CN104017645B - The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction - Google Patents
The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction Download PDFInfo
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- CN104017645B CN104017645B CN201410300110.XA CN201410300110A CN104017645B CN 104017645 B CN104017645 B CN 104017645B CN 201410300110 A CN201410300110 A CN 201410300110A CN 104017645 B CN104017645 B CN 104017645B
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Abstract
The table crystalline substance copolymerization that the invention discloses a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprise the following steps that and peony seed oil is heated to 70 90 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, being cooled to 50 65 DEG C, being subsequently adding the surfactant of peony seed oil weight 0.08 0.15%, slow cooling the most under agitation, to stopping stirring, growing the grain, centrifugation when 58 DEG C, take edible vegetable oil, standby;Edible vegetable oil upwards adds ethanol solution, stands in being transferred to separatory funnel, separatory, take off layer oil, repeat extraction once, take off layer oil, finally remove ethanol solution.Surfactant is combined by the present invention with ethanol extraction phase, can obtain that viscosity is little, good fluidity and the bright dewaxed oil of color clarification, improve that tradition dewaxing technique dewaxing effect is poor, in oil wax ester can not effectively Ex-all and the oils and fats that brings occurs to early viscous and even forms wax-like phenomenon.
Description
Technical field
The invention belongs to peony product deep process technology field, the table crystalline substance copolymerization being specifically related to a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction.
Background technology
The dewaxing technique of oils and fats starts from later 1940s, attains full development in the 1970s and 1980s and popularizes.After the nineties, along with making rapid progress and the demand of high-quality plants oil of science and technology, dewaxing status during vegetable oil refining seems more and more important.Owing to wax crystallization in oil is not to become solid waxiness crystal grain as people are imagined, it is also not possible to unconfined slow cooling, i.e. wax can not all crystallize into bulky grain.Wax, wax crystalline substance in oil suspendible body is a kind of plastic solid particle, affected bigger by temperature, pressure, when temperature impact and pressure change, wax crystallization granule is easily deformed, form fine particle or molecule, in order to avoid suspendible body wax crystalline substance in separating transport process is pulverized by shearing force, general employing centrifugal filtration or plate-and-frame filtration during tradition dewaxing technique, the meanwhile very thin thickness of filter cloth, under the effect of centrifugal force and pressure, in wax crystallization granule, some becomes fine particle, in addition during in oil, the most uncrystallized waxy molecules group or the small nucleus of waxiness pass through filter cloth entrance dewaxed oil through extruding, so that the wax content in dewaxed oil is considerably beyond normal value.In existing DEWAXING TECHNIQUE, dewaxing with freezing and crystallizing conventional method, advantage is that equipment is simple, reduced investment, processing ease, and shortcoming is that oil-wax separates not exclusively, and dewaxed oil yield is relatively low and cloud point is high.Surfactant method defat method, advantage is beneficially wax-oil separating, shortcoming is in oils and fats after interpolation surfactant, and surfactant is difficult to thoroughly separate with oils and fats, after long-time placement, owing to defat dewaxing effect is poor, perhaps the molecule that in oil, wax fat is remaining, can not effectively be removed totally by filters, and the oils and fats brought occurs the most wax-like oils and fats solidification presentation that waits of viscous after 3 months, have a strong impact on Vegetable Oil Quality, becoming sour too early of oil even occurs.
Peony seed oil is as new resources, paraffin content in oil the most clearly measures, technical study for peony seed oil defat dewaxing also has no report, dewaxing for peony seed oil does not has fairly perfect preferable technique so far, and unique feature of the unsaturated fatty acid of the high-load being had due to peony seed oil itself, it is impossible to merely use traditional dewaxing technique to dewax.Therefore, improving traditional dewaxing technique dewaxing effect inconspicuous, the technical study exploring peony seed oil defat dewaxing is the key technical problem to be solved of the present invention and a difficult problem.
Summary of the invention
The table crystalline substance copolymerization that it is an object of the invention to provide a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, surfactant is combined by the method with ethanol extraction phase, can obtain that viscosity is little, good fluidity and the bright dewaxed oil of color clarification, improve that tradition dewaxing technique dewaxing effect is poor, in oil wax ester can not effectively Ex-all and the oils and fats that brings occurs to early viscous and even forms wax-like phenomenon.
The present invention realizes above-mentioned purpose and the technical scheme is that the table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprises the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 70-90 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, dissolving is cooled to 50-65 DEG C after completing, the surfactant of peony seed oil weight 0.08-0.15% is added the most while stirring in peony seed oil, slow cooling the most under agitation, control to reduce 2-3 DEG C per hour, controlling mixing speed in temperature-fall period is 10-15r/min, it is cooled to when 5-8 DEG C stop stirring, and be incubated 4-8h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 15-20min, take edible vegetable oil, standby;
Edible vegetable oil upwards adds ethanol solution, after stirring 1-1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, layer oil adds ethanol solution that quality is analytical pure level still further below, stirs 1-1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil.
Described surfactant is fatty alcohol-polyoxyethylene ether or sucrose ester.
The weight ratio adding ethanol solution and upper edible vegetable oil in described upwards edible vegetable oil is 2-3:0.5-1.5,2-6 times that ethanol solution is lower floor's weight of oil added in lower floor's oil.
Described ethanol solution is that dehydrated alcohol, generally analytical pure and top grade are pure, but for reduce cost, the dehydrated alcohol of analytical pure level can meet defat dewaxing technological requirement, i.e. dehydrated alcohol be mass concentration be the analytical pure level ethanol solution of 99.5-99.9 %.
Beneficial effects of the present invention:
The present invention utilizes some group and the affinity of wax or adsorption in surfactant to form the copolymer with wax, thus contribute to the crystallization of wax and the growth of crystal grain, it is beneficial to wax-oil separation, after being performing centrifugal separation on, possibly together with a small amount of copolymer residual and free fatty and wax in peony seed oil.Then similar compatibility principle is utilized, and the feature that ethanol is close with the dielectric constant of free fatty and wax, bigger with the dielectric constants of oils and fats and oryzanol, use alcohol solvent extraction, the surfactant crystallite of residual is separated out in ethanol, separates from peony seed oil further.By this method, not only the surfactant remained in crystallite in oil is removed, further improves the removal efficiency of the wax of crystallite copolymer form.
The process for dewaxing that the present invention provides is by being combined surfactant with ethanol extraction phase, break away from the vegetable oil tradition unconspicuous shortcoming of dewaxing technique dewaxing effect, peony seed oil clear after the method dewaxes, bright color, mobility is preferable, and transdermal characteristic strengthens, nutrition will not be destroyed, after long-term placement, color and luster and mobility are constant, can be used in medicine, cosmetics and food service industry, as being promoted to medical oil or cosmetic oil etc. further.
Detailed description of the invention
The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprises the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 70-90 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, dissolving is cooled to 50-65 DEG C after completing, the surfactant of peony seed oil weight 0.08-0.15% is added the most while stirring in peony seed oil, slow cooling the most under agitation, control to reduce 2-3 DEG C per hour, controlling mixing speed in temperature-fall period is 10-15r/min, it is cooled to when 5-8 DEG C stop stirring, and be incubated 4-8h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 15-20min, take edible vegetable oil, standby;
Edible vegetable oil upwards adds ethanol solution, after stirring 1-1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, layer oil adds ethanol solution still further below, stirs 1-1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil.
Described surfactant is fatty alcohol-polyoxyethylene ether or sucrose ester.
The ethanol solution added in described upwards edible vegetable oil is 2-3:0.5-1.5 with the weight ratio of upper edible vegetable oil, 2-6 times that ethanol solution is lower floor's weight of oil added in lower floor's oil.
Below in conjunction with specific embodiment, the present invention will be further described:
Embodiment
1
:
The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprises the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 70 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, dissolving is cooled to 50 DEG C after completing, the surfactant of peony seed oil weight 0.08% is added the most while stirring in peony seed oil, surfactant is fatty alcohol-polyoxyethylene ether, slow cooling the most under agitation, control to reduce by 2 DEG C per hour, controlling mixing speed in temperature-fall period is 10r/min, it is cooled to when 5 DEG C stop stirring, and be incubated 4h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 15min, take edible vegetable oil, standby;
Upwards adding the ethanol solution of the analytical pure level that mass concentration is 99.5% in edible vegetable oil, ethanol solution is 2:0.5 with the weight ratio of upper edible vegetable oil, after stirring 1h, stand in being transferred to separatory funnel, separatory, takes off layer oil, adds the ethanol solution that mass concentration is the analytical pure level being 99.5% of 2 times of its weight still further below in layer oil, stirring 1h, stand in being transferred to separatory funnel, separatory, take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil.
Embodiment
2
:
The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprises the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 90 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, dissolving is cooled to 65 DEG C after completing, the surfactant of peony seed oil weight 0.15% is added the most while stirring in peony seed oil, surfactant is sucrose ester, slow cooling the most under agitation, control to reduce by 3 DEG C per hour, controlling mixing speed in temperature-fall period is 15r/min, it is cooled to when 8 DEG C stop stirring, and be incubated 8h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 20min, take edible vegetable oil, standby;
Upwards adding the ethanol solution of the analytical pure level that mass concentration is 99.5 in edible vegetable oil, ethanol solution is 3:1.5 with the weight ratio of upper edible vegetable oil, after stirring 1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, the mass concentration of add its weight still further below in layer oil 6 times be 99.5 analytical pure ethanol solution, stirring 1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil.
Embodiment
3
:
The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprises the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 80 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, dissolving is cooled to 60 DEG C after completing, the surfactant of peony seed oil weight 0.12% is added the most while stirring in peony seed oil, surfactant is fatty alcohol-polyoxyethylene ether, slow cooling the most under agitation, control to reduce by 3 DEG C per hour, controlling mixing speed in temperature-fall period is 12r/min, it is cooled to when 7 DEG C stop stirring, and be incubated 6h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 18min, take edible vegetable oil, standby;
Upwards adding the ethanol solution of the pure level of top grade that mass concentration is 99.9 % in edible vegetable oil, ethanol solution is 2.5:1 with the weight ratio of upper edible vegetable oil, after stirring 1.2h, stand in being transferred to separatory funnel, separatory, takes off layer oil, adds the pure ethanol solution of the top grade that mass concentration is 99.9 % of 4 times of its weight still further below in layer oil, stirring 1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil.
Embodiment
4
:
The table crystalline substance copolymerization of a kind of peony seed oil is combined the method carrying out dewaxing with alcohol extraction, specifically comprises the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 70 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, dissolving is cooled to 60 DEG C after completing, the surfactant of peony seed oil weight 0.1% is added the most while stirring in peony seed oil, surfactant is fatty alcohol-polyoxyethylene ether, slow cooling the most under agitation, control to reduce by 3 DEG C per hour, controlling mixing speed in temperature-fall period is 12r/min, it is cooled to when 7 DEG C stop stirring, and be incubated 6h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 18min, take edible vegetable oil, standby;
Upwards adding the pure ethanol solution of top grade that mass concentration is 99.9 % in edible vegetable oil, ethanol solution is 2.5:1 with the weight ratio of upper edible vegetable oil, after stirring 1h, stand in being transferred to separatory funnel, separatory, takes off layer oil, adds the pure ethanol solution of the top grade that mass concentration is 99.9 % of 4 times of its weight still further below in layer oil, stirring 1.5h, stand in being transferred to separatory funnel, separatory, take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil.
Experimental data
Through degumming, deacidification, decolouring and the peony seed oil totally 7 parts of deodorize, 1st part of direct measurement absorbance, 2nd part uses measurement absorbance after freezing method dewaxing, 3rd part uses measurement absorbance after the dewaxing of sucrose ester surfactants method, 4th part uses measurement absorbance after the dewaxing of fatty alcohol-polyoxyethylene ether surfactant method, 5th part uses measurement absorbance after the dewaxing of anhydrous ethanol solvent method, 6th part uses measurement absorbance after sucrose ester and ethanol extraction dewaxing, 7th part uses measurement absorbance after fatty alcohol-polyoxyethylene ether and ethanol extraction dewaxing, 6th part and the 7th part of method used are the defat lost-wax process of the peony seed oil that the present invention provides.
Above-mentioned different types of peony seed oil being respectively adopted ultraviolet spectrophotometry, surveys its absorbance at 315nm, measurement result is as shown in table 1:
Table 1:
In table 1, its absorbance is little, and light transmittance is the biggest, and oil viscosity is less, and mobility is relatively good.
Being contrasted by above-mentioned data analysis, peony seed oil uses the optimal defat lost-wax process that method is peony seed oil that fatty alcohol-polyoxyethylene ether and ethanol extraction combine.
Above 7 parts of oil are placed for a long time, and 1-5 part started to engender caking phenomenon respectively at about 3 months, lumpd completely after 6 months, and the dewaxing effect that the 6th part and the 7th part of oil, color and luster and mobility keep is the most general.
Claims (1)
1. the table crystalline substance copolymerization of a peony seed oil is combined the method carrying out dewaxing with alcohol extraction, it is characterised in that: specifically comprise the following steps that
Learnt from else's experience degumming, deacidification, the peony seed oil of decolouring and deodorize is as raw material, peony seed oil is heated to 70-90 DEG C, until after the waxiness crystal separated out during room temperature is completely dissolved in peony seed oil, it is cooled to 50-65 DEG C, the surfactant of peony seed oil weight 0.08-0.15% is added the most while stirring in peony seed oil, described surfactant is sucrose ester, slow cooling the most under agitation, control to reduce 2-3 DEG C per hour, controlling mixing speed in temperature-fall period is 10-15r/min, it is cooled to when 5-8 DEG C stop stirring, and be incubated 4-8h and carry out growing the grain, growing the grain terminate after under 3000r/min rotating speed centrifugation 15-20min, take edible vegetable oil, standby;
Edible vegetable oil upwards adds ethanol solution, after stirring 1-1.5h, stands in being transferred to separatory funnel, separatory, take off layer oil;Layer oil adds ethanol solution still further below, stirs 1-1.5h, stand in being transferred to separatory funnel, separatory, again take off layer oil, finally remove ethanol solution remaining in lower floor's oil under reduced pressure, i.e. complete the dewaxing of peony seed oil;The ethanol solution added in described upwards edible vegetable oil is 2-3:0.5-1.5 with the weight ratio of upper edible vegetable oil, 2-6 times that ethanol solution is lower floor's weight of oil added in lower floor's oil.
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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 |
CN104277913B (en) * | 2014-10-20 | 2017-06-23 | 河南工业大学 | Flocculation material removal methods in a kind of sesame oil |
CN104877757B (en) * | 2015-06-05 | 2018-02-16 | 武汉轻工大学 | Peracid value rice bran oil synchronization depickling dewaxing technique |
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 |
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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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