CN113292626B - Rice bran oil oryzanol production process - Google Patents
Rice bran oil oryzanol production process Download PDFInfo
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- CN113292626B CN113292626B CN202110749061.8A CN202110749061A CN113292626B CN 113292626 B CN113292626 B CN 113292626B CN 202110749061 A CN202110749061 A CN 202110749061A CN 113292626 B CN113292626 B CN 113292626B
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- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
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Abstract
The invention belongs to the technical field of rice bran oil production, in particular to a rice bran oil oryzanol production process, which combines a physical process with a process for extracting oryzanol by a solvent method, so that the yield of refined rice bran oil is improved compared with that of an alkali-dissolving and acid-separating method, the traditional saponification is carried out at high temperature for a long time, the traditional saponification causes oryzanol hydrolysis, and the yield is reduced. The crude rice bran oil must be alkali-refined by complex alkali liquor in the past, so that the main oryzanol of the oil is enriched in the secondary alkali-refined soapstock, the invention does not use complex alkali liquor for treatment, the pollution degree of the production to the environment is greatly reduced, the total yield of the oryzanol is improved by solvent extraction, the high-quality product standard is reached, the production cost of the oryzanol is greatly reduced, the limited raw rice bran oil material is fully utilized, and the economic benefit is higher.
Description
Technical Field
The invention belongs to the technical field of rice bran oil production, and particularly relates to a production process of rice bran oil oryzanol.
Background
According to data issued by the national statistical bureau, the Chinese rice yield in 2018 is 19330 ten thousand tons, the rice bran yield is 7 percent, and the rice bran yield in the country is 1353.1 ten thousand tons. The rice bran contains 64 percent of important nutrient components of rice and more than 90 percent of essential elements of human bodies, so the rice bran is called as 'natural nutrient treasury', and is a byproduct resource with wide development value. Wherein the rice bran oil has effects of reducing old sterol, resisting hyperlipemia, resisting oxidation and cancer, and maintaining health; the rice bran phytic acid has good oxidation resistance, is safe and nontoxic, and has antistatic capability; many studies have shown that oryzanol prevents vegetative nerve functional disorders and endocrine disorders. The phytosterol part in oryzanol also has the function of inhibiting the absorption of cholesterol, and the ferulic acid has the function of promoting the function of gallbladder. The comprehensive expression effect of each component is that the oryzanol reduces the level of liver lipid, lipid peroxide, low-density lipoprotein cholesterol and very low-density lipoprotein cholesterol in serum, increases the content of high-density lipoprotein cholesterol, hinders the cholesterol from depositing on the artery wall, and reduces the cholelithiasis formation index. Oryzanol is a ferulic acid ester mixture which takes triterpene alcohol as a main component in Amelanchier oil, and has the functions of regulating autonomic nerve dysfunction and endocrine balance disorder. At present, oryzanol is mainly extracted from crude bran oil, and the oryzanol content in the crude bran oil is as high as 1.8-3.0%. Because the oryzanol has the similar properties with phenols, is easy to be absorbed by alkaline soapstock, and also has the characteristics of alkali dissolution and acid precipitation in methanol solution, the oryzanol is mainly extracted from the raw bran oil industrially by utilizing the properties, and the method mainly comprises a secondary alkali refining method, an acidification distillation separation method, a weak acid substitution method, a methanol extraction method, a nonpolar solvent extraction method and the like. The yield of the oryzanol by the acidification distillation separation method is low, the production period is long, the process is complex, the extraction rate of the oryzanol by the weak acid substitution method is low and is only 1/3, the high-acid rice bran oil is not applicable, the methanol extraction is realized, the methanol consumption is high, and the recovery process is complicated. The development of a rice bran oil oryzanol production process is urgently needed by the technical personnel in the field to meet the existing market demand.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a rice bran oil oryzanol production process.
The invention is realized by the following technical scheme:
a production process of rice bran oil oryzanol comprises the following steps:
the method adopts ion exchange resin alkali refining, is a physical refining process, not only improves the yield of finished oil, but also effectively protects the physiological active substances in the oil, such as oryzanol, vitamin E and the like.
(1) Pumping the crude rice bran oil into an exchange resin alkali refining pot, stirring at a speed of 150-200 rpm quickly, heating to 60 ℃, stopping heating, uniformly adding strong-base styrene anion exchange resin with the mass of 30-35% of that of the crude rice bran oil for 10-15 minutes under quick stirring, stirring for reaction for 8-10 hours, heating to 55-60 ℃, preserving heat for reaction for 1-2 hours, filtering, and collecting saponin for later use; the ion exchange resin can remove part of free fatty acid in the raw bran oil, reduce the acid value, and simultaneously remove the impurities such as phospholipid, colloid and the like in the oil, thereby being beneficial to trapping the oryzanol.
(2) Supplementary saponification: stirring and heating the soapstock to 50-55 ℃, uniformly adding alkali liquor with the mass of 10-15% of that of the anion exchange resin, continuously heating to 90-95 ℃, stirring and saponifying for 1-2 hours, and filtering to obtain filter residue;
the soapstock is a mixture of fatty acid sodium salt, neutral oil, free alkali and water, and is easy to delaminate when being statically stored, so that the uniformity of the next procedure is influenced, and the operation is difficult. Therefore, a saponification method of supplementing a little alkali liquor is adopted, which is beneficial to production;
(3) placing filter residues into a reaction kettle, adding a liquid-liquid extraction solvent, wherein the liquid-liquid extraction solvent is a mixed liquid of ethylene glycol monomethyl ether-methanol-water, the mass contents of the ethylene glycol monomethyl ether, the methanol and the water are 61-65%, 25-29% and 10% respectively, separating oryzanol in a liquid phase, stirring at a stirring speed of 150-200 rpm in the reaction kettle, heating to dissolve, heating to 65-70 ℃, keeping the temperature, continuing stirring and refluxing for 20-30 minutes, stopping the reaction, slowly cooling the saponified liquid to 45-50 ℃ by using cooling water, performing vacuum suction filtration, and pumping the filtrate into an acidification reaction kettle to obtain an extractant mother liquid; (4) storing the extractant mother liquor in an acid precipitation reaction kettle, heating the extractant mother liquor under the condition of continuously stirring at 150-200 rpm, dropwise adding a dilute hydrochloric acid mixed solution to adjust the pH to 6.8-7 when the temperature rises to 40-45 ℃, dropwise adding acetic acid with the mass fraction of 2-3% when the temperature rises to 50 ℃, heating the mixture to 60 ℃, reacting for 30 minutes, adjusting the pH to 6.5-6.7, stopping heating, extracting the oryzanol to return to ethylene glycol monomethyl ether, desolventizing the ethylene glycol monomethyl ether phase to obtain a oryzanol concentrate, and performing resin gel permeation, wherein the volume of the oryzanol concentrate is 60-70 times that of the resin gel, and the pH is 6.5-6.7;
(4) extracting oryzanol from rice bran oil soapstock by liquid-liquid extraction, resin gel permeation, elution, washing and refining. The liquid-liquid extraction solvent is used for separating oryzanol in a liquid phase, neutralizing with hydrochloric acid and acetic acid to obtain oryzanol concentrate, and then performing resin gel permeation and elution refining;
(5) and (3) elution and refining: eluting with acidic methanol with the pH of 2-3 for 12-24 h, volatilizing the solvent, crushing, sieving with a 12-mesh sieve, washing with distilled water at 80 ℃ for several times to remove inorganic salt impurities until the washed oryzanol has no salty taste;
the crude oryzanol contains impurities such as lipid, pigment and inorganic salt, and is refined by washing, crystallization and purification;
(6) and (3) crushing the filtered oryzanol, sieving the oryzanol with a 12-mesh sieve, loading the oryzanol into a drying chamber, controlling the thickness of the oryzanol powder in the plate to be 2-3 cm, controlling the drying temperature to be 75-80 ℃ and the drying time to be 8 hours, and drying to obtain the oryzanol.
Further, the alkali liquor in the step (2) is a sodium hydroxide solution with the mass fraction of 15-20%.
Further, resin gel permeation is adopted in the step (4), wherein the volume of the oryzanol concentrate is 60-70 times of the volume of the resin gel, and the pH value is 6.5-6.7. Further, the dilute hydrochloric acid mixed solution in the step (4) is a methanol-25% hydrochloric acid solution.
The invention has the beneficial effects that:
the invention adopts ion exchange resin and resin gel permeation to adsorb oryzanol by using an adsorption principle and then elute the oryzanol by using a solvent, thereby purifying the oryzanol, being easy to manufacture into an adsorption column, simultaneously being difficult to deteriorate, having quite strong adsorption capacity and being convenient for regeneration. The crude bran oil is treated with ion exchange resin to remove fatty acids, at which point the oryzanol concentration is concentrated to about 3.5%, while adsorption is performed, to extract the oryzanol from the rice bran oil soapstock in a four-step process comprising liquid-liquid extraction, resin gel permeation, crystallization and recrystallization. Extracting solvent with liquid-liquid to obtain refined oryzanol product. The basic ion exchange resin treatment of the oil soapstock is less likely to occur, and the conventional saponification is carried out at a high temperature for a long time, which causesOryzanol is hydrolyzed, thereby reducing its yield, so that the degradation of oryzanol is minimized during processing. The crude rice bran oil must be alkali-refined by complex secondary alkali liquor to enrich the essential oryzanol in the secondary alkali-refined soapstock, the invention is not used, the alkali refining is carried out by adopting strong-base anion exchange resin, and the anion exchange resin carries exchangeable OH - Can release OH - The ion can reach the purpose of deacidification, simultaneously has certain impurity adsorption effect, simplifies the operation, has no waste liquid discharge, and can regenerate and reuse the ion exchange resin.
Compared with the prior art, the invention has the following advantages:
the invention combines the physical process with the solvent method extraction oryzanol production process, so that the yield of refined rice bran oil is improved compared with the alkali dissolution and acidification method, the production process of the alkali dissolution and acidification method comprises the first step of alkali refining, alkali dissolution, filtration and recovery, and the waste materials such as oil residue, lipid, fatty acid and the like are discharged in multiple processes, and the waste materials are processed into useful fatty acid, and a large amount of inorganic acid and alkali are consumed, so that certain environmental pollution is caused. The solvent extraction method production process adopts an advanced physical refining deacidification process on oil refining, so that alkali refining oil residue is not generated, and oryzanol is extracted without removing lipid and black fatty acid, so that the pollution of production to the environment is basically eliminated. The yield of refined rice bran oil is improved compared with that of an alkali-dissolving and acid-separating method, the traditional saponification is carried out at high temperature for a long time, the traditional saponification causes the hydrolysis of oryzanol, and the yield is reduced. The crude rice bran oil must be alkali-refined by complex alkali liquor in the past, so that the main oryzanol of the oil is enriched in the secondary alkali-refined soapstock, the invention does not use complex alkali liquor for treatment, the pollution degree of the production to the environment is greatly reduced, the total yield of the oryzanol is improved by solvent extraction, the high-quality product standard is reached, the production cost of the oryzanol is greatly reduced, the limited raw rice bran oil material is fully utilized, and the economic benefit is higher.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
The crude rice bran oil is obtained by removing impurities, degumming and decoloring, and is a product in the Dongbo rice industry of Anhui, wherein the crude rice bran oil contains 0.6% of impurities, 3.6mgKOH/g of acid value, 0.38% of water, 35% of yellow (25.4 mm groove), 4.0% of red, 2.8meq/kg of peroxide value and 1.93% of oryzanol. The method comprises the following steps: (1) pumping the crude rice bran oil into an exchange resin alkali refining pot, stirring at a speed of 150rpm quickly, heating to 60 ℃, stopping heating, uniformly adding Amberlite IRA400 strongly basic styrene anion exchange resin with the mass of 30% of the crude rice bran oil for 10 minutes under the condition of quick stirring, stirring for reaction for 8 hours, heating to 55 ℃, carrying out heat preservation reaction for 1 hour, filtering, and collecting saponin for later use; (2) supplementary saponification: stirring and heating the soapstock to 50 ℃, uniformly adding an alkali solution with the mass percent of 15% of that of the anion exchange resin, namely a sodium hydroxide solution, continuously heating to 90 ℃, stirring and saponifying for 1 hour, filtering to obtain filter residue, and detecting to obtain the oryzanol content of 1.79%, wherein the loss of the oryzanol content is less in the treatment process; (3) placing filter residues in a reaction kettle, adding a liquid-liquid extraction solvent, wherein the liquid-liquid extraction solvent is a mixed solution of ethylene glycol monomethyl ether, methanol and water, the mass contents of the ethylene glycol monomethyl ether, the methanol and the water are 65%, 25% and 10% respectively, separating oryzanol in a liquid phase, stirring at the speed of 150rpm in the reaction kettle, heating to 65 ℃, stopping heating, keeping the temperature, performing reflux reaction for 20 minutes while continuing stirring, stopping heating, sampling to determine that the pH value is 9, then slowly cooling the saponified solution to 50 ℃ by using cooling water, performing vacuum suction filtration, and pumping the filtrate into an acidification reaction kettle to obtain an extractant mother solution; (4) storing the extractant mother liquor in an acid-out reaction kettle, heating gradually under the condition of continuously stirring at 150rpm, when the temperature rises to 45 ℃, dropwise adding a dilute hydrochloric acid methanol-25% hydrochloric acid solution to adjust the pH to 6.8, when the temperature rises to 50 ℃, dropwise adding acetic acid with the mass fraction of 2%, wherein the acetic acid is one fourth of the amount of the dilute hydrochloric acid, heating to 60 ℃, reacting for 30 minutes, adjusting the pH to 6.5, stopping heating, extracting oryzanol to return to ethylene glycol monomethyl ether, desolventizing the ethylene glycol monomethyl ether phase to obtain a oryzanol concentrate, and permeating by adopting Toyopearl HW-40C resin gel, wherein the volume of the oryzanol concentrate is 60 times that of the resin gel, and the pH is 6.5; (5) and (3) elution and refining: eluting with acidic methanol with pH of 2 for 12h, washing with 70% hot methanol solution for several times, volatilizing solvent, crushing, sieving with 12 mesh sieve, washing with 80 deg.C distilled water for several times to remove inorganic salt impurities until no salt taste of oryzanol is obtained; (6) and (3) crushing the filtered oryzanol, sieving the oryzanol with a 12-mesh sieve, loading the oryzanol into a drying chamber, controlling the thickness of the oryzanol powder in the plate to be 2 cm, controlling the drying temperature to be 75 ℃ and the drying time to be 8 hours, and drying to obtain the oryzanol.
The product quality is as follows: the oryzanol content is more than 98%, the color is white, the volatile matter is less than 1%, the ash content is less than 0.3%, and the methoxyl group value is 4.99.
Example 2
A rice bran oil oryzanol production process, the rice bran oil is to remove miscellaneous, come unstuck, decolorize and get crude rice bran oil, crude rice bran oil is to Anhui Dongbo rice industry, wherein crude rice bran oil impurity 0.5%, acid number 3.4mgKOH/g, water 0.38%, color (25.4 mm trough) yellow 35, red 4.0, peroxide number 3.2meq/kg, oryzanol content 1.91%, (1) pump crude rice bran oil into exchange resin alkali-refining pot, stir fast 200rpm and heat up to 60 duC, stop heating up, add crude rice bran oil quality 35% Amberlite eIRA strong base 400 styrene anion exchange resin under fast stirring for 10 minutes, heat up to 60 duC after stirring and reacting for 8 hours, the reaction for 2 hours of heat preservation, filter, collect the Chinese honeylocust for use; (2) supplementary saponification: stirring and heating the soapstock to 55 ℃, uniformly adding alkali liquor accounting for 15% of the mass of the anion exchange resin, continuously heating to 95 ℃, stirring and saponifying for 2 hours, filtering to obtain filter residue, detecting to obtain the oryzanol content of 1.78%, and reducing the loss of the oryzanol content in the treatment process; (3) placing filter residues in a reaction kettle, adding a liquid-liquid extraction solvent, wherein the liquid-liquid extraction solvent is an ethylene glycol monomethyl ether-methanol-water mixed solution, the mass contents of ethylene glycol monomethyl ether, methanol and water are respectively 61%, 29.0% and 10%, separating oryzanol in a liquid phase, stirring at the speed of 200rpm in the reaction kettle, heating to 70 ℃, stopping heating when a reflux phenomenon occurs in a methanol reflux device, keeping the temperature, carrying out reflux reaction for 30 minutes while continuously stirring, sampling, determining the pH value to be 9, slowly cooling the saponified liquid to 50 ℃ by using cooling water, carrying out vacuum suction filtration, and pumping the filtrate into an acidification reaction kettle to obtain an extractant mother solution; (45) storing the extractant mother liquor in an acid-out reaction kettle, heating gradually under the condition of continuously stirring at 200rpm, when the temperature rises to 45 ℃, dropwise adding a methanol-25% hydrochloric acid solution to adjust the pH to 7, when the temperature rises to 50 ℃, dropwise adding acetic acid with the mass fraction of 3% which is one fourth of the weight of the dosage of dilute hydrochloric acid, heating to 60 ℃, reacting for 30 minutes, adjusting the pH to 6.7, stopping heating, extracting oryzanol to return to ethylene glycol monomethyl ether, desolventizing the ethylene glycol monomethyl ether phase to obtain a oryzanol concentrate, and performing gel permeation by adopting Toyopearl HW-40C resin, wherein the volume of the oryzanol concentrate is 70 times of the volume of the resin gel, and the pH is 6.7; (5) and (3) elution and refining: eluting with acidic methanol with pH of 3 for 24 hr, washing with 80% hot methanol solution, volatilizing solvent, crushing, sieving with 12 mesh sieve, washing with 80 deg.C distilled water for several times to remove inorganic salt impurities until no salt taste of oryzanol is obtained; (6) and (3) crushing the filtered oryzanol, sieving the oryzanol with a 12-mesh sieve, loading the oryzanol into a drying chamber, controlling the thickness of the oryzanol powder in the plate to be 3 cm, controlling the drying temperature to be 80 ℃, and drying for 8 hours to obtain the oryzanol.
The product quality index is as follows: the oryzanol content is more than 98%, the color is white, the volatile matter is less than 0.5%, the ash content is less than 0.3%, and the methoxyl group value is 4.98.
Note: the detection method comprises the following steps: GB/T5520-2011 (insoluble impurities test); GB/T5530-2005 (acid value test), GB/T5528-2008 (moisture and volatile test); GB/T5538-2005 (peroxide number test); GB/T5525-2008 (color test); GB19112-2003 (rice bran oil standard); LS/T6121.1-2017 spectrophotometry for detecting oryzanol content in vegetable oil.
Claims (5)
1. A rice bran oil oryzanol production process is characterized in that rice bran oil is rice bran crude oil obtained by removing impurities, degumming and decoloring, and comprises the following steps: (1) pumping the crude rice bran oil into an exchange resin alkali refining pot, adding strong-basicity styrene anion exchange resin, stirring, preserving heat, filtering, and collecting saponin for later use; (2) supplementary saponification: stirring and heating the soapstock to 50-55 ℃, uniformly adding alkali liquor with the mass of 10-15% of that of the anion exchange resin, continuously heating to 90-95 ℃, stirring and saponifying for 1-2 hours, and filtering to obtain filter residue; (3) placing filter residues in a reaction kettle, adding a liquid-liquid extraction solvent, wherein the liquid-liquid extraction solvent is a mixed solution of ethylene glycol monomethyl ether, methanol and water, the mass contents of the ethylene glycol monomethyl ether, the methanol and the water are respectively 61-65%, 25-29% and 10%, separating oryzanol in a liquid phase, stirring at the speed of 150-200 rpm, heating to 65-70 ℃, continuously stirring at a constant temperature for reflux reaction for 20-30 min, cooling the saponified solution to 45-50 ℃, performing vacuum suction filtration, and pumping the filtrate into an acidification reaction kettle to obtain an extractant mother solution; (4) heating the extractant mother liquor under the stirring of 150-200 rpm, dropwise adding a dilute hydrochloric acid mixed solution to adjust the pH to 6.8-7 when the temperature is raised to 40-45 ℃, dropwise adding acetic acid with the mass fraction of 2-3% when the temperature is raised to 50 ℃, adjusting the pH to 6.5-6.7, raising the temperature to 60 ℃, stopping the reaction for 30min, extracting the oryzanol, returning the oryzanol to ethylene glycol monomethyl ether, desolventizing the ethylene glycol monomethyl ether phase to obtain a oryzanol concentrate, and permeating the oryzanol concentrate by adopting resin gel; (5) and (3) elution and refining: eluting with acidic methanol with the pH of 2-3 for 12-24 h, volatilizing the methanol, crushing, sieving, and washing with distilled water at 80 ℃ until the oryzanol has no salty taste; (6) and (3) crushing and sieving the filtered oryzanol, and drying for 8 hours at the drying temperature of 75-80 ℃ to obtain the oryzanol.
2. The rice bran oil oryzanol production process as claimed in claim 1, wherein the alkali liquor in the step (2) is 15-20% sodium hydroxide solution by mass fraction.
3. The rice bran oil oryzanol production process as claimed in claim 1, wherein the stirring and filtering step (1) is to rapidly stir at 150-200 rpm and heat up to 60 ℃, stop heating, uniformly add strongly basic styrene anion exchange resin with a mass of 30-35% of the crude rice bran oil for 10-15 minutes under rapid stirring, stir for 8-10 hours, heat up to 55-60 ℃, and perform heat preservation reaction for 1-2 hours.
4. The rice bran oil and oryzanol production process as claimed in claim 1, wherein the step (4) adopts resin gel permeation, wherein the volume of the oryzanol concentrate is 60-70 times that of the resin gel, and the pH value is 6.5-6.7.
5. The process for producing rice bran oil and oryzanol as claimed in claim 1, wherein the diluted hydrochloric acid mixed solution of step (4) is methanol-25% hydrochloric acid solution.
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