CN1869182A - Method of extracting cotton seed oil - Google Patents

Method of extracting cotton seed oil Download PDF

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Publication number
CN1869182A
CN1869182A CN 200610090688 CN200610090688A CN1869182A CN 1869182 A CN1869182 A CN 1869182A CN 200610090688 CN200610090688 CN 200610090688 CN 200610090688 A CN200610090688 A CN 200610090688A CN 1869182 A CN1869182 A CN 1869182A
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oil
filter
cooling
oleum gossypii
gossypii semen
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CN 200610090688
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CN100408660C (en
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白长军
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Abstract

The invention relates to cotton oil dividing-extraction method. It adopts dry process vacuum crystallization dividing-extraction technique to process dividing-extraction, diaphragm press filtration, compressed air to sweep pressure filter, and hot oil to dissolve residual solid fat. The processed cotton oil can use as first level salad oil. Its lucidity time can reach over 240 hours at zero centigrade degree. The processed solid fat can be used as the material for broil oil, margarine, cocoa butter, saturated fatty acid, and so on.

Description

The method that a kind of cotton seed oil is carried
Affiliated technical field
The present invention relates to the oil and foodstuffs manufacture field, relate to a kind of greasy method of refining, be specifically related to the method that a kind of cotton seed oil is put forward.
Background technology
Oleum Gossypii semen is the byproduct of cotton planting industry, is one of edible oil of countries in the world.Oleum Gossypii semen is a kind of good frying oil, and good stability during frying is used the Oleum Gossypii semen deep fried foodstuff, and color and luster is vivid, excellent in taste, so Oleum Gossypii semen is modulated into mixed oil with rapeseed oil, soybean oil usually, it is very suitable being used for cooking.Owing to contain abundant essential fatty acid in the Oleum Gossypii semen, wherein oleic acid and linoleic content 70%-80% also have the saturated fatty acid of 20%-30% in addition.The saturated fatty acid zero pour is higher, and during low tempertaure storage, these dystectic saturated fatty acids can be separated out from oil, makes its retrogradation and even solidifies, and causes the oil product poor mobile performance, is difficult for storage.Also contain a small amount of wax in the grease, the wax of trace (5PPM) can make cloud point and cloud point raise, the transparency and the digestibility of oil product are reduced, and when grease is cooked, can smolder and produce the people's smell of choking, make flavour and palatability variation, thereby reduced the quality of the nutritive value and the fatty foods of edible oil.On the other hand, wax is important industrial raw material, can be used for making paraffin paper, water-resisting agent, gloss-imparting agent etc.The grease branch is carried and can be classified into single relatively product with forming complicated natural fats and oils, improves the conformability of grease to different service requirementss, enlarges greasy purposes, improves greasy use value and economic worth.
Be subjected to the grease branch to put forward technology limitation at present, the industrial liquid oil and the isolating operation of solid fat that can only realize with different melting points.This fusing point difference of utilizing dissimilar sweet three esters calls degreasing to solid fat in the natural fats and oils and liquid oils separating process.Degreasing has two kinds of purposes, and a kind of is for developing, utilize solid fat; Usually adopt degree of saturation to be used for the solid-state fat of shortening, oleomargarine, substitute of cocoa fat production usefulness than higher grease, the solid fat that generally obtains is many and liquid oils is fewer; Another kind is for improving the low temperature use properties of liquid oil, adopt the lower grease production salad oil of degree of saturation usually, and the liquid oils that obtains is many and solid fat is fewer.It is a kind of that the Oleum Gossypii semen degreasing belongs to the back exactly.There is acyloxy in the wax molecule in the cotton oil, make wax have faint polarity, therefore wax is a kind of lipophilic compound that has the slightly water-wet base, when temperature is higher than 40 ℃ a little less than the polarity of wax, be dissolved in the grease, the ester bond polarity of wax strengthened when temperature was lower than 30 ℃, and wax forms crystallization and separates out, and goes into more stable colloid system.It is exactly the process of degreasing dewaxing that the branch of cotton oil is carried.Divide at present the technology of carrying to be applied to industrially mainly contain that the tensio-active agent branch is carried, the solvent branch is carried and the dry method branch is carried.
The 1950's, the tensio-active agent fractionation technology has the branch that is used for plam oil and palm-kernel oil lipid acid etc. on a small scale to carry.Liquid oil and solid fat adopt disk centrifugal separator to improve separation efficiency.Today, because the pollution that high cost and the finished product are subjected to tensio-active agent, this technology has lost its magnetism.Solvent branch formulation is used for producing the fusing point product similar to theobroma oil.Carry plam oil intermediate component PMF as plam oil with the solvent method branch, PMF is as the raw material of producing cocoa butter equivalent CBE (Cocoa Butter Equivalent).The characteristics that the solvent branch is carried are that branch is carried the efficient height, Gu the fat constituent mass is good.But its cost of investment is big, productive expense is high, requires design of workshop, extra safety control is provided when producing as the inflammableness of the hexane of solvent, acetone, Virahol.Therefore, the solvent branch is carried and only is used for production added value high product.It is the simplest and the most cheap separating technology that the dry method branch is carried.Under controlled chilling, melt oily partial crystallization to outlet temperature, adopt vacuum filter or filter press membrane to remove residual liquid subsequently.Because dry method divides extracting method constantly to develop, increasing various fat are just with maybe carrying with the branch that this method is carried out highly selective.Usually carry the various products that to produce with the solvent branch, equally also can carry and obtaining with the dry method branch.Development along with crystallisation by cooling, filtering technique, the dry method fractionation technology is widely used in multiple greasy processing, by selective freezing condition, separation temperature, adopt different routes can obtain multiple different branch and carry product, because the dry method branch is carried and is the physically modified process, no trans acids generates in the production, catalyst-free pollutes, so the dry method branch is carried and being had a extensive future.
Summary of the invention
Greasy branch is carried and is divided into three big steps: the 1st, and freezing, the 2nd, crystallization, the 3rd, filter.Divide the quality of putting forward effect to depend primarily on this three big step and selected minute extracting method.The frozen liq temperature that the grease branch is carried is-5 ℃~-10 ℃ at the cooling liqs medium of crystallizer generally, frozen liq circulated in adding in the cover of crystallizer, general factory adopts chilled brine, but salt solution can corrode crystallizer, we adopt ethylene glycol solution to do medium, the good non-corrosiveness of heat exchange effect.Crystallization is the key that branch is carried, and it relates to the composition of product and distinctness that thus obtained branch is put forward cut rerum natura aspect changes.Cooling and lock out operation must carry out in a kind of more experimental mode under very strict control condition.Require crystallization to form big, spheric, crystal grain uniform and stable, that anti-mechanical stress is strong.The total characteristics of crystallizer will have big cooling area, high heat transfer coefficient [k=150-170W/ (m 2. ℃)], stir well-balanced, speed control by frequency variation.Aspect controlled cooling technology, according to the characteristics of raw material with from product requirement, by selective freezing condition and separation temperature, PLC controlled chilling speed.Usually oil cools off according to predetermined temperature of cooling water curve, or cools off according to oil and cooling circulating water difference curve, to form suitable crystal seed and to control it good condition that provides of filtering is provided.In the process of freezing and crystallizing, crystallizer and water cycle vacuum pump link together, and form vacuum in jar, help reducing the crystalline temperature.Filter general vacuum filter and/or the membrane filtration machine of adopting, the more advantage that arrives with vacuum filter thin in comparison membrane filtration function, as liquid oil yield height, the filter operations and maintenance is convenient etc., after filter had filtered, the fluid oil of blowing with pressurized air had in the wet cyclone of filler through top earlier and separates the back entering temporary the filling, also dissolves clean solid fat with deep fat, and filter also has the hot water heating cycle, is beneficial to clean residual solid fat.For the advance and the convenience of technology, we carry with the dry method branch.For economy with the requirement of producing, the diaphragm filter press that we select the energy continous way to produce filters production technique.
Adopt the technology of this invention can obtain following beneficial effect: 1 emits no waste water; 2 have adopted vacuum crystallization, and crystallization effect is good, and crystal is big and solid, is beneficial to filtration; 3 process continous-stables, the material turnover is convenient; 4 quality producies are better, and the yield of liquid oil is than higher, without any the pollution of solvent cleaner; 5 reduce production costs with any solvent owing to not needing;
Whole technological process mainly is divided into following three phases: the one, and cooling, the 2nd, crystallization, the 3rd, filter.
1, cooling
As cooling for the first time in the decolouring Oleum Gossypii semen watercooler of raw material, the decolouring Oleum Gossypii semen is reduced to about 70 ℃ from about 110 ℃, enters oil-oil heat exchanger then and carries out cooling second time, and the Oleum Gossypii semen that decolours is reduced to about 45 ℃ from about 70 ℃.This twice cooling mainly is to make oil cooling fully before entering crystallizer, and oiling-oil heat exchanger is for heat is utilized fully.
2, crystallization
Temperature by crystallizer coil pipe internal cooling liquid in the CONTROL PROCESS realizes the control to the cotton oil crystallisation process.The control of chilled liquid temperature is by temperature sensor, and PLC finishes for the control valve of basic temperature regulator and band steady arm.Refrigerative decolouring Oleum Gossypii semen enters crystallizer, the cooling area and the whipping process of crystallizer have material impact for crystallisation process, the Cooling Design of crystallizer inside, the design of cooling tube no matter be flat spin or vertical around, all need to guarantee enough cooling areas, cooling area is at 7m 2/ m 3-8m 2/ m 3Can obtain crystallization effect preferably,, can increase chuck to guarantee cooling area at the crystallization tank skin in order to prevent extreme case.Cooling area is not enough, can cause phenomenons such as grease is clamminess, crystal dissolves again, filter cake is defective, the pressure filter deslagging is not smooth easily.Whipping device normally is with mechanically operated propeller stirrer, stirring velocity is based on the Frequency Converter Control of PLC, stirring helps realizing greasy controlled cooling and crystallization, the cooling grease stirs can realize the heat transmission better, make that liberated heat can in time be distributed in the crystallisation process, the assurance mixing of materials is even, promotes crystalline to grow up, and suitable stirring velocity is 10r/min~15r/min, can stir quicker during beginning, crystal is collided mutually, and heat scatters, but can not be too fast, can smash crystal too soon, in the growing the grain stage, can slow down stirring velocity, so that go into big and hard crystal.The time that stops in crystallizer is 24h-36h, the crystalline heat-eliminating medium is an ethylene glycol solution, ethylene glycol solution is done medium, good and the non-corrosiveness of heat exchange effect, the temperature of heat-eliminating medium is-5 ℃~-10 ℃, the crystalline temperature is 5 ℃~7 ℃, refrigerative speed can not be too fast, too fast crystal growth is bad, brings difficulty to filtration, with 2 ℃ of-4 ℃/h for well.Temperature recovery is controlled in 0.5 ℃ in the crystallisation process.Temperature recovery is too high, just is unfavorable for crystal growth, and the serious need of situation avoid the measure that grease crystallization latter temperature gos up normally to adjust the cooling menu this batch grease crystallization again, prolong rearing crystal time, and the heat of crystals is distributed as far as possible.In the process of freezing and crystallizing, crystallizer and water cycle vacuum pump link together, and form vacuum in jar, and the vacuum tightness in jar helps reducing the crystalline temperature so generally at 30-40mbar, promotes crystallization.If the crystalline result is not very desirable, this soup compound can send back to petroleum tank and reprocess then by the Crude oil heater heating that circulates again.
3, filter
Adopt the barrier film press filtration, the press filtration area is Oleum Gossypii semen 6m per ton 2-8m 2, pressure filter presses together filter plates by hydraulic efficiency plant, filter plates alternately is made up of two kinds of filter plates, a kind of be diaphragm plate (membrane plate) a kind of be chamber panel (chamber plate).Plate is covered by filter cloth, and the filter cloth material is a polypropylene, so that separate fully with filter cake, and cleans easily.Membranous material also is a polypropylene, and diaphragm and filter cloth contact part have the circular flat projection, supports so that good filtrate channel and filter cloth to be provided.When cutting out, pressure filter forms filter chamber between the filter plate, liquid enters the filter chamber rear filtrate and discharges from the hole on the filter plate by filter cloth, and filter cake is trapped in the filter chamber, and filter cloth and filter cake form resistance to oil-feed, increasing when resistance, stop oil-feed when in filter chamber, forming closely filter cake.Feed the barrier film extrusion medium in diaphragm plate, drain the filter cake in the filter chamber, with pressurized air filter is purged at last, the liquid oil of purging has the cyclonic separator of filter screen through top, enters temporary jar of liquid oil then, collects oily oil pump and returns recycle.Opening pressure filter after the pressure release is discharged to filter cake in the stearic receiving tank.Solid fat on the filter cloth is melted in the filter frame internal recycle with the hot water of hot-water cylinder and flows, the solid fat of fusing is gone in the stearic receiving tank, be the washing and filtering device, deposit a spot of deep fat in the deep fat jar, by pump at the filter internal recycle, melt all resistatess, this part oil regathers the deep fat jar or collects in the oil tank recycling.Definite quality with filter cake of press filtration pressure is a standard, and general operation pressure is about 15bar, and filter pressure is: 1.2~1.5bar, and filter cake is solid, does not contain liquid oils, and adhesion has certain plasticity.Time of filter pressing is determined by the setting of crystalline condition and filter pressure and squeeze pressure that usually extrusion time is 15-20min.At any time observe fuel-displaced situation during filtration, as oil mass occurs and obviously reduce, illustrate that the filter filter residue is blocked up, answer switch valve to another filter.Pressure filter cleans filter cloth once behind every continuous filtration 24h, filter cloth can not fold between filter plate, with the antisitic defect filter cloth, influences filter effect.
The specific embodiment of the present invention
Embodiment 1
1, cooling, as cooling for the first time in the decolouring Oleum Gossypii semen watercooler of raw material, the decolouring Oleum Gossypii semen is reduced to about 70 ℃ from about 110 ℃, enters oil-oil heat exchanger then and carries out cooling second time, and the Oleum Gossypii semen that decolours is reduced to about 45 ℃ from about 70 ℃;
2, crystallization enters the crystallizer crystallization with the refrigerative Oleum Gossypii semen that decolours, and cooling area is 7m 2/ m 3Stirring velocity is 10r/min, the time that stops in crystallizer is 24h, the crystalline heat-eliminating medium is an ethylene glycol solution, and the temperature of heat-eliminating medium is-5 ℃, and the crystalline temperature is 5 ℃, rate of cooling is 2 ℃, temperature recovery is controlled in 0.5 ℃ in the crystallisation process, forms vacuum in jar, and vacuum tightness is at 30mbar;
3, the barrier film press filtration is adopted in press filtration, and filtration area is Oleum Gossypii semen 6m per ton 2, working pressure is about 15bar, filter pressure is 1.2bar, extrusion time is 15min, purge pressure filter with the oil circulation utilization of collection liquid with pressurized air in the pressure-filtering process, and the deep fat that is entered in the pressure filter by compressed-air line dissolves residual solid fat, recycling.
Divide the cotton oil after carrying, 0 ℃ of clearing time was more than 240 hours, and smell, flavour and good mouthfeel can be used as the one-level salad oil, also can produce mixed oil and aioli etc.Divide the raw material oil that solid fat after carrying can frying oil, the raw material oil of oleomargarine and shortening is produced the raw material oil of substitute of cocoa fat, produces the raw material oil of saturated fatty acid.
Embodiment 2
1, cooling is with embodiment 1.
2, crystallization enters the crystallizer crystallization with the refrigerative Oleum Gossypii semen that decolours, and cooling area is 8m 2/ m 3Stirring velocity is 15r/min, the time that stops in crystallizer is 36h, the crystalline heat-eliminating medium is an ethylene glycol solution, and the temperature of heat-eliminating medium is-10 ℃, and the crystalline temperature is 7 ℃, rate of cooling is 4 ℃/h, temperature recovery is controlled in 0.5 ℃ in the crystallisation process, forms vacuum in jar, and vacuum tightness is at 40mbar;
3, the barrier film press filtration is adopted in press filtration, and filtration area is Oleum Gossypii semen 8m per ton 2, working pressure is about 15bar, filter pressure is 1.5bar, extrusion time is 20min, purge pressure filter with the oil circulation utilization of collection liquid with pressurized air in the pressure-filtering process, and the deep fat that is entered in the pressure filter by compressed-air line dissolves residual solid fat, recycling.
Divide the cotton oil after carrying, 0 ℃ of clearing time was more than 240 hours, and smell, flavour and good mouthfeel can be used as the one-level salad oil, also can produce mixed oil and aioli etc.Divide the raw material oil that solid fat after carrying can frying oil, the raw material oil of oleomargarine and shortening is produced the raw material oil of substitute of cocoa fat, produces the raw material oil of saturated fatty acid.

Claims (8)

1. a branch is put forward the method for Oleum Gossypii semen, it is characterized in that: adopt cooling, crystallization, filtering method to realize dividing and carries Oleum Gossypii semen, what wherein crystallisation step adopted is vacuum crystallization.
2. the method described in claim 1, it is characterized in that: the vacuum tightness of vacuum crystallization is 30-40mbar.
3. the method described in claim 1 or 2 is characterized in that: the cooling area that vacuum crystallization adopts is 7m 2/ m 3-8m 2/ m 3, stirring velocity is 10r/min~15r/min, the time that stops in crystallizer is 24h-36h, the temperature of heat-eliminating medium is-5 ℃~-10 ℃, the crystalline temperature is 5 ℃~7 ℃, and rate of cooling is 2 ℃ of-4 ℃/h, and temperature recovery is controlled in 0.5 ℃ in the crystallisation process.
4. the method described in claim 3 is characterized in that: adopt ethylene glycol as refrigerant in the crystallisation process.
5. as each described method in the claim 1,2,4, it is characterized in that: twice method of cooling adopted in cooling, uses watercooler for the first time, and the Oleum Gossypii semen that will decolour is cooled to about 70 ℃ from about 110 ℃; With oil-oil heat exchanger, the Oleum Gossypii semen that will decolour is cooled to about 45 ℃ from about 70 ℃ for the second time.
6. as each described method in the claim 5, it is characterized in that: adopt the barrier film press filtration, working pressure is about 15bar, and filter pressure is 1.2~1.5bar, and extrusion time is 15-20min.
7. the method described in claim 6 is characterized in that: purge pressure filter to collect the oil circulation utilization of liquid with pressurized air in the pressure-filtering process.
8. the method described in claim 7 is characterized in that: deep fat enters dissolving residual solid fat in the pressure filter, recycling by compressed-air line.
CNB2006100906882A 2006-07-07 2006-07-07 Method of extracting cotton seed oil Expired - Fee Related CN100408660C (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101591586B (en) * 2008-05-29 2012-02-08 金光食品(宁波)有限公司 Secondary fractionation product of palm oil and preparation method thereof
CN102113603B (en) * 2009-12-31 2013-04-24 嘉里特种油脂(上海)有限公司 Cocoa butter replacer composition as well as preparation method and application thereof
CN103666760A (en) * 2013-12-11 2014-03-26 晨光生物科技集团股份有限公司 Method for fractionating cottonseed oil with high freezing resistance
CN104194928A (en) * 2014-07-31 2014-12-10 青岛海智源生命科技有限公司 Method for fractionation of DHA microalgae oil
CN104450182A (en) * 2015-01-01 2015-03-25 湖南东祥油脂有限公司 Rice bran oil grease and oil separation method
CN104531347A (en) * 2014-12-09 2015-04-22 会同县贤胜油业有限责任公司 Oscillation type condensation factor removing system used in walnut oil production process
CN104726204A (en) * 2015-04-09 2015-06-24 天门市诚鑫化工有限公司 Production technology of low-cold-point oleic acid
CN105524712A (en) * 2015-09-23 2016-04-27 湖北元大粮油科技有限公司 Rapeseed oil degreasing device and technology
CN106367202A (en) * 2015-07-22 2017-02-01 中粮营养健康研究院有限公司 Method for shortening cottonseed oil separation extraction time, cottonseed oil separation extraction method, and uses of extremely hydrogenated vegetable oil as crystallization promoting agent
CN108753456A (en) * 2018-07-23 2018-11-06 盘中餐粮油食品(长沙)有限公司 One vegetable oil process for dewaxing

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JPS60262894A (en) * 1984-06-11 1985-12-26 日清製油株式会社 Winter process
US5045243A (en) * 1988-07-01 1991-09-03 Fuji Oil Company, Limited Method for dry fractionation of fats and oils
CN1560015A (en) * 2004-02-20 2005-01-05 焱 徐 Process for producing conjugated diolefine linoleic acid, palmic acid by cotton seed oil

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101591586B (en) * 2008-05-29 2012-02-08 金光食品(宁波)有限公司 Secondary fractionation product of palm oil and preparation method thereof
CN102113603B (en) * 2009-12-31 2013-04-24 嘉里特种油脂(上海)有限公司 Cocoa butter replacer composition as well as preparation method and application thereof
CN103666760B (en) * 2013-12-11 2015-11-18 晨光生物科技集团股份有限公司 Point extracting method of high frost resistance Oleum Gossypii semen
CN103666760A (en) * 2013-12-11 2014-03-26 晨光生物科技集团股份有限公司 Method for fractionating cottonseed oil with high freezing resistance
CN104194928A (en) * 2014-07-31 2014-12-10 青岛海智源生命科技有限公司 Method for fractionation of DHA microalgae oil
CN104531347A (en) * 2014-12-09 2015-04-22 会同县贤胜油业有限责任公司 Oscillation type condensation factor removing system used in walnut oil production process
CN104450182A (en) * 2015-01-01 2015-03-25 湖南东祥油脂有限公司 Rice bran oil grease and oil separation method
CN104726204A (en) * 2015-04-09 2015-06-24 天门市诚鑫化工有限公司 Production technology of low-cold-point oleic acid
CN106367202A (en) * 2015-07-22 2017-02-01 中粮营养健康研究院有限公司 Method for shortening cottonseed oil separation extraction time, cottonseed oil separation extraction method, and uses of extremely hydrogenated vegetable oil as crystallization promoting agent
CN106367202B (en) * 2015-07-22 2019-10-15 中粮营养健康研究院有限公司 Shorten cotton seed oil and proposes the purposes of the method for time, the fractionation method of cottonseed oil and deep hydrogenation vegetable oil as crystallization-promoter
CN105524712A (en) * 2015-09-23 2016-04-27 湖北元大粮油科技有限公司 Rapeseed oil degreasing device and technology
CN105524712B (en) * 2015-09-23 2016-09-28 湖北元大粮油科技有限公司 The degreasing plant of a kind of Oleum Brassicae campestris and technique thereof
CN108753456A (en) * 2018-07-23 2018-11-06 盘中餐粮油食品(长沙)有限公司 One vegetable oil process for dewaxing

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