, centrifugally obtains Rice bran crude oil.
The present embodiment gained Rice bran crude oil GB/T5530-2005 prescriptive procedure measures, and acid value is 1.0 (KOH) (mg/g); Measure with GB/T5537-2008 prescriptive procedure, phosphorus content is 67ppm; Rice bran crude oil extraction yield is 78.3%; Thiaminogen component content is 1.86%; Tocopherol content is 889ppm, remains a large amount of thiaminogen and tocopherol.
Embodiment 5
Rice bran crude oil is prepared by following steps:
(1) rice bran stabilization: thin layer fresh rice bran being paved into thickness 5mm, is placed in medium short wave infrared drying oven, and setting equilibrium temperature is 80 DEG C, and heat-up time is 60min.
(2) rice bran extraction depickling dephosphorization: solvent extraction method will be adopted through the rice bran of step (1) stabilization treatment, using and extracting reagent is 95% (volume) ethanol, and extracting times is 1 time, and solid-liquid ratio is 1:4, extraction temperature is 30 DEG C, and extraction time is 1h.
(3) Rice bran crude oil extracts: the dry rice bran 200g after step (2) depickling dephosphorization is placed in 2000mL beaker, extraction temperature is room temperature, solid-liquid ratio is 1:5, extraction time is 3h, extracting times is 1 time, reaction mixture carries out vacuum filtration, and filtrate is carried out vacuum and revolved steaming, centrifugally obtains Rice bran crude oil.
The present embodiment gained Rice bran crude oil GB/T5530-2005 prescriptive procedure measures, and acid value is 0.7 (KOH) (mg/g); Measure with GB/T5537-2008 prescriptive procedure, phosphorus content is 55ppm; Rice bran crude oil extraction yield is 78.2%; Thiaminogen component content is 1.85%; Tocopherol content is 883ppm, remains a large amount of thiaminogen and tocopherol.
Embodiment 6: extracting method is on the impact of Rice bran crude oil quality
(1) conventional n-hexane extraction method:
The step of conventional normal hexane extraction method is: the rice bran of infra-red stabilization directly uses n-hexane extraction, and extraction times is 2 times, and solid-liquid ratio is 1:3, and extraction time is 2h/ time.
The crude oil acid value extracted by the present invention is 21.5 (KOH) (mg/g); Phosphorus content is 299ppm; Rice bran crude oil color and luster Huang 40, red 4.6, blue 3.Later stage refining procedures include come unstuck, dewax, depickling, decolouring, the step such as deodorization.And the Rice bran crude oil color and luster Huang 31 that embodiment 1-5 method obtains, red 4.1, blue 1, later stage refining only has decolouring, greatly reduces refining cost.
(2) stabilization method is on the impact of Rice bran crude oil quality
The most general method of current rice bran stabilization is that microwave and extruding puffing are stablized, and invention has been the control experiment that rice bran microwave is stable.Concrete steps are as follows: fresh rice bran bed thickness 5mm, microwave power 900w, microwave time 90s, and the crude oil acid value that under this condition, the rice bran of stabilization directly adopts n-hexane extraction to obtain is 22.4 (KOH) (mg/g); Phosphorus content 302ppm; Crude oil color and luster Huang 66, red 7, blue 4, illustrates rice bran seriously brown stain.As can be seen here, the stabilization method of this research has obvious advantage.
(3) alcoholic solution is on the impact of Rice bran crude oil quality
Adopt the ethanol of in Virahol, dehydrated alcohol, 90% ethanol replacement embodiment 1 95% to carry out rice bran depickling dephosphorization respectively, other steps and embodiment 1 are consistent.Found that, the loss of isopropanol extraction process crude oil is serious, dehydrated alcohol extraction rate only has 33%, 90% ethanol oil extracting rate to only have 57%.
Although the present invention with preferred embodiment openly as above; but it is also not used to limit the present invention, any person skilled in the art, without departing from the spirit and scope of the present invention; all can do various changes and modification, what therefore protection scope of the present invention should define with claims is as the criterion.
Claims (9)
1. the preparation method of a low acid number and low phosphorus content Rice bran crude oil, it is characterized in that, described method first carries out stabilization treatment to rice bran, then adopts alcohol extraction to carry out depickling dephosphorization to rice bran, then extract Rice bran crude oil from the rice bran after depickling dephosphorization treatment.
2. method according to claim 1, is characterized in that, the ethanol that the alcohol that described alcohol extraction uses is volume fraction is 94-96%.
3. method according to claim 1, is characterized in that, described depickling dephosphorization is in the rice bran after stabilization, add alcoholic solution and carry out lixiviate, extracting times is 1 ~ 2 time, and extraction temperature is 0 ~ 40 DEG C, solid-liquid ratio is 1:3 ~ 1:5, and extraction time is 30 ~ 90min.
4. method according to claim 1, is characterized in that, described stabilization treatment, is to adopt medium short wave Infrared Heating stabilization, and wherein equilibrium temperature is 60 ~ 80 DEG C, and steady time is 15 ~ 60min, and material thickness is 3 ~ 8mm.
5. method according to claim 1, is characterized in that, described extraction Rice bran crude oil adopts normal hexane restricted-access media Rice bran crude oil.
6. method according to claim 1, is characterized in that, the extraction solvent of described extraction Rice bran crude oil is normal hexane, and extracting times is 1 ~ 3 time, and solid-liquid ratio is 1:3 ~ 1:5, and extraction temperature is normal temperature, and extraction time is 1 ~ 3h.
7. method according to claim 1, is characterized in that, described method specifically comprises the steps:
(1) rice bran stabilization: fresh rice bran is through medium short wave Infrared Heating stabilization, and stable condition is temperature 60 ~ 80 DEG C, and steady time is 15 ~ 60min, and material thickness is 3 ~ 8mm;
(2) rice bran extraction depickling dephosphorization: the rice bran through step (1) stabilizing treatment is mixed with the ethanol of volume fraction 95%, adopt extraction depickling dephosphorization, extracting times is 1 ~ 2 time, extraction temperature is 0 ~ 40 DEG C, solid-liquid ratio is 1:3 ~ 1:5, and extraction time is 30 ~ 90min;
(3) Rice bran crude oil extracts: the raw rice bran after step (2) depickling dephosphorization is at room temperature evaporated and removed residual ethanol, and adopt restricted-access media Rice bran crude oil, extraction solvent is normal hexane; Extracting times is 1 ~ 3 time, and solid-liquid ratio is 1:3 ~ 1:5, and extraction temperature is normal temperature, and extraction time is 1 ~ 3h; Vacuum filtration, vacuum revolves steaming, centrifugal, namely obtains Rice bran crude oil.
8. according to the Rice bran crude oil that the arbitrary described method of claim 1-7 obtains.
9. the application of Rice bran crude oil described in claim 8 in food, health care.
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| CN108342247A (en) * | 2018-04-11 | 2018-07-31 | 安徽德运粮油有限公司 | A kind of method of three phase separation aqueous enzymatic extraction rice bran oil |
| CN109221871A (en) * | 2018-10-24 | 2019-01-18 | 南京财经大学 | A kind of method of infra-red radiation auxiliary rice bran fast and stable |
| CN115975719A (en) * | 2023-02-21 | 2023-04-18 | 江苏得乐康生物科技有限公司 | Crude oil extraction process of rice bran |
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Application publication date: 20160113 |