CN101317611A - Multi-stage molecular distillation continuous depickling technique for oil and fat with high acidity number - Google Patents
Multi-stage molecular distillation continuous depickling technique for oil and fat with high acidity number Download PDFInfo
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Abstract
The invention discloses a high acid-value grease depickling novel technology. The technology of the invention applies advanced molecular distillation technique to high acid-value grease depickling and can separate the grease from the fatty acid better on the basis of not damaging the original compositions of the raw material so as to reduce the oil acid-value; furthermore, the depickling effect can be improved by multi-stage serial connection and the continuous operation can be carried out. The acidified oil is dehydrated by fine filtration, saturated NaCl water washing and film braising and is pumped into a first-stage molecular distiller by a first-stage delivery pump so as to distil part of fatty acid; the distilled residue in the first-stage is taken as the raw material of the second-stage molecular distiller and pumped into the second-stage molecular distiller by a second-stage delivery pump so as to distil the residual fatty acid; the distilled residue is taken as the raw material of the third-stage; the circulation is repeatedly to the required N-stage; wherein, N is more than or equal to 2 and less than or equal to 5; the best stage number is 3 or 2. The technology of the invention has the advantages that the fatty acid is separated; meanwhile, the raw material composition of the grease is not damaged; the distilled high-quality fatty acid has extremely high application value by the further disposal; furthermore, multi-stage molecular distilling is beneficial to the continuous operation so as to complement the shortages of single-stage separation capability, thus providing beneficial conditions for the industrialization in large scale.
Description
Technical field
The present invention relates to a kind of high-acid value grease depickling new technology, this technology is applied to advanced person's molecular distillation technique the acidifying lipin deacidifying of high acid value, not only can on the basis of not destroying original composition, better reduce the acid number of grease, can also obtain the higher aliphatic acid of purity, and can improve removal effect by the form of plural serial stage distillation and realize continuous operation.
Background technology
Since grease collect and storage and transport process in be subjected to the influence of environment, self moisture content and lipase, can hydrolysis generate a large amount of free fatties (FFA), cause its acid number to rise and the final oil that becomes sour that forms, the trench wet goods that vegetable fat higher such as water content, that lipase activity is strong and environment of living in are comparatively abominable.
For the processing of these high acid lipids, method commonly used is chemical alkali refining and the depickling of water vapour stripping.For the high acid value oil product, the alkali consumption of chemical alkali refining is very big, and alkali with the N-process of free fatty in, also saponification a large amount of neutral grease, make refining yield on the low side; The depickling of physical refining water vapour stripping, grease need be handled under the high temperature of long period, influences oil quality, and product colour is darker, some active ingredients such as V in the grease
EOverflow with the water vapour stripping with meetings such as sterols, for the V that is rich in as wheat-germ oil
EGrease, reduced healthy nutritive value.Other processing method also comprises solvent extraction, supercritical CO
2Extraction, esterification or film separation etc., but exist also that efficient is low, cost is high or problem such as technology is not mature enough.
Molecular clock is at the industrial short-path distillation that is also referred to as, it is a kind of flexible efficiently liquid liquid thermal Release Technology, its special structure can be distilled material after the match at low temperature, has the holdup time weak point, advantages such as separative efficiency height, the easy maintenance of raw material rerum natura, especially the processing to HMW, high viscosity, heat sensitive material provides a new way.In food and oil prodution industry, this technology has been successfully applied to the separation of aliphatic acid and derivative thereof and has purified, as the depickling of grape seed oil, wheat-germ oil depickling, separate eicosapentaenoic acid (EPA) and DHA (DHA) in the deep sea fish oil, to high acid value Fructus Zanthoxyli oil depickling etc.
This patent applies to the multiple-grade molecular distillation technology in the deacidifying process of high-acid value grease, remedy the deficiency of single-stage molecular clock separating power by multiple-grade molecular distillation, not only can on the basis of not destroying the original composition of grease, effectively reduce the acid number of grease, can also obtain high-quality aliphatic acid; And efficient, energy-conservation and environmental protection are applicable to extensive, continuous operation.
Summary of the invention
The present invention is in order to overcome the deficiency of the conventional acid stripping method of high-acid value grease, and improves the effect of depickling and realize continuous operation with multistage form.
In order to achieve the above object, the present invention takes following technical scheme to be achieved:
A kind of multiple-grade molecular distillation process of high-acid value grease depickling, its main flow process is described below:
Through after filtration treatment removes mechanical admixture, grease washs with saturated NaCl solution, and washing grease later is pumped to and carries out removing of moisture and light component in the thin film evaporator, enters after qualified and carries out in the molecular distillation equipment separating of aliphatic acid and grease.According to the composition of different material and different aliphatic acid, need the process conditions of many molecular distillation equipments of control series connection, reach the purpose that better distills out aliphatic acid and do not destroy original composition.
In the molecular clock process, the vapo(u)rizing temperature of upper level molecular distillation equipment is comparable to the vapo(u)rizing temperature of next stage molecular distillation equipment, the light component that upper level distills is handled as the fatty acid product products for further of separating, and heavy ends are then distilled once more as the distillating material of next stage.
And so forth, plural serial stage can be reached in this way, when improving the lipin deacidifying effect, continuous operation can be realized.
The glyceride stock composition was not destroyed when the advantage that multiple-grade molecular distillation reduces the high-acid value grease acid number was that aliphatic acid is separated, and the high-quality aliphatic acid that distills also has very high using value through further processing; And multiple-grade molecular distillation helps continuous operation to remedy the deficiency of single-stage separating power, for extensive industrialization provides advantage.
High-acid value grease depickling multiple-grade molecular distillation process among the present invention comprises following flow process:
The a fine filtering;
The saturated NaCl washing of b;
The c thin film evaporation;
D removes the acidifying oil of moisture and light component, pumps into the partial fatty acid that distills out in the one-level molecular still wherein by the one-level dehvery pump.The aliphatic acid that distills is by the processing of one-level discharging pump as byproduct input one-level pans products for further.
The distillation residue that the e first order distills is as the raw material of second level molecular still, pumps into by the secondary feed pump and further distills out remaining partial fatty acid in the molecular still of the second level.The aliphatic acid that distills pumps in the secondary pans by the secondary discharging pump and waits for further and handling, and the distillation residue is then as the raw material of the third level.
In the such scheme, from described flow process e, the material that is not distilled out in the third level still can be imported through the level Four dehvery pump according to the needs of boiling range and distill out the cut that needs in the fourth stage molecular still, analogize therewith, employing and secondary, three grades of charging and discharging modes that the molecule distiller is identical, polyphone form multiple-grade molecular distillation high-acid value grease deacidifying process.After through the distillation of n level, fatty acid component is distilled fully, at n level molecule distiller, final distillate is pending through n level discharging pump input n level pans etc., and the grease that distillation finishes is handled through waiting for further in grease discharging pump (or n+1 level feed pump) the input finished product jar.
Described multiple-grade molecular distillation high-acid value grease depickling molecular clock progression scope is 2≤n≤5, and best progression recommends 3 or 2.
The vapo(u)rizing temperature of molecular stills at different levels, because the existence of a small amount of light component, and reduce step by step, therefore vacuums at different levels are slightly different.
Can realize the agent set of multiple-grade molecular distillation high-acid value grease deacidifying process described in the present invention, comprise a thin film evaporator, with many molecular stills that structure is identical.The top of molecular still is provided with the charging valve and can links to each other with the feedstock pump pipeline, the outer light components outlet valve of purpose boiling range can link to each other with cold-trap, have heating agent turnover valve on the external jacket, in order to be connected with the heating agent supply system, the bottom is provided with vacuum outlet and is connected with vacuum system, there is cooling water turnover valve the bottom in order to link to each other with cooling water system, and distillation can link to each other with discharging pump with distillation residue outlet valve; The described high-acid value grease that removes moisture and light component through fine filtering, saturated NaCl washing and thin film evaporation, by the one-level feed pump that is connected with one-level molecular still charging valve, pump in the one-level molecular still, evaporate the purpose component at evaporating surface after distributing by liquid distribution trough.Its essential characteristic is, distillation is condensed on built-in condenser, and the discharging opening by the bottom pumps into the product pans through discharging pump, and the light component outside boiling range also can be distilled out but most ofly taken away by vacuum, is condensed in cold-trap; Distillation residue on the evaporating surface then pumps in subordinate's molecular still by subordinate's feed pump and distills.By parity of reasoning, until distilling to the n level that needs.
The inventive concept of above-mentioned technology is:
Remove the high-acid value grease of moisture and light component through fine filtering, saturated NaCl washing and thin film evaporation, mechanical admixture, micromolecular water soluble substance and the moisture that can impact subsequent processes have been removed wherein, remaining step is to remove wherein fatty acid component by molecular clock, but separate unit molecular still flow process is not enough, can not reach fully and remove, need the series connection of many molecular stills to distill and improve removal effect, the progression of molecular still series connection need according to acidizing degree and wherein the concrete composition of aliphatic acid determine.Because removing of light component is not very complete in the thin film evaporator, can influence the vacuum in the molecular still, but along with the increase of progression, this influence can ease up, and vacuum also increases, and vapo(u)rizing temperature can suitably be turned down.Therefore forwardly adopt higher temperature in the fractionated molecule distiller, distill out partial fatty acid wherein; In the mid portion molecular still, adopt the temperature that is lower than slightly in the forward part molecular still, distill out rest parts aliphatic acid wherein; In the molecular still of rear section, adopt low or identical slightly temperature, distill out wherein remaining fatty acid.
Every grade of distillation residue by the higher level reaches connection as the mode of the distillating material of subordinate, and so forth, reaches distillation fully until all aliphatic acid, perhaps reaches the proper acidity value.
The invention has the beneficial effects as follows, this device utilizes its high vacuum (0.1Pa-1Pa) condition, under the temperature of setting, the difference of the different molecular mean motion free path between grease molecule and fatty acid molecule realizes separating of these two kinds of liquid mixtures, have liquid and force film forming, raw material is difficult for sticking, residence time of material is short, distillation efficiency is high and vapo(u)rizing temperature is low, grease and fatty acid composition advantage such as be not damaged, the vacuum drawn that the lower end has can further be separated the light component that can not remove fully in the thin film evaporator lights removal process, promptly reach the purpose of gas clean-up, improving also can grease purity.So adopt multiple-grade molecular distillation high-acid value grease depickling new technology of the present invention, in deacidification, grease consumption, the esterification exacting terms that can not occur in the alkali refining require and the steam stripped long-time high-temperature process of water vapour, can not occur the phenomenon such as coking, cracking in the conventional decompression distillation yet, and not have secondary pollutions such as salkali waste, spent acid, waste water.
Because vapo(u)rizing temperature is low, the separative efficiency height can significantly cut down the consumption of energy; High vacuum, low temperature distill after the match, can guarantee the quality of distillage preferably.If add can be supporting robot control system(RCS), can make then that the operation of whole device is simpler, operation is more stable.
Description of drawings
Below in conjunction with accompanying drawing and embodiment multiple-grade molecular distillation high-acid value grease deacidifying process is further specified.
Fig. 1 is three grades of molecule distil process flow charts of the present invention.
Pass through the acidification oil of fine filtering and saturated NaCl washing, pump into through feed pump P101 and carry out preheating among the preheater EX101, Acidification oil after the preheating enters among the thin film evaporator LFE101 and removes moisture; The light components such as moisture are taken away by vacuum, in EX102 Be condensed; Remove acidification oil behind the moisture through the temporary tank V101 buffer memory of material after, P102 pumps into the one-level knifing through the one-level feed pump Carry out separating of aliphatic acid and grease among the formula molecular still DZ101; Separated aliphatic acid enters fat with the form of condensate Wait for further among the temporary tank V102 of acid material and processing; The distillation residue then through behind the temporary tank V103 buffer memory of material as two The raw material of level molecule distiller DZ102 carries out separating of remainder aliphatic acid and grease; In like manner, separated aliphatic acid is with cold The form of condensate enters among the temporary tank V104 of aliphatic acid material and waits for further processing; The distillation residue is then temporary through material Raw material as three grades of molecule distiller DZ103 behind the tank V105 buffer memory carries out separating of decline aliphatic acid and grease;
Wherein, every grade of molecule distiller all is provided with the light component grabber with the protection vacuum; The acid number of acidification oil reduces step by step, After reach required value.
If progression is greater than three grades, the rest may be inferred, repeats no more.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment detailed description is done in technological process of the present invention.
Embodiment 1
Three grades of molecule distillations of a kind of high acid value (35-40mgKOH/g) lard deacidifying process, its main flow process is described below:
A. will pump among the preheater EX101 through the acidifying lard of fine filtering and saturated NaCl washing through feed pump P101, be preheated to about 100 ℃ after, enter and remove moisture and light component among the thin film evaporator LFE101; 100 ℃ of evaporating temperatures, operation pressure (absolute pressure) 2000Pa, light component is by the condensation of EX102 institute.
B. the acidifying lard that removes moisture and light component enters among the temporary jar V101 of material.
C. the acidifying lard that removes moisture pumps among the one-level scraped film type molecular still DZ101 through one-level feed pump P102.
170-180 ℃ of one-level molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.5-0.7Pa, inlet amount 8kg/h, 65 ℃ of material inlet temperature, residence time of material is less than 5min;
One-level discharging acid value of oil and fat 7-8mgKOH/g, aliphatic acid GC detects mass fraction 94-97%, aliphatic acid removal efficiency 92-95% (calculating with the charging of one-level molecular clock).
D. the aliphatic acid that is evaporated in one-level scraped film type molecular still DZ101 enters after the inner condenser condensation of molecular still among the temporary jar V102, the light component of minute quantity enters the further condensation of cold-trap EX103, and heavy ends are conveyed into secondary scraped film type molecular still by dehvery pump P104 after entering temporary jar V103.
160-175 ℃ of secondary molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.4-0.6Pa, inlet amount 8kg/h, 110-120 ℃ of material inlet temperature, residence time of material is less than 5min;
Secondary discharging acid value of oil and fat 1-2mgKOH/g, aliphatic acid GC detects mass fraction 95-98%, aliphatic acid removal efficiency 85-90% (calculating with the charging of secondary molecular clock).
E. the aliphatic acid that is evaporated in secondary scraped film type molecular still DZ102 enters after the inner condenser condensation of molecular still among the temporary jar V104, the light component of minute quantity enters the further condensation of cold-trap EX104, and heavy ends are conveyed into three grades of scraped film type molecular stills by dehvery pump P106 after entering temporary jar V105.
160-175 ℃ of three grades of molecule distiller vapo(u)rizing temperature, operation pressure (absolute pressure) 0.3-0.6Pa, inlet amount 8kg/h, 110-120 ℃ of material inlet temperature, residence time of material is less than 5min;
Three grades of discharging acid value of oil and fat 0.4-0.7mgKOH/g, aliphatic acid GC detects mass fraction 96-99%, aliphatic acid removal efficiency 79-84% (calculating with three grades of molecule distillation chargings).
F. third level distillation residue is as the depickling qualified products, and P108 pumps by the product discharging pump.
A kind of high acid value rapeseed oil secondary molecular clock deacidifying process, its main flow process is described below:
A. will pump among the preheater EX101 through the acidifying rapeseed oil of fine filtering and saturated NaCl washing through feed pump P101, be preheated to about 60C after, enter and remove moisture and light component among the thin film evaporator LFE101; 100 ℃ of evaporating temperatures, operation pressure (absolute pressure) 2000Pa, light component is by the condensation of EX102 institute.
B. the acidifying rapeseed oil that removes moisture and light component enters among the temporary jar V101 of material.
C. the acidifying rapeseed oil that removes moisture pumps among the one-level scraped film type molecular still DZ101 through one-level feed pump P102.
170-190 ℃ of one-level molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.5-0.7Pa, inlet amount 8kg/h, 65 ℃ of material inlet temperature, residence time of material is less than 5min;
One-level discharging acid value of oil and fat 4-5mgKOH/g, aliphatic acid GC detects mass fraction 94-97%, aliphatic acid removal efficiency 92-95% (calculating with the charging of one-level molecular clock).
D. the aliphatic acid that is evaporated in one-level scraped film type molecular still DZ101 enters after the inner condenser condensation of molecular still among the temporary jar V102, the light component of minute quantity enters the further condensation of cold-trap EX103, and heavy ends are conveyed into secondary scraped film type molecular still by dehvery pump P104 after entering temporary jar V103.
160-175 ℃ of secondary molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.4-0.6Pa, inlet amount 8kg/h, 110-120 ℃ of material inlet temperature, residence time of material is less than 5min;
Secondary discharging acid value of oil and fat 0.3-0.7mgKOH/g, aliphatic acid GC detects mass fraction 95-98%, aliphatic acid removal efficiency 85-90% (calculating with the charging of secondary molecular clock).
E. distillation residue in the second level is as the depickling qualified products, and P106 pumps by the product discharging pump.
Claims (6)
1. high-acid value grease multiple-grade molecular distillation deacidifying process, preprocessing process comprise that fine filtering, saturated NaCl washing and thin film evaporation remove moisture, and the multiple-grade molecular distillation system removes wherein aliphatic acid to reduce acid number; It is characterized in that: the prime molecular clock distills out partial fatty acid wherein, and the distillation residue enters subordinate's molecular still as raw material and distills out the remaining fatty acid component; By multiple-grade molecular distillation so, grease is better separated with fatty acid component and do not destroy grease and the original composition of aliphatic acid, when reducing acid value of oil and fat, can recycle aliphatic acid again.
2. deacidifying process according to claim 1, its flow process is:
The a fine filtering;
The saturated NaCl washing of b;
The c thin film evaporation;
D removes the acidifying oil of moisture and light component, pumps into the partial fatty acid that distills out in the one-level molecular still wherein by the one-level dehvery pump.The aliphatic acid that distills is by the processing of one-level discharging pump as byproduct input one-level pans products for further.
The distillation residue that the e first order distills is as the raw material of second level molecular still, pumps into by the secondary feed pump and further distills out remaining partial fatty acid in the molecular still of the second level.The aliphatic acid that distills pumps in the secondary pans by the secondary discharging pump and waits for further and handling, and the distillation residue is then as the raw material of the third level.
F such as e are reciprocal, until reaching needed n level, 2≤n≤5, best progression recommendation 3 or 2.
3. three grades of molecule distillations of high acid value lard according to claim 2 depickling new technology is characterized in that:
170-180 ℃ of one-level molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.5-0.7Pa, inlet amount 8kg/h, 65 ℃ of material inlet temperature, residence time of material is less than 5min; Discharging acid value of oil and fat 7-8mgKOH/g, aliphatic acid GC detects mass fraction 94-97%, aliphatic acid removal efficiency 92-95% (calculating with the charging of one-level molecular clock).
160-175 ℃ of secondary molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.4-0.6Pa, inlet amount 8kg/h, 110-120 ℃ of material inlet temperature, residence time of material is less than 5min; Discharging acid value of oil and fat 1-2mgKOH/g, aliphatic acid GC detects mass fraction 95-98%, aliphatic acid removal efficiency 85-90% (calculating with the charging of secondary molecular clock).
160-175 ℃ of three grades of molecule distiller vapo(u)rizing temperature, operation pressure (absolute pressure) 0.3-0.6Pa, inlet amount 8kg/h, 110-120 ℃ of material inlet temperature, residence time of material is less than 5min; Discharging acid value of oil and fat 0.4-0.7mgKOH/g, aliphatic acid GC detects mass fraction 96-99%, aliphatic acid removal efficiency 79-84% (calculating with three grades of molecule distillation chargings).
4. high acid value rapeseed oil secondary molecular clock depickling new technology according to claim 2 is characterized in that:
170-190 ℃ of one-level molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.5-0.7Pa, inlet amount 8kg/h, 65 ℃ of material inlet temperature, residence time of material is less than 5min; Discharging acid value of oil and fat 4-5mgKOH/g, aliphatic acid GC detects mass fraction 94-97%, aliphatic acid removal efficiency 92-95% (calculating with the charging of one-level molecular clock).
160-175 ℃ of secondary molecular still vapo(u)rizing temperature, operation pressure (absolute pressure) 0.4-0.6Pa, inlet amount 8kg/h, 110-120 ℃ of material inlet temperature, residence time of material is less than 5min; Discharging acid value of oil and fat 0.3-0.7mgKOH/g, aliphatic acid GC detects mass fraction 95-98%, aliphatic acid removal efficiency 85-90% (calculating with the charging of secondary molecular clock).
5. process unit of realizing the depickling of high-acid value grease multiple-grade molecular distillation comprises: a thin film evaporator, and with many molecular stills that structure is identical.The top of molecular still is provided with the charging valve and can links to each other with the feedstock pump pipeline, the outer light components outlet valve of purpose boiling range can link to each other with cold-trap, have heating agent turnover valve on the external jacket, in order to be connected with the heating agent supply system, the bottom is provided with vacuum outlet and is connected with vacuum system, there is cooling water turnover valve the bottom in order to link to each other with cooling water system, and distillation can link to each other with discharging pump with distillation residue outlet valve; Described through fine filtering, saturated NaCl washing with the one-level feed pump of acidifying oil after thin film evaporation removes moisture by being connected with one-level molecular still charging valve, pump in the one-level molecular still, evaporate the purpose component at evaporating surface after distributing by liquid distribution trough.
6. realize high-acid value grease multiple-grade molecular distillation depickling technical matters device for one kind, its essential characteristic is, distillation is condensed on built-in condenser, discharging opening by the bottom pumps into the product pans through discharging pump, and the light component outside boiling range also can be distilled out but most of taken away by vacuum, is condensed in cold-trap; Distillation residue on the evaporating surface then pumps in subordinate's molecular still by subordinate's feed pump and distills.By parity of reasoning, until distilling to the n level that needs.
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