CN108753458A - Improve the refinery practice of microbial grease stability and safety - Google Patents

Improve the refinery practice of microbial grease stability and safety Download PDF

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Publication number
CN108753458A
CN108753458A CN201810880337.4A CN201810880337A CN108753458A CN 108753458 A CN108753458 A CN 108753458A CN 201810880337 A CN201810880337 A CN 201810880337A CN 108753458 A CN108753458 A CN 108753458A
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grease
safety
deodorization
water
stability
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瞿瀚鹏
曹晟
王身健
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Priority to PCT/CN2019/086376 priority patent/WO2020024645A1/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter

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  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

The present invention relates to Rrefinement of Fungal Oil fields, disclose a kind of refinery practice improving microbial grease stability and safety, including first wash, degumming, acid refining, second wash, alkali refining, third time washing, winterization, decoloration and deodorization.The Rrefinement of Fungal Oil technique of the present invention, devises multiple tracks washing step;Unique program cooling low temperature winterization technique is taken in winterization process;Using compound adsorbents such as silica in bleaching process;The temperature of grease is controlled in deodorization procedures and is stripped using vacuum.Using the technique, the content of trans-fatty acid, 3 chloropropyl alcohols and glycidol aliphatic ester etc. in grease is can control, the content and pesticide residue of polycyclic aromatic hydrocarbon is reduced, improves stability and the safety of microbial grease.The microbial grease nutritive value handled by this method is high, in good taste, stablizes, and harmful components are low, is especially suitable for making dispensed food for baby, healthy food and health food.

Description

Improve the refinery practice of microbial grease stability and safety
Technical field
The present invention relates to Rrefinement of Fungal Oil fields, and in particular to a kind of raising microbial grease stability and safety Refinery practice.
Background technology
Content of polyunsaturated fatty acid is high in microbial grease, and the saturation degree of grease is low, and easy oxidation results in microorganism Oil stability is poor.Fat degumming, de- soap, decoloration especially deodorising process are carried out under higher temperature condition, and high Temperature, oxygen are two key factors of Oxidation of Fat and Oils.
The refinery practice of existing how unsaturated microbial grease is from the refinery practice of the vegetable fat such as rapeseed oil, work Skill control is more rough, can not prevent the generation of oxidation.
The deodorizing technology of existing microbial grease generally carries out under 190-220 DEG C of temperature condition, and technical process compared with Long, one side high temperature will more easily lead to Oxidation of Fat and Oils, isomerization, on the other hand also be easy to cause the production of trans-fatty acid It is raw, it is larger with safety effects to Oil stability, also create production loss.
In the production process of microbial grease, the nuisances such as pesticide residue and polycyclic aromatic hydrocarbon in fermentation medium also can It is brought into microbial grease, influences the safety of grease.And existing microbial grease Scouring Technology to pesticide residue and The removal effect of polycyclic aromatic hydrocarbon is limited.
The harmful components that vegetable fat raw material and processing aid itself carry, what improper fabrication process condition was formed is harmful into Grade, can be moved in grease with course of oil processing, if do not taken during oil seed production efficient control and Removing sulfuldioxide, these harmful components will eventually remain in product oil and can exceed threshold limit values, to the quality safety of grease It threatens and is detrimental to health.Research report, inventor's achievement in research and the practical inspection for producing product of associated mechanisms Survey the result shows that, during vegetable fat high temperature refinery, during especially 200 DEG C or more of grease deodorization, vegetable fat It will produce the harmful side products such as trans-fatty acid, chloropropanol ester, ethylene oxidic ester.Glycidol aliphatic ester is generated from edible By-product in oil and fat refining process, can be hydrolyzed into dehydration glycerine in the gastrointestinal tract, and dehydration glycerine has genetoxic and cause It is carcinous.Chloropropyl alcohol class compound is generally acknowledged food contaminant, has Toxicity of Kidney, genotoxicity, immunosupress and potential cause It is carcinous.Meanwhile if the raw material used in vegetable fat production is contaminated, manufacturing condition is improper, process equipment defect or former Barrier and raw material or product the reasons such as are polluted during shipping storage by environment and packaging material, may all be caused using oil Contain a certain amount of polycyclic aromatic hydrocarbon (PAH) in fat.In order to avoid trans-fatty acid, glycidol aliphatic ester, 3 chloropropyl alcohols, PAH Deng health problem caused by possibility, countries in the world especially EU Committee has given being distinctly claimed to its limitation requirement.
Invention content
The purpose of the invention is to overcome technique of the existing technology rough, the generation of Oxidation of Fat and Oils can not be prevented, The problems such as easy ting produce trans-fatty acid, 3 chloropropyl alcohols, glycidol aliphatic ester provides a kind of raising microbial grease stabilization Property and safety refinery practice, which has and can preferably prevent oxidation, the isomerism of unsaturated microbial grease Change, improves the stability of grease;The generation that can prevent trans-fatty acid, remove or be greatly reduced pesticide residue in grease, The harmful substances such as polycyclic aromatic hydrocarbon, 3 chloropropyl alcohols, glycidol aliphatic ester, improve the safety of grease.
To achieve the goals above, the present invention provides a kind of refining work improving microbial grease stability and safety Skill, including the following process that carries out successively:Degumming, acid refining, alkali refining, winterization, decoloration and deodorization, also, between above-mentioned operation It is added to multiple washing process;The technique of the wherein described deodorization procedures is that under the vacuum condition of 20-600Pa, grease is heated To 130-200 DEG C, it is passed through the deoxygenated water steam stripping for accounting for oil weight 2-30%, deodorization time is no less than 60 minutes, broken with High Purity Nitrogen Vacuum.
In conjunction with the characteristic that 3 chloropropanol esters are soluble easily in water, in refining process, inventor is washed by design with using multiple Technique, design and the technique of deodorization stripped vapor is generated using deoxidation pure water, come reduce glycidol aliphatic ester this One precursor substance, control and the content for reducing by 3 chloropropyl alcohols;Entire refining uses the pure water of two-pass reverse osmosis with water, described The conductivity of reverse-osmosis pure water is 2-10us/cm, free chlorine contents≤0.05mg/L.
Preferably, the multiple washing step is respectively:1. the first wash before the Degumming Procedures:Addition accounts for The reverse-osmosis pure water of oily weight 10%, the citric acid of oily weight 3 ‰ are heated to 85 DEG C, are stirred 20 minutes with the rotating speed of 80rpm;It is quiet 2 hours descendant's work point water is set, or divides water immediately using two-phase centrifuge;2. the second wash before the alkali refining process: The reverse-osmosis pure water for accounting for oily weight 20% is added, is heated to 85 DEG C, is stirred 20 minutes with the rotating speed of 80rpm;Stand 2 hours descendants Work point water, or divide water immediately using two-phase centrifuge;3. the third time washing before the winterization process:Addition accounts for oil weight 20% reverse-osmosis pure water is heated to 85 DEG C, is stirred 20 minutes with the rotating speed of 80rpm;2 hours descendant's work point water is stood, or Divide water immediately using two-phase centrifuge.
Preferably, the bleaching process is that under the conditions of nitrogen charging, grease is heated to 35-80 DEG C;Add 1-2wt% Silica, arbitrary two kinds or three kinds in the atlapulgite of 1-2.5wt% and the activated carbon of 1-2.5wt%, stir 30- Plate-frame filtering is used after sixty minutes, or is filtered using leaf filter.
It is further preferred that in the bleaching process, the heating temperature of grease is 65-75 DEG C.
Preferably, in the bleaching process, the silica of 1.5wt%, the atlapulgite of 2wt% and 2wt% is added Activated carbon in arbitrary two or three.
Since heavy metal, PAH etc. are easily adsorbed by substances such as atlapulgite, silica, activated carbons, decoloration work of the invention Sequence uses two or three of combination in atlapulgite, silica dry glue and activated carbon to be used as decolorizing adsorbent, can be efficient Remove the pollutants such as PAH.
Preferably, in the deodorization procedures, the vacuum condition is 50-100Pa.
Preferably, in deodorization procedures, it is 160-190 DEG C that the deodorization of the grease, which maintains temperature,.
It is further preferred that in deodorization procedures, the heating temperature of the grease is 170-185 DEG C.
Preferably, in deodorization procedures, the deoxygenated water steam stripping for accounting for oil weight 10-20%, deodorization time 120-180 are passed through Minute.
Due to microbial grease and other plant grease be more prone at high temperature trans-fatty acid, ethylene oxidic ester and 3 chloropropanol esters, method of the invention reduces the temperature of grease deodorization, shortens the time of deodorization processing, i.e., by conventional 190- 220 DEG C of grease deodorization temperature is reduced to 170-185 DEG C of optimize technique of the present invention, vacuum degree 50-100Pa.
The microbial grease of the refinery practice refining using the present invention for improving microbial grease stability and safety, contains Have no more than the glycidol aliphatic ester of 200 μ g/kg, 3 chloropropyl alcohols no more than 200 μ g/kg, anti-no more than 0.8wt% Formula aliphatic acid, the dissolvent residual not higher than 1.0mg/kg, the unsaponifiable matter not higher than 3.5wt%, not higher than the Huang of 4.0 μ g/kg Aspertoxin B1, total arsenic not higher than 0.1mg/kg and not higher than the lead content of 0.1mg/kg, the OSI values at 80 DEG C are not less than 5 hours, color and luster used the coloration that " Gardner's colour photometer " detects for 1.7-3.1.
Through the above technical solutions, pass through in the how unsaturated microbial grease of refining, anisidine value≤10, acid value (with KOH is counted) it is not higher than 0.8mg/g, peroxide value≤3meq/kg, moisture≤0.08% and clean taste, without greasy feeling.
The refinery practice provided by the invention for improving microbial grease stability and safety, is used for how unsaturated microorganism Grease is primarily referred to as the docosahexaenoic acid (DHA) in algae oil source and fish oil source, the eicosatetraenoic acid of originated from fungus (ARA).It can also be used for other edible vegetable oil and fats, including but not limited to palm oil, rapeseed oil, peanut oil, tea-seed oil, soybean Oil, olive oil, sunflower oil.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
In the present invention, the production, transhipment and the storage process that entirely refine all take the measure of vacuum or nitrogen charging, are completely cutting off It is carried out in the case of oxygen, acid refining, alkali refining, decoloration and the deodorization procedures of refining carry out at relatively mild temperature, especially Deodorization procedures, using under 185 DEG C of relatively low temperature conditions, the deodorizing technology of High efficiency stripping effectively prevents more insatiable hungers The generation of oxidation and trans-fatty acid with microbial grease, it is residual that decolorization adsorption process removes more pesticides with deodorising process It stays and polycyclic aromatic hydrocarbon.
The present invention will be described in detail by the following examples, the stream of the refining process of all embodiments as shown in Figure 1 Cheng Jinhang.In following embodiment, crude oil used is the Mortierella alpina grease and split pot algae oil fat that inventor obtains in production. Nitrogen is 99.99% nitrogen by the content that mating nitrogen making machine group (High Seience Technology Co., Ltd. of being piled mountain high in Guangdong, JH-PN49-10) generates Gas is the high pure nitrogen that content is 99.999% used in deodorization procedures.It vacuumizes by the limited public affairs of horse Debao vacuum equipment group The vacuum source system of ZJP1200C, ZJ600B, ZJ300B three-level Roots vaccum pump and 2BE1-202 the water ring vacuum pumps composition of department It carries out, which adds two level sliding vane rotary vacuum pump to form by level-one water ring pump.All water used are reverse osmosis pure water, It is made by mating reverse osmosis water manufacturing system (Jiangsu Dexing environmental protection Co., Ltd, DX3000), control underwater gold category ion, Chlorine ion concentration creates conditions for the influence of subsequent metal ion pair product quality, the control of 3-MCPD.Winterization is in 3m3Winterization Tank carries out, and low temperature is kept by indirect refrigeration medium cooling;Plate and frame filter press uses the XA/GF40/800- of Shandong Jing Jin companies The product of UK types, filter cloth use polypropylene material filter cloth, pressure to be set by plate and frame filter press;Dehydration carries out in drain sump, can Set temperature, pressure;Leaf filter uses the NYB-7 products of Jiangsu Ju Neng mechanical equipments Co., Ltd.Deoxidation water vapour is by Ningbo The GMF360-0.8 boilers of wave power Wei Ge environmental protection equipments Co., Ltd generate.Anisidine value and peroxide value, OSI values, PAH (or Polycyclic aromatic hydrocarbon) content, content of trans fatty acids, 3-MCPD contents etc. be all made of national standard method and measure, and agents useful for same is Commercially available common product.
Embodiment 1
Using the crude oil of Mortierella alpina grease, handle in the steps below.
1) first wash:The reverse-osmosis pure water for accounting for oily weight 10% is added, the citric acid of oily weight 3 ‰ is heated to 85 DEG C, It is stirred 20 minutes with the rotating speed of 80rpm;Divide water using two-phase centrifuge.
2) degumming:The reverse-osmosis pure water that oil weighs 10% is added, is heated to 85 DEG C, is stirred 20 minutes with the rotating speed of 80rpm; Divide water with two-phase centrifuge.
3) acid refining:Acid-refining tank is taken out into negative pressure to -0.1MPa, is delivered grease in acid-refining tank with the mode of negative-pressure adsorption; The tank pressure that negative pressure forms micro-positive pressure is broken with nitrogen;Oil is heated to 75 DEG C;The citric acid that addition accounts for oily weight 4 ‰ (is configured to concentration It is added for 50% aqueous solution), it is stirred 40 minutes with the rotating speed of 80rpm.85 DEG C of hot water of oily weight 10% are added, stir 20 points Clock divides water with two-phase centrifuge.
4) second wash:The reverse-osmosis pure water for accounting for oily weight 20% is added, is heated to 85 DEG C, is stirred with the rotating speed of 80rpm It mixes 20 minutes;Divide water using two-phase centrifuge.
5) alkali refining:Alkali refining tank is first taken out into negative pressure, grease in acid-refining tank is sent to nitrogen in alkali refining tank.Oil is heated to 45 DEG C, caustic dosage (caustic dosage=7.13 × 10 are calculated according to acid value of lipids-4× acid value × oil weight), 40% sodium hydroxide is added Solution is stirred 50 minutes with the rotating speed of 80rpm;Grease temperature is warming up to 80 DEG C, adds 85 DEG C of pure water of oily weight 5%, It is stirred 15 minutes with the speed of 80rpm, centrifugation removes gleditsia sinensis with two-phase centrifuge.
6) third time is washed:The reverse-osmosis pure water that oil weighs 20% is added, is heated to 85 DEG C, is stirred with the rotating speed of 80rpm 20 minutes, divide water with two-phase centrifuge.
7) winterization:Drain sump is first taken out into negative pressure, alkali refining oil is sent to nitrogen in drain sump, then grease is warming up to 85 DEG C, continue to take out negative pressure to -0.1MPa, is dehydrated 40 minutes.Dehydrated oil is pressed into the room temperature winterization tank for taking out negative pressure, room temperature winterization temperature 25 DEG C, 20 hours time are spent, the filtering of plate filter frame, filter pressure 0.1MPa.Grease is sent in drain sump and is dehydrated again, is taken off Water condition is the same as dehydration for the first time.Grease is sent to nitrogen in low temperature winterization tank again, (cooling process is shown in Table program cooling degree 1) low temperature winterization processing, -5 DEG C of low temperature winterization temperature, 90 hours time, with plate-frame filtering, filter pressure 0.2MPa, are carried out.
Table 1
8) it decolourizes:Grease after winterization is heated to 65 DEG C in the environment of vacuum nitrogen, and the dioxy for accounting for oily weight 1% is added SiClx is stirred 60 minutes with the speed of 120rpm;The activated carbon for adding the atlapulgite for accounting for oily weight 1% and accounting for oily weight 1%, with The speed of 120rpm stirs 60 minutes, is filtered with leaf filter.
9) it is deodorized:Grease through decoloration is heated to 170 DEG C, under 50Pa vacuum environments, is passed through and accounts for weight of oil 10% Deoxidation steam stripping 120 minutes, after 99.999% High Purity Nitrogen vacuum breaker, the product oil for delivering grease to vacuum nitrogen is temporary In tank.
In the present embodiment, it is all two-pass reverse osmosis pure water to refine water used, free chlorine contents≤0.05mg/ in water L;In the deodorization procedures of step 9), it is the two-pass reverse osmosis pure water heating gained by deoxidation treatment to strip steam used Steam, and the pipeline of steam be S316L materials stainless steel pipes.
Embodiment 2
Using the crude oil for splitting pot algae oil fat, handle in the steps below.
1) first wash:The oily reverse-osmosis pure water for weighing 10% of addition, oil weigh 3 ‰ citric acid, are heated to 85 DEG C, with The rotating speed of 80rpm stirs 20 minutes, stands 2 hours descendant's work point water.
2) degumming:The reverse-osmosis pure water that oil weighs 10% is added, is heated to 85 DEG C, is stirred 20 minutes with the rotating speed of 80rpm, Stand 2 hours descendant's work point water.
3) acid refining:Acid-refining tank is taken out into negative pressure to -0.1MPa, is delivered grease in acid-refining tank with the mode of negative-pressure adsorption; The tank pressure that negative pressure forms micro-positive pressure is broken with nitrogen;Oil is heated to 60 DEG C, the citric acid that addition accounts for oily weight 6 ‰ (is configured to concentration Aqueous solution for 50%), it is stirred 40 minutes with the rotating speed of 80rpm.85 DEG C of hot water of oily weight 10% are added, are stirred 20 minutes, Stand 3 hours descendant's work point water.
4) second wash:The reverse-osmosis pure water for accounting for oily weight 20% is added, is heated to 85 DEG C, is stirred with the rotating speed of 80rpm It mixes 20 minutes;Stand 2 hours descendant's work point water.
5) alkali refining:Alkali refining tank is first taken out into negative pressure, grease in acid-refining tank is sent to nitrogen in alkali refining tank.Oil is heated to 70 DEG C, caustic dosage (caustic dosage=7.13 × 10 are calculated according to acid value of lipids-4× acid value × oil weight), 40% sodium hydroxide is added Solution is stirred 60 minutes with the rotating speed of 80rpm;Grease temperature is warming up to 80 DEG C, adds 85 DEG C of pure water of oily weight 5%, It is stirred 20 minutes with the speed of 80rpm;Gleditsia sinensis is filtered using millipore filter after standing 3 hours and is removed.
6) third time is washed:The reverse-osmosis pure water that oil weighs 20% is added, is heated to 85 DEG C, is stirred with the rotating speed of 80rpm 20 minutes;Stand 2 hours descendant's work point water.
7) winterization:Drain sump is first taken out into negative pressure, alkali refining oil is sent to nitrogen in drain sump, then grease is warming up to 90 DEG C, continue to take out negative pressure to -0.1MPa, is dehydrated 40 minutes.Dehydrated oil is pressed into the room temperature winterization tank for taking out negative pressure, room temperature winterization temperature 35 DEG C, 40 hours time are spent, the filtering of plate filter frame, filter pressure 0.1MPa.Grease is sent in drain sump and is dehydrated again, is taken off Water condition is the same as dehydration for the first time.Grease is sent to nitrogen in low temperature winterization tank again, (cooling process is shown in Table program cooling degree 2) low temperature winterization processing, 0 DEG C of low temperature winterization temperature, 120 hours time, with plate-frame filtering, filter pressure 0.2MPa, are carried out.
Table 2
Program number 1 2 3 4 5 6 7 8 9 10 11 12 13
Temperature (DEG C) 75 65 55 45 42 39 36 32 28 25 21 19 17
Time (divides) 30 30 30 60 60 60 60 90 90 90 120 90 90
Program number 14 15 16 17 18 19 20 21 22 23 24 25 26
Temperature (DEG C) 16 15 14 13 12 12.2 12.4 12.7 13.1 13.5 14 12 10
Time (divides) 60 60 60 60 60 60 60 60 60 60 60 60 60
Program number 27 28 29 30 31 32 33 34 35 36 37 38
Temperature (DEG C) 8 6 4 2 0 0 0 0 0 0 0 0
Time (divides) 60 60 60 60 60 600 600 900 900 900 900 420
8) it decolourizes:Grease after winterization is heated to 75 DEG C in the environment of vacuum nitrogen, and the dioxy for accounting for oily weight 2% is added SiClx and the atlapulgite for accounting for oily weight 2.5% use plate-frame filtering after sixty minutes with the rotating speed stirring of 120rpm.
9) it is deodorized:Under the condition of negative pressure of 100Pa, the grease through decoloration is heated to 185 DEG C, is passed through and accounts for weight of oil 20% Deoxidation steam stripping 180 minutes, after 99.999% High Purity Nitrogen vacuum breaker, the product oil for delivering grease to vacuum nitrogen is temporary It deposits in tank.
In the present embodiment, it is all two-pass reverse osmosis pure water to refine water used, free chlorine contents≤0.05mg/ in water L;In the deodorization procedures of step 9), it is the two-pass reverse osmosis pure water heating gained by deoxidation treatment to strip steam used Steam, and the pipeline of steam be S316 materials stainless steel pipes.
Comparative example 1
Using the crude oil of Mortierella alpina grease, with reference to embodiment 1 using washing degumming, alkali refining washing, winterization, decoloration, The normal refinery activities of deodorization, unlike, it except dehydration, does not vacuumize in addition to deodorizing technology, whole process not nitrogen charging;The decoloration Process is:Grease is heated to 70 DEG C, addition oil weighs 1.5% activated carbon, is stirred 70 minutes with the speed of 120rpm, uses leaf filter Filtering;In the deodorization procedures, process conditions are:210 DEG C of temperature, 4 hours time, vacuum degree 200Pa, vacuum breaker nitrogen are pure 99.99% is spent, water used is softened water in technique.
Comparative example 2
Using splitting the crude oil of pot algae oil fat according to embodiment 2 using washing degumming, alkali refining washing, winterization, decoloration, deodorization Normal refinery activities, unlike, it except dehydration, does not vacuumize in addition to deodorizing technology, whole process not nitrogen charging;The bleaching process For:Grease is heated to 75 DEG C, addition oil weighs 2% atlapulgite, is stirred 60 minutes with the speed of 120rpm, with leaf filter mistake Filter;The process conditions of deodorization are:210 DEG C of temperature, 4 hours time, vacuum degree 200Pa, vacuum breaker nitrogen gas purity 99.99%, work Water used is softened water in skill.
To using finished product grease detection anisidine value, peroxide value that the above method refines, OSI values, PAH contents, trans- Content of fatty acid, 3-MCPD contents etc., testing result is as shown in table 3.
Table 3
Embodiment 1 Embodiment 2 Comparative example 1 Comparative example 2
Moisture (%) 0.02 0.024 0.032 0.028
Acid value (in terms of KOH) (mg/g) 0.18 0.14 0.43 0.51
Peroxide value (meq/kg) 0.04 0.06 1.5 2.1
Anisidine value 2.3 2.9 11 13
Free fatty (%) Nothing Nothing 0.32 0.28
Trans-fatty acid (%) Nothing Nothing 1.02 1.08
Unsaponifiable matter (%) 2.51 2,48 3.61 3.78
Solvent residual amount (mg/kg) Nothing Nothing 0.81 0.78
Lead (in terms of Pb) (mg/kg) 0.01 0.02 1.21 1.27
Arsenic (in terms of As) (mg/kg) Nothing Nothing 1.15 1.31
Aflatoxin B1 (μ g/kg) ND ND 1.6 2.1
Polychlorinated biphenyls (PCB) (ppm) 0.23 0.35 1.54 2.31
3-MCPD(μg/kg) 76 82 325 412
PAH(ppb) 0.81 0.75 1.35 1.78
GEs glycidols aliphatic ester (μ g/kg) 68 79 423 398
OSI values (80 DEG C) (h) 16.2 15.9 5.8 6.3
Ghana obtains coloration 2.12 2.46 3.64 3.75
The embodiment using refinery practice of the present invention is can be seen that by the result of table 3, inoxidizability is stronger, You Haicheng Divide content lower, there is apparent preferably stability and safety.
The refinery practice of raising the microbial grease stability and safety of the present invention, can be used for algae oil source and fish oil comes The docosahexaenoic acid (DHA) in source, the eicosatetraenoic acid (ARA) of originated from fungus and other edible vegetable oil and fats, mainly Refer to the refining of palm oil, rapeseed oil, peanut oil, tea-seed oil, soybean oil, olive oil, sunflower oil etc..
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention In art conception range, technical scheme of the present invention can be carried out a variety of simple variants, including each technical characteristic with it is any its Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to Protection scope of the present invention.

Claims (10)

1. it is a kind of improve microbial grease stability and safety refinery practice, which is characterized in that including carry out successively with Lower process:Degumming, acid refining, alkali refining, winterization, decoloration and deodorization, also, multiple washing process is added between above-mentioned operation; The technique of the deodorization procedures is, under the vacuum condition of 20-600Pa, grease is heated to 130-200 DEG C, is passed through and accounts for oil weight The deoxygenated water steam stripping of 2-30%, deodorization time >=60 minute, with High Purity Nitrogen vacuum breaker.
2. the refinery practice according to claim 1 for improving microbial grease stability and safety, which is characterized in that institute Stating multiple washing step is respectively:1. the first wash before the Degumming Procedures:Addition accounts for the reverse osmosis of oily weight 10% Pure water, the citric acid of oily weight 3 ‰ are heated to 85 DEG C, are stirred 20 minutes with the rotating speed of 80rpm;Stand 2 hours descendant's work points Water, or divide water immediately using two-phase centrifuge;2. the second wash before the alkali refining process:Addition accounts for oily weight 20% Reverse-osmosis pure water is heated to 85 DEG C, is stirred 20 minutes with the rotating speed of 80rpm;2 hours descendant's work point water is stood, or uses two Phase centrifuge divides water immediately;3. the third time washing before the winterization process:The reverse osmosis pure for accounting for oily weight 20% is added Water is heated to 85 DEG C, is stirred 20 minutes with the rotating speed of 80rpm;2 hours descendant's work point water is stood, or vertical using two-phase centrifuge Divide water.
3. the process according to claim 1 for improving how unsaturated microbial grease stability and safety, special Sign is that the bleaching process is, under the conditions of nitrogen charging, grease is heated to 35-80 DEG C;The silica of addition 1-2wt%, Two or three in the atlapulgite of 1-2.5wt% and the activated carbon of 1-2.5wt%, stirring uses sheet frame after 30-60 minutes Filtering, or filtered using leaf filter.
4. the refinery practice according to claim 3 for improving microbial grease stability and safety, which is characterized in that institute It states in bleaching process, the heating temperature of grease is 65-75 DEG C.
5. the refinery practice according to claim 3 for improving microbial grease stability and safety, which is characterized in that institute It states in bleaching process, is added two kinds or three in the activated carbon of the silica of 1.5wt%, the atlapulgite of 2wt% and 2wt% Kind.
6. the refinery practice according to claim 1 for improving microbial grease stability and safety, which is characterized in that institute It states in deodorization procedures, the vacuum condition is 50-100Pa.
7. the refinery practice according to claim 1 for improving microbial grease stability and safety, which is characterized in that In deodorization procedures, the deodorization temperature of the grease is 160-190 DEG C.
8. the refinery practice according to claim 7 for improving microbial grease stability and safety, which is characterized in that institute The deodorization temperature for stating grease is 170-185 DEG C.
9. the refinery practice according to claim 1 for improving microbial grease stability and safety, which is characterized in that In deodorization procedures, it is passed through the deoxygenated water steam stripping for accounting for oil weight 10-20%, deodorization time 180-240 minutes.
10. a kind of microbial grease, which is characterized in that it is refined and is obtained according to claim 1-9 any one of them refinery practices, Containing the glycidol aliphatic ester no more than 200 μ g/kg, 3 chloropropyl alcohols no more than 200 μ g/kg and:
1) anisidine value is not higher than 10;
2) acid value (in terms of KOH) is not higher than 0.8mg/g;
3) peroxide value is not higher than 3meq/kg;
4) unsaponifiable matter content is not higher than 3.5%;
5) the μ g/kg of aflatoxin B1≤4;
6) content of trans fatty acids is no more than 0.8%;
7) moisture is not higher than 0.08%;
8) 80 DEG C of OSI values are not less than 5 hours;
9) it is 1.7-3.1 that Ghana, which obtains coloration,.
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WO2020024645A1 (en) * 2018-08-03 2020-02-06 梁云 Refining process for improving stability and safety of microbial oil
WO2020024644A1 (en) * 2018-08-03 2020-02-06 梁云 Method for improving stability and safety of microbial oils and fats
CN113122386A (en) * 2019-12-30 2021-07-16 丰益(上海)生物技术研发中心有限公司 Rice oil and preparation method thereof
CN113122386B (en) * 2019-12-30 2023-11-24 丰益(上海)生物技术研发中心有限公司 Rice oil and preparation method thereof
CN111233813A (en) * 2020-03-05 2020-06-05 浙江伊宝馨生物科技股份有限公司 Method for removing glycidyl ester in mixed tocopherol
WO2021239797A1 (en) * 2020-05-28 2021-12-02 Société des Produits Nestlé S.A. Prevention of mcpd formation by high temperature washing
CN112300864A (en) * 2020-10-22 2021-02-02 安徽天凯生物科技有限公司 Method for improving stability of docosahexaenoic acid
CN114574282A (en) * 2021-06-29 2022-06-03 嘉必优生物技术(武汉)股份有限公司 Refined microbial oil and refining method
CN114343021A (en) * 2021-12-22 2022-04-15 嘉必优生物技术(武汉)股份有限公司 Application of DHA (docosahexaenoic acid) algae oil with improved fishy smell in edible oil
CN114343021B (en) * 2021-12-22 2024-04-05 嘉必优生物技术(武汉)股份有限公司 Application of DHA algae oil for improving fishy smell in edible oil
CN114657022A (en) * 2022-03-23 2022-06-24 东北农业大学 Deodorization method for improving quality of microalgae oil rich in DHA

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