CN102599261B - Soybean oil powder grease and preparation method thereof - Google Patents
Soybean oil powder grease and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 10
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- Edible Oils And Fats (AREA)
- General Preparation And Processing Of Foods (AREA)
- Fats And Perfumes (AREA)
- Medicinal Preparation (AREA)
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Abstract
The invention relates to soybean oil powder grease and a preparation method thereof. Concretely, soybean first-grade oil is used as a raw material to be used as core materials, a microencapsulation embedding technology is adopted, and a novel series soybean oil powder grease product with excellent processing characteristics and rich and mass nutrients is developed through the selection of an embedding agent, a filling agent and an emulsifying agent and the optimization of process conditions. The improvement is carried out on the trial test study, an industrialized production and test recipe is obtained. During the proportioning, the soybean oil powder grease comprises the following ingredients in percentage by weight: 9.25 percent to 27.25 percent of core material, 1.35 percent to 2.7 percent of embedding agent, 13.925 percent to 33.8375 percent of filling agent, 0.5625 percent to 1.125 percent of emulsifying agent and 55 percent of water. Compared with ordinary liquid-stage grease products, the product has various advantages that the quality guarantee period of the product is prolonged, the product functionality is improved, the product water solubility is improved, and the product application range is enlarged.
Description
Technical field
The present invention relates to a kind of soybean oil powdered oil and preparation method thereof, belong to food processing field.
Background technology
Most of food belong to a kind of multicomponent colloid admixture with labyrinth, the various nutrients that formed by multicomponent, also all very easily be subjected to the impact of extraneous poor environment factor (light, temperature, pH value, oxygen, water etc.) and bad change and loss occur, especially more there is this problem in soybean wet goods liquid fat.Soybean oil contains 80% unrighted acid, and trophism is extremely strong, but exists the problem of easy oxidation.Microcapsules technology has following function: can protect by the core of embedding, avoid it and other component generation bad reaction; Itself and extraneous poor environment factor are completely cut off, when keeping the original color of core, reduced bad loss on transmission mistake or extended and guaranteed the quality the time, improved product quality; The material that makes some be difficult for storing or process becomes the solid of stable and good fluidity, expands the scope of application, simplifies production technology.Utilize the serial powdered oil product of microencapsulation technology production that following characteristics are arranged: water-soluble, emulsibility is good, can satisfy the processing needs in different food products field; The microencapsulation product more easily transports, stores, and is difficult for oxidation, good stability, and local flavor is difficult for scattering and disappearing; But the fatty consumption in the products such as Partial Replacement milk powder reduces costs; Can be according to client and the various specific breeds of different application exploitation.
The research for powdered oil abroad started from for 20 beginnings of the century, rise the fifties to have begun that abroad powdered oil is had patent report, but adopted at that time be mostly cooling curing method or absorption method, product quality is not fully up to expectations, range of application is restricted always.Along with going deep into of research, microencapsulation technology is applied to the production of powdered oil.The kind of feedstock oil expands to nearly all grease by lard, coconut wet goods, comprises peanut oil, soybean oil, barley germs oil, rice bran oil, corn oil and cottonseed wet goods.Nineteen eighty-two, Japanology the pulverizing technology of one vegetable oil, the making that prepared powdery oil is specially adapted to make cake and is used for other fast food.Main method is that grease is joined in the soy protein suspension of partial hydrolysis, makes it to form a kind of oil--water-in-oil emulsion, more spray-dried, namely obtains the powdered oil goods.In the same year, in order to produce Powdered sesame oil, research finds to add emulsifying agent, alkali salt, water-solubility protein intermixture in oil, through fully mix, drying, just can make powdered oil.Nowadays external microencapsulation powdered oil has been realized industrialization production, and its product is widely used in bakery product, facilitates leisure food, in the middle of cold drink, dairy products.
China starts late to the research of powdered oil, and nearly more than ten years, many R﹠D institutions carried out the research of these aspects, the focusing on aromatic condiment essential oil, health-related grease and culinary art oil of research.Use soybean protein isolate, maltodextrin and the xanthans such as Xie Liang as Wuxi Light Industry Univ. are made the wall material, adopt spray-dired method, fennel oil microcapsules (" the drying process with atomizing research of fennel oil microencapsulation ", food and machinery, the 5th phase in 1999) have been made.The Liu Jianhui of drug research chamber, China Preventive Medicial Science Institute institute of industrial health etc. makes the wall material with sodium alginate, by coacervation, zanthoxylum oil microcapsule is made powdery product (" research of zanthoxylum oil microcapsule preparation process condition ", China's flavouring, the 6th phase in 1997).The She Gangzhe of University Of Shantou etc. selects complex coacervation to prepare the stability that eel animal oil microcapsules etc. have improved fish oil, and microcapsules have enteric solution characteristic, make that its application is very extensive, convenient, safety (" research of eel animal oil microcapsules technology " Chinese grain and oil journal, the 4th phase in 1996).
Most raw materials of the microencapsulation powdered oil product of domestic production at present are solid-state fat, the raw material majority of for example cooking milk tea, formula milk, ice cream powder is coconut oil, palm wet goods, technical difficulty is relatively low, and to being that the research of microencapsulation product of soybean primary oil of liquid is less under normal temperature, because the short-and-medium chain unsaturated fatty acid content of soybean one-level grease is higher, be liquid under normal temperature, therefore embedding effect and the embedding intensity of microcapsules had higher requirement.In this respect, be lost etc. microencapsulation powder soybean grease wall material and emulsifying agent condition be studied (" research of microencapsulation powder soybean grease wall material and emulsifying agent " in the rich school of country's soybean Engineering Technical Research Centre, the soybean circular, the 2nd phase in 2005), but up to now, the industrialization of soybean powder oil product and market are used and are still belonged to blank, and research also rests on laboratory stage.
The present invention is directed to above technological difficulties, by common micro-encapsulation technology and formula are carried out the novelty improvement, researched and developed successfully the industrialized manufacturing technique condition of microencapsulation soybean grease, and complete to build and produce one of 3000 tons of soybean powder oil production line per year.China's soybean grease industry that is embodied as of the present invention provides a kind of new oil product, not only applied range, application are wide, and extended the production chain of soybean grease enterprise, strengthen the market competitiveness of soybean grease enterprise and resisted the ability of risk, significant to the development that promotes China's soybean grease industry.
Summary of the invention
The purpose of this invention is to provide a kind of good stability, dissolubility is good, the grease embedding rate is high soybean oil powdered oil.
Another object of the present invention is to provide a kind of simple possible, and preparation condition holds the industrialization production method of manageable soybean oil powdered oil.
For realizing above goal of the invention, the concrete scheme that the present invention adopts is as follows:
A kind of soybean oil powdered oil, the percentage by weight of this powdered oil each component when batching is:
Core: 9.25%-27.25%
Embedding medium: 1.35%-2.7%
Filler: 13.925%-33.8375%
Emulsifying agent: 0.5625%-1.125%
Water: 55%
Wherein,
Described core is the soybean primary oil,
Described embedding medium be in casein sodium, converted starch and soybean protein isolate any or any two,
Described filler is any in maltodextrin, malt syrup or HFCS,
Described emulsifying agent is comprised of monoglyceride and sucrose ester.
Wherein, described filler is preferably maltodextrin.
Any two in the preferred casein sodium of wherein said embedding medium or converted starch or soybean protein isolate, the mixture of casein sodium and converted starch more preferably, wherein, casein sodium and converted starch mass ratio are 0.8-1.25: 1, be preferably 1: 1.
Wherein, in described emulsifying agent, the mass ratio of monoglyceride and sucrose ester is 0-2.4: 1, be preferably 0.25: 1.
A kind of soybean oil powdered oil, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 9.25%
Casein sodium: 0.675%
Converted starch: 0.675%
Monoglyceride: 0.1125%
Sucrose ester: 0.45%
Maltodextrin: 33.8375%
Water: 55%
A kind of soybean oil powdered oil, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 13.75%
Casein sodium: 0.675%
Converted starch: 0.675%
Monoglyceride: 0.1125%
Sucrose ester: 0.45%
Maltodextrin: 29.3375%
Water: 55%
A kind of soybean oil powdered oil, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 18.25%
Casein sodium: 1.0125%
Converted starch: 1.0125%
Monoglyceride: 0.225%
Sucrose ester: 0.9%
Maltodextrin: 23.6%
Water: 55%
A kind of soybean oil powdered oil, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 22.75%
Casein sodium: 1.125%
Converted starch: 1.125%
Monoglyceride: 0.225%
Sucrose ester: 0.9%
Maltodextrin: 18.875%
Water: 55%
A kind of soybean oil powdered oil, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 27.25%
Casein sodium: 1.35%
Converted starch: 1.35%
Monoglyceride: 0.225%
Sucrose ester: 0.9%
Maltodextrin: 13.925%
Water: 55%
A kind of preparation method of soybean oil powdered oil, carry out as follows:
A. water heating: heating steam pressure:＜0.2MPa, water temperature: 60 ℃;
B. prepare burden: add successively embedding medium, filler, emulsifying agent, core by above-mentioned part by weight in water, make emulsion after high speed shear;
C. refinement: with colloid mill with above-mentioned emulsion refinement;
D. emulsification: steam pressure:＜0.2MPa, 65 ℃ of emulsifying temperatures, emulsification times 20min;
E. homogeneous: homogenization pressure a: 18Mpa, second homogenate pressure: 30Mpa;
F. spray-drying: inlet temperature: 150-155 ℃, outlet temperature: 85-90 ℃, charging high-pressure pump pressure:: 5-20Mpa;
G. anticaking agent adds: the silica addition accounts for the 0.9%-1.3% of material addition;
H. cooling: the cooling dry powder that obtains in fluid bed, air mass flow is 3.12m
3/ min;
I. pack: the brown paper with metering 25Kg liner moisture barrier bag is packed;
J. equipment cleans: hot water temperature: 80 ℃; The buck temperature: 80 ℃, buck concentration 1.5-2%.
The present invention adopts technique scheme, has the following advantages:
(1) select suitable embedding medium and filler, press the compound wall material of rational proportion preparation, to guarantee that microcapsules are not destroyed substantially in dry run;
(2) add compound emulsifying agent, and by multistage homogeneous and the centrifugal wet capsule solution of high stability that is mixed with.Technique is to guarantee that the microencapsulation grease forms the important measures of stable emulsion after rehydration;
(3) batch temperature is controlled at 60 ℃ of left and right, adopts high speed shear, and meticulous emulsion process mixes rapidly the batchings such as embedding medium, filler, emulsifying agent, core, forms the oil mixing with water system of meticulous emulsification.
(4) adopt high pressure charging, high temperature air intake, air draft, fine powder agglomeration, add the spray-drying related process approach such as anticaking agent, fluidized bed drying and make powdered oil after with wet microencapsulation grease drying.This technology is the ongoing emphasis of the present invention, its basic principle guarantees to be dried capsule in the instantaneous capsule dehydration of wetting exactly, and guarantee that in this process, capsule is not destroyed, simultaneously, compare with traditional spray drying tower, added the cyclone separator with agglomeration, by the fine powder agglomeration, little dried capsule and droplet are bonded together, make the product formation diameter remain on even, cavernous particle between 0.5-1mm, help the formation of particle and improve the embedding effect, in addition, reduce the generation of fine powder, thereby improved the product instant capacity; At this mechanical anticaking agent that adds in spray drying tower exit, improvement interpolation operation is beneficial to assurance product sanitary index and stablizes and the product mobility in addition.
Description of drawings
Fig. 1 is that single embedding medium is to the influence curve figure of powdered oil embedding effect;
Fig. 2 is that compound embedding medium is to the influence curve figure of powdered oil embedding effect;
Fig. 3 is that single embedding medium and compound embedding medium are to the influence curve figure of powdered oil embedding effect;
Fig. 4 is the drying process with atomizing flow chart that the industrialization of soybean oil powdered oil is produced;
Fig. 5 is the process chart that the industrialization of soybean oil powdered oil is produced.
Description of reference numerals:
A-soybean protein isolate and converted starch; B-soybean protein isolate and casein sodium; C-converted starch and casein sodium.
The specific embodiment
1 test material
1.1 test raw material
1.2 test reagent
It is pure that all reagent are domestic analysis:
1.3 lab scale testing equipment
2. lab scale craft flow process
At first the present invention is optimized the lab scale production technology of microencapsulation soybean oil powdered oil, carries out on this basis the research that industrialization is produced again.
2.1 batching
At first by the experimental design formula, wall material, emulsifying agent and soybean primary oil are weighed up stand-byly, add successively wall material, emulsifying agent, soybean oil to stir into uniform emulsion after then getting the water of the weighed amount of 1000ml beaker, then cross colloid mill.
2.2 refinement
At first after opening condensed water and then opening colloid mill and regulate gap 0.5-2mm, with deployed emulsion, cross colloid mill, repeatedly carry out three times, make the emulsion uniformity without grumeleuse, then carry out emulsification.
2.3 emulsification
Open in advance the water bath chader design temperature to assigned temperature, then measure and regulate water temperature with thermometer at assigned temperature, then emulsion is put into water bath chader, regulate agitator and stir and timing to the speed of setting, after the time of insulation appointment, carry out at once homogeneous.
2.4 homogeneous
At first valve-off, open the homogenizer condensed water, adds emulsion after circulation in modulation, then opens the homogenizer switch, is transferred to 20Mpa pressure, then modulates outer circulation and carry out homogeneous, repeatedly carries out twice.
2.5 spray-drying
Adopt the BUCHI-190 spray drying tower, emulsion after homogeneous is carried out spray-drying, at first assembling spray thing drying equipment, then open air pump, condensed water, air draft, heater successively, regulates air draft 2Mbar, open air pressure pump when being heated to after pressure stability after requiring temperature, open the charging button and regulate with clear water, inlet temperature is controlled at 180-190 ℃, and outlet temperature is controlled at 80-90 ℃, after stable, clear water is changed to the emulsion of handling well, carries out spray-drying.Along with the carrying out of experiment, the cloth bag permeability reduces, and should regulate according to experiment parameter.
3 detection methods
3.1 the embedding rate of powdered oil and total Determination of method
Total Determination of method: at first precision takes sample 2g, is placed in the 50ml Boiling tube, adds 8ml water, adds 10ml hydrochloric acid after mixing again; Then test tube is put into 70-80 ℃ of water-bath, is stirred once with glass bar every 5-10min, to treatments of the sample fully till, about 40-50min.
Then take out test tube, add 10ml ethanol, mix.After cooling, mixture is moved in 100ml tool plug graduated cylinder, wash test tube with the gradation of 25ml ether, pour in graduated cylinder in the lump.After ether was all poured graduated cylinder into, the jolting 1min that jumps a queue carefully opened plug, emitted gas, then filled in, and static 12min carefully opens plug, and the fat that adheres to benzinum-ether equivalent mixed liquor washout plug and nozzle.Static 10-20min treats that upper liquid is clear, and the sucking-off supernatant then adds the 5ml ether in tool plug graduated cylinder in the conical flask of constant, jolting, static after, will upper strata ether sucking-off, put into former conical flask.Conical flask is put evaporate to dryness in water-bath, put dry 2h in 95-105 ℃ of baking oven, take out and put weighing after cooling 0.5h in drier.
Computing formula:
In formula: the content of fat in the X-sample, %
m
1The quality of-receiving flask and fat, g
m
0The quality of-receiving flask, g
m
2The quality of-sample, g
The assay method of embedding rate: surperficial Determination of oil: accurately take the 1g sample, be tiled in Buchner funnel, use 30ml normal hexane washing sample, collect wash filtrate in suction filtration, reclaims n-hexane, claims to such an extent that flushing oil heavily is surface oil heavily.
Computing formula:
3.2 the assay method of emulsion stability
After oil, water, wall material mixing, and at a high speed (10,000rpm) disperse 3min, namely get emulsion.Get the 50ml emulsion and be placed in 50ml tool plug graduated cylinder, be placed in the volume that the water bath with thermostatic control 5h of 30 ℃ reads free water layer.
3.3 the mensuration of acid value
Take soybean oil 3-5g (ml) and inject conical flask, add isopropyl alcohol 50ml, shake and make the soybean oil dissolving, add again three phenolphthalein indicators, be titrated to 0.1mol/L NaOH and blush occurs, do not disappear in 30s, write down the NaOH milliliter number (V) of consumption.
Acid value of lipids calculates as follows:
In formula: the sodium hydroxide solution volume that the V-titration consumes, ml;
The c-concentration of sodium hydroxide solution, mol/L;
M-soybean oil quality, g;
The molal weight of 40-NaOH, g/mol.
3.4 the mensuration of peroxide value
Take sample (soybean oil) approximately 2g in conical flask, add the saturated KI solution of 10ml chloroform and 1ml glacial acetic acid and 1ml to add a cover vibration evenly, the standing 5min of dark place lucifuge.Add 75ml distilled water and 1ml starch solution, shake up.Then become colorless by blueness with sodium thiosulfate solution titrated to solution, do not disappear in 30s, write down the sodium thiosulfate milliliter number (V) of consumption.
The oil peroxidation value is calculated as follows:
In formula: V
2The volume of the hypo solution that spends in-sample, ml;
V
1The volume of the hypo solution that-blank test spends, ml;
The concentration of C-hypo solution, mol/L;
The quality of m-soybean oil, g.
3.5 the mensuration of moisture
Take approximately 5g sample, be accurate to 0.001g, in the aluminum dish of known constant weight, be placed in the air blast Constant Temp. Oven of 103 ± 2 ℃ (ware lid tiltedly be placed on ware limit), heating 2～4h adds a cover taking-up.Cooling 0.5h in drier, weighing.Be placed in the air blast Constant Temp. Oven of 103 ± 2 ℃, heating 1h adds a cover taking-up again.Cooling 0.5h in drier, weighing.The operation of Repeat-heating 1h is until the poor 0.002g that is no more than of double weighing is constant weight.Be as the criterion with minimum weighing.
Water content is greater than 20% sample, takes in the air blast Constant Temp. Oven that first is placed in 70～85 ℃ after sample, and then heating 2～4h is warming up to 103 ± 2 ℃, by the above-mentioned steps operation.
Calculate by formula:
In formula: x
1---moisture in food (quality percentage), %;
m
1---the quality before sample and aluminum dish baking, g;
m
2---the quality after sample and aluminum dish baking, g;
The quality of m---sample, g.
Allowable error: twice measured value of same sample poor, every 100g sample must not surpass 0.2g.
Further describe the present invention below in conjunction with specific embodiment, advantage and disadvantage of the present invention will be more clear along with description.But these embodiment are only exemplary, scope of the present invention are not consisted of any restriction.It will be understood by those skilled in the art that lower without departing from the spirit and scope of the present invention and can modify or replace details and the form of technical solution of the present invention, but these modifications and replacement all fall within the scope of protection of the present invention.
The impact of embodiment 1 wall material on powdered oil embedding effect
Adopt microcapsules technology, spray drying process is produced the soybean powder oil product, and groundwork is to filter out effective microcapsule wall material.The main component that forms the wall material is again embedding medium, film material, lapping etc., is a large molecule organic material of class.The wall material should possess suitable physical property, be fit to the Protein denaturation method of economical rationality, and can match with core material and chemical reaction, nontoxic does not occur, and also should have suitable permeability, hygroscopicity, dissolubility and stability simultaneously.The embedding medium that uses in the production of microencapsulation powdered oil mainly contains gelatin substance, polysaccharide, starchy material, cellulose, protein etc.This test is chosen required " skeleton " material---the embedding medium of this test by the analysis to various film forming matter character, and selects suitable filler from all kinds of " fillers ".Beat a metaphor of image, build the house not only needs reinforcing bar also to need cement and sandstone simultaneously, and this is like " skeleton thing " above-mentioned and " filler ".
(1) single factor experiment:
At first this test compares (seeing Table 1) to maltodextrin, malt syrup, three kinds of polysaccharide fillers of HFCS,
The contrast of table 1 maltodextrin, malt syrup, HFCS
As can be known maltodextrin little sweet, instant capacity good, viscosity is less and slightly emulsibility therefore this test select maltodextrin to do filler research.Also can select maltose and HFCS partly to substitute maltodextrin according to characteristics and the processing conditions restriction of development.
Then casein sodium, gelatin, converted starch and four kinds of embedding mediums of soybean protein isolate are compared.The test technological process as previously mentioned, the test recipe of different single embedding mediums sees Table 2.
The test recipe of the different single embedding mediums of table 2
The soybean powder oil of producing according to test technology flow process and method detects, due to gelatin not good dissolving and the high temperature smell bad, on the processing of product and the impact of product quality, therefore test does not consider that its embedding effect directly abandons its application.Other three kinds of embedding medium test results are respectively: the single factor experiment take soybean protein isolate as embedding medium, and total lipid content 49.51%, embedding rate are 59.60%, moisture 2%; Single factor experiment take converted starch as embedding medium, total lipid content 51.04%, embedding rate are 75.15%, moisture is 2.5%; Single factor experiment take casein sodium as embedding medium, total lipid content 50.08%, embedding rate are 84.32%, moisture is 2.5%.Result curve figure sees Fig. 1.Judge relatively that by embedding rate four kinds of single embedding mediums are respectively to the influence degree of grease embedding effect.
Can find out significantly respectively single factor experiment with soybean protein isolate, converted starch, three kinds of embedding mediums of casein sodium by Fig. 1, total lipid content is all round 50% oil-containing left and right, embedding rate raising gradually, and moisture is consistent substantially.The moisture 2-2.5% of the powdered oil that processes and basically identical illustrates that powdered oil process and spray-drying process are more stable.Three single factor experiment total lipid contents differ 2% up and down, and its main cause is by weighing, and in mixing and testing process, error causes.Can find out from the embedding rate curve of the single factor experiment of three kinds of embedding mediums, be respectively with casein sodium, converted starch, soybean protein isolate in the test of single embedding medium, impact on the powdered oil embedding rate is progressively successively decreased, effect take casein sodium as single embedding medium is best, effect take converted starch as single embedding medium is better, and is relatively poor with the effect of the single embedding medium of soybean protein isolate.
(2) compound embedding medium test:
The selection of compound embedding medium, be reference according to the single factor experiment of casein sodium, gelatin, converted starch, soybean protein isolate, maltodextrin on indexs such as the situation that affects of powdered oil embedding effect, materiel machining characteristics, the smell bad due to gelatin after heating and poorly solublely affect product processing.Therefore composite experimental design with converted starch, casein sodium, three kinds of materials of soybean protein isolate, is got C
3 2Carry out in the ratio of 1: 1 composite, compound embedding medium consist of soybean protein isolate and casein sodium, soybean protein isolate and converted starch, casein sodium and converted starch.
This test is take the soybean primary oil as core, adopts two kinds of embedding mediums 1: 1 composite, take monoglyceride and sucrose ester (1: 4) as emulsifying agent, each material component put into beaker after by the weighing of table 3 formula add water 300 grams, and compound concentration is 40% emulsion.After making soybean powder oil according to aforesaid process, detect total lipid content and embedding rate, judge that by embedding rate three kinds of compound embedding mediums are respectively to the influence degree of powdered oil embedding effect.
The test recipe of table 3 different composite embedding medium
Testing result is respectively: soybean protein isolate and converted starch (a), and total lipid content 49.20%, embedding rate are 80.87%, moisture is 2%; Soybean protein isolate and casein sodium (b), total lipid content 51.44 weight portions, embedding rate are 76.53%, moisture is 2%; Converted starch and casein sodium (c), total lipid content 48.88%, embedding rate are 89.21%, moisture is 1.5%.Composite result of the test curve map is seen Fig. 2.
Can be found out significantly respectively with soybean protein isolate and converted starch (a), soybean protein isolate and casein sodium (b), converted starch and three kinds of compound embedding mediums of casein sodium (c) respectively with in composite test in 1: 1 by Fig. 2, total lipid content is in 50% left and right, embedding rate is c＞a＞b successively, the moisture 2% of the powdered oil that processes and basically identical.The fluctuation range of the content by moisture is less, illustrates that the powdered oil process is more stable.total lipid content has suitable fluctuation, its main cause is caused by journey amount and mismachining tolerance, may affect the textual criticism that the embedding effect also need be tested, but the error of total fat is less and do not affect the calculating of embedding rate, so can reflect that the compound embedding medium of soybean protein isolate and converted starch or casein sodium is close on the impact of powdered oil embedding rate, and the embedding effect of compound embedding medium is better than the single type embedding medium, the embedding effect that soybean protein isolate is described is bad, though with converted starch or its embedding effect of the compound raising of casein sodium, but can not arrive its embedding effect preferably.And in compound embedding medium, the compounded combination of converted starch and casein sodium is that in three kinds of compound embedding mediums, the embedding effect is best, and is larger to powdered oil embedding influential effect.
(3) single type embedding medium and compound embedding medium are to powdered oil embedding Contrast on effect:
Compound embedding medium curve is all above the single type embedding medium as seen from Figure 3, illustrate that compound embedding medium is more effective to the powdered oil embedding than single type embedding medium, especially the embedding effect of the compound embedding medium of soybean protein isolate and soybean protein isolate single type embedding medium alters a great deal.Single type embedding medium embedding effect is casein sodium＞converted starch＞soybean protein isolate, compound embedding medium embedding effect is casein sodium and converted starch＞converted starch and soybean protein isolate＞casein sodium and soybean protein isolate, the embedding effect of compound embedding medium has same trend with single type embedding medium embedding effect as can be known, but compound embedding medium converted starch and soybean protein isolate＞casein sodium and soybean protein isolate are different with its trend, and its reason requires further study.
The research of embodiment 2 emulsion stabilities
Various greases are due to the difference of chemical constitution, and the compatibility of they and emulsifying agent is also different.Therefore various greases are when emulsified, and the HLB value of required adaptation is also different.Selection to emulsifying agent is also just very necessary.But common a kind of emulsifying agent is HLB value of correspondence only, can't satisfy the needs of the HLB value of any oil and fat product.Therefore the present invention is by adopting composite this problem that solves of monoglyceride and sucrose ester.
(1) impact of HLB value on emulsion stability
Total inventory configures with 100g, get soybean primary oil 50%, adding compound embedding medium---the mass ratio of casein sodium and converted starch (1: 1) 5%, maltodextrin 43%, compound emulsifying agent 2%, the selected sucrose ester of compound emulsifying agent, monoglyceride was respectively 10: 0,9: 1,8: 2,7: 3,6: 4, after putting into beaker and adding water 100g and stir, after mixing by three high speed shear of colloid mill, put into 60 ℃ of water-bath oscillators, mixing speed 50r/min, the emulsion that obtains after insulation 15min is standby., determine the best proportioning of emulsifying agent and draw the optimum HLB value of emulsification as testing index with emulsion stability (5h mensuration) and viscosity.The mensuration temperature of viscosity is 30 ℃, reading after rotor rotation 15s.The impact (see Table 4) of HLB value on soybean oil emulsification liquid stability and viscosity.
The impact of table 4 HLB value on emulsion stability and viscosity
As can be seen from Table 4, when the ratio of monoglyceride and sucrose ester is 1: 4, namely the HLB value is 12.8 o'clock, and emulsion stability is best, and this moment, the viscosity of emulsion was 64mPas.This illustrates in the situation that viscosity is lower, the emulsion that just can obtain having good stability, so this test determines that emulsifier proportion is monoglyceride: sucrose ester=1: 4.
(2) impact of the addition of emulsifying agent on emulsion stability
Total inventory configures with 100g, get soybean primary oil 50%, add compound embedding medium---casein sodium and converted starch (1: 1) 5%, compound emulsifying agent monoglyceride and sucrose ester are 4: 1, the compound emulsifying agent addition gets respectively 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, the filler maltodextrin is respectively from 44.5% to 42% and successively decreases, and making total quality of material is 100%; With each material put into beaker add mix by three high speed shear of colloid mill after water 100g stirs after, put into 60 ℃ of water-bath oscillators, mixing speed 50r/min, the emulsion that obtains after insulation 15min is standby.Determining compound emulsifying agent monoglyceride and sucrose ester is 4: 1 o'clock, changes the emulsifying agent addition to stability and the viscosity of emulsion.When emulsion stability was good, the minimum of emulsifier was benefit.Table 5 is that the emulsifying agent addition is on the impact of emulsion stability.
The impact of table 5 emulsifying agent addition on emulsion stability
As shown in Table 5, emulsifying agent stability all increases along with the increase of emulsifying agent addition with viscosity, but in material the addition of emulsifying agent greater than 3% the time emulsion stability not in the impact that is subjected to addition and viscosity still increases gradually.Two emulsifications of profit were uniform and stable when the addition that emulsifying agent in material is described was 3%, then the amount that increases emulsifying agent only can improve liquid viscosity, and are all unfavorable to processing and the price of product.The consumption (except special product) of minimum when therefore the selection of emulsifier reaches emulsifying effectiveness.In the emulsion preparation, compound embedding medium itself has emulsion stabilizing effect, therefore adopts the emulsion that does not add compound embedding medium to carry out the emulsion stability test, and the content of emulsifying agent can corresponding minimizing in the emulsion that adds compound embedding medium.
(3) impact of emulsification condition on emulsion stability
Total quality of material configures with 100g.Get soybean primary oil 50%, add compound embedding medium-casein sodium and converted starch (1: 1) 5%, compound emulsifying agent monoglyceride and sucrose ester are 4: 1, the compound emulsifying agent addition is respectively 2%, 2.5%, 3%, maltodextrin is respectively 43%, 42.5%, 42%, after putting into beaker and adding water 100g and stir, by three high speed shear of colloid mill, emulsification times, temperature, rotating speed are as shown in table 6, and the emulsion that obtains after mixing is standby.
By take emulsifying temperature, emulsification times, processing rotating speed and 4 conditions of emulsifying agent addition as factor, study different emulsification conditions to the research of emulsion emulsion stability in test.Each factor is got three levels, and the design orthogonal experiment as index, is determined best emulsification condition by orthogonal test with emulsion stability, and optimum emulsification condition combination is A3B2C1D1 as shown in Table 6.
The table as a result of table 6 optimum emulsification condition
When variance analysis, calculate as testing index with emulsion stability.But consider that also viscosity index is reference, because spray dryer used in the present invention is the press spray drier, this just requires the viscosity of emulsion can not be excessive, therefore weighs emulsion and whether can carry out spray-drying by measuring viscosity.Due in actual production, after the emulsion preparation, can directly carry out spray-drying, even be subject to certain delay, time can be not long (otherwise because the nutrition of emulsion self is abundanter yet, can be subject to microorganism or the invading of oxygen and cause rotten in environment), so the minute of emulsion stability is 10 hours.
According to the extreme difference size as can be known, each factor is sequentially B＞A＞D＞C on the primary and secondary of result of the test impact, i.e. emulsifying temperature＞emulsification times＞emulsifying agent addition＞processing rotating speed.Emulsifying temperature, emulsification times have appreciable impact to emulsion stability person as can be known by analysis of variance table 7.
Table 7 analysis of variance table
Determining of embodiment 3 soybean powder oil optimization formulas
The material gross mass is configured with 200g, get 50% soybean primary oil as core, the mass percent of rest materials according to the form below is carried out weighing and is put into respectively beaker, adds water 300g, after stirring, by three high speed shear of colloid mill, the emulsion that obtains after mixing is standby; After batching is completed, emulsion is put into 60 ℃ of insulations of water-bath 20 minutes, mixing speed is 50r/min; Then carry out carrying out spray-drying after 18Mpa homogeneous 2 times.This test is got respectively three levels, the design orthogonal experiment with compound embedding medium casein sodium and converted starch ratio and content, emulsifying agent sucrose ester and monoglyceride ratio and four factors of content.
Orthogonal experiments sees Table 8.
Table 8 powdered oil optimum formula orthogonal experiments
Can obtain optimum emulsification condition combination according to orthogonal experiments is A2B3C2D2.By range analysis as can be known, each factor is sequentially B＞C＞A＞D on the primary and secondary of result of the test impact.According to analysis of variance table 9 as can be known, embedding medium content is the most remarkable, the compound proportion of embedding medium to the embedding effect greater than emulsifier content and and the composite ratio of emulsifying agent.Its reason is to determine in single factor experiment that due to emulsifying agent the emulsifying effectiveness of scope is better, and the filler such as embedding medium and maltodextrin has also played emulsification in addition, so the change of emulsifying agent is little to the embedding influential effect.The compound proportion of embedding medium is better in the higher effect of caseinic acid sodium content, this empirical tests in single factor experiment.
Table 9 variance analysis
Drawing fat content in material by orthogonal test is that 50% soybean powder oil optimization formula is: soybean primary oil 50%, casein sodium 2.5%, converted starch 2.5%, monoglyceride 0.5%, sucrose ester 2%, maltodextrin 42.5%, adding water configuration material concentration is 40%.
According to above experimental design scheme, design respectively fat content in material and be the formula of 20%, 30%, 40%, 60% soybean oil powdered oil product.Orthogonal test method is the same.
Optimum formula such as the table 10 of the soybean oil powdered oil product lab scale test of different fat contents:
The optimum formula (in 500g) of the soybean oil powdered oil lab scale test of the different fat contents of table 10
Embodiment 4 industrialization pilot productions
By the analysis to above lab scale test method and result, carry out industrialization production.Industrialization is produced to produce per year the production line of 3000 tons of soybean powder oils and is implemented, the materials such as the material-compound tank with the shearing disk high-speed electric expreess locomotive that industrialization is used in producing, colloid mill, insulation emulsion tank, homogenizer are processed and storage facilities, and high-pressure pump, spray drying tower, cyclone separator, anticaking agent add the equipment that spray drying device, packaging facilities and the cleaning equipments such as equipment, fluid bed are general routine in industry industrialization production.Content of the test is that in the industrialization production material, fat content is respectively 20%, 30%, 40%, 50%, 60% soybean oil powdered oil.
Due to industrialization production equipment ability higher than the lab scale level, therefore test parameters will be adjusted according to actual conditions.At first be the adjustment of formula, dosage and the material concentration of core soybean primary oil slightly are improved on the basis of lab scale optimum formula, and correspondingly the dosage of filler maltodextrin decreases.Next is the adjustment of production technology, in the batching stage, increases the high speed shear batching, plays the pre-emulsification effect, therefore, and can the more simple static emulsifying process of adopting process when emulsification.in addition, different from common spray drying tower is, added agglomeration equipment (referring to Fig. 4) above soybean oil powdered oil spray drying tower of the present invention, so-called agglomeration be exactly in spray-drying process material be transported to tower top by high-pressure pump and spray, droplet moisture flash evapn in tower forms particle, obtain product after particle is fallen fluid bed uniformly, and entering the bottom that cyclone separator is gathered in separator, tiny particle (fine powder) by dust feed device, fine powder is transported to again the top of tower, by the fine powder agglomeration, little dried capsule and droplet are bonded together, make the product formation diameter remain between 0.5-1mm evenly, cavernous particle, help the formation of particle, improve the embedding effect, in addition, reduced the generation of fine powder, thereby improve product instant capacity and production efficiency.In addition, due to industrialization production, powdered oil easily produces the phenomenon of caking, therefore, has added anticaking agent to add equipment in the spray drying tower exit.Anticaking agent in the present invention is selected silica, because silica has large specific area, make it play the effect of interval dose between the particle of powdered rubber, promoted simultaneously flowing freely of powdered rubber, its moisture pick-up properties is very big, has also strengthened agglomeration resistance effect and suction-operated.
Fig. 5 is the process chart that the industrialization of soybean oil powdered oil is produced, and concrete production procedure and processing parameter are as follows:
1, water heating: heating steam pressure:＜0.2MPa, water temperature: 60 ℃.
2, batching:
(1) with 800 kilograms of total inventorys, wherein inventory is 360 kilograms, and water is 440 kilograms, and compound concentration is 45% for example, and in material, the formula of different fat contents is as follows:
20% grease: 74 kilograms of soybean primary oils, 5.4 kilograms of converted starches, 5.4 kilograms of casein sodiums, 3.6 kilograms of Sucrose Fatty Acid Esters, 0.9 kilogram of monoglyceride, 270.7 kilograms of maltodextrins, 440 kilograms, water.
30% grease: 110 kilograms of soybean primary oils, 5.4 kilograms of converted starches, 5.4 kilograms of casein sodiums, 3.6 kilograms of Sucrose Fatty Acid Esters, 0.9 kilogram of monoglyceride, 234.7 kilograms of maltodextrins, 440 kilograms, water.
40% grease: 146 kilograms of soybean primary oils, 8.1 kilograms of converted starches, 8.1 kilograms of casein sodiums, 7.2 kilograms of Sucrose Fatty Acid Esters, 1.8 kilograms of monoglycerides, 188.8 kilograms of maltodextrins, 440 kilograms, water.
50% grease: 182 kilograms of soybean primary oils, 9 kilograms of converted starches, 9 kilograms of casein sodiums, 7.2 kilograms of Sucrose Fatty Acid Esters, 1.8 kilograms of monoglycerides, 151 kilograms of maltodextrins, 440 kilograms, water.
60% grease: 218 kilograms of soybean primary oils, 10.8 kilograms of converted starches, 10.8 kilograms of casein sodiums, 7.2 kilograms of Sucrose Fatty Acid Esters, 1.8 kilograms of monoglycerides, 111.4 kilograms of maltodextrins, 440 kilograms, water.
(2) mix-order is successively: water, converted starch, maltodextrin, casein sodium, Sucrose Fatty Acid Ester, monoglyceride, soybean primary oil.
(3) technological requirement: 2800r/min high speed shear batching plays the pre-emulsification effect, and mixing time is the emulsion of 10 minutes formation uniformities.
3, refinement
The colloid mill gap is 0.1-5mm, carries out the refinement of emulsion.
4, emulsification
Emulsifying device: interlayer heated type insulation emulsion tank
Emulsifying manner: static insulation emulsification
Steam pressure:＜0.2MPa
Emulsifying temperature: 65 ℃
Emulsification times: 20min
5, homogeneous
Homogenization pressure a: 18Mpa
Second homogenate pressure: 30Mpa
6, spray-drying
Material is squeezed in tower by high-pressure pump, high-pressure pump pressure: 5-20Mpa
Inlet temperature: 150-155 ℃
Outlet temperature: 85-90 ℃
Temperature in tower: 92 ℃ of left and right
7, add anticaking agent: addition accounts for total powder outlet quantity and calculates, and this production equipment flour extraction design is greater than 90%, and the silica addition is 3.24 kilograms-4.68 kilograms, and therefore accounting for material percentage is 0.9%-1.3%
8, cooling: air mass flow is 3.12m
3/ min, cooling in fluid bed, obtain dry powder.
9, packing: the brown paper packing of package metro-measuring 25Kg liner moisture barrier bag.
10, carry out equipment after production finishes and clean (CIP cleaning): hot water temperature: 80 ℃; The buck temperature: 80 ℃, buck concentration 1.5-2%.
Product physics and chemistry and sanitary index:
Be that 50% soybean primary oil powdered oil industrialization product detects according to aforesaid detection method to fat content in material, result such as table 11.
Table 11 physics and chemistry and sanitary index
Annotate: table 11 is only enumerated the physics and chemistry sanitary index of the soybean powder oil product of 50% fat content.Other products all detect, and do not enumerate at this.
The physical and chemical index of all products all satisfies the company standard that this product is formulated, sanitary index is near company standard, reason may be because pipeline is not produced continuously, makes the floras such as bacterium, yeast higher, but can reduce the pollution of microorganism when reality is produced continuously.
Claims (13)
1. a soybean oil powdered oil, is characterized in that, the percentage by weight of this powdered oil each component when batching is:
Core: 9.25%-27.25%
Embedding medium: 1.35%-2.7%
Filler: 13.925%-33.8375%
Emulsifying agent: 0.5625%-1.125%
Water: 55%
Wherein,
Described core is the soybean primary oil,
Described embedding medium be in casein sodium, converted starch and soybean protein isolate any or any two,
Described filler is any in maltodextrin, malt syrup or HFCS,
Described emulsifying agent is comprised of monoglyceride and sucrose ester.
2. soybean oil powdered oil as claimed in claim 1, is characterized in that, described filler is maltodextrin.
3. soybean oil powdered oil as claimed in claim 1, is characterized in that, described embedding medium is selected from any two in casein sodium or converted starch or soybean protein isolate.
4. soybean oil powdered oil as claimed in claim 3, is characterized in that, described embedding medium is the mixture of casein sodium and converted starch, and wherein, casein sodium and converted starch mass ratio are 0.8-1.25:1.
5. soybean oil powdered oil as claimed in claim 4, is characterized in that, casein sodium and converted starch mass ratio are 1:1.
6. soybean oil powdered oil as claimed in claim 1, is characterized in that, in described emulsifying agent, the mass ratio of monoglyceride and sucrose ester is 0.25-2.4:1.
7. soybean oil powdered oil as claimed in claim 6, is characterized in that, in described emulsifying agent, the mass ratio of monoglyceride and sucrose ester is 0.25:1.
8. soybean oil powdered oil as described in claim 1-7 any one, is characterized in that, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 9.25%
Casein sodium: 0.675%
Converted starch: 0.675%
Monoglyceride: 0.1125%
Sucrose ester: 0.45%
Maltodextrin: 33.8375%
Water: 55%.
9. soybean oil powdered oil as described in claim 1-7 any one, is characterized in that, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 13.75%
Casein sodium: 0.675%
Converted starch: 0.675%
Monoglyceride: 0.1125%
Sucrose ester: 0.45%
Maltodextrin: 29.3375%
Water: 55%.
10. soybean oil powdered oil as described in claim 1-7 any one, is characterized in that, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 18.25%
Casein sodium: 1.0125%
Converted starch: 1.0125%
Monoglyceride: 0.225%
Sucrose ester: 0.9%
Maltodextrin: 23.6%
Water: 55%.
11. soybean oil powdered oil as described in claim 1-7 any one is characterized in that, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 22.75%
Casein sodium: 1.125%
Converted starch: 1.125%
Monoglyceride: 0.225%
Sucrose ester: 0.9%
Maltodextrin: 18.875%
Water: 55%.
12. soybean oil powdered oil as described in claim 1-7 any one is characterized in that, the percentage by weight of this powdered oil each component when batching is:
Soybean primary oil: 27.25%
Casein sodium: 1.35%
Converted starch: 1.35%
Monoglyceride: 0.225%
Sucrose ester: 0.9%
Maltodextrin: 13.925%
Water: 55%.
13. a method for preparing soybean oil powdered oil as claimed in claim 1 is characterized in that, carries out as follows:
A. water heating: heating steam pressure:＜0.2MPa, water temperature: 60 ℃;
B. prepare burden: add successively embedding medium, filler, emulsifying agent, core by described part by weight in water, make emulsion after high speed shear;
C. refinement: with colloid mill with above-mentioned emulsion refinement;
D. emulsification: steam pressure:＜0.2MPa, 65 ℃ of emulsifying temperatures, emulsification times 20min;
E. homogeneous: homogenization pressure a: 18Mpa, second homogenate pressure: 30Mpa;
F. spray-drying: inlet temperature: 150-155 ℃, outlet temperature: 85-90 ℃, charging high-pressure pump pressure: 5-20Mpa;
G. anticaking agent adds: the silica addition accounts for the 0.9%-1.3% of material addition;
H. cooling: the cooling dry powder that obtains in fluid bed, air mass flow is 3.12m
3/ min;
I. pack: the brown paper with metering 25Kg liner moisture barrier bag is packed;
J. equipment cleans: hot water temperature: 80 ℃; The buck temperature: 80 ℃, buck concentration 1.5-2%.
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| CN112641090A (en) * | 2020-12-18 | 2021-04-13 | 广州白云山汉方现代药业有限公司 | High-energy-density high-protein full-nutrition milk and preparation method thereof |
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