CN102397777B - Preparation method of activated rice husk ash and application of activated rice husk ash to purification of biodiesel - Google Patents
Preparation method of activated rice husk ash and application of activated rice husk ash to purification of biodiesel Download PDFInfo
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- CN102397777B CN102397777B CN2011103045388A CN201110304538A CN102397777B CN 102397777 B CN102397777 B CN 102397777B CN 2011103045388 A CN2011103045388 A CN 2011103045388A CN 201110304538 A CN201110304538 A CN 201110304538A CN 102397777 B CN102397777 B CN 102397777B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses a preparation method of activated rice husk ash. The method comprises the following steps: 1) hydrochloric acid immersion: immersing the rice husk ash with 3mol/L hydrochloric acid for 2-6 h; 2) washing and draining: washing to neutral and draining; 3) high temperature treatment: sintering at 500-600 DEG C for 2-8 h to obtain the activated rice husk ash. The method of the invention is simple, and prepared activated rice husk ash has large specific surface area, strong adsorption capability and low cost. The invention also discloses application of the prepared activated rice husk ash to purification of biodiesel. Applied to purification of biodiesel, the activated rice husk ash has advantages of simple equipment, easy operation, zero washing, waste water discharge reduction and environmental pollution reduction.
Description
Technical field
The invention belongs to technical field of biochemical industry, be specifically related to a kind of preparation method and application in purifying biological diesel oil thereof that activates rice hull ash.
Background technology
At present, often take vegetable oil, animal tallow as raw material, adopt homogeneous phase base-catalyzed transesterification reaction preparation biodiesel.The method has advantages of the reaction condition gentleness, the production time is shorter, productive rate is higher.But the homogeneous phase base catalysis prepares biodiesel and also has some problems.Such as, produced soap in ester-exchange reaction; Especially when using the higher raw material of free fatty acid content, also produced simultaneously the by-product glycerin of ester exchange.And the residual biodiesel that soap and dissociative glycerin are arranged can have a strong impact on the normal operation of diesel engine when burning, even greatly shortens its working life.Therefore, the quality standard that biodiesel is relevant has strictly limited the residual quantity of soap and dissociative glycerin.
Be the requirement that biodiesel is reached quality standards, need to carry out purification process to biodiesel.Publication number is that the Chinese patent application of CN101735845A discloses with thin film evaporator biodiesel coarse product is carried out degassed and distillation procedure, obtains coarse biodiesel; The coarse biodiesel product that again separation is obtained carries out the alkaline earth depickling, obtains the purifying biological diesel oil that acid number meets national standard.Its alkaline earth deacidification agent used is by alkaline Peng Run soil or zeolite powder and a certain amount of Na
2CO3, NaHCO3, Na
2The saturated solution of SO4, NaOH, KOH etc. mixes under heat-retaining condition and gets.Publication number is that the Chinese patent application of CN101475824 has been described a kind of method for preparing biodiesel for the higher feedstock oil of acid number.Then free fatty in the first separate raw materials oil of the method carries out acid esters reaction and ester exchange reaction to aliphatic acid and triglycerides after separating respectively, and system is to coarse biodiesel.With the method for adsorption filtration, coarse biodiesel is made with extra care again.It is sorbent used is the atlapulgite of 2%-7%.Publication number is that the Chinese patent application of CN101939068A has been described the method for using the adsorbent purifying biological diesel oil of powder, granular or extruding.Adsorbent used comprises the bleaching clay of charcoal, silica, zeolite, metal silicate, bleaching clay or activation.In addition, the method is to come purifying biological diesel oil with the adsorption column system.The patent No. is that 4629588 United States Patent (USP) has been described the various forms of adsorbents of use silica, as the film of silica gel, precipitated silica, silica, the purified monoglycerides such as silica of calcining, to remove phosphatide in glyceride, metal ion etc.Although these methods have effect preferably to purifying biological diesel oil, or purification step is complicated, and the adsorbent cost that perhaps uses is higher.
Publication number is that the Chinese patent application of CN101457176 has been described and used rice hull ash the feedstock oil as production of biodiesel to be carried out the method for purifying.The object of its purifying is mainly free fatty, phosphatide, carrotene, sterol, protein, amino acid and vitamin, does not mention the purifying to dissociative glycerin.And the rice hull ash of using is not activated, and specific area is less, and adsorption capacity is limited.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of activation rice hull ash simple and convenient, with low cost.The activation rice hull ash specific area of preparation is large, high adsorption capacity.
Another technical problem to be solved by this invention is to provide a kind of application process of rice hull ash in purifying biological diesel oil that activate.
For solving first technical problem of the present invention, the technical solution used in the present invention comprises the steps:
1) salt acid soak: first with the salt acid soak 2-6h of rice hull ash with 3mol/L;
2) washing drains: then be washed to neutrality and drain;
3) high-temperature process: namely get the activation rice hull ash again after firing 2-8h at 500-600 ℃ of temperature.
For solving second technical problem of the present invention, the technical solution used in the present invention comprises following technical step:
1) absorption: will activate rice hull ash and add in biodiesel, absorption soap and dissociative glycerin wherein;
2) separate: have the activation rice hull ash of soap and dissociative glycerin to separate with biodiesel absorption, get purifying biological diesel oil.
For solving second technical problem of the present invention, also can adopt following technical scheme:
1) composite: one or more that will activate rice hull ash and silica gel, active carbon, atlapulgite, aluminium oxide, diatomite, white carbon are composite, and the content that makes the activation rice hull ash gets composite activation rice hull ash more than 50%;
2) absorption: composite activation rice hull ash is added in biodiesel absorption soap and dissociative glycerin wherein;
3) separate: have the composite activation rice hull ash of soap and dissociative glycerin to separate with biodiesel absorption, get purifying biological diesel oil.
Further, in described adsorption step, the temperature of material is 30-120 ℃, and mixing speed is 100-3000r/min, and adsorption time is 5-120min, and the adsorbent addition is the 1%-5% of biodiesel weight.
Further, described separating step adopts centrifugal or isolated by filtration mode.
Beneficial effect of the present invention is:
1) rice husk is the accessory substance of rice processing, and rice hull ash is the waste material after rice husk is used for burning boiler, the preparation activation rice hull ash take rice hull ash as raw material, and raw material sources are extensive, and are with low cost.Activated make the activation rice hull ash after, the unburned further carbonization of organic matter completely in rice hull ash, specific area also significantly improves, adsorption capacity is enhanced.
2) with being used for the purifying of biodiesel after rice hull ash activation preparation activation rice hull ash, not only solved a waste disposal difficult problem, and can be enterprise and the considerable economic worth of social creativity.
3) adopt that purification via adsorption-based process biodiesel equipment is simple, processing ease; Need not washing, reduced discharge of wastewater and environmental pollution.
The specific embodiment
The following stated embodiment understands the present invention in detail.
Embodiment 1
Take the 500g rapeseed oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2928ppm, and free glycerol content is 0.29%).
Rice hull ash is first used the salt acid soak 2h of 3mol/L; Then be washed to neutrality and drain; Obtain activating rice hull ash after firing 6h at 550 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 278m
2/ g.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 40 ℃, then add oil to weigh 2% activation rice hull ash; Mixing speed is to adsorb 20min under the condition of 3000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 62ppm, and the dissociative glycerin residual quantity is 0.05%).
Embodiment 2
Take the 500g soybean oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute ethyl alcohol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methacrylate layer in separatory funnel is isolated methacrylate layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2588ppm, and free glycerol content is 0.25%).
Rice hull ash is first used the salt acid soak 6h of 3mol/L; Then be washed to neutrality and drain; Obtain activating rice hull ash after firing 6h at 600 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 289m
2/ g.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 30 ℃, then add oil to weigh 1% activation rice hull ash; Mixing speed is to adsorb 40min under the condition of 2000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 370ppm, and the dissociative glycerin residual quantity is 0.11%).
Embodiment 3
Take the 500g rapeseed oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2928ppm, and free glycerol content is 0.29%).
Rice hull ash is first used the salt acid soak 4h of 3mol/L; Then be washed to neutrality and drain; Obtain activating rice hull ash after firing 3h at 500 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 263m
2/ g.To activate rice hull ash and atlapulgite is composite, and get composite activation rice hull ash, the weight that wherein activates rice hull ash accounts for 60% of composite activation rice hull ash gross weight.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 80 ℃, then add oil to weigh 5% composite activation rice hull ash; Mixing speed is to adsorb 100min under the condition of 1000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (soap residual quantity and dissociative glycerin residual quantity all do not detect).
Embodiment 4
Take 500g lard in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2163ppm, and free glycerol content is 0.26%).
Rice hull ash is first used the salt acid soak 2h of 3mol/L; Then be washed to neutrality and drain; Obtain activating rice hull ash after firing 6h at 550 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 278m
2/ g.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 120 ℃, then add oil to weigh 2% activation rice hull ash; Mixing speed is to adsorb 120min under the condition of 300r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 187ppm, and the dissociative glycerin residual quantity is 0.07%).
Embodiment 5
Take the 500g cottonseed oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 3165ppm, and free glycerol content is 0.31%).
Rice hull ash is first used the salt acid soak 5h of 3mol/L; Then be washed to neutrality and drain; Obtain activating rice hull ash after firing 2h at 600 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 291m
2/ g.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 100 ℃, then add oil to weigh 1% activation rice hull ash; Mixing speed is to adsorb 60min under the condition of 1000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 493ppm, and the dissociative glycerin residual quantity is 0.12%).
Embodiment 6
Take the 500g soybean oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2588ppm, and free glycerol content is 0.25%).
Rice hull ash is first used the salt acid soak 3h of 3mol/L; Then be washed to neutrality and drain; Obtain activating rice hull ash after firing 4h at 500 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 272m
2/ g.To activate rice hull ash and white carbon and atlapulgite composite, get composite activation rice hull ash, wherein activate rice hull ash weight and account for 50% of composite activation rice hull ash gross weight, white carbon weight accounts for 20% of composite activation rice hull ash gross weight, and atlapulgite weight accounts for 30% of composite activation rice hull ash gross weight.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 30 ℃, then add oil to weigh 3% composite activation rice hull ash; Mixing speed is to adsorb 120min under the condition of 100r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 15ppm, and the dissociative glycerin residual quantity is 0.02%).
Embodiment 7
Take the 500g soybean oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2588ppm, and free glycerol content is 0.25%).
Rice hull ash is first used the salt acid soak 6h of 3mol/L; Then be washed to neutrality; Obtain activating rice hull ash after firing 8h at 600 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 296m
2/ g.To activate rice hull ash and white carbon and atlapulgite composite, get composite activation rice hull ash, wherein activate rice hull ash weight and account for 70% of composite activation rice hull ash gross weight, white carbon weight accounts for 20% of composite activation rice hull ash gross weight, and atlapulgite weight accounts for 10% of composite activation rice hull ash gross weight.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 50 ℃, then add oil to weigh 5% composite activation rice hull ash; Mixing speed is to adsorb 60min under the condition of 1500r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (soap residual quantity and dissociative glycerin residual quantity all do not detect).
Embodiment 8
Take 500g lard in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2163ppm, and free glycerol content is 0.26%).
Rice hull ash is first used the salt acid soak 3h of 3mol/L; Then be washed to neutrality; Obtain activating rice hull ash after firing 6h at 500 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 270m
2/ g.To activate rice hull ash and white carbon, atlapulgite, silica gel and diatomite composite, get composite activation rice hull ash, wherein activate rice hull ash weight and account for 50% of composite activation rice hull ash gross weight, white carbon weight accounts for 20% of composite activation rice hull ash gross weight, atlapulgite weight accounts for 10% of composite activation rice hull ash gross weight, silica gel weight accounts for 10% of composite activation rice hull ash gross weight, and diatomite weight accounts for 10% of composite activation rice hull ash gross weight.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 90 ℃, then add oil to weigh 4% composite activation rice hull ash; Mixing speed is to adsorb 80min under the condition of 2000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (soap residual quantity and dissociative glycerin residual quantity all do not detect).
Embodiment 9
Take the 500g rapeseed oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 2928ppm, and free glycerol content is 0.29%).
Rice hull ash is first used the salt acid soak 4h of 3mol/L; Then be washed to neutrality; Obtain activating rice hull ash after firing 3h at 600 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 283m
2/ g.Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 30 ℃, then add oil to weigh 1% activation rice hull ash; Mixing speed is to adsorb 30min under the condition of 1000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 287ppm, and the dissociative glycerin residual quantity is 0.07%).
Embodiment 10
Take the 500g cottonseed oil in beaker, put into the heat-collecting magnetic stirring device and be preheated to 50 ℃.Be to measure absolute methanol at 6: 1 by molar ratio of methanol to oil, add oil to weigh 1% NaOH, fully stir, NaOH is dissolved fully.The methanol solution that then will be dissolved with NaOH slowly adds oil under stirring condition in, reaction 1h.After reaction is completed, change the mixed solution in beaker over to separatory funnel standing.Methyl esters layer in separatory funnel is isolated the methyl esters layer with after glycerin layer is separated fully, namely obtains rough biodiesel (soap content is 3165ppm, and free glycerol content is 0.31%).
Rice hull ash is first used the salt acid soak 3h of 3mol/L; Then be washed to neutrality; Obtain activating rice hull ash after firing 7h at 500 ℃ of temperature.Specific area with the rear rice hull ash of activation before activation is respectively 115m
2/ g and 267m
2/ g.To activate rice hull ash and white carbon, atlapulgite and aluminium oxide composite, get composite activation rice hull ash, wherein activate rice hull ash weight and account for 60% of composite activation rice hull ash gross weight, white carbon weight accounts for 20% of composite activation rice hull ash gross weight, atlapulgite weight accounts for 10% of composite activation rice hull ash gross weight, alumina weight accounts for 10% of composite activation rice hull ash gross weight.
Take the rough biodiesel of 50g and be placed in beaker, put into constant temperature blender with magnetic force and be preheated to 50 ℃, then add oil to weigh 3% composite activation rice hull ash; Mixing speed is to adsorb 40min under the condition of 2000r/min; Then filter out spent sorbents and obtain purifying biological diesel oil (the soap residual quantity is 13ppm, and the dissociative glycerin residual quantity is 0.03%).
Claims (4)
1. one kind activates the application of rice hull ash in purifying biological diesel oil, and it is characterized in that: it comprises the following steps:
1) absorption: will activate rice hull ash and add in biodiesel, absorption soap and dissociative glycerin wherein;
2) separate: have the activation rice hull ash of soap and dissociative glycerin to separate with biodiesel absorption, get purifying biological diesel oil;
Described activation rice hull ash adopts following method to prepare:
A) salt acid soak: first with the salt acid soak 2-6h of rice hull ash with 3mol/L;
B) washing drains: then be washed to neutrality and drain;
C) high-temperature process: namely get the activation rice hull ash again after firing 2-8h at 500-600 ℃ of temperature.
2. the application of activation rice hull ash according to claim 1 in purifying biological diesel oil, it is characterized in that: it comprises the following steps:
1) composite: one or more that will activate rice hull ash and silica gel, active carbon, atlapulgite, aluminium oxide, diatomite, white carbon are composite, and the content that makes the activation rice hull ash gets composite activation rice hull ash more than 50%;
2) absorption: composite activation rice hull ash is added in biodiesel absorption soap and dissociative glycerin wherein;
3) separate: have the composite activation rice hull ash of soap and dissociative glycerin to separate with biodiesel absorption, get purifying biological diesel oil.
3. the application of activation rice hull ash according to claim 1 and 2 in purifying biological diesel oil, it is characterized in that: in described adsorption step, the temperature of material is 30-120 ℃, mixing speed is 100-3000r/min, adsorption time is 5-120min, and the adsorbent addition is the 1%-5% of biodiesel weight.
4. the application of activation rice hull ash according to claim 1 and 2 in purifying biological diesel oil is characterized in that: described separating step adopts centrifugal or isolated by filtration mode.
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| CN103908946B (en) * | 2013-01-07 | 2018-04-06 | 丰益(上海)生物技术研发中心有限公司 | A kind of mixed adsorbent, grease and preparation method thereof |
| CN104119948B (en) * | 2013-04-23 | 2016-08-03 | 中国石油化工股份有限公司 | A kind of method of biodiesel imurity-removal |
| CN103949211A (en) * | 2014-04-03 | 2014-07-30 | 安庆师范学院 | Method for producing adsorbent by using rice hull ash and application thereof |
| CN104531350B (en) * | 2014-12-05 | 2017-10-27 | 昆明理工大学 | A kind of method for purifying biodiesel |
| CN105524644B (en) * | 2016-01-15 | 2017-08-25 | 广西阔能霸能源科技开发有限责任公司 | A kind of synthetic method of biodiesel |
| CN105969419B (en) * | 2016-01-15 | 2018-10-26 | 浙江海鸿工业产品设计有限公司 | A kind of preparation method of high-quality biodiesel |
| CN108905982A (en) * | 2018-07-18 | 2018-11-30 | 广西南宁荣威德新能源科技有限公司 | It is a kind of for removing the preparation method of the adsorbent of aflatoxin in peanut oil |
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