CN106479673A - A kind of method of purification Fructus Hippophae skin residual oil - Google Patents

A kind of method of purification Fructus Hippophae skin residual oil Download PDF

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CN106479673A
CN106479673A CN201611014647.5A CN201611014647A CN106479673A CN 106479673 A CN106479673 A CN 106479673A CN 201611014647 A CN201611014647 A CN 201611014647A CN 106479673 A CN106479673 A CN 106479673A
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oil
filter
temperature
open
valve
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刘志会
张祖奎
马荣山
颜廷才
巴志刚
李伟
王艳平
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Chaoyang Fengyuan Biotechnology Co Ltd
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Chaoyang Fengyuan Biotechnology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/006Refining fats or fatty oils by extraction

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  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention provides a kind of method of purification Fructus Hippophae skin residual oil, using ethanol degumming technology, the extraction efficiency of Fructus Hippophae dreg oil can be greatly improved, and product impurity is few, decrease later-period purification technique, reduce the production cost of Fructus Hippophae dreg oil, this technology belongs to physical method, the nutritional labeling of Oleum Hippophae is fully retained, has had good effect to human body cardiovascular and cerebrovascular vessel, metabolism, immune system, digestive system and respiratory system;Also there is defencive function to human liver, there are anticancer, anti-aging effects.The method operating procedure is simple, easily realization, and degumming effect is notable, is that the production of Fructus Hippophae skin slag fruit oil provides effective and feasible production method.

Description

A kind of method of purification Fructus Hippophae skin residual oil
Technical field
The present invention relates to food processing field, especially, it is related to a kind of method of purification Fructus Hippophae skin residual oil.
Background technology
Fructus Hippophae, Elaeangnaceae plant.It is commonly called as vinegar willow, acid thorn, black thorn.Every 100g contains soluble sugar 8g-12g, organic acid 1g-3g, carotenoid 3-4g, vitamin C 300mg, vitamin e1 5mg, particularly also contain abundant trace element, Fructus Hippophae Many active substances such as flavone, plant sterol, phenols and organic acid, triterpene, steroid compound, have many work( Effect.Can be applied to prevent and treat cardiovascular and cerebrovascular disease, tumor, immune disease, gastrointestinal disturbances tract disease etc., also have and significantly resist Aging, infection and promotion organization cell regeneration effect, have very big pharmaceutical developmentses and are worth.
Oleum Hippophae is the material being extracted from Fructus Hippophae by certain physical means, and it is a kind of high nutrition, height The natural materials of economic worth.It contains multivitamin, various trace elements, several amino acids and other biological activity thing Matter.The former Russian scholar research finds that in Oleum Hippophae, contained active component has reached 1060 kinds of (wherein 6 kinds of fatsoluble vitamin, fat 22 kinds of fat acid, 42 kinds of lipid, flavone and 36 kinds of phenols.Its oneself separated main component identifying is broadly divided into vitamin Class:Mainly there are Vitamin E, vitamin A, provitamin A (carotene), vitamin K, vitamin C, vitaminF etc..Liang Denian Show 580mg-800mg containing vitamin c in 100g Fructus Hippophae etc. result of study, and contained vitamin c quite stable.Dimension life Content in Fructus Hippophae for the plain A is also to enrich very much, and the every hectogram of Fructus Hippophae that Azerbaijan produces is dried in marc and contains 40mg, in Fructus Hippophae 168mg-215mg is contained in oil.Contain total tocopherol 28mg in marc, oil contains total tocopherol 112mg-154mg.Vitamin E is Activated Vitamin E-α the type being to account for vitamin 51% one 65%, Vitamin E race is the Oleum Hippophae Natural antioxidant, content Higher, Oleum Hippophae is more stable.Triterpene, phytosterin compound:Such composition in about 52 is contained, main inclusion paddy steroid in Oleum Hippophae Alcohol, amyrin, ring lanosterol, ergostene glycol, ursolic acid, ring one Pilus Caprae seu Oviss steroid glycol, bean steroid dienone, ergostene Alcohol, ergostene tetrol, 24 monomethyl ring A Erta alcohol, lemon flavol, stigmastenol (△ 7), avenasterol (△ 5, △ 7), dish Oily enol (△ 7), campesterol etc..Yin Fushan etc. adopts silica gel column chromatography and application of gas chromatorgraphy/mass technology to Fructrs Hippophae seed oil not saponification portion Analyzed, identification removes Vitamin E and 10 steroids:As ring-Pilus Caprae seu Oviss steroid-glycol, bean steroid dienone, Ergota steroid Enol, ergostene tetrol etc..Demonstrate simultaneously and also contain in Fructrs Hippophae seed oil and fruit oil identical composition, such as α-amyrin, β- Amyrin, ring-Pilus Caprae seu Oviss steroid one glycol, ergostenol glycol etc..Lipid component:Abundant fatty acid, content is contained in Oleum Hippophae Reach 60-70%, mainly have stearic acid, palmitic acid, Oleic acid, linoleic acid, linolenic acid, arachidic acid, myristic acid, palmitic olefinic acid, the moon Cinnamic acid etc.;Additionally, also containing 13 kinds of monohydroxies and 4 kinds of double hydroxy acid in Oleum Hippophae, and 7 kinds of lists, double and three epoxyeicosatrienoic acids;Fructus Hippophae In contain more than 100 kind of lipid composition, in Oleum Hippophae content of phospholipid be 0.9-1.0%.Including lecithin, cephalin, phospholipid phthalein gallbladder Alkali, phospholipid phthalein glycerol, phospholipid phthalidyl alcohol, phospholipid phthalein cholamine, lysophosphatide phthalidyl alcohol, LYSOLECITHIN SUNLECITHIN A, N mono- phthalidyl phospholipid phthalein Alcohol, haemolysis N mono- second phthalein phosphatidic acid cholamine etc..Flavones ingredient:In Fructus Hippophae and leaf, flavones ingredient is certified Cortex querci dentatae Element, isorhamnetin, kaempferol and its glycoside, myricetin, chlorogenic acid, pigweed glycosides, catechuic acid, astragaloside etc., different Fructus Hippophae product Kind, different parts and different place of production sea buckthorn resources, flavones content is different;Fruit maturity, collection period are to flavones ingredient Have a major impact.Phenol and organic acid:The organic acid such as malic acid, citric acid, oxalic acid, tartaric acid, succinic acid is contained in Oleum Hippophae Composition, total content is 3.86-4.52%.Its polyphenol compound includes maloic acid, a- coumarin, coumarin, phenolic acid, Salvia japonica Thunb. Phenol, Salvia japonica Thunb. phenolic acid, n- methyl Salvia japonica Thunb. phenolic acid etc..Volatile oil composition:Ripe fresh China obtains pale yellow through steam distillation Color has shape thing.Yield is 175mg/Kg, is solidified as semisolid after cooling, shows that this oil contains more free fatty through TLC Hydrocarbon component with polarity very little.Its chemical composition is analyzed using GC-MS method, in 89 given peaks, oneself removes in identification 82 compounds.Oneself identification from Chinese sea buckthorn, Fructus rhamni (Rhamnus davurica Pall.) Fructus Hippophae and subsp.neurocarpa removes more than 200 kind of volatile ingredient so far.Finland Produce 36 kinds of components containing volatile ingredient in Fructus Hippophae, analyze 60 kinds of fragrance ingredients, mainly lower fatty acid fat.Shaanxi HUANGLONG Remove seed Chinese sea buckthorn 1.23-1.69% containing volatile oil component, 36 kinds of components of detection are it is determined that 32 kinds therein.Qinghai Qilian County Subsp.neurocarpa quintessence oil oil yield is 0.1-0.14%, and the component that fresh fruit essential oil content is more than 0.1% has more than 160 kinds, Preliminary Identification Go out 52 kinds, content accounts for more than the 80% of quintessence oil total composition, wherein alcohol, aldehyde, lower fatty acid lipid accounts for significant proportion.Micro unit Element:Contain 30 various trace elements in Oleum Hippophae, including the necessary trace element of human body, such as ferrum, zinc, manganese, aluminum, selenium, nickel, Stannum, silicon, vitriol etc..Other compositions:Ester, ether, aldehyde, ketone, simultaneously alkene and other heterocyclic compounds is also contained in Oleum Hippophae;Also simultaneously There are hydrocarbon compound, the mainly linear paraffin of cl6-34.
Fructus Hippophae is doctor's food dual purpose plant, has very high economic worth and potentiality to be exploited,《Chinese Pharmacopoeia》, Tibetan medicine's masterpiece《Four Portion cures allusion quotation》In all effect of Fructus Hippophae is expressly recited.Oleum Hippophae extracts from sea buckthorn fruit or seed, containing polyunsaturated fat Acid and other biological activity composition.Therefore, Oleum Hippophae is as special functional oils and fatss, in food, Medicines and Health Product, cosmetics etc. Field has wide practical use.Oleum Hippophae, as the source of industrial chain, has vital effect to its deep development.Right The effect of cardiovascular system:Oleum Hippophae has the effect of anti-myocardial ischemia, can extend the time-to-live of mice, to myocardial ischemia Also there is certain protective effect.Fructus Hippophae whole part 62.08mg/kg lumbar injection, all can significantly increase mice hypoxia-bearing capability, Showing as the mouse survival time significantly extends, and also compared with matched group, there were significant differences for keto consumpting speed and remaining oxygen amount, and 31.04mg/ Kg intravenously administrable has significant protective effect to Acute Myocardial Ischemia in Rats.The effect of anti-tumor aspect;Oleum Hippophae has substantially Radiation resistance;Hepatoprotective effect Experimental report, Fructus Hippophae concentrated fruit juice and Fructrs Hippophae seed oil have obvious hepatoprotective effect;Spine oil is to dynamic Physical property inflammation has obvious effect:Oleum Hippophae lumbar injection has antioxidative effect and prevents fatty liver from acting on, and can adjust group Knit speed and the Vitamin E levels of middle lipid peroxidation.Oleum Hippophae is similar with Vitamin E, the blood that high cruel serum is damaged Pipe smooth muscle cell has protective effect, can substantially reduce high cruel consumption and hinder containing of the lipid peroxide increasing in smooth muscle cell Amount, and the activity of SOD can be significantly improved, the high cruel damage to cell membrane for the serum can be mitigated, protect and promote the health of cell raw Long;Fructus Hippophae also has immunological enhancement.
On domestic market, oil degumming methods mainly have aquation method.Fructus Hippophae oil degumming methods are also adopted by the method, and the method takes off Glue effect is general, and needs to consume great lot of water resources.A large amount of colloids are contained, wherein some is pectin, really in Oleum Hippophae Glue runs into ethanol easily Precipitation, does not apply at present in oil plant degumming.This research invention focuses primarily upon ethanol degumming On, the widely used aquation method degumming of current manufacturing enterprise, degumming ratio is relatively low, and production cost is higher, so manufacturing enterprise is less.Husky Spine peel residue product region is strong, lacks the best brand of product in the impact whole nation, and the market sales volume is limited.Therefore it is necessary that research is a kind of The method of purification Fructus Hippophae skin residual oil, improves the extraction efficiency of Fructus Hippophae dreg oil, reduces impurity, thus decreasing later-period purification work Skill, reduces the production cost of Fructus Hippophae dreg oil.
Content of the invention
Present invention aim at providing a kind of method of purification Fructus Hippophae skin residual oil, to solve technical problem.
A kind of method of purification Fructus Hippophae skin residual oil, comprises the following steps:Crude oil → ethanol degumming → filtration → mensure acid value Store in → alkali refining (deacidification) → dehydration → decolouring → deodorize → freezing dewaxing → fine straining → importing finished product oil tank.
Preferably, described ethanol degumming comprises the following steps:Add the ethanol of Fructus Hippophae skin residual oil 40-60% volume molten Liquid, stirring and evenly mixing fully precipitates colloid, stands under room temperature, separates oil reservoir and ethanol, centrifugation colloid, ethanol recycles, Oleum Hippophae carries out next step filter progress again.
Preferably, the volumetric concentration of described ethanol solution is 75%.
Preferably, during described filtration, pressure is gradually risen, final pressure controls in 0.2-0.3MPa;Just started During filter, in filter, filter cake is not yet formed, and clean in order to dregs in oil are filtered, Stress control is between 0.05~0.1Mpa; After stopping filtering, connect air compressor, with air extrusion 25-35 minute, then unload folder cleaning filter cake.
Preferably, described alkali refining operation (low temperature process alkali refining), comprises the following steps:Detection degummed oil acid value, according to acid Valency calculates theoretical caustic dosage and excess alkali quantity, so that it is determined that caustic dosage.
Theoretical caustic dosage GNaON=7.13 × 10-4*G oil × VA;
In formula:GNaON:Alkali refining needs the quality (Kg) of pure solid sodium hydroxide;
G oil:The quality (Kg) of oil;
VA:The acid value of oil.
Excess alkali quantity:The general percent accounting for oil quality with pure solid caustic soda represents, rule of thumb, the preferable hair of quality Oil is general to use oil weight 0.05-0.25% excess alkali quantity.
According to acid value, determine concentration of lye.
Table one:Crude oil acid value and the relation of concentration of lye.
Crude oil acid value Concentration of lye0Be
Less than 3 10
3-5 11
5-8 12
8-10 14
More than 10 16
Alkali refining purpose:Free fatty in removing crude oil, increases the transparency of oil, reduces smoke point, prevents oxidation deterioration.
Decoloration process is batch production, is suitable for the decolouring of qualified various edible oil materials after degumming, deacidification, dehydration Journey.
Preferably, described decolouring, comprises the following steps:(1) check the liquid level of decolouring oil tank, determine the weight of oil, enter And determine the addition of adjuvant;(2) produce adjuvant used and water, electricity, vapour etc. should be made adequate preparation;(3) automatic discharge filter Answer adequate preparation good, security filter filter bag should correctly be installed;(4) each valve should be at tram;(5) in preparation On the premise of completing, first turn on water-ring vacuum pump, by bleacher, automatic discharge filter evacuation, vacustat- More than 0.085Mpa;(6) open the steam valve of bleacher, after exclusion condensed water, open drain valve, to the oil heating of decolouring oil tank; (7) when the oil temperature of the oil tank that decolours is to 105 DEG C, hargil and activated carbon are added from hargil inlet port, when hargil and activated carbon add After start timing, decolour 30 minutes, temperature control is between 105-110 DEG C;(8) when bleaching time then, start automatic discharge Filter, opens decolouring pump, starts to filter.
Deodorize:Deodorize purpose is the removing oil abnormal flavour that abnormal flavour, the course of processing are brought in itself and moisture content.
Preferably, described deodorize, comprises the following steps:Deodorizing tank evacuation:When bleached oil entrance deodorizing tank starts, With Roots vaccum pump, deodorizing tank is evacuated close -0.1Mpa, starts heat-conducting oil furnace simultaneously and start to warm up;When oil temperature is raised to When more than 130 DEG C, open live (open) steam, start cooling water recirculation system simultaneously, close deodorizing tank Inlet and outlet water valve, open vacuum Cooler water-inflow and drain valve on pipeline;Live (open) steam amount will be controlled, and oil droplet must not be made to be splashed to tank top, be evacuated pipe and be extracted into very Empty set system goes;Continue to use heat-conducting oil heating simultaneously, until tank temperature rise to 180 DEG C about;Keep this temperature, continue to take out very Sky, vacuum maintains -0.01Mpa;It is raised to 180 DEG C of beginning timing, deodorization time 6-8 hour from temperature;Deodorising process terminates Afterwards, claw the unburned coal cinder in heat-conducting oil furnace, open cooling water turnover valve cooling deodorised oil, oil temperature drops to less than 70 DEG C Afterwards, break deodorizing tank vacuum, bought oil toward freezing oil tank after accurate filter filtration with oil pump and carry out freezing dewaxing.
Preferably, described freezing dewaxing, comprises the following steps:Crystallize growing the grain, filtration and melt cured.
The method of the purification Fructus Hippophae skin residual oil of the present invention, using ethanol degumming technology, can greatly improve Fructus Hippophae dreg oil Extraction efficiency, and product impurity is few, decreases later-period purification technique, reduces the production cost of Fructus Hippophae dreg oil, this skill Art belongs to the nutritional labeling that physical method has been fully retained Oleum Hippophae, to human body cardiovascular and cerebrovascular vessel, metabolism, immune system, disappears Change system and respiratory system have good effect;Also there is defencive function to human liver, there are anticancer, anti-aging effects.This side Method operating procedure is simple, easily realization, and degumming effect is notable, is that the production of Fructus Hippophae skin slag fruit oil provides effective and feasible producer Method.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages. The present invention is further detailed explanation below.
Specific embodiment
Hereinafter embodiments of the invention are described in detail, but the present invention can limit according to claim and cover Multitude of different ways implement.
Embodiment
A kind of method of purification Fructus Hippophae skin residual oil, comprises the following steps:Crude oil → ethanol degumming → filtration → mensure acid value Store in → alkali refining (deacidification) → dehydration → decolouring → deodorize → freezing dewaxing → fine straining → importing finished product oil tank.
Described ethanol degumming comprises the following steps:Add the ethanol solution of Fructus Hippophae skin residual oil 50% volume, stirring and evenly mixing Fully precipitation colloid, stands under room temperature, separates oil reservoir and ethanol, centrifugation colloid, ethanol recycles, Oleum Hippophae is carried out again Next step filter progress.
The volumetric concentration of described ethanol solution is 75%.
During described filtration, pressure is gradually risen, final pressure controls in 0.2-0.3MPa;When just starting to filter, mistake In filter, filter cake is not yet formed, and clean in order to dregs in oil are filtered, Stress control exists
Between 0.05-0.1Mpa;After stopping filtering, connect air compressor, with air extrusion 30 minutes, then unload folder Cleaning filter cake.
Described alkali refining operation (low temperature process alkali refining), comprises the following steps:Detection degummed oil acid value, calculates according to acid value Theoretical caustic dosage and excess alkali quantity, so that it is determined that caustic dosage.
Theoretical caustic dosage GNaON=7.13 × 10-4*G oil × VA;
In formula:GNaON:Alkali refining needs the quality (Kg) of pure solid sodium hydroxide;
G oil:The quality (Kg) of oil;
VA:The acid value of oil.
Excess alkali quantity:The general percent accounting for oil quality with pure solid caustic soda represents, rule of thumb, the preferable hair of quality Oil is general to use oil weight 0.05-0.25% excess alkali quantity.
According to acid value, determine concentration of lye.
Described decolouring, comprises the following steps:(1) check the liquid level of decolouring oil tank, determine the weight of oil, and then determine auxiliary The addition of material;(2) produce adjuvant used and water, electricity, vapour etc. should be made adequate preparation;(3) automatic discharge filter should be fully accurate Get ready, security filter filter bag should correctly be installed;(4) each valve should be at tram;(5) before preparation is completed Put, first turn on water-ring vacuum pump, by bleacher, automatic discharge filter evacuation, vacustat is in -0.085Mpa More than;(6) open the steam valve of bleacher, after exclusion condensed water, open drain valve, to the oil heating of decolouring oil tank;(7) when de- When the oil temperature of color oil tank is to 105 DEG C, add hargil and activated carbon from hargil inlet port, start to count after hargil and activated carbon add When, decolour 30 minutes, temperature control is between 105-110 DEG C;(8) when bleaching time then, start automatic discharge filter, beat Exoneration color pump, starts to filter.
Described deodorize, comprises the following steps:Deodorizing tank evacuation:When bleached oil entrance deodorizing tank starts, use Roots Vacuum pump, deodorizing tank is evacuated close -0.1Mpa, starts heat-conducting oil furnace simultaneously and starts to warm up;When oil temperature be raised to 130 DEG C with When upper, opened live (open) steam, and started cooling water recirculation system simultaneously, close deodorizing tank Inlet and outlet water valve, open on vacuum line Cooler water-inflow and drain valve;Live (open) steam amount will be controlled, and oil droplet must not be made to be splashed to tank top, be evacuated pipe and be extracted into vacuum system Go;Continue to use heat-conducting oil heating simultaneously, until tank temperature rise to 180 DEG C about;Keep this temperature, continue evacuation, vacuum Degree maintains -0.01Mpa;It is raised to 180 DEG C of beginning timing, deodorization time 6-8 hour from temperature;After deodorising process terminates, claw Unburned coal cinder in heat-conducting oil furnace, opens cooling water turnover valve cooling deodorised oil, after oil temperature drops to less than 70 DEG C, breaks Deodorizing tank vacuum, is bought oil toward freezing oil tank after accurate filter filtration with oil pump and carries out freezing dewaxing.
Described freezing dewaxing, comprises the following steps:Crystallize growing the grain, filtration and melt cured.
Described crystallization growing the grain process operations:Start freezing unit, open freezing unit, will be cold for ethanol coolant (cold carrier) Freeze stand-by to -10 DEG C of degree.After crystallization maturator fills deep fat, oil temperature in record tank, if oil temperature, more than 70 DEG C, is opened Coolant supply valve be passed through coolant into maturator, first oil temperature is down to 70 DEG C, then according to《Dewaxing crystallization rearing crystal time and temperature Degree degree of passing table》In require cooling rate to oil cooling in tank, open stirring simultaneously, 10 turns per minute, and carry out itemized record.If Cooling rate is too fast, should take the circumstances into consideration to turn down coolant supply valve opening degree;Conversely, opening big.Require cooling slow, do not allow rapidly Cooling:" actual temperature " should try one's best close to " requiring cooling temperature ".Holding stage should be fixed time and is passed through coolant into maturator, protect Hold the no big change of temperature.Temperature-fall period should often be patrolled and be freezed unit working condition, note abnormalities and should process in time.Every knot Brilliant maturator oiling corresponds to every batch deodorised oil, is forbidden to intersect oiling.If finding, growing the grain situation is poor should again melt for a certain crystallization Cured recrystallization growing the grain.
Filter progress operates:Clean out dewaxing filter, filter cloth is balanced suitable, do not allow filter cloth to have Fold (should go through), and filter plate left and right edges are arranged into a line.After inspection is errorless, prepare oil strain.Open the good growing the grain of growing the grain The fuel-displaced valve of tank, opens filter pump terminal valve and return valve, and filter pump outlet valve guides filter.Start filter pump to Oil filter fuel feeding.Oil filter oil inlet valve is opened in slow-action, and open degree is between 1/3--1/2.Then adjust filter pump to import and export Reflux inlet, so that pump discharge pressure is controlled in 0.3Mpa about.After all fuel-displaced water nozzles of oil filter have oil out after, observe water nozzle Fuel-displaced situation.Fuel-displaced should be limpid, if finding to have the fuel-displaced muddiness of indivedual mouths should close this fuel-displaced water nozzle immediately.5-10 minute Afterwards, connect oily half cup with clean beaker from oil outlet, rusting cup will be contained and shine light compared with oil reservoir in benefit observation cup.If finding in oil Suspended crystal, should keep observation, until the transparent no suspended crystal of oil reservoir shows that in oil, cured crystalline substance is completely cleared, now should Turn down oil inlet valve, and rapid discharge roily oil in oil-containing groove in roily oil case (is shaved with scraper plate), then will be clear for oil-containing groove guiding Hydraulic fluid port, and inlet valve is recovered former open position, enter normal filtration.During normal filtration, it is still to observe profit mouth at any time Fuel-displaced situation, finds there is fuel-displaced muddiness, water nozzle should be closed immediately.During filtration, inlet pressure can gradually rise, if this stage When having a large amount of permeability phenomenon between filter plate and filter cloth, suitably filter plate compression hydraulic system can be opened and filter plate is compressed again.If When inlet pressure rises to 0.4Mpa, oil-feed can be stopped, closing inlet valve, stop filter pump.The filter stopping filtering is connect oil Groove oil-out guides roily oil mouth, and opens compressed air valve at oil-in and be blown into compressed air into filter and carry out blowing cake.Open Beginning blows tolerance during cake should be less, now should open all fuel-displaced water nozzle entering oil filter closing, first will be substantial amounts of in filter chamber Unfiltered oil presses out, and is then gradually opened compressed air valve, by Residual oil blow pressure in cured cake out.Treat fuel-displaced water nozzle substantially no Oil out when can close compressed air, then carry out melt cured operation.By the complete liquidation of bright for the overflow connecing in cured groove oil to roily oil In oil-containing groove.Also excess oil in oil-containing groove is cleaned out simultaneously.Periodically filtration roily oil is squeezed into and recrystallize after refrigerated cylinder.Incited somebody to action Product tank squeezed into by filtering oil.
Melt cured process operations:First boiler temperature be raised to more than 95 DEG C stand-by.After dewaxing filter end of operation, Open into hot water valve, start hot water circulating pump, carry out molten cured, molten cured during it is ensured that certain hot water temperature, treat all of Go out La Kou all no cured outflow when, open air cock, carry out blowback from oil-out, whne all of go out La Kou all no cured outflows when, can With think molten cured finish, close hot water valve and heat-exchanger pump, open cold water and start dewaxing filter is lowered the temperature until filter For room temperature.Carry out the filtration of subsequent cycle.The cured timely barrelling flowed out transports workshop.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, made any repair Change, equivalent, improvement etc., should be included within the scope of the present invention.

Claims (8)

1. a kind of method of purification Fructus Hippophae skin residual oil is it is characterised in that comprise the following steps:Crude oil → ethanol degumming → filtration → Measure in acid value → alkali refining (deacidification) → dehydration → decolouring → deodorize → freezing dewaxing → fine straining → importing finished product oil tank and store.
2. the method for purification Fructus Hippophae skin residual oil as claimed in claim 1 is it is characterised in that described ethanol degumming, including with Lower step:Add the ethanol solution of Fructus Hippophae skin residual oil 40-60% volume, stirring and evenly mixing fully precipitates colloid, stand under room temperature, point From oil reservoir and ethanol, centrifugation colloid, ethanol recycles, and Oleum Hippophae carries out next step filter progress again.
3. the method for purification Fructus Hippophae skin residual oil as claimed in claim 2 is it is characterised in that the volume of described ethanol solution is dense Spend for 75%.
4. the method for purification Fructus Hippophae skin residual oil as claimed in claim 1 is it is characterised in that during described filtration, by pressure by Edge up height, and final pressure controls in 0.2-0.3MPa;When just starting to filter, in filter, filter cake is not yet formed, in order in oil Dregs filter totally, and Stress control is between 0.05-0.1Mpa;After stopping filtering, connect air compressor, use air extrusion 25-35 minute, then unload folder cleaning filter cake.
5. the method for purification Fructus Hippophae skin residual oil as claimed in claim 1 is it is characterised in that the operation of described alkali refining, including with Lower step:Detection degummed oil acid value, calculates theoretical caustic dosage and excess alkali quantity according to acid value, so that it is determined that caustic dosage;
Theoretical caustic dosage GNaON=7.13 × 10-4*G oil × VA;
In formula:GNaON:Alkali refining needs the quality (Kg) of pure solid sodium hydroxide;
G oil:The quality (Kg) of oil;
VA:The acid value of oil;
Excess alkali quantity:The general percent accounting for oil quality with pure solid caustic soda represents, rule of thumb, the preferable crude oil of quality one As with oil weight 0.05-0.25% excess alkali quantity;
According to acid value, determine concentration of lye.
6. the method for purification Fructus Hippophae skin residual oil as claimed in claim 1, it is characterised in that described decolouring, walks including following Suddenly:(1) check the liquid level of decolouring oil tank, determine the weight of oil, and then determine the addition of adjuvant;(2) will be auxiliary used by production Material and water, electricity, vapour are made adequate preparation;(3) adequate preparation of automatic discharge filter is good, and security filter filter bag is correctly installed;(4) each Valve is in tram;(5) under the premise of preparation is completed, first turn on water-ring vacuum pump, by bleacher, certainly Dynamic filtering machine evacuation, vacustat is more than -0.085Mpa;(6) open the steam valve of bleacher, exclude condensed water After open drain valve, to decolouring oil tank oil heating;(7) when the oil temperature of the oil tank that decolours is to 105 DEG C, add from hargil inlet port Hargil and activated carbon, start timing after hargil and activated carbon add, and decolour 30 minutes, temperature control is between 105-110 DEG C; (8) when bleaching time then, start automatic discharge filter, open decolouring pump, start filter.
7. the method for purification Fructus Hippophae skin residual oil as claimed in claim 1, it is characterised in that described deodorize, walks including following Suddenly:Deodorizing tank evacuation:When bleached oil enters deodorizing tank and starts, with Roots vaccum pump, by deodorizing tank be evacuated close- 0.1Mpa, starts heat-conducting oil furnace simultaneously and starts to warm up;When oil temperature is raised to more than 130 DEG C, opens live (open) steam, start cold simultaneously But water circulation system, closes deodorizing tank Inlet and outlet water valve, opens cooler water-inflow and drain valve on vacuum line;Control live (open) steam Amount, must not make oil droplet be splashed to tank top;Continue to use heat-conducting oil heating simultaneously, until tank temperature rise to 180 DEG C about;Keep This temperature, continues evacuation, and vacuum maintains -0.01Mpa;It is raised to 180 DEG C of beginning timing from temperature, deodorization time 6-8 is little When;After deodorising process terminates, claw the unburned coal cinder in heat-conducting oil furnace, open cooling water turnover valve cooling deodorised oil, After oil temperature drops to less than 70 DEG C, break deodorizing tank vacuum, with oil pump through accurate filter filtration after toward freezing oil tank buy oil into Row freezing dewaxing.
8. the method for purification Fructus Hippophae skin residual oil as claimed in claim 1 is it is characterised in that described freezing dewaxing, including with Lower step:Crystallize growing the grain, filtration and melt cured;
Described crystallization growing the grain process operations:Start freezing unit, open freezing unit, by ethanol coolant be refrigerated to -10 DEG C with Under stand-by;Crystallization maturator fill deep fat after, record tank in oil temperature, if oil temperature is more than 70 DEG C, open coolant supply valve to It is passed through coolant in maturator, first oil temperature is down to 70 DEG C, then according to requiring cooling rate to oil cooling in tank, open simultaneously and stir Mix, 10 turns per minute, and carry out itemized record;If cooling rate is too fast, should take the circumstances into consideration to turn down coolant supply valve opening degree;Instead It, open big;Require cooling slow, do not allow rapid cooling:" actual temperature " should try one's best close to " requiring cooling temperature ";Insulation Stage should be fixed time and is passed through coolant into maturator, the no big change of keeping temperature;Temperature-fall period should often be patrolled freezing unit Working condition, notes abnormalities and should process in time;Every crystallization maturator oiling corresponds to every batch deodorised oil, is forbidden to intersect oiling; If finding, growing the grain situation is poor should again melt cured recrystallization growing the grain for a certain crystallization;
Filter progress operates:Clean out dewaxing filter, filter cloth is balanced suitable, do not allow filter cloth to have Fold, and will Row is into a line for filter plate left and right edges;After inspection is errorless, prepare oil strain;Open the good fuel-displaced valve of maturator of growing the grain, opened Filter pump terminal valve and return valve, filter pump outlet valve guides filter;Start filter pump to oil filter fuel feeding;Slow-action is opened Open oil filter oil inlet valve, open degree is between 1/3--1/2;Then adjust filter pump and import and export reflux inlet, make pump discharge pressure Power controls in 0.3Mpa;After all fuel-displaced water nozzles of oil filter have oil out after, observe the fuel-displaced situation of water nozzle;Fuel-displaced should be Limpid, if finding to have the fuel-displaced muddiness of indivedual mouths should close this fuel-displaced water nozzle immediately;After 5-10 minute, with clean beaker from fuel-displaced Mouth connects oily half cup, will contain rusting cup and shine light compared with oil reservoir in benefit observation cup;If finding suspended crystal in oil, should keep Observe, until the transparent no suspended crystal of oil reservoir shows that in oil, cured crystalline substance is completely cleared, now should turn down oil inlet valve, and rapidly Roily oil in oil-containing groove is discharged in roily oil case, then oil-containing groove is guided edible vegetable oil mouth, and inlet valve is recovered former open position, enter Enter normal filtration;During normal filtration, it is still to observe the fuel-displaced situation of profit mouth at any time, find there is fuel-displaced muddiness, water nozzle should stand Close;During filtration, inlet pressure can gradually rise, if having a large amount of permeability phenomenon between this stage filter plate and filter cloth, can Suitably filter plate compression hydraulic system is opened and filter plate is compressed again;If inlet pressure rises to 0.4Mpa, can stop into Oil, closes inlet valve, stops filter pump;By the filter oil-containing groove oil-out stopping filtering guiding roily oil mouth, and open oil-in Place's compressed air valve is blown into compressed air into filter to carry out blowing cake;Starting to blow tolerance during cake should be less, now should be by oil-feed The all fuel-displaced water nozzle that filter cuts out is opened, and first presses out unfiltered oil substantial amounts of in filter chamber, is then gradually opened compression Air door, by Residual oil blow pressure in cured cake out;Whne the basic oil-free of fuel-displaced water nozzle out when can close compressed air, Ran Houjin Row melts cured operation;By the complete liquidation of bright for the overflow connecing in cured groove oil to roily oil oil-containing groove;Simultaneously also will be clear for excess oil in oil-containing groove Reason is clean;Periodically filtration roily oil is squeezed into and recrystallize after refrigerated cylinder;Squeeze into product tank by filtering edible vegetable oil;
Melt cured process operations:First boiler temperature be raised to more than 95 DEG C stand-by;After dewaxing filter end of operation, open Enter hot water valve, start hot water circulating pump, carry out molten cured, molten cured during it is ensured that certain hot water temperature, treat all of go out cured Mouth all no cured outflow when, open air cock, carry out blowback from oil-out, whne all of go out La Kou all no cured outflows when, can recognize For molten cured finish, close hot water valve and heat-exchanger pump, it is normal for open cold water starting dewaxing filter is lowered the temperature until filter Temperature;Carry out the filtration of subsequent cycle;The cured timely barrelling flowed out transports workshop.
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CN109603789A (en) * 2019-01-07 2019-04-12 枣阳市金鹏化工有限公司 Reduce active carbon oil content blows charcoal method
CN110540892A (en) * 2019-08-21 2019-12-06 洞口县亿丰农林牧科技有限公司 operation method in tea seed oil pressing process
CN112251284A (en) * 2020-10-11 2021-01-22 甘肃省科学院生物研究所 Method for extracting and refining sea-buckthorn whole fruit oil
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109603789A (en) * 2019-01-07 2019-04-12 枣阳市金鹏化工有限公司 Reduce active carbon oil content blows charcoal method
CN110540892A (en) * 2019-08-21 2019-12-06 洞口县亿丰农林牧科技有限公司 operation method in tea seed oil pressing process
CN112251284A (en) * 2020-10-11 2021-01-22 甘肃省科学院生物研究所 Method for extracting and refining sea-buckthorn whole fruit oil
JP7108992B1 (en) * 2021-10-27 2022-07-29 宇航人ジャパン株式会社 Composition containing ingredient derived from pericarp of sea buckthorn

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