CN104017645A - Method for dewaxing peony seed oil by combination of surfactant-crystallization copolymerization and alcohol extraction - Google Patents
Method for dewaxing peony seed oil by combination of surfactant-crystallization copolymerization and alcohol extraction Download PDFInfo
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- CN104017645A CN104017645A CN201410300110.XA CN201410300110A CN104017645A CN 104017645 A CN104017645 A CN 104017645A CN 201410300110 A CN201410300110 A CN 201410300110A CN 104017645 A CN104017645 A CN 104017645A
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Abstract
The invention discloses a method for dewaxing peony seed oil by combination of surfactant-crystallization copolymerization and alcohol extraction, which comprises the following steps: heating peony seed oil to 70-90 DEG C until the wax crystal precipitated at normal temperature is completely dissolved in the peony seed oil, cooling to 50-65 DEG C, adding a surfactant which accounts for 0.08-0.15 wt% of the peony seed oil, slowly cooling while stirring, stopping stirring when the temperature drops to 5-8 DEG C, growing the grain, carrying out centrifugal separation, and taking the supernatant oil for later use; adding an anhydrous ethanol solution into the supernatant oil, transferring into a separating funnel, standing, separating, taking the understratum oil, extracting once, taking the understratum oil, and finally, removing the ethanol solution. By combining the surfactant and ethanol extract phase, the low-viscosity favorable-flowability dewaxed oil with clear and bright color can be obtained; and the method improves the phenomena of premature adhesion and even waxing due to poor dewaxing effect and incapability of effectively removing wax in oil in the traditional dewaxing process.
Description
Technical field
The invention belongs to peony product deep process technology field, the method dewaxing is combined in the brilliant copolymerization of table that is specifically related to a kind of peony seed oil with alcohol extracting.
Background technology
The dewaxing technique of grease starts from later 1940s, in the 1970s and 1980s, attains full development and popularizes.After the nineties, along with making rapid progress and the demand of high-quality plants oil of science and technology, the status of dewaxing in vegetable oil refining process seems more and more important.Due to the crystallization of wax in oil be not people imagine become like that solid wax crystal grain, also can not unconfined slow cooling, wax can not all crystallize into macrobead.Wax, wax crystalline substance in oil suspendible body is a kind of plastic solid particle, affected by temperature, pressure larger, when temperature impact and pressure change, wax crystallization particle is easy to distortion, form fine particle or molecule, for fear of suspendible body wax crystalline substance in separated transport process, be subject to shearing force and pulverize, general centrifuging or the Plate Filtration of adopting in tradition dewaxing technique process, the very thin thickness of filter cloth meanwhile, under the effect of centrifugal force and pressure, in wax crystallization particle, some becomes fine particle, in addition in oil, still uncrystallized waxy molecules group or the small nucleus of wax pass through filter cloth through extruding and enter in pressed oil, thereby make wax content in pressed oil considerably beyond normal value.In existing DEWAXING TECHNIQUE, with the dewaxing of freezing and crystallizing conventional method, advantage is that equipment is simple, reduced investment, and processing ease, shortcoming is that oil-wax is not exclusively separated, pressed oil yield is lower and cloud point is high.Surfactant method degreasing method, advantage is to be beneficial to wax-oil separating, shortcoming be in grease, add tensio-active agent after, it is thoroughly separated with grease that tensio-active agent is difficult to, after long-time placement, because degreasing dewaxing effect is poor, perhaps the molecule of wax fat remnants in oil, can not effectively remove totally by filtration means, and the even wax-like curing presentation of grease that waits of viscous occurred after 3 months the grease bringing, have a strong impact on Vegetable Oil Quality, becoming sour too early of oil even occurs.
Peony seed oil is as new resources, wax content in oil is not also clearly measured, technical study for peony seed oil degreasing dewaxing also has no report, for the dewaxing of peony seed oil perfect desirable technique without comparison so far, and unique feature of the unsaturated fatty acids of the high-content having due to peony seed oil itself, can not merely adopt traditional dewaxing technique to dewax.Therefore, improve traditional dewaxing technique dewaxing effect not obvious, the technical study of exploring peony seed oil degreasing dewaxing is key technical problem and the difficult problem that wish of the present invention solves.
Summary of the invention
The method dewaxing is combined in the brilliant copolymerization of table that the object of this invention is to provide a kind of peony seed oil with alcohol extracting, the method combines tensio-active agent with alcohol extraction, can access that viscosity is little, good fluidity and color clarify bright pressed oil, improved that traditional dewaxing technique dewaxing effect is poor, effectively Ex-all and viscous occurs too early for the grease that brings even forms wax-like phenomenon of wax ester in oil.
The present invention realizes the technical scheme that above-mentioned purpose adopts: the method dewaxing is combined in a kind of brilliant copolymerization of table of peony seed oil with alcohol extracting, concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 70-90 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, after completing, dissolving is cooled to 50-65 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.08-0.15% in peony seed oil, slow cooling under agitation condition again, control reduction 2-3 ℃ per hour, in temperature-fall period, controlling stirring velocity is 10-15r/min, while being cooled to 5-8 ℃, stop stirring, and be incubated 4-8h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 15-20min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, add ethanol solution, stir after 1-1.5h, be transferred to separating funnel interior standing, separatory, take off layer oil, in Zai Xiang lower floor oil, adding quality is the ethanol solution of analytical pure level, stirs 1-1.5h, is transferred in separating funnel standing, separatory, take off layer oil, finally remove ethanolic soln remaining in lower floor's oil under reduced pressure, complete the dewaxing of peony seed oil.
Described tensio-active agent is fatty alcohol-polyoxyethylene ether or sucrose ester.
In described upwards edible vegetable oil, adding the weight ratio of ethanol solution and upper edible vegetable oil is 2-3:0.5-1.5, is 2-6 times of lower floor's weight of oil to the ethanol solution adding in lower floor's oil.
Described ethanolic soln is dehydrated alcohol, be generally analytical pure and top grade is pure, but for reducing costs, the dehydrated alcohol of analytical pure level can meet the processing requirement of degreasing dewaxing, and dehydrated alcohol is that mass concentration is the analytical pure level ethanol solution of 99.5-99.9 %.
Beneficial effect of the present invention:
The present invention utilizes some group and the avidity of wax or the interpolymer of adsorption formation and wax in surfactant, thereby contribute to the crystallization of wax and the growth of crystal grain, be beneficial to wax-oil separation, after centrifugation, in peony seed oil, also contain a small amount of interpolymer residual and free fatty acids and wax.Then utilize similar compatibility principle, and the specific inductivity of ethanol and free fatty acids and wax approaches, differ larger feature with the specific inductivity of grease and thiaminogen, adopt alcohol solvent extraction, residual tensio-active agent crystallite is separated out in ethanol, further from peony seed oil, separate.By this method, not only the tensio-active agent remaining in oil with crystallite is removed, also further improved the decreasing ratio of the wax of crystallite interpolymer form.
Process for dewaxing provided by the invention is by combining tensio-active agent with alcohol extraction, broken away from the unconspicuous shortcoming of vegetables oil tradition dewaxing technique dewaxing effect, peony seed oil clear after this method dewaxing, color and luster is bright, and mobility is better, and transdermal characteristic strengthens, nutrition can not destroyed, after long-term placement, color and luster and mobility are constant, can be used in medicine, makeup and food service industry, as being further promoted to medical oil or used for cosmetic wet goods.
Embodiment
The method dewaxing is combined in the brilliant copolymerization of the table of peony seed oil with alcohol extracting, concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 70-90 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, after completing, dissolving is cooled to 50-65 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.08-0.15% in peony seed oil, slow cooling under agitation condition again, control reduction 2-3 ℃ per hour, in temperature-fall period, controlling stirring velocity is 10-15r/min, while being cooled to 5-8 ℃, stop stirring, and be incubated 4-8h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 15-20min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, add ethanol solution, stir after 1-1.5h, be transferred to separating funnel interior standing, separatory, take off layer oil, in Zai Xiang lower floor oil, add ethanol solution, stir 1-1.5h, be transferred in separating funnel standing, separatory, take off layer oil, finally remove ethanolic soln remaining in lower floor's oil under reduced pressure, complete the dewaxing of peony seed oil.
Described tensio-active agent is fatty alcohol-polyoxyethylene ether or sucrose ester.
The ethanol solution adding in described upwards edible vegetable oil is 2-3:0.5-1.5 with the weight ratio of upper edible vegetable oil, is 2-6 times of lower floor's weight of oil to the ethanol solution adding in lower floor's oil.
below in conjunction with specific embodiment, the present invention will be further described:
embodiment 1:
The method dewaxing is combined in the brilliant copolymerization of the table of peony seed oil with alcohol extracting, concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 70 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, after completing, dissolving is cooled to 50 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.08% in peony seed oil, tensio-active agent is fatty alcohol-polyoxyethylene ether, slow cooling under agitation condition again, control 2 ℃ of reductions per hour, in temperature-fall period, controlling stirring velocity is 10r/min, while being cooled to 5 ℃, stop stirring, and be incubated 4h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 15min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, adding mass concentration is the ethanol solution of 99.5% analytical pure level, the weight ratio of ethanolic soln and upper edible vegetable oil is 2:0.5, stir after 1h, be transferred in separating funnel standing, separatory, take off layer oil, the ethanol solution of the analytical pure level that the mass concentration of 2 times that adds its weight in Zai Xiang lower floor oil is 99.5%, stir 1h, be transferred to separating funnel interior standing, separatory, takes off layer oil, finally remove ethanolic soln remaining in lower floor's oil under reduced pressure, complete the dewaxing of peony seed oil.
embodiment 2:
The method dewaxing is combined in the brilliant copolymerization of the table of peony seed oil with alcohol extracting, concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 90 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, after completing, dissolving is cooled to 65 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.15% in peony seed oil, tensio-active agent is sucrose ester, slow cooling under agitation condition again, control 3 ℃ of reductions per hour, in temperature-fall period, controlling stirring velocity is 15r/min, while being cooled to 8 ℃, stop stirring, and be incubated 8h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 20min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, adding mass concentration is the ethanol solution of 99.5 analytical pure level, and the weight ratio of ethanolic soln and upper edible vegetable oil is 3:1.5, after stirring 1.5h, be transferred in separating funnel standing, separatory, takes off layer oil, the analytical pure ethanol solution that the mass concentration of 6 times that adds its weight in Zai Xiang lower floor oil is 99.5, stir 1.5h, be transferred to separating funnel interior standing, separatory, takes off layer oil, finally remove ethanolic soln remaining in lower floor's oil under reduced pressure, complete the dewaxing of peony seed oil.
embodiment 3:
The method dewaxing is combined in the brilliant copolymerization of the table of peony seed oil with alcohol extracting, concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 80 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, after completing, dissolving is cooled to 60 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.12% in peony seed oil, tensio-active agent is fatty alcohol-polyoxyethylene ether, slow cooling under agitation condition again, control 3 ℃ of reductions per hour, in temperature-fall period, controlling stirring velocity is 12r/min, while being cooled to 7 ℃, stop stirring, and be incubated 6h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 18min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, adding mass concentration is the ethanol solution of the pure level of top grade of 99.9 %, the weight ratio of ethanolic soln and upper edible vegetable oil is 2.5:1, stir after 1.2h, be transferred in separating funnel standing, separatory, take off layer oil, the mass concentration of 4 times that adds its weight in Zai Xiang lower floor oil is the pure ethanol solution of top grade of 99.9 %, stir 1.5h, be transferred to separating funnel interior standing, separatory, takes off layer oil, finally remove ethanolic soln remaining in lower floor's oil under reduced pressure, complete the dewaxing of peony seed oil.
embodiment 4:
The method dewaxing is combined in the brilliant copolymerization of the table of peony seed oil with alcohol extracting, concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 70 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, after completing, dissolving is cooled to 60 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.1% in peony seed oil, tensio-active agent is fatty alcohol-polyoxyethylene ether, slow cooling under agitation condition again, control 3 ℃ of reductions per hour, in temperature-fall period, controlling stirring velocity is 12r/min, while being cooled to 7 ℃, stop stirring, and be incubated 6h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 18min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, adding mass concentration is the pure ethanol solution of top grade of 99.9 %, and the weight ratio of ethanolic soln and upper edible vegetable oil is 2.5:1, stirs after 1h, be transferred in separating funnel standing, separatory, takes off layer oil, and the mass concentration of 4 times that adds its weight in Zai Xiang lower floor oil is the pure ethanol solution of top grade of 99.9 %, stir 1.5h, be transferred to separating funnel interior standing, separatory, takes off layer oil, finally remove ethanolic soln remaining in lower floor's oil under reduced pressure, complete the dewaxing of peony seed oil.
experimental data
Through coming unstuck, depickling, totally 7 parts of the peony seed oils of decolouring and deodorization, directly measure absorbancy for the 1st part, the 2nd part adopts the rear absorbancy of measuring of cold method dewaxing, the 3rd part adopts the rear absorbancy of measuring of sucrose ester surfactant method dewaxing, the 4th part adopts the rear absorbancy of measuring of fatty alcohol-polyoxyethylene ether surfactant method dewaxing, the 5th part adopts the rear absorbancy of measuring of anhydrous ethanol solvent method dewaxing, the 6th part adopts sucrose ester and the rear absorbancy of measuring of extraction using alcohol dewaxing, the 7th part adopts fatty alcohol-polyoxyethylene ether and the rear absorbancy of measuring of extraction using alcohol dewaxing, the 6th part and the 7th part of method adopting are the degreasing wax fractionation process of peony seed oil provided by the invention.
Above-mentioned dissimilar peony seed oil is adopted respectively to ultraviolet spectrophotometry, survey its absorbancy at 315nm place, measuring result is as shown in table 1:
Table 1:
In table 1, its absorbancy is little, and transmittance is larger, and oil viscosity is less, and mobility is relatively good.
Known by above-mentioned data analysis contrast, peony seed oil adopts the best degreasing wax fractionation process that the method for fatty alcohol-polyoxyethylene ether and extraction using alcohol combination is peony seed oil.
Above 7 parts of oil are placed for a long time, and 1-5 part starts to engender respectively caking phenomenon about 3 months, after 6 months, lump completely, and the 6th part and the 7th part of oil, the dewaxing effect that color and luster and mobility keep is general as before.
Claims (3)
1. the method dewaxing is combined in the brilliant copolymerization of the table of peony seed oil with alcohol extracting, it is characterized in that: concrete steps are as follows:
Learnt from else's experience and came unstuck, depickling, the peony seed oil of decolouring and deodorization is as starting material, peony seed oil is heated to 70-90 ℃, until after the wax crystal of separating out during normal temperature is dissolved in peony seed oil completely, be cooled to 50-65 ℃, then while stirring to the tensio-active agent that adds peony seed oil weight 0.08-0.15% in peony seed oil, slow cooling under agitation condition again, control reduction 2-3 ℃ per hour, in temperature-fall period, controlling stirring velocity is 10-15r/min, while being cooled to 5-8 ℃, stop stirring, and be incubated 4-8h and carry out growing the grain, after growing the grain finishes under 3000r/min rotating speed centrifugation 15-20min, get edible vegetable oil, standby,
Upwards in edible vegetable oil, add ethanol solution, stir after 1-1.5h, be transferred to separating funnel interior standing, separatory, takes off layer oil; In Zai Xiang lower floor oil, add ethanol solution, stir 1-1.5h, be transferred to separating funnel interior standing, separatory, takes off layer oil again, finally removes ethanolic soln remaining in lower floor's oil under reduced pressure, completes the dewaxing of peony seed oil.
2. the method dewaxing is combined in the brilliant copolymerization of the table of a kind of peony seed oil as claimed in claim 1 with alcohol extracting, it is characterized in that: described tensio-active agent is fatty alcohol-polyoxyethylene ether or sucrose ester.
3. the method dewaxing is combined in the brilliant copolymerization of the table of a kind of peony seed oil as claimed in claim 1 with alcohol extracting, it is characterized in that: the ethanol solution adding in described upwards edible vegetable oil is 2-3:0.5-1.5 with the weight ratio of upper edible vegetable oil, is 2-6 times of lower floor's weight of oil to the ethanol solution adding in lower floor's oil.
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Cited By (8)
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| CN104224633A (en) * | 2014-09-30 | 2014-12-24 | 河南科技大学 | Pure peony skin-care essential oil and preparation method thereof |
| CN104277913A (en) * | 2014-10-20 | 2015-01-14 | 河南工业大学 | Method for removing floccules in sesame oil |
| CN104877757A (en) * | 2015-06-05 | 2015-09-02 | 武汉轻工大学 | High-acid-value rice bran oil synchronous deacidification and dewaxing process |
| CN105602712A (en) * | 2016-03-09 | 2016-05-25 | 中国农业科学院油料作物研究所 | Vegetable oil processing method |
| CN107937130A (en) * | 2017-11-18 | 2018-04-20 | 陈馨雅 | A kind of soybean oil treatment process for capacitor impregnant |
| CN109234019A (en) * | 2018-11-14 | 2019-01-18 | 陈同翔 | A kind of edible fat production technique process for dewaxing |
| CN111019760A (en) * | 2019-12-26 | 2020-04-17 | 云南省玉溪市云溪香精香料有限责任公司 | Grease wax separation process and device for dewaxing and degreasing by dynamic freezing crystallization |
| CN113528237A (en) * | 2020-04-22 | 2021-10-22 | 华中农业大学 | Process for deodorizing edible oil by steam distillation with nonionic surfactant |
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| CN104224633A (en) * | 2014-09-30 | 2014-12-24 | 河南科技大学 | Pure peony skin-care essential oil and preparation method thereof |
| CN104224633B (en) * | 2014-09-30 | 2017-07-21 | 河南科技大学 | A kind of pure tree peony heal-care essential oil and preparation method thereof |
| CN104277913A (en) * | 2014-10-20 | 2015-01-14 | 河南工业大学 | Method for removing floccules in sesame oil |
| CN104877757A (en) * | 2015-06-05 | 2015-09-02 | 武汉轻工大学 | High-acid-value rice bran oil synchronous deacidification and dewaxing process |
| CN104877757B (en) * | 2015-06-05 | 2018-02-16 | 武汉轻工大学 | Peracid value rice bran oil synchronization depickling dewaxing technique |
| CN105602712A (en) * | 2016-03-09 | 2016-05-25 | 中国农业科学院油料作物研究所 | Vegetable oil processing method |
| CN105602712B (en) * | 2016-03-09 | 2019-10-01 | 中国农业科学院油料作物研究所 | One vegetable oil processing method |
| CN107937130A (en) * | 2017-11-18 | 2018-04-20 | 陈馨雅 | A kind of soybean oil treatment process for capacitor impregnant |
| CN109234019A (en) * | 2018-11-14 | 2019-01-18 | 陈同翔 | A kind of edible fat production technique process for dewaxing |
| CN111019760A (en) * | 2019-12-26 | 2020-04-17 | 云南省玉溪市云溪香精香料有限责任公司 | Grease wax separation process and device for dewaxing and degreasing by dynamic freezing crystallization |
| CN113528237A (en) * | 2020-04-22 | 2021-10-22 | 华中农业大学 | Process for deodorizing edible oil by steam distillation with nonionic surfactant |
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