CN104974857A - Method for preparing horse oil through ethyl esterification and prepared horse oil - Google Patents
Method for preparing horse oil through ethyl esterification and prepared horse oil Download PDFInfo
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- CN104974857A CN104974857A CN201510389147.9A CN201510389147A CN104974857A CN 104974857 A CN104974857 A CN 104974857A CN 201510389147 A CN201510389147 A CN 201510389147A CN 104974857 A CN104974857 A CN 104974857A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
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Abstract
The invention relates to a method for preparing horse oil from horse fat through ethyl esterification and the horse oil prepared by using the method, belonging to the technical field of processing and refining of animal fat. The method comprises the following steps: adding crude horse oil into a reaction container, dissolving a catalyst in absolute ethyl alcohol in terms of the mass of the crude horse oil and according to an alcohol-oil ratio of 3-5: 1 and a catalyst addition amount of 0.4%, adding the dissolved catalyst into the reaction container, starting a stirrer at the same time, carrying out uniform and full mixing and then carrying out a reaction at 50 to 70 DEG C at a rotating speed of 40 to 80 r/min for 90 min; after completion of the reaction, recovering ethanol and centrifuging an obtained mixture of glycerin and fatty acid ethyl ester; and after completion of centrifugation, taking an oil liquid at an upper layer so as to obtain refined horse oil. The preparation method has the advantages of high horse oil yield, small usage amount of raw materials and the catalyst, short reaction time, etc.
Description
Technical field:
The present invention relates to a kind of take horse fat as the ethyl esterified house oil preparation method of raw material, and relates to the obtained house oil of the method, belongs to animal grease processing and refining technical field.
Background technology:
Colt oil and horse fat, white, yellow or orange-yellow ointment shape, containing alpha-linolenic acid and linolic acid amount up to more than 15%, be rich in unsaturated fatty acids, vitamin A and vitamin-E, horse fat melts the liquid fat and house oil that obtain.Kazak medical science is thought, horse fat is hot in nature, and seepage force is strong, can promoting blood circulation and removing obstruction in channels, the strong body of nourishing, the broken dissipating bind of change.Horse fat fat is commonly used to assisting therapy coronary heart disease, high blood viscosity, hypertension, fracture solution heals, body of suffering from a deficiency of the kidney loses or the symptom such as cervical spondylosis, softening malunion of fracture; When severe scald, burn, colt oil is applied to affected part can fully recover very soon, and preventing from scar; Permanently effective to omarthritis, cold disease, goinyalgia, pain in the back; To the excellent treatment effect of the bedsore disease of patient bedridden in long term; Also can be used to hairdressing, skin care, ecchymose removing, dye method, Wu Fa etc.; The symptom Be very effective such as antagonism senile plaque, alopecia, wrinkle, allergic rhinitis, eczema, pollinosis, the ringworm of the foot, atopic dermatitis, pachylosis; Swelling and pain relieving effect is had to general wound; By the fracture of the softening old malunion of colt oil (horse fat fat), joint dislocation and ankylosis, do not need anesthesia and operation, do not need other medicines and cross many condition, do not stay operative scar, particularly wound is little, and institute of traditional Chinese medicine of Xinjiang Yili of China autonomous prefecture, Altay Ha Yi hospital and position, Xinjiang more than 10 doctor among the people have abundant Couple herbs.The Kazak people also generally understand house oil and soften the reduction more again of malunion of fracture solution, fixing treatment.By investigation among the people, the kazakh masses are generally familiar with the effect to horseflesh, horse fat fat.Just the nutritive ingredient of mechanism to horse fat fat is had to give abundant affirmation abroad at the seventies, and be raw material with horse fat fat and other plant, develop the products such as makeup, softener, shampoo, hair growth promoting agent, but expensive, be not subject to market accreditation.Slightly carrying than being easier to of horse fat, but crude fat has the special odor of kind of very bad news, and color and luster is comparatively dark, also have impact on applying of horse fat.
The research relevant to refining horse fat, published patent is as follows:
The Chinese invention " horse fat extracts and industrial application " of publication number CN1456648A discloses a kind of collection horse body adipose tissue, extract the method for thick horse fat and refining horse fat, and disclose its application in industrial aspect, extracting the horse fat relative density obtained is 0.912-0.930, specific refractory power (20 DEG C) 1.468, fusing point 25-45 DEG C, acid number (mg/g)≤2.0, iodine number 70-86, saponification value 195-201, moisture≤0.5%, unsaponifiables 0.2-0.5.Food, washing cosmetic, Medicines and Health Product, the leather processing nursing lubricant of auxiliary agent, textile auxiliary agent and precision meter, rust-preventive agent and inhibiter etc. can be widely used in.
The horse fat extracted with conventional boil technique contains palmitic acid fat≤29%, glyceryl stearate≤7%, olein≤55%, linoleic acid fat≤7%.
The disclosed house oil production technique of Chinese invention " production method of refined horse oil " of application number 92106187.0 is: adopt with the rough house oil of alkali lye, heating washing, steam air lift removes peculiar smell, discoloring agent imurity-removal and color, and the technique of filtering and obtained colourless light yellow clear, refined horse oil without any peculiar smell, its quality can reach makeup requirement.The yield of house oil prepared by this method is very low, and saponification phenomenon is obvious, is not suitable for large-scale industrial production.
The Chinese invention " grease being rich in unsaturated fatty acids and preparation method thereof " of publication number CN103409224A relates to unsaturated fatty acids extractive technique field, disclosed preparation method is: the first step, horse fat is rubbed, and the horse fat after rubbing is carried out heating the grease and house oil that obtain liquid state; Second step, after 1:2 to 1:5 mixes in mass ratio by house oil and saponifying agent, obtains saponification liquor after carrying out saponification reaction 0.5-3h under temperature is 50-90 DEG C of condition.This invention carries out solvent crystallization according to the difference of component crystallizes temperature each in house oil, further acquisition unsaturated fatty acids, in house oil, unsaturated fatty acids comprises oleic acid, linolic acid, linolenic acid, Zoomeric acid, this method can extract mono-unsaturated glyceride (oleic acid, Zoomeric acid) and polyunsaturated fatty acid (linolic acid, linolenic acid) by Sync enrichment, and method is easy, service temperature is low and yield is higher.The yield that the first step heating method of this method obtains house oil is low, critical defect is in high-temperature heating process, the middle unsaturated fatty acids major part deterioration by oxidation of house oil, late enrichment mono-unsaturated glyceride (oleic acid, Zoomeric acid) and polyunsaturated fatty acid (linolic acid, linolenic acid), do not know where to begin.
In sum, there is following problem in prior art:
1. the heating infusion method tentatively slightly proposing employing can make unsaturated fatty acids acid oxidase in house oil, thus loses most effect;
2. process for purification is roughly divided into saponification method and solvent extraction method two kinds, and common drawback is: refined horse oil yield is low, has dissolvent residual, and solvent extraction method is not suitable for suitability for industrialized production.
Include in middle National IP Network, Xinjiang Agricultural Univ, the master thesis " acid extraction of house oil unsaturated fatty acids and enrichment research " that author is Zheng Jing relates to enzymolysis process and extracts thick house oil, then carries out ethyl esterified by base catalysis method to house oil, finally applies molecular distillation method enrichment unsaturated fatty acids.But exist ethyl esterified after the water washing operations that carries out, reduces ethyl esterified house oil yield to a great extent, and quite significantly saponification reaction can occur, and it is large to there is raw material dosage, the defects such as long reaction time.
Summary of the invention:
The deficiency that the present invention exists in developing mainly for current house oil, make full use of the natural resources that Xinjiang is abundant, play the advantage of folk tradition medicine, in conjunction with modern advanced theory and scientific and technical means, developing a kind of is raw material with horse fat, after processing treatment, at utmost retain the unsaturated fatty acids that it is abundant, also effectively can reduce its molten boiling point, and it is in stable condition, be easy to the ethyl esterified house oil product of absorption of human body, for later stage molecular distillation enrichment unsaturated fatty acids lays the foundation.Consider reaction times, reaction conditions and equipment etc., employing alkali catalyzed alcoholysis method of the present invention carries out the ethyl esterified processing of house oil.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A kind of ethyl esterified house oil preparation method, comprises the steps:
Thick house oil is added in reaction vessel, in house oil quality, according to alcohol oil rate 3-5:1, catalyst loading 0.3-0.4%, by catalyst dissolution after dehydrated alcohol, add reaction vessel, simultaneously turn on agitator, fully mix, at 50-70 DEG C, under rotating speed 40-80r/min condition, clock reaction (90-100min; After reaction terminates, reclaim ethanol, the glycerine obtained and fatty acid ethyl ester mixture are carried out centrifugal treating.Treat centrifugal end, get upper strata fluid, refining house oil can be obtained;
Described catalyzer is analytical pure sodium hydroxide; Described dehydrated alcohol is analytical pure;
Described reaction vessel is the closed reaction vessel that stirring and condensation reflux unit are housed;
Preferably, described reaction vessel is reactor or three-necked bottle;
Described reactor is interlayer heating glass constant temperature stirred autoclave, and condensation reflux unit is housed.
Described sodium hydroxide is catalyzer, owing to not having the participation of water in whole reaction system, avoids the generation of saponification reaction.Its principle is that sodium hydroxide and ethanol synthesis generate sodium ethylate, sodium ethylate again with triglyceride level generation permutoid reaction, generate glycerine trisodium and fatty-acid ethyl ester.Due to the difference of molecular weight and textural association form
,glycerine trisodium can be deposited on lower floor after centrifugation, and fatty-acid ethyl ester and refined horse oil are enriched in upper strata.Now sodium hydroxide detaches house oil with the form of glycerine trisodium.
Base catalysis method alcoholysis reaction, reaction formula is as follows:
NaOH
↓
R
1OCOR+R
2OH→R
2OCOR+R
1OH
Described recovery ethanol, uses Rotary Evaporators, and constant temperature 45 DEG C, reclaim ethanol 40min-50min under rotating speed 40r/min-50r/min, the rate of recovery can reach more than 90%.
Described centrifugal treating, namely selects rotating speed 4000r/min-5000r/min, time 5min-10min.
The present invention provides above-mentioned preparation method the house oil obtained simultaneously; The ethyl esterified degree of described house oil is higher, and unsaturated fatty acids retention rate reaches more than 40%, wherein ethyl oleate >=30%, ethyl linoleate >=10%, ethyl palmitate >=30%, and containing a small amount of Ethyl arachidonate.
Beneficial effect:
1, raw materials for production cost is low
Raw materials for production used are horse fat, and it is with low cost, and wide material sources achieve and turn waste into wealth, and take full advantage of horse fat resource.
2, equipment investment cost is little
The equipment manufacturing cost such as preparation required reactor, agitator, whizzer, Rotary Evaporators are moderate, and the course of processing is very little to the degree of injury of equipment, does not affect the work-ing life of equipment.
3, products obtained therefrom Functionality, quality and appealing design
The horse fat product absorptivity adopting this method to obtain is good, and unsaturated fatty acids retention rate is high, and oil clarification is bright, without the pungent grease taste of thick horse fat, best in quality.
4, end-use is wide
The house oil of process for processing of the present invention is strong to human body skin seepage force, stretchability good, skin absorbs fast, skin-protecting face nursing, can replace lanolin for cosmetics.In addition, also can be used for senior liquid washing agent, the leather processing nursing lubricant of auxiliary agent, textile auxiliary agent and precision meter, rust-preventive agent and inhibiter etc.Improve class and the added value of product, extend industrial chain, add the comprehensive benefit of industry.
5, preparation method's house oil yield of the present invention is high, saponification reaction does not occur, and adopts centrifuging separation of glycerin and carboxylate, not only saves time, and is separated completely, and more easy to operate, ethyl esterified efficiency of pcr product is high.The advantages such as and it is few to have raw material dosage, catalyst levels is few, and the reaction times is short.Raw material and catalyst levels are not as good as disclosed in prior art 1/2nd, and the reaction times but shortens 1/3rd, significantly reduces production cost, improves technological feasibility, wide market.
Embodiment
The following stated is only the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have change and change.All any amendments done within the spirit and principles in the present invention, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Embodiment 1
Take the thick house oil of 100g and be placed in 2L three-necked bottle, again according to alcohol oil rate 3:1, catalyst loading 0.4% takes dehydrated alcohol and sodium hydroxide is respectively 300g and 0.4g, and both are poured on dissolved hydrogen sodium oxide in beaker, and completely to be dissolved, all pour in three-necked bottle.Two, the left and right mouth of three-necked bottle is connected condensing reflux pipe, makes ethanol pump around circuit.Middle bottleneck connects motor stirrer, 50 DEG C, under 40r/min condition, and clock reaction 90min.After reaction terminates, reaction soln is poured into 1L and revolve in steaming bottle, constant temperature 45 DEG C, under the rotating speed of 40r/min-50r/min, reclaim ethanol 40min-50min.To be recycled to 3min without ethanol drip into reclaim terminate, after glycerine and fatty acid ethyl ester mixture are poured in 500mL Centrifuge Cup, at rotating speed 4000r/min-5000r/min, centrifugal under time 5min-10min condition, due to the difference of molecular weight and textural association form, glycerine trisodium can be deposited on lower floor after centrifugation, and fatty-acid ethyl ester and refined horse oil are enriched in upper strata.Be separated and obtain refined horse oil, ethyl esterified yield >=90.00%.
Embodiment 2
Take the thick house oil of 12kg and be placed in 100L glass closed reactor, again according to alcohol oil rate 3.8:1, catalyst loading 0.35% takes dehydrated alcohol and sodium hydroxide is respectively 45.6kg and 42g, and both are poured on dissolved hydrogen sodium oxide in stainless steel cask, completely to be dissolved, all pour in reactor.Reactor upper end is connected with condensation reflux unit, 62.5 DEG C, under 60r/min condition, and clock reaction 98min.After reaction terminates, reaction soln is poured into 50L in batches and revolve in steaming bottle, constant temperature 45 DEG C, under the rotating speed of 40r/min-50r/min, reclaim ethanol 40min-50min.To be recycled to 3min without ethanol drip into reclaim terminate, after glycerine and fatty acid ethyl ester mixture are poured in 4L Centrifuge Cup, at rotating speed 4000r/min-5000r/min, centrifugal under time 5min-10min condition.Be separated and obtain refined horse oil, ethyl esterified yield 94.69%.
Embodiment 3
Take the thick house oil of 10kg and be placed in 100L glass closed reactor, again according to alcohol oil rate 5:1, catalyst loading 0.4% takes dehydrated alcohol and sodium hydroxide is respectively 50kg and 40g, and both are poured on dissolved hydrogen sodium oxide in stainless steel cask, and completely to be dissolved, all pour in reactor.Reactor upper end is connected with condensation reflux unit, 70 DEG C, under 80r/min condition, and clock reaction 90min.After reaction terminates, reaction soln is poured into 50L in batches and revolve in steaming bottle, constant temperature 45 DEG C, under the rotating speed of 40r/min-50r/min, reclaim ethanol 40min-50min.To be recycled to 3min without ethanol drip into reclaim terminate, after glycerine and fatty acid ethyl ester mixture are poured in 4L Centrifuge Cup, at rotating speed 4000r/min-5000r/min, centrifugal under time 5min-10min condition.Be separated and obtain refined horse oil, ethyl esterified yield >=90.00%.
The embodiment of the present invention 2 is preparation method be compared with the prior art, and result is as following table:
As can be seen from above correlation data, preparation method of the present invention under the prerequisite keeping higher ethyl ester interest rate, can save time, and saves cost and is more conducive to realizing suitability for industrialized production.And embodiment 2 effect is particularly outstanding.
The final index of the refined horse oil that preparation method of the present invention obtains: unsaturated fatty acid ethyl ester>=40% (ethyl oleate>=30%, ethyl linoleate>=10%
), ethyl palmitate>=30%, and containing a small amount of Ethyl arachidonate.
Preparation method of the present invention, by optimization Test parameter, can save (auxiliary material except raw material) cost more than 50%, further improving production efficiency, saves energy consumption; By Optimizing Process Parameters, more can adapt to suitability for industrialized production, requirement harsh especially do not had to conversion unit, if meet there is sealing, controlled Heating temperature, can stir, the equipment of the condition of condensable backflow; While having above advantage, final ethyl esterified yield still can be made to remain on higher level (more than 90%), and unsaturated fatty acids retention rate reaches more than 40%.
Claims (10)
1. an ethyl esterified house oil preparation method, comprises the steps:
Thick house oil is added in reaction vessel, in house oil quality, according to alcohol oil rate 3-5:1, catalyst loading 0.3-0.4%, by catalyst dissolution after dehydrated alcohol, add reaction vessel, simultaneously turn on agitator, fully mix, at 50-70 DEG C, under rotating speed 40-80r/min condition, clock reaction 90-100min; ; After reaction terminates, reclaim ethanol, the glycerine obtained and fatty acid ethyl ester mixture are carried out centrifugal treating; Treat centrifugal end, get upper strata fluid, refining house oil can be obtained;
Described catalyzer is analytical pure sodium hydroxide; Described dehydrated alcohol is analytical pure.
2. ethyl esterified house oil preparation method according to claim 1, is characterized in that, described reaction vessel is the closed reaction vessel that stirring and condensation reflux unit are housed.
3. ethyl esterified house oil preparation method according to claim 2, it is characterized in that, described reaction vessel is reactor or three-necked bottle.
4. ethyl esterified house oil preparation method according to claim 3, it is characterized in that, described reactor is interlayer heating glass constant temperature stirred autoclave.
5. ethyl esterified house oil preparation method according to claim 1, is characterized in that, described recovery ethanol, uses Rotary Evaporators to carry out, constant temperature 45 DEG C, reclaims ethanol 40min-50min under rotating speed 40r/min-50r/min.
6. ethyl esterified house oil preparation method according to claim 1, is characterized in that, described centrifugal treating, rotating speed 4000r/min-5000r/min, time 5min-10min.
7. ethyl esterified house oil preparation method according to claim 1, comprises the steps:
According to three-necked bottle capacity, take appropriate thick house oil and be placed in one, in thick house oil quality, according to alcohol oil rate 3:1, catalyst loading 0.4%, take dehydrated alcohol and sodium hydroxide respectively, after sodium hydroxide is dissolved in dehydrated alcohol completely, all pour in three-necked bottle; Three-necked bottle is connected condensing reflux pipe, make ethanol pump around circuit; Middle bottleneck connects motor stirrer, 50 DEG C, under 40r/min condition, and clock reaction 90min; After reaction terminates, reaction soln is poured into revolve and steam in bottle, constant temperature 45 DEG C, under the rotating speed of 40r/min-50r/min, reclaim ethanol 40min-50min; To be recycled to 3min without ethanol drip into reclaim terminate, after by glycerine and fatty acid ethyl ester mixture, at rotating speed 4000r/min-5000r/min, centrifugal under time 5min-10min condition; Be separated upper strata fluid and namely obtain refined horse oil.
8. ethyl esterified house oil preparation method according to claim 1, comprises the steps:
According to interlayer heating glass constant temperature stirred autoclave capacity, take appropriate thick house oil to be placed in one, in thick house oil quality, according to alcohol oil rate 3.8:1, catalyst loading 0.35%, take dehydrated alcohol and sodium hydroxide respectively, after sodium hydroxide is dissolved in dehydrated alcohol completely, all pour in reactor; Reactor upper end is connected with condensation reflux unit, 62.5 DEG C, under 60r/min condition, and clock reaction 98min; After reaction terminates, reaction soln is poured into revolve in batches and steam in bottle, constant temperature 45 DEG C, under the rotating speed of 40r/min-50r/min, reclaim ethanol 40min-50min; To be recycled to 3min without ethanol drip into reclaim terminate, after by glycerine and fatty acid ethyl ester mixture, at rotating speed 4000r/min-5000r/min, centrifugal under time 5min-10min condition; Be separated upper strata fluid and namely obtain refined horse oil.
9. ethyl esterified house oil preparation method according to claim 1, comprise the steps:
According to interlayer heating glass constant temperature stirred autoclave capacity, take appropriate thick house oil to be placed in one, in thick house oil quality, according to alcohol oil rate 5:1, catalyst loading 0.4%, take dehydrated alcohol and sodium hydroxide respectively, after sodium hydroxide is dissolved in dehydrated alcohol completely, all pour in reactor; Reactor upper end is connected with condensation reflux unit, 70 DEG C, under 80r/min condition, and clock reaction 90min; After reaction terminates, reaction soln is poured into revolve in batches and steam in bottle, constant temperature 45 DEG C, under the rotating speed of 40r/min-50r/min, reclaim ethanol 40min-50min; To be recycled to 3min without ethanol drip into reclaim terminate, after by glycerine and fatty acid ethyl ester mixture, at rotating speed 4000r/min-5000r/min, centrifugal under time 5min-10min condition; Be separated upper strata fluid and namely obtain refined horse oil.
10. according to the house oil that the arbitrary described ethyl esterified house oil preparation method of claim prepares.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181883A (en) * | 2018-10-24 | 2019-01-11 | 新疆工程学院 | A kind of production technology of refined horse oil ethyl ester |
| CN109666533A (en) * | 2019-01-25 | 2019-04-23 | 新疆天药生物科技有限公司 | Refined horse oil and its refining extracting method and application |
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Application publication date: 20151014 |