CN1759697A - Method for preparing freeze dried superfines of persimmon - Google Patents
Method for preparing freeze dried superfines of persimmon Download PDFInfo
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Abstract
A process for preparing the superfine freeze-dried persimmon powder with high solubility and chemical activity includes such steps as providing fresh hard persimmon, removing puckery taste, vacuum freeze drying, and superfine pulverizing by airflow grinder. Its advantage is no loss in special smell and nutrients.
Description
Technical field:
The present invention relates to persimmon be carried out method for processing with vacuum freezing drying dehydration technology and airflow milling technology.
Background technology
Persimmon has another name called Zhu fruit, is widely grown in the northern China and the Huanghe valley, the cultivation history in existing more than 3,000 year.Persimmon is that a kind of nutritional labeling is abundant, the fruit that nutritive value is very high.By analysis: in the bright persimmon of 1kg, contain 110g carbohydrate, 1g fat, 7g protein, contain 1.6mgV
A, 0.1mgV
B1, 0.2mgV
B2, 160mgVc, 100mg calcium, 190mg phosphorus, 2mg iron, 80-84mg iodine, 80mg cobalt, 40mg manganese, 0.4mg selenium, 6.76mg zinc or the like element; Still 18 seed amino acids that contain needed by human in the fruit, its total sugar content 8-11%.Be a kind of fruit in season that people like, but that it easily go mouldy is rotten, freshness date is extremely short, can't long preservation.Utilize the vacuum freezing drying dehydration technology can solve this difficult problem.The vacuum freezing drying dehydration technology is one vegetables, fruit, meat etc. is protected look, fresh-keeping, the high-new process technology of guaranteeing the quality, abbreviates freeze-drying as.This technology is taked at low temperatures, material is carried out freezing rapidly, makes a kind of lyophilization method of the moisture of material by solid-state direct convert gaseous then under high vacuum.This process technology has been avoided defectives such as the variable color that traditional drying and dewatering technology brings, rotten off-flavour component run off, can't reduce, and can keep shape, look, the flavor of former material constant, and it is good, lossless to have a dry fruit rehydration, lightweight advantage.Therefore, the freeze dried and antistaled technology of research persimmon helps the Long-term Storage and the deep processing of persimmon.At present, Shang Weijian is about the bibliographical information of freeze dried superfines of persimmon process technology content.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of freeze dried superfines of persimmon, with solve persimmon fresh-keeping, deposit with deep processing in a difficult problem.
Technical scheme of the present invention is realized by the following step: a kind of preparation method of freeze dried superfines of persimmon, be divided into five stages of pre-treatment, prefreezing, lyophilization, parsing-desiccation, ultra-fine grinding of material, and it is characterized in that
Pretreatment stage: select ripe very likely persimmon for use, after taking away the puckery taste with warm water, persimmon is cut into small pieces, the dryness storehouse quick-frozen is put in sabot then;
The prefreezing stage: in the prefreezing stage, the prefreezing temperature of material should reach following 5～10 ℃ of its eutectic temperature, and temperature of charge can distil below eutectic point, and does not thaw;
The lyophilization stage: when material central temperature in the dryness storehouse reaches it and freezes fully below eutectic temperature, constant temperature keeps 1～1.5h, make the material deep colling, implement again to vacuumize, heat, promptly begin lyophilization, should guarantee that in this stage material freezes portion temperature and is lower than its plait point temperature, vacuum and condenser temperature must keep corresponding technological requirement value simultaneously, keep this process to all ice crystal distillations;
The parsing-desiccation stage: after the ice crystal distillation finishes, must continue one section parsing-desiccation process, what be about to partly not freeze in the material removes by evaporation in conjunction with water, should guarantee that temperature of charge is below the maximum permissible temperature of disintegration temperature this moment, when material remnant moisture reaches 3%-5%, finish freeze-drying process;
The ultra-fine grinding stage: after the freeze-drying of persimmon piece, should adopt the plant pulverizer to roughly grind immediately, carry out ultramicro grinding with the airflow milling pulverizer at last, thereby obtain freeze dried superfines of persimmon.
Prefreezing stage wherein: raw meal particle size is 0.5cm * 0.5cm, and material thickness is 10mm-15mm, and material pre-freeze temperature is-20 ℃ of-25 ℃ of intervals, and pre-freeze speed is 0.03-0.05h/mm.
Wherein distil the freeze-drying stage: dryness storehouse vacuum 20-40Pa, 20 ℃-30 ℃ of temperature of heating plate, temperature of charge-20 ℃--25 ℃, cold sunken temperature-35 ℃, when freezing dried rate was 95%, its freeze drying rate was 0.53-0.55h/mm.
Desorption phase wherein: below the dryness storehouse pressure 20Pa, 20 ℃-25 ℃ of temperature of charge, 25 ℃ of temperature of heating plate, cold sunken temperature＜-35 ℃.
Ultra-fine grinding stage wherein: air-flow grinding machine operating pressure is 6Pa-12Pa, and the material inlet granularity is 0.5-10mm, finished product granularity＜10-100 μ m.
The freeze dried superfines of persimmon of producing with the inventive method has unique physical and chemical performance, good dispersiveness, adsorptivity, dissolubility, chemism, complete reservation intrinsic fragrance and the nutrition of persimmon, freeze dried superfines of persimmon can be used as the preparation persimmon beverage, fruit is brilliant, the primary raw material of soft sweets, also can be used as the additive of fruit food, but and long preservation, color is constant.
Description of drawings
Fig. 1 is the three-phase equilibrium schematic diagram of water.
Fig. 2 is persimmon freeze-drying curve figure.
Specific embodiment
Introduce the technological process of persimmon vacuum freeze drying below in detail, and to the measurement and the control of the technological parameters such as eutectic point of the temperature in this technological process programme-control, the technological process, vacuum, freeze-drying curve, persimmon material thickness, persimmon, analyze and research, determined the cryodesiccated optimum operation condition of persimmon, actual freeze drying production has been had certain directive significance.
1, test material and method
1.1 Vacuum Freezing ﹠ Drying Technology principle
Vacuum Freezing ﹠ Drying Technology (abbreviation freeze-drying) is will to freeze through the material after the pre-treatment earlier, then in vacuum tank, under certain vacuum, material is heated, make that moisture is steam state from solid-state direct distillation in the material, and water vapour is drained by vacuum system, thereby remove the moisture in the wet stock, obtain dried product (abbreviation freeze-drying prods).
The distillation principle of freeze-drying process is based on the three-phase equilibrium figure of water, as shown in Figure 1, the ternary transformation temperature of water is directly relevant with pressure, and pressure reduces, and the freezing point of water changes little, boiling point then reduces with the reduction of pressure, when pressure hanged down to a certain value, the boiling point of water promptly coincided with freezing point, promptly reaches the three-phase equilibrium point to water, at this moment pressure is called three phase point pressure P 0 and is 610.5Pa., and corresponding temperature is called three phase point temperature T 0 and is 00980C.When pressure was lower than P0, water just from the solid-state steam state that is converted into, was called distillation, and the heat that is absorbed when distillation is called the heat of sublimation.The basic principle of freeze-drying is exactly the solid conversion process of vapour on the AD line.Ice can be gas phase by solid transformation directly just.
But because in the fresh feed, except that containing moisture, also have inorganic salts, sugar and vitamin etc. to coexist as in the cell, and the content of each composition of different material is also inequality, they are dissolved in water and form solution, the freezing point that causes water descends, and temperature was referred to as eutectic point when the solution that becomes to be grouped into when water and resolvability was icing, and so-called eutectic point temperature just is meant that the scars material is in the intensification sublimation process, when reaching a certain temperature, the temperature when beginning liquid state to occur in the solid claims that this is an eutectic point.Therefore, different material has different eutectic points and eutectic point.The existence form of moisture mainly is free water and irreducible water in the material, and free water accounts for the overwhelming majority of water content, removes free water, and reducing water activity is the main purpose of food drying.When freezing material to eutectic point the time, in cell and the space between cells in free water be frozen into the ice crystal that particle does not wait, in the environment of higher vacuum, these ice crystals will at first distil on the material surface, and from outward appearance to inner essence outside effusion water vapour, moisture in the material is removed, cryodesiccated basic principle that Here it is.
1.2, experimental facilities
This test adopts the FD-0.5 vacuum freeze drier to carry out the test of persimmon freeze-dry process.This equipment mainly is made up of following five parts.
1) dryness storehouse, it is freezing and dry to be used for material, is the case body equipment of a heat transfer and mass transfer.
2) water vessel (claiming water condenser or cold-trap again), being used for condensing captures distillation and the desorption phase condensing plant from material effusion steam.
3) refrigerating plant, totally two refrigeration systems, one is used for cool drying case material, and another system is for water vessel cooling, and institute's liberated heat when taking away condensation of moisture makes water vessel maintain-34 ℃～-45 ℃ low temperature;
4) vacuum system is used for distillation and desorption process, keeps the vacuum of drying box and water vessel, guarantees that freeze drying carries out smoothly.
5) heating system is used for the control of temperature of heating plate.
6) control and measuring system, control and measurement distillation and desorption process state parameter.
These equipment major technology performance indications are:
The effectively total drying area of single mount dish is 0.5m
2
Dryness storehouse working vacuum degree scope: 13.3～133Pa (time of full load forvacuum degree (30Pa) is 10min);
The cold-trap operating temperature :-35 ℃～-45 ℃ (maximum is caught the water yield: 25kg);
Lyophilization cycle (comprising the defrosting of charging and discharging and cold-trap): 10～20h;
1.3, experimental procedure
The vacuum freeze drying process generally is divided into pre-treatment, prefreezing, lyophilization, the parsing-desiccation four-stage of material.
Pretreatment stage: select ripe very likely persimmon for use, after taking away the puckery taste with warm water, persimmon is cut into length of side 5mm or the square fritter of 1cm, the dryness storehouse quick-frozen is put in sabot then.
The prefreezing stage: in the prefreezing stage, the prefreezing temperature of material should reach following 5 ℃～10 ℃ of its eutectic temperature.Temperature of charge can distil below eutectic point, and does not thaw.
The lyophilization stage: when material central temperature in the dryness storehouse reached it and freezes fully below eutectic temperature, constant temperature kept 1～1.5h, makes the material deep colling.Implement again to vacuumize, heat, promptly begin lyophilization.Should guarantee that in this stage material freezes portion temperature and is lower than its plait point temperature (vacuum and condenser temperature must keep corresponding technological requirement value simultaneously), keep this process to all ice crystal distillations.
The parsing-desiccation stage: after the ice crystal distillation finishes, must continue one section parsing-desiccation process, what soon part was not freezed in the material removes by evaporation in conjunction with water, and should guarantee that temperature of charge is below the maximum permissible temperature of disintegration temperature this moment.When material remnant moisture reaches 3%-5%, finish freeze-drying process.
1.4, the technological parameter method of testing
1.4.1 the mensuration of eutectic point and eutectic point: what the assay method of eutectic point was commonly used is the resistance measurement method.Principle is to utilize material in freezing process, and temperature is removed to freezing point, and ice crystal begins to form, and along with temperature of charge descends, ice crystal increases gradually.When the moisture that temperature is reduced in certain some material is all iced knot, at this moment resistance can increase suddenly, almost is infinitely great, and the temperature of this moment is exactly the eutectic temperature of material.
The eutectic point temperature just is meant the scars material in the intensification sublimation process, when reaching a certain temperature, begins in the solid liquid state to occur, and resistance value reduces suddenly, and this temperature is called the eutectic point of solution.Its assay method is identical with the assay method of eutectic point, and both are more or less the same.
1.4.2 pre-freeze speed: unit thickness material pre-freeze is during to the eutectic temperature of material following 5 ℃ or 10 ℃, and required cooling time: unit is h/mm.
1.4.3 freeze-drying rate: be the ratio that the dehydration quality accounts for the material moisture total amount after the material freeze-drying, assay method commonly used is a weight method, represents with difference and homogenous quantities fresh fruit and its ratio of drying the difference of back quality of quality after homogenous quantities fresh fruit and its freeze-drying.
1.4.4 freeze drying rate: under same freeze-drying rate, the freeze-drying time of unit thickness material, and the ratio of the freeze-drying time (h) of material and material thickness (mm), unit is h/mm.
2, result of the test and discussion
2.1 the eutectic point of persimmon and eutectic point, we record persimmon resistance change-11 ℃～-14 ℃ the time with electric-resistivity method and turnover takes place sharply increase, and this turning point temperature should be the eutectic temperature of persimmon.Equally, record persimmon resistance change-13 ℃～-10 ℃ the time with electric-resistivity method and turnover takes place from large to small.Should be the eutectic point temperature of persimmon.The prefreezing temperature of material should be eutectic point or below the eutectic point temperature 5 ℃～10 ℃.In view of the above, our the prefreezing temperature of selecting material is-20 ℃～-25 ℃ intervals.
2.2 material thickness
The thickness of material directly influences freeze drying rate, thin thickness, and freeze-drying time can reduce greatly.But can reduce the device processes ability.Thickness thickens, and freeze-drying time is with big leap ahead.And in the distillation freeze-drying process, along with the growth of distillation time, when the freeze-drying layer formed gradually, heating plate can make the temperature on freeze-dried material top layer raise, and causes that the form of material and color change.In the experiment, we have investigated the influence of the thickness of material to freeze drying rate under other controlled conditions and freeze-drying rate fixation case, see Table 1.The material thickness that experiment is finally chosen is 10mm～15mm; In the freeze-drying rate is 95% o'clock, and its freeze drying rate is 0.53～0.55h/mm.
Table 1: the thickness of material is to the influence of freeze drying rate
| Material thickness (mm) | 20 | 17.5 | 15 | 10 | 5 |
| Freeze-drying time (h) | 13.5 | 11 | 8.5 | 5.5 | 3.5 |
| Freeze drying rate (h/mm) | 0.68 | 0.63 | 0.53 | 0.55 | 0.7 |
2.3 pre-freeze speed and pre-freeze temperature
Pre-freeze speed directly influences the quality of rate of drying and product.When freezing slowly, the ice crystal particle is big, helps the distillation of article, and rehydration speed is fast; But the food nerve is poor; Quick freezing, the crystal ice granule of generation is little, and it is slower to distil, and rehydration speed is slow, but the nerve of dried product is good.The thickness of pre-freeze speed and material and dryness storehouse prefreezing temperature correlation.When material thickness was 10mm～15mm, the prefreezing temperature was～20 ℃～-25 ℃ intervals, and the material pre-freeze speed that we select is 0.03～0.05h/mm;
2.4 the condition of sublimation stage control
2.4.1 temperature of charge in dryness storehouse and the storehouse
The sublimation stage temperature of charge should be lower than its eutectic point temperature, and it is too many that temperature of charge is lower than the eutectic point temperature, and rate of sublimation is low, the distillation time is long; Be higher than the eutectic point temperature.Product melts, and influences product quality and dry run.In view of the above, the temperature of charge that we select material is-20 ℃～-25 ℃ intervals, and the dryness storehouse temperature is a little less than temperature of charge 1-2 ℃.
2.4.2 temperature of heating plate
The temperature of freeze-drying curve is exactly the heating-up temperature of dryness storehouse, and the control temperature plays an important role to the quality of freeze-dried products.The latent heat of phase change that needs during the material distillation is mainly supplied with by heating plate.But should guarantee heating plate institute heating load size at sublimation stage, material is heated up be higher than its eutectic point temperature.Under the dryness storehouse different temperatures, the heat of sublimation of ice sees Table 2.In desorption phase, temperature of heating plate just is lower than maximum permissible temperature.Otherwise the maximum temperature that the material central temperature surpasses material can occur, the material disintegration is melted, the surface is burnt or is out of shape.In the test, the temperature of heating plate that we select is 20 ℃～30 ℃ intervals.
Table 2: the saturated vapor pressure of ice and distillation hotlist
| Temperature (℃) | Vapour pressure (Pa) | The heat of sublimation (Kj/kg) |
| -10 | 260.2 | 2837.4 |
| -15 | 130.6 | 2837.8 |
| -20 | 103.5 | 2838.4 |
| -25 | 63.2 | 2837.9 |
| -30 | 38.1 | 2839.0 |
| -35 | 22.4 | 2839.2 |
2.4.3 the vacuum of sublimation stage dryness storehouse
The dryness storehouse temperature level influences the heat and mass of lyophilization process.The pressure height, heat-transfer effect is good, but is unfavorable for the effusion of steam; Pressure is low, and heat-transfer effect is poor, helps the effusion of steam.Whole sublimation process is exactly a heat and mass transfer process.Have only pressure suitable, an economic rate of drying just can be arranged.
Usually should the force value of dryness storehouse be controlled at a little less than the highest sublimation temperature corresponding saturated vapor pressure 1/2nd.The saturated vapor pressure of ice sees Table 2.The dryness storehouse internal pressure scope of experiment that we select is 20～40Pa.
2.4.4 condenser temperature: when condenser temperature is low more, the water vapour pressure difference is big more between distillation interface and water vessel surface, can accelerate drying time.We select condenser temperature for use is-35 ℃.
2.5 desorption condition
Desorption phase is not freezed ice because of not existing in the material, product temperature can rise to the highest permissive temperature rapidly and keep a period of time under this temperature, make in conjunction with water and the enough energy of water acquisition that are adsorbed in the drying layer and from Molecular Adsorption, parse, product temperature is generally 20～25 ℃, and temperature of heating plate is a little more than the product temperature several years.And dryness storehouse pressure is dropped to below the 20Pa, help steam and from product, overflow.The temperature of desorption phase water vapour coagulator can reduce because of steam vapour amount subtracts greatly to load, and causes its temperature to descend to some extent.
2.6 the research of the best lyophilisation condition of persimmon
To influencing the main technique condition that the persimmon freeze-drying is produced, we adopt orthogonal design to implement the exploration of best distillation lyophilisation condition.Inquired into dryness storehouse vacuum, temperature of heating plate, condenser temperature is to the influence of persimmon freeze-drying rate.EE with the results are shown in Table 3.
Through experiment repeatedly, by range analysis in the table 3 as seen: 5mm is square at raw meal particle size, and when material thickness was 10mm～15mm, the freeze-dry process condition to the primary and secondary ordering of persimmon freeze-drying result influence was: hothouse vacuum＞temperature of heating plate＞condenser temperature; The best of persimmon distillation lyophilisation condition is: dryness storehouse vacuum 20Pa, 25 ℃ of temperature of heating plate, condenser temperature-35 ℃.
Table 3: orthogonal design L9 (33) EE and result
| The test sequence number | Dryness storehouse vacuum (Pa) | Temperature of heating plate (℃) | Trap temperature cold as ice and frost (℃) | Freeze-drying rate (%) |
| 1 | 20 | 20 | -40 | 93 |
| 2 | 20 | 25 | -35 | 97 |
| 3 | 20 | 30 | -30 | 93 |
| 4 | 30 | 20 | -35 | 94 |
| 5 | 30 | 25 | -30 | 93 |
| 6 | 30 | 30 | -40 | 92 |
| 7 | 40 | 20 | -30 | 93 |
| 8 | 40 | 25 | -40 | 91 |
| 9 | 40 | 30 | -35 | 90 |
| I | 283 | 280 | 279 | R is the extreme difference value |
| II | 279 | 281 | 281 | |
| III | 274 | 275 | 276 | |
| R | 9 | 6 | 5 |
2.7 persimmon freeze-drying curve
The persimmon freeze-drying curve is the curve of record temperature of heating plate, temperature of charge, condenser temperature and dry vacuum time to time change, and we have implemented monitoring result to each factor in the actual production and seen Fig. 2 according to the best freeze-dry process condition of above-mentioned persimmon.Should it have certain directive significance to actual production.
2.8 freeze-drying persimmon product characteristics
2.8.1 dry back persimmon product is porous spongy, volume, shape invariance, no drying shrinkage phenomenon, fabulous rehydration is arranged, the freeze-drying persimmon is immersed in 50mi 20n in the normal-temperature water, presses reconstitution rate=[weight after (weight after the rehydration-dry product weight)/rehydration] * 100% and calculate, reconstitution rate is 80%.The moisture content of the fresh persimmon that records simultaneously is 82.5%, and visible persimmon rehydration is fine, and this can recover original proterties after persimmon rehydration also is described substantially.Internal structure is preserved good.
2.8.2 because dry run is carried out under vacuum, readily oxidizable substance is protected; And can kill a large amount of bacteriums under the vacuum state, suppress to recover original proterties substantially after part bacterium and the rehydration.Internal structure is preserved good.
2.8.3 because dry run carries out at low temperatures, in the food loss of the nutritional labeling of volatile component and heated denaturalization very little, keep original color of food and nutritional labeling to greatest extent.
2.8.4 the freeze-drying prods residual water content is very low, is generally 3%～5%, but long preservation.
3, conclusion
The best freeze-dry process condition of persimmon is: the prefreezing stage: raw meal particle size 5mm is square, and material thickness is 10mm～15mm; Material pre-freeze temperature is-20 ℃～-25 ℃ intervals, pre-freeze speed 0.03～0.05h/mm; The distillation freeze-drying stage: below the dryness storehouse vacuum 20Pa, temperature of charge-10～-22 ℃, 25 ℃ of temperature of heating plate, condenser temperature-35 ℃.
4, ultra-fine grinding
4.1 coarse crushing: after the freeze-drying of persimmon piece, the persimmon piece is spongy, only surplus 3-5% is very crisp for water content, also very easily gets damp, and should adopt the plant pulverizer to roughly grind immediately, the corase grind granularity is 10-100mm, the persimmon freeze-dried powder of roughly grinding is sent to vacuum drying cabinet rapidly, vacuumizes with aluminium platinum paper, sealing is preserved, and is strictly on guard against and gets damp.
4.2 ultramicro grinding: because the plant pulverizer is when pulverizing the freeze-drying persimmon, because of easily heating of machine operation, thus can not the freeze-drying persimmon process very thin.Show through multiple breaking method experimental result, select the method effect of airflow milling machined freeze-drying persimmon ultra micro powder best.
Airflow milling claims that again fluid energy mill or jet mill are to utilize compressed air or superheated steam to produce high pressure and produce the carrier of supersonic airstream for material particles by nozzle for working medium, make particle obtain huge kinetic energy.Collision mutually takes place or impacts with fixed head in the particle of two bursts of move toward one another, thereby reaches the purpose of pulverizing.Compare with standard machinery formula micronizer, it is very thin that the airflow milling pulverizer can further be pulverized freeze-drying persimmon meal, and particle size distribution is little, and granularity is more even, persimmon freeze-dried powder finished product granularity＜10-25 μ m.See Table 4, can lower the temperature because gas expands at the nozzle place, not association of crushing process heat, it is very low to heat up during pulverizing, selects the machined ultra micro powder of airflow milling for use for the higher persimmon raw material of thermal sensitivity, and its nutritive value is not suffered a loss substantially.
Table 4 freeze-drying persimmon grinding particle size type
| Pulverize type | Raw material granularity/mm | Finished product granularity/mm | Pulverize type | Raw meal particle size/mm | Finished product granularity/um |
| Coarse crushing | 10-100 | 5-10 | Micro mist is broken | 5-10 | ＜100um |
| Fine powder is broken | 5-50 | 0.1-5 | Ultramicro grinding | 0.5-5 | ＜10-25um |
4.3 when the freeze-drying persimmon reaches the required standard granularity through air-flow grinding machine ultramicro grinding, immediately at aseptic hothouse, vacuumize with senior aluminide-coating bag component and to pack, storage life can reach 3-5 and never degenerate.
5, the measurement result of freeze-drying persimmon ultra micro powder nutrition sees Table 5
The nutrition measurement result of table 5 freeze-drying persimmon ultra micro powder
| Amino acid (g/100ml) | Inorganic elements (μ g/g) | Other composition (%) | |||
| Aspartic acid (ASP) | 0.3434 | Na | 240.6 | Total acid | 0.64 |
| Threonine (Thr) | 0.1628 | Ca | 832.0 | Crude fat | 4.98 |
| Serine (Ser) | 0.1645 | Mg | 508.1 | Crude protein | 3.27 |
| Glutamic acid (Glu) | 0.4495 | P | 790.0 | Total reducing sugar | 49.5 |
| Proline (Pro) | 0.1448 | K | 620.0 | Glucose | 20.2 |
| Glycine (Gly) | 0.1693 | Cu | 1.25 | Fructose | 25.7 |
| Alanine (Ala) | 0.1521 | Fe | 103.4 | Crude fibre | 6.66 |
| Cystine (Cys) | 0.01204 | Mn | 5.83 | Moisture | 3.95 |
| Valine (Val) | 0.1537 | Zn | 6.75 | Ash content | 2.07 |
| Methionine (Met) | 0.05513 | Se | 0.04 | Tannin | 0.89 |
| Isoleucine (Lieu) | 0.1690 | I | 504.1 | Vitamin (mg/100g) | |
| Leucine (Len) | 0.2500 | Co | 480.2 | V E | 1.833 |
| Tyrosine (Tyr) | 0.1144 | V C | 37.0 | ||
| Phenylalanine (Phe) | 0.1692 | V B2 | 0.07 | ||
| Lysine (Lys) | 0.2195 | V B1 | 0.03 | ||
| Histidine (His) | 0.06069 | V A1 | 13.56 | ||
| Arginine (Arg) | 0.1486 | ||||
6, the organoleptic indicator of freeze-drying persimmon ultra micro powder sees Table 6.
The organoleptic indicator of table 6 freeze-drying persimmon ultra micro powder.
| Project | Index |
| Granularity/μ m | Common flour＜100 μ m high-quality powder 10-25 μ m |
| Color and luster | Pale yellow or deep yellow |
| Fragrance | Has unique bright persimmon fragrance |
| Mouthfeel | Very sweet astringency-less persimmon flavor |
| Dissolution phenomena | Distribute persimmon fragrance look Huang after the dissolving persimmon powder precipitation is arranged |
| Style | Individual style with persimmon |
Annotate: subjective appreciation is a freeze-drying persimmon ultra micro powder comprehensive review group evaluation result
Claims (6)
1, a kind of preparation method of freeze dried superfines of persimmon is divided into five stages of pre-treatment, prefreezing, lyophilization, parsing-desiccation, ultra-fine grinding of material, it is characterized in that
Pretreatment stage: select seven or eight fens ripe persimmons for use, after taking away the puckery taste with warm water, persimmon is cut into small pieces, the dryness storehouse quick-frozen is put in sabot then;
The prefreezing stage: in the prefreezing stage, the prefreezing temperature of material should reach following 5 ℃～10 ℃ of its eutectic temperature, and temperature of charge can distil below eutectic point, and does not thaw;
The lyophilization stage: when material central temperature in the dryness storehouse reaches it and freezes fully below eutectic temperature, constant temperature keeps 1～1.5h, make the material deep colling, implement again to vacuumize, heat, promptly begin lyophilization, should guarantee that in this stage material freezes portion temperature and is lower than its plait point temperature, vacuum and condenser temperature must keep corresponding technological requirement value simultaneously, keep this process to all ice crystal distillations;
The parsing-desiccation stage: after the ice crystal distillation finishes, must continue one section parsing-desiccation process, what be about to partly not freeze in the material removes by evaporation in conjunction with water, should guarantee that temperature of charge is below the maximum permissible temperature of disintegration temperature this moment, when material remnant moisture reaches 3%-5%, finish freeze-drying process;
The ultra-fine grinding stage: after the freeze-drying of persimmon piece, should adopt the plant pulverizer to roughly grind immediately, carry out ultramicro grinding with the airflow milling pulverizer at last, thereby obtain freeze dried superfines of persimmon.
2, the preparation method of a kind of freeze dried superfines of persimmon as claimed in claim 1, it is characterized in that the prefreezing stage: raw meal particle size is 0.5cm * 0.5cm, material thickness is 10mm-15mm, and material pre-freeze temperature is-20 ℃--25 ℃ of intervals, pre-freeze speed are 0.03-0.05h/mm.
3, the preparation method of a kind of freeze dried superfines of persimmon as claimed in claim 1, the freeze-drying stage is characterized in that distilling: dryness storehouse vacuum 20-40Pa, 20 ℃-30 ℃ of temperature of heating plate, temperature of charge-20 ℃--25 ℃, cold sunken temperature-35 ℃, when freezing dried rate was 95%, its freeze drying rate was 0.53-0.55h/mm.
4, the preparation method of a kind of freeze dried superfines of persimmon as claimed in claim 1 is characterized in that desorption phase: below the dryness storehouse pressure 20Pa, and 20 ℃-25 ℃ of temperature of charge, 25 ℃ of temperature of heating plate, cold sunken temperature＜-35 ℃.
5, the preparation method of a kind of freeze dried superfines of persimmon as claimed in claim 1 is characterized in that the ultra-fine grinding stage: air-flow grinding machine operating pressure is 6Pa-12Pa, and the material inlet granularity is 0.5-10mm, finished product granularity＜10-100 μ m.
6, the preparation method of a kind of freeze dried superfines of persimmon as claimed in claim 3, the freeze-drying stage is characterized in that distilling: dryness storehouse vacuum 20Pa, 25 ℃ of temperature of heating plate, temperature of charge-10 ℃～-22 ℃, condenser temperature-35 ℃.
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