CN101979484B - Method for refining pressing flaxseed oil through solid adsorption and vacuum filtration - Google Patents
Method for refining pressing flaxseed oil through solid adsorption and vacuum filtration Download PDFInfo
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Abstract
The invention relates to a method for refining edible flaxseed oil. The method for refining pressing flaxseed oil through solid adsorption and vacuum filtration is characterized by comprising the following steps of: 1) adsorption: contacting 100 weight parts of pressing flaxseed oil with 0.5 to 10 weight parts of kieselguhr adsorbent calcined by a flux at the temperature of between 30 and 50 DEG C for 30 minutes or more; 2) winterization: cooling to the temperature of between 5 and 10 DEG C, freezing for not less than 3 hours, and filtering to remove solids; 3) vacuum filtration: at the temperature of between 50 and 55 DEG C, performing vacuum filtration on the flaxseed oil of which the solids are removed in an active alumina/silicon oxide filled vacuum filtering machine to obtain the refined clean flaxseed oil; and 4) storage under the protection of inert gas: filling the inert gas into the refined clean flaxseed oil for protective storage. By the method, harmful substances can be removed from the flaxseed oil, the quality grade of the flaxseed oil is improved, and the flavor of the oil cannot be influenced. The method has a simple and effective process and is convenient to implement and apply industrially.
Description
Technical field
The present invention relates to a kind of method of refining of edible linseed oil, belong to the food oils processing technique field.
Background technology
For a long time; (be commonly called as: siritch) production and consumption mainly is confined to the flax main producing region to edible linseed oil; Because its commercialized degree is low, the overwhelming majority is processing on a small scale, squeezing consumption on the spot on the spot; The processing facility on the basis of the existing conditions no matter how simple and crude, to pressed oil (squeezing linseed oil) take as simple not even refining of refining such as filtrations, sedimentation, because of the condition deficiency also seldom carry out quality test just conduct the finished product edible oil.Cold pressed flax seed oil has a kind of hot moulding linseed oil of fragrance flavor after propagandizing hotly that is similar to nut and then has strong siritch fragrance; But in case carry out inspection by sampling; Problems such as often rationalization and sanitary index be defective take place; Particularly may spontaneous or exogenous some foreign matters or the toxic substance brought in the course of processing, as: excessively fry Jiao that seed causes and stick with paste that bitter taste, benzopyrene exceed standard, the lubricated wet goods of press machines, under cover food safety risk; No matter be hot moulding linseed oil or cold pressed flax seed oil in addition, after storing for some time, will produce some flockss and be attended by dense bitter taste, influence the oil product sales and marketing and promote.The bad bitter taste that has about linseed oil; Ludger Br ü hl [Eur.J.LipidSci.Technol.2008,110,625-631] has carried out systematic study; Think to exist in the linseed oil a kind of inferior oily peptide E (cyclolinopeptide E of annular material ring that constitutes by eight amino acid of trace; But present this material is not also estimated edible safety except that influencing the bad taste of linseed oil CLE).Consider it is to carry out suitable purified like this from grease edible safety aspect.
And to some larger processing enterprises; Because its oil product listing will receive the mandatory technological constraint of national standard and standard, must carry out refining, is " four take off " refinery practice mostly in the employing of refinery practice; Be hydration degum, alkali-refining deacidification, adsorption bleaching, high temperature (220～240 ℃) vacuum deodorization; Through this technology refining,, can bring the other problem though satisfied technical requirements; Lose linseed oil inherent fragrance flavor and have offending fishy smell like the finished product linseed oil, this fishy smell also is difficult to accept to the consumers in general of first edible linseed oil.About linseed oil " four take off " refinery practice, Wang Changqing [Chinese oil, 2008 Vol.33 No.3] systematic study lipid acid and V in " four take off " refinery practice process
EChanging Pattern, discover that through " four take off " refining, the function lipid acid alpha-linolenic acid content of siritch drops to 47.99% by 53.06%, natural V
EContent then is reduced to 29.3mg/100g by 57.0mg/100g, explain linseed oil behind " four take off " refinery practice havoc the interior quality of oil product, " four take off " technology is not suitable for the linseed oil refining.
To sum up analyze, need research a kind ofly can effectively keep linseed oil nutrition and flavour substances, can effectively guarantee product physics and chemistry and sanitary index requirement and be different from the as above linseed oil refinery practice of " four take off " refinery practice again.
Summary of the invention
The object of the present invention is to provide the method for a kind of solid absorption and the refining of vacuum oil strain squeezing linseed oil, this method can remove objectionable impurities in the linseed oil, and can not cause adverse influence to greasy local flavor.
For realizing above-mentioned purpose, the technical scheme that the present invention taked is: the method for solid absorption and vacuum oil strain refining squeezing linseed oil is characterized in that it comprises the steps:
1) absorption: through 100 weight parts squeezing linseed oil being contacted 30 minutes or the longer time (the contact Best Times is 0.5～1.5 hour) with the process fusing assistant incinerating diatomite adsorbant of 0.5-10 weight part at 30-50 ℃;
2) winterization: be cooled to again 5-10 ℃ freezing, keep being not less than 3 hours freezing times (Best Times is 3～15 hours), solids removed by filtration things then;
3) vacuum oil strain: under temperature 50-55 ℃, the linseed oil of removing solids through being filled with the vacuum oil-filter of activated alumina/silicon oxide, is carried out the vacuum oil strain, obtain cleaning linseed oil after the refining;
4) protection of inert gas stores: cleaning linseed oil filling with inert gas is protected storage after the refining.
The described calcining by conventional calcining process by fusing assistant and zeyssatite through fusing assistant incinerating diatomite adsorbant forms, and fusing assistant and diatomaceous part by weight are 3～8: 100; Wherein, fusing assistant is any one or any mixing that (contains any two kinds) more than two kinds in Pottasium Hydroxide, sodium hydroxide, calcium hydroxide, salt of wormwood, yellow soda ash, the lime carbonate, and any is any proportioning when (containing any two kinds) more than two kinds and mixing.
Described rare gas element is high pure nitrogen, high-purity carbon dioxide gas or high-purity argon gas, and purity is not less than 99.9wt%.
Described squeezing linseed oil is cold pressed flax seed oil or hot moulding linseed oil.
Further set forth in the face of the effect of technological process down:
Zeyssatite is a kind of flocculating aids when being widely used in need filtering grease in the grease course of processing, filters and all adds some zeyssatite like grease activated carbon decolorizing after-filtration, the dewaxing of grease winterization.General zeyssatite production is the powder that calcining forms under 900-1200 ℃ of condition, has the hole of a large amount of diameters at 100-1000nm, and porosity has reasonable adsorptive power up to 60-90%.Through discovering; Adding accounts for weight and is no more than 10% alkaline auxiliary flux in the diatomite calcination process; Make the zeyssatite pore surface not only have highly porous; Also had suitable basic active group; This highly porous and have basic active group through fusing assistant incinerating diatomite adsorbant under not being higher than 50 ℃ of temperature to some the micro-polar materials in the grease; Have very strong adsorptive power like objectionable impuritiess such as bitter substance, phosphatide, benzopyrene, free fatty acidies, and can not cause adverse influence to greasy local flavor, this point significantly is different from the activated decoloration agent and causes very heavy bilgy odour after to grease-decolor and must carry out follow-up vacuum deodorization technological process.About alkaline auxiliary flux; Through experimental study; In the certain proportion scope, 3～8% of zeyssatite weight is adopted in test, adopts these several kinds of fusing assistant incinerating diatomite adsorption effects such as sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood all can reach the ideal adsorption effect; Add a certain proportion of calcium hydroxide or lime carbonate and substitute fusing assistant incinerating zeyssatite, its adsorption effect also can reach the ideal adsorption effect.The present invention has at first adopted in technology and has made linseed oil and the technological process that contacts absorption through fusing assistant incinerating diatomite adsorbant.
Usually behind oil and fat refining; Can there be some HMP materials in the grease; Under the lower situation of temperature, can separate out floss, make grease transparency index defective, the present invention directly is cooled to linseed oil greasy winterization temperature after adsorbing and carries out winterization with contact through fusing assistant incinerating diatomite adsorbant; Just become winterization crystalline nucleus through fusing assistant incinerating diatomite adsorbant; Make the winterization crystallization bigger, and process fusing assistant incinerating diatomite adsorbant itself is a kind of flocculating aids, it is greatly convenient to come for like this grease transition band.
After contacting absorption and freezing and filtering through fusing assistant incinerating diatomite adsorbant; Grease is through being filled with the strainer oil strain of activated alumina/silicon oxide under the 50-55 ℃ of condition in vacuum and temperature; To remove volatile material here, micro-moisture is also removed.
At last; Because linseed oil is a kind of grease of as easy as rolling off a log oxidation, though refining process of the present invention has kept the antioxidant natural VE in the grease to greatest extent, at grease with after air contacts; Natural VE will be by rapid oxidation consumption; Make the linseed oil deterioration by oxidation, for fear of deterioration by oxidation in the grease storage process, the present invention is employed in the method for filling with inert gas in the storage vessel and carries out the preservation of linseed oil.
The invention has the beneficial effects as follows: adopt solid absorption and vacuum oil strain that the squeezing linseed oil is carried out refining (through adsorbing through fusing assistant incinerating diatomite adsorbant; Through the vacuum oil strain); Can remove objectionable impurities in the linseed oil (like bitter substance, phosphatide, benzopyrene, free fatty acids), and can not impact greasy local flavor.The present invention can improve linseed oil quality grade, reduces edible safety risk, the maintenance intrinsic local flavor of linseed oil of squeezing linseed oil and removes the linseed oil bitter taste; Entire method is simple and effective, is convenient to implement and industrial applications.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following embodiment.
In the reaction vessel that has stirring and temperature-control device; Confirm good squeezing linseed oil and process fusing assistant incinerating diatomite adsorbant ratio in laboratory study; Start stirring; Be lower than 30 ℃ like temperature, open temperature control unit and be heated to 30-50 ℃ for a jar interior squeezing linseed oil, adopt the automatic control design temperature usually as 45 ℃; Absorption was not less than 30 minutes duration of contact, and absorption surpasses 1 hour duration of contact, 1.0,1.5 hours duration of contact, does not observe the remarkable enhancing of adsorption effect, was generally contacting adsorption time in 1.5 hours; After absorption is accomplished, the grease that is mixed with through fusing assistant incinerating diatomite adsorbant is transferred in the refrigerated cylinder of band stirring and freezing temp control, intermittent type starts whipping appts; Here stirring velocity generally is not higher than 30rpm; Controlled temperature adopts automatic control to set controlled temperature as 8 ℃ 5-10 ℃ of scope usually, and the winterization time was at 3-15 hour; Adopt mechanical filter equipment, filter like flame filter press, whizzer, vane type filtration machine; The limpid grease that filtration obtains gets into the vacuum oil-filter that is filled with activated alumina/silicon oxide and carries out the vacuum oil strain; The clean grease of final purification is sent into the hold-up vessel storage of filling with inert gas protection, as the finished product linseed oil.Adopt refinery practice technology of the present invention to the refining of squeezing linseed oil, can reach GB/T 8235-2008 linseed oil one-level oil tech standard-required.
Embodiment 1:
The method of solid absorption and vacuum oil strain refining squeezing linseed oil, it comprises the steps:
1) absorption: being taken at room temperature is expressed cold pressed flax seed oil under 35 ℃ of conditions, and smell presents a kind of nut fragrance flavor, vapidity; The spinning solid impurity, the grease clear and transparent, chemical examination acid value 1.3mgKOH/g oil, peroxide number 5.2mmol/kg, 2.54cm groove colour examining pool is Y19, R1.4,280 ℃ of heat tests, color with oil color becomes aterrimus, and visible precipitate is arranged;
Get the process fusing assistant incinerating diatomite adsorbant of above-mentioned cold pressed flax seed oil of 100 weight parts and 2 weight parts, stir 30 minutes (stirring contact) at 45 ℃ of following constant temperature;
The described calcining by conventional calcining process by fusing assistant and zeyssatite through fusing assistant incinerating diatomite adsorbant forms, and fusing assistant and diatomaceous part by weight are 5: 100; Wherein, fusing assistant is a Pottasium Hydroxide.
2) winterization: put then under 7 ℃ of temperature of constant temperature freezing 5 hours, and started in per 1 hour and to stir 5 minutes, take out solids removed by filtration thing (promptly filtering out mechanical impurity).
3) vacuum oil strain: configuring the temp autocontrolled of vacuum oil-filter that is filled with activated alumina/silicon oxide is 55 ℃, and the linseed oil that separates solids is dropped into the vacuum oil-filter oil strain, obtains refrigerant grease; Chemical examination acid value 0.4mgKOH/g oil, peroxide number 4.0mmol/kg, 2.54cm groove colour examining pool is Y19, R1.3; 280 ℃ of heat tests; Color deepens phenomenon, does not have visible precipitate, obtains cleaning linseed oil after the refining.
4) protection of inert gas stores: the cleaning linseed oil pours in the transparent vessel that fills high pure nitrogen (purity is not less than 99.9wt%) and seals up for safekeeping after the refining, and the room temperature lucifuge is deposited.
Get refrigerant cold pressed flax seed oil and seal up for safekeeping in another transparent vessel, the room temperature lucifuge is deposited, as control samples 1.
After placing 90 days, observe, adopts cold pressed flax seed oil (being to clean linseed oil after the refining) clear and transparent after the technical finesse of the present invention, it is thus clear that the control samples oil product has significantly floss and deposition, and each item technical indicator detected value is seen table 1.
Cold pressed flax seed oil reaches the technical requirements of GB/T 8235-2008 one-level squeezing linseed oil after technology refining of the present invention.Significantly the sense organ variation is the variation (being that the present invention can not cause adverse influence to greasy local flavor) of transparency and flavour (slight bitter taste).
Table 1 cold pressed flax seed oil refining effect relatively
Embodiment 2:
The method of solid absorption and vacuum oil strain refining squeezing linseed oil, it comprises the steps:
1) absorption: the linseed oil of the 120 ℃ of bakings of learning from else's experience adopts oil press zhai squeezing system oil, and expressed hot moulding linseed oil, smell present a kind of giving off a strong fragrance flavor, vapidity; The spinning solid impurity, the color with oil color blackout, chemical examination acid value 1.6mgKOH/g oil, peroxide number 6.0mmol/kg, 2.54cm groove colour examining pool is Y30, R1.9,280 ℃ of heat tests, color with oil color becomes aterrimus, and visible precipitate is arranged;
Get the process fusing assistant incinerating diatomite adsorbant of above-mentioned hot moulding linseed oil of 100 weight parts and 2.5 weight parts, stir 30 minutes (stirring contact) at 45 ℃ of following constant temperature.
The described calcining by conventional calcining process by fusing assistant and zeyssatite through fusing assistant incinerating diatomite adsorbant forms, and fusing assistant and diatomaceous part by weight are 5: 100; Wherein, fusing assistant is a sodium hydroxide.
2) winterization: put then under 7 ℃ of temperature of constant temperature freezing 5 hours, and started in per 1 hour and to stir 5 minutes, take out solids removed by filtration thing (promptly filtering out mechanical impurity).
3) vacuum oil strain: configuring the temp autocontrolled of vacuum oil-filter that is filled with activated alumina/silicon oxide is 55 ℃, and the linseed oil that separates solids is dropped into the vacuum oil-filter oil strain, obtains refrigerant grease; Chemical examination acid value 0.6mgKOH/g oil, peroxide number 3.5mmol/kg, 2.54cm groove colour examining pool is Y30, R1.6; 280 ℃ of heat tests; Color has the intensification phenomenon, does not have visible precipitate, obtains cleaning linseed oil after the refining.
4) protection of inert gas stores: the cleaning linseed oil pours in the transparent vessel that fills high pure nitrogen and seals up for safekeeping after the refining, and the room temperature lucifuge is deposited.
Get refrigerant hot moulding linseed oil and seal up for safekeeping in another transparent vessel, the room temperature lucifuge is deposited, as control samples 2.
After placing 90 days, observe, adopt hot moulding linseed oil (being to clean linseed oil after the refining) clear and transparent of technical finesse of the present invention, control samples oil product container bottom has tangible throw out, and each item technical indicator detected value is seen table 2.The present invention does not cause adverse influence to greasy local flavor.
The hot moulding linseed oil reaches the technical requirements of GB/T 8235-2008 one-level squeezing linseed oil after technology refining of the present invention.
Table 2 hot moulding linseed oil refining effect relatively
Embodiment 3:
The method of solid absorption and vacuum oil strain refining squeezing linseed oil, it comprises the steps:
1) absorption: through 100 weight parts squeezing linseed oil (cold pressed flax seed oil is with embodiment 1) being contacted 30 minutes with the process fusing assistant incinerating diatomite adsorbant of 0.5 weight part at 30 ℃;
The described calcining by conventional calcining process (being zeyssatite production) by fusing assistant and zeyssatite through fusing assistant incinerating diatomite adsorbant forms, and fusing assistant and diatomaceous part by weight are 8: 100; Wherein, fusing assistant is a Pottasium Hydroxide.
2) winterization: be cooled to again 5 ℃ freezing, freezing 4 hours, solids removed by filtration thing then;
3) vacuum oil strain: under 50 ℃ of temperature,, carry out the vacuum oil strain, obtain cleaning linseed oil after the refining with the vacuum oil-filter (for existing suite of equipment) of the linseed oil of removing solids through being filled with activated alumina/silicon oxide;
4) protection of inert gas stores: cleaning linseed oil filling with inert gas (high-purity carbon dioxide gas, purity is not less than 99.9wt%) is protected storage after the refining, in transparent vessel, seals up for safekeeping.
After placing 90 days, observe, adopts cold pressed flax seed oil (being to clean linseed oil after the refining) clear and transparent after the technical finesse of the present invention, it is thus clear that acid value 0.8mgKOH/g oil, control samples 1 oil product have significantly floss and deposition.Cold pressed flax seed oil reaches the technical requirements of GB/T 8235-2008 one-level squeezing linseed oil after technology refining of the present invention.
Table 3 cold pressed flax seed oil refining effect relatively
Embodiment 4:
The method of solid absorption and vacuum oil strain refining squeezing linseed oil, it comprises the steps:
1) absorption: through 100 weight parts squeezing linseed oil (the hot moulding linseed oil is with embodiment 2) being contacted 1.5 hours with the process fusing assistant incinerating diatomite adsorbant of 10 weight parts at 50 ℃;
The described calcining by conventional calcining process by fusing assistant and zeyssatite through fusing assistant incinerating diatomite adsorbant forms, and fusing assistant and diatomaceous part by weight are 3: 100; Wherein, fusing assistant is a salt of wormwood.
2) winterization: be cooled to again 10 ℃ freezing, freezing 15 hours, solids removed by filtration thing then;
3) vacuum oil strain: under 55 ℃ of temperature, the linseed oil of removing solids through being filled with the vacuum oil-filter of activated alumina/silicon oxide, is carried out the vacuum oil strain, obtain cleaning linseed oil after the refining;
4) protection of inert gas stores: cleaning linseed oil filling with inert gas (high-purity argon gas, purity is not less than 99.9wt%) is protected storage after the refining.
After placing 90 days, observe, adopt hot moulding linseed oil (being to clean linseed oil after the refining) clear and transparent of technical finesse of the present invention, control samples 2 oil product container bottoms have tangible throw out.The hot moulding linseed oil reaches the technical requirements of GB/T8235-2008 one-level squeezing linseed oil after technology refining of the present invention.Greasy local flavor is not caused adverse influence.
Table 4 hot moulding linseed oil refining effect relatively
Claims (2)
1. the method for solid absorption and the refining of vacuum oil strain squeezing linseed oil is characterized in that it comprises the steps:
1) absorption: through 100 weight parts squeezing linseed oil being contacted 30 minutes or the longer time with the process fusing assistant incinerating diatomite adsorbant of 0.5-10 weight part at 30-50 ℃;
The described calcining by conventional calcining process by fusing assistant and zeyssatite through fusing assistant incinerating diatomite adsorbant forms, and fusing assistant and diatomaceous part by weight are 3～8: 100; Wherein, fusing assistant is any one or any mixing more than two kinds in Pottasium Hydroxide, sodium hydroxide, calcium hydroxide, salt of wormwood, yellow soda ash, the lime carbonate, and any is any proportioning when mixing more than two kinds;
2) winterization: be cooled to again 5-10 ℃ freezing, keep being not less than 3 hours freezing times, solids removed by filtration thing then;
3) vacuum oil strain: under temperature 50-55 ℃, the linseed oil of removing solids through being filled with the vacuum oil-filter of activated alumina/silicon oxide, is carried out the vacuum oil strain, obtain cleaning linseed oil after the refining;
4) protection of inert gas stores: cleaning linseed oil filling with inert gas is protected storage after the refining.
2. the method for solid absorption according to claim 1 and vacuum oil strain refining squeezing linseed oil, it is characterized in that: described rare gas element is high pure nitrogen, high-purity carbon dioxide gas or high-purity argon gas, and purity is not less than 99.9wt%.
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| RU2505593C1 (en) * | 2012-05-10 | 2014-01-27 | Открытое Акционерное Общество "Казанский Жировой Комбинат" | Method of purifying vegetable oil |
| CN103120223B (en) * | 2013-02-05 | 2014-01-29 | 陕西关中油坊油脂有限公司 | Method of extracting linseed oil based on nitrogen covering water agent method |
| CN104073339B (en) * | 2014-07-09 | 2016-06-15 | 甘肃陇郁香粮油工业有限责任公司 | A kind of method of refine siritch |
| CN104046511B (en) * | 2014-07-09 | 2016-05-25 | 宁夏六盘珍坊生态农业科技有限公司 | Improve the linseed oil preparation method of linseed oil quality |
| CN104403791A (en) * | 2014-12-18 | 2015-03-11 | 宁夏伊斯兰仁存药膳食品有限公司 | Vegetable oil fresh-keeping and cold-pressing process |
| CN104830527B (en) * | 2015-05-27 | 2018-06-22 | 中国农业科学院油料作物研究所 | Extraordinary flavor grease adsorbs refinery practice |
| CN106753781A (en) * | 2017-01-04 | 2017-05-31 | 杭州智华杰科技有限公司 | A kind of method of bitter taste in removal linseed oil |
| CN107619716B (en) * | 2017-01-22 | 2023-04-07 | 李石平 | Method for removing bitter substances in linseed oil |
| CN107090351A (en) * | 2017-04-13 | 2017-08-25 | 荣海生物科技有限公司 | A kind of linseed oil method of refining |
| CN107227203A (en) * | 2017-04-21 | 2017-10-03 | 荣海生物科技有限公司 | A kind of efficient linseed oil dewaxing device |
| CN108753458A (en) * | 2018-08-03 | 2018-11-06 | 梁云 | Improve the refinery practice of microbial grease stability and safety |
| CN113088385A (en) * | 2019-12-23 | 2021-07-09 | 丰益(上海)生物技术研发中心有限公司 | Method for improving stability of grease and grease prepared by method |
| CN112156760A (en) * | 2020-09-24 | 2021-01-01 | 常熟理工学院 | Method for decolorizing rapeseed oil by using composite diatomite |
| CN112481017A (en) * | 2020-11-13 | 2021-03-12 | 宁夏瑞福祥粮油食品有限公司 | Production method of linseed oil |
| CN113388449A (en) * | 2021-06-18 | 2021-09-14 | 余海龙 | Flaxseed oil fishy smell removing agent and application thereof |
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| RU2245902C2 (en) * | 2003-03-11 | 2005-02-10 | Пятачков Андрей Александрович | Method for adsorption refining of vegetable oil and fat matters |
| CN101275101A (en) * | 2007-03-28 | 2008-10-01 | 刘洪举 | Low-temperature cold pressing method for linseed oil |
| CN101658211B (en) * | 2009-09-15 | 2012-05-23 | 中国农业科学院油料作物研究所 | Extracting debitterizing method of edible linseed oil |
| CN101768511B (en) * | 2010-01-27 | 2013-02-06 | 卢玉胜 | Low-temperature refining method for tea seed oil and refining adsorbent |
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