CN104351171A - Plant leaf flour-milling freezing-drying process - Google Patents
Plant leaf flour-milling freezing-drying process Download PDFInfo
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- CN104351171A CN104351171A CN201410618063.3A CN201410618063A CN104351171A CN 104351171 A CN104351171 A CN 104351171A CN 201410618063 A CN201410618063 A CN 201410618063A CN 104351171 A CN104351171 A CN 104351171A
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Abstract
The invention discloses a plant leaf flour-milling freezing-drying process. The plant leaf flour-milling freezing-drying process is characterized in that by comprising the following steps: removing withered and yellow leaves and foreign substances from raw materials as 6-10-year plant leaves, rinsing the selected plant leaves with 3.5% D-2.3.5.6-tetrahydroxyl-2-hexenoic acid-gamma-lactonic sodium and 1.5% deacetyl chitin, draining, drying under a vacuum condition at 10-20 DEG C, and refrigerating at 2-6 DEG C for standby use; starting a freezing concentration device, feeding feed liquid into the freezing concentration device, and carrying out freezing concentration within a set time period, wherein the feed liquid is separated into a high-concentration solution and waste water, and the content of solid of the high-concentration solution is not more than 40%; delivering the solution into a spray freezing tower and delivering the waste water into a water cooling box, wherein the water cooling box is provided with a primary heat pump and is used as a cold source of a secondary heat pump and a heat source of the primary heat pump; and carrying out drying, namely, carrying out spray freezing granulation on the feed liquid at below 40-below 60 DEG C, wherein the sprayed particles are frozen instantly at the low temperature to prepare the freeze-dried powder. The preparation method is simple and the yield is high.
Description
Technical field
The present invention relates to a kind of leaves of plants powder process freeze-dry process.
Background technology
Existing in biology preservation field, one of the most well-known the most successful method is freeze-drying method.Freeze drying makes product freezing to extract most moisture in product out under a high vacuum, then by vacuum chamber in this product of heated under vacuum to extract the method for remaining a small amount of moisture in the product.
At first implementing freeze-drying method period in World War II is method as preserving blood plasma and medicine.Finally, the method becomes the method for the biological products that generally acknowledged preservation fruit, vegetables and other market occur.Particularly nearest, freeze-drying method is used to chemically process the various technical fields manufacturing calculator superconductor.Prevailing freeze drying operation is those process fruit, vegetables, medicinal herbs and other there is the operation of the commercial use consumer goods.The main purpose adopting freeze-drying method is not economic aim, but it is proved to be to extract the most successful store method of moisture in product, wherein minimally damage the cell structure in product, better revert to the nature before closest to drying to make product.
Utilizable small-sized, medium-sized and large-scale commercial lyophilization system is there is in business management.Typically, to each company that freeze drying is served of other provider of unit, there is maximum commercial freezer systems.Some systems utilize multiple (20 or more) vacuum chamber, and the diameter of each vacuum chamber is equal to, or greater than 6 feet.These systems usually can be contracted to large-scale commerce scale and be carried out the system of work as the unit in batches of drying many batches of products simultaneously.
There are solid, liquid, gas 3 kinds of forms in material, under certain vacuum and temperature condition, material directly can be transformed from the solidified state into gaseous state, this process is sublimation process, utilize sublimating technologe to material and solution thereof carry out freezing after, and be aided with vacuum, the solid-state direct distillation of the solvent in material under freezing is made to be gas, carried secretly away by vacuum system, thus under the prerequisite keeping material stability, drying process is carried out to material.Adopt the material after freeze drying process, have better stability, the storage life extends, and when again dissolving, has good dissolubility.Freeze Drying Technique is extensive in biological products, pharmacy and food industry applications, and constantly extends to other field.
Geo-stationary process is mainly taked in existing freeze drying, namely there is not relative motion relative to for thermosphere in material, refrigeration of the prior art, quick freezing, freeze drying and other heat-exchange apparatus, because evaporator is stationary structure, cause in evaporator tube and between liquid refrigerant and tube wall, form flow boundary layer (laminar flow), evaporator tube is outer and form flow boundary layer between air, steam or other liquid coolant, these two flow boundary layers (laminar flow) make heat exchange efficiency low, thus cause overall freeze-drying time to extend.Such as: feed liquid is positioned in pallet, ampoule bottle, utilize the heat energy of bottom, the solvent in material is distilled.This process time is long, and energy consumption is high, and especially when carrying out the freeze drying of pallet, material bed variable thickness, evaporation rate difference is large, causes extend drying time, final freeze-dried powder caking, weak effect when again dissolving, dosing freeze-drying again again after need pulverizing.Meanwhile, pellet type freeze-dry process need process a large amount of pallets, comprises the spatula of pallet, transport, cleaning etc., has larger hall space needs, directly bring cost to increase.
The basic element of character of lyophilization system is vacuum chamber bracing frame for placing product, condenser, condenser refrigeration unit, heat transfer/cooling system for the vavuum pump from vacuum to vacuum chamber and integration that provide, in most of the cases product shelf uses temperature control heating and cooling.Lyophilization system is operated by the control panel of the program providing control temperature, vacuum pressure, time etc. usually.Different product types needs different control measure to produce best freeze drying effect.In some relatively simple situations, condenser is not housed, heat fused ice is made it after running at one section, described condenser is positioned at the described chamber of the water vapour existed with the form of ice for collection, but ice can be removed mechanically, as by cutting a hole or scraping, or by making ice melt to condenser spray water.
The generation of waste water is the one side of freeze-drying method, and generally claim waste water to be effluent in this manual, described waste water is that the moisture extracted from dried product obtains.The mode of described method work is that table plague was carried out before bearing vacuum is freezing.Under higher vacuum, by maintaining the non-equilibrium state between ice and described temperature/vacuum condition, the water being in freezing state does not evaporate through liquid stage (distillation).The water vapour produced from solid ice finally becomes ice crystal at colder condenser.Condenser can adopt several form, such as coil system, conical device, row's plate etc.The temperature using refrigeration unit to make condenser be cooled to lower than chamber temperature under vacuum, makes the steam extracted on condenser, be collected as the form of ice crystal.
After temperature rises, thawing in operation at taking-up cryodesiccated product, ice crystal melts and on the base plate dropping to vacuum chamber (internal condensation device) or condenser casing (if in outside) usually.Can make strike off in manual methods or chisel out ice, as mentioned above; Or use such as water or other material that ice is melted.The form of described moisture usually with waste water from device is output.
CN101126593 discloses a kind of supersonic freeze drying method and comprises the steps: that the solution dissolving material to be dried is put into supersonic freeze drying machine by 1., start the ultrasonic of supersonic freeze drying machine and refrigerating plant, under ultrasonication, material depth is cooled, make material be even solid granulates; 2. stop refrigeration, start vacuum plant, under vacuum and ultrasonication, heat energy supply is carried out to material, the solvent in material is distilled, is taken away by vacuum system, after finally eliminating solvent, obtain freeze-dried powder.Need before carrying out freeze-drying operation extract from raw material and refine desired substance, raw material can be extracted with appropriate solvent, fermentation, refining, extracting method is selected from but is not limited to following method: as immersion, backflow, microwave, the extractive technique such as ultrasonic, overcritical; Extraction solvent is selected from but is not limited to following solvent: can be ethanol, acetone and other organic solvent, also can be water, can also be water and the mixing or acid-base solution of organic solvent; Subtractive process is selected from but is not limited to following process for purification: the technology such as heavy in alcohol precipitation, depositing in water acid, alkali heavy, purifying resin, extraction, rectifying, micro-filtration.The material prepared until supersonic freeze drying normally filters after refining material to be dried is by suitable auxiliary material and dissolution with solvents, described auxiliary material comprises conventional freeze-dried powder auxiliary material, as cosolvent, thickener, supensoid agent, isotonic regulator, proppant etc.; Solvent can adopt water, glycerine, ethanol and a certain proportion of mixed solvent thereof; Filtration can adopt ultrafiltration, micro-filtration, nanofiltration etc.Ultrasonic freezing method utilizes hyperacoustic pulverizing, immixture, makes freeze-dried material form homogeneous particle and in heating up process, promote the transmission of heat.Generally, the frequency 2 ~ 20kHz of ultrasonication is advisable; The temperature of material cooling, at least lower than 20 DEG C, its freezing point, for preventing material generation bumping in the decompression process of subsequent step, being led and being subsided, thus affecting stripping and the outward appearance of final products, preferably controls at least lower than 40 DEG C, its freezing point; Above-mentioned vacuum preferably 0.01 ~ 5mbar.Described step 2 pair material heat supplying process adopts different programs according to the heterogeneity of material, heats up stage by stage, ensures to obtain freeze-dried powder that is even, good water solubility.
Supersonic freeze drying machine (supersonic lyophilizer) comprising: a closed container putting material, and this closed container has sealable dog-house and discharging opening; The vacuum plant be connected with closed container and solvent recovery unit; To the heating combined equipment of closed container heat supply; The refrigerating plant of cooling closed container; The heat-insulation layer of closed container and related seals and attaching parts; And one the material in closed container is fully disperseed, mixed uniformly Vltrasonic device, this Vltrasonic device comprises multiple ultrasonic device, ultrasonic device is divided into ultrasonic generator and ultrasonic vibrator two parts, at least one ultrasonic vibrator is placed in closed container, other ultrasonic vibrator is distributed in outside closed container, directly contacts with the outer wall of closed container.
Summary of the invention
The object of the invention is to propose a kind of leaves of plants powder process freeze-dry process.
For reaching this object, the present invention by the following technical solutions:
A kind of leaves of plants powder process freeze-dry process, it is characterized in that, with 6 years to 10 years growing plants leaves for raw material, reject withered and yellow leaf and field trash, with chitin rinsing, the draining of the deacetylation of D-2.3.5.6-tetrahydroxy-2-hexenoic acid-gamma lactone acid sodium+1.5% concentration of 3.5% concentration of preparation, again after vacuum drying at low temperature 10-20 DEG C temperature, at 2-6 degree temperature, stored refrigerated is for subsequent use; Open freezing concentrating device, feed liquid sends into freezing concentrating device, and in setting-up time, complete freeze concentration process, feed liquid is separated into highly concentrated solution and waste water, and the solid content of highly concentrated solution is the highest is no more than 40%; Solution sends into spray chilling tower, and waste water sends into water cooling box, and water cooling box is provided with one-level heat pump; The low-temperature receiver of water cooling box as secondary heat pump and the thermal source of one-level heat pump; Dry run is: the granulation of feed liquid spray chilling, and the temperature of spray chilling granulation controls at-40 ~-60 DEG C, and under low-temperature condition, the particle that spraying produces is frozen instantaneously, makes freeze-dried powder.
Embodiment
Embodiment 1
A kind of leaves of plants powder process freeze-dry process, it is characterized in that, with 6 years to 10 years growing plants leaves for raw material, reject withered and yellow leaf and field trash, with chitin rinsing, the draining of the deacetylation of D-2.3.5.6-tetrahydroxy-2-hexenoic acid-gamma lactone acid sodium+1% concentration of 5% concentration of preparation, again after vacuum drying at low temperature 35 DEG C of DEG C of temperature, at 1 DEG C of DEG C of temperature, stored refrigerated is for subsequent use; Open freezing concentrating device, feed liquid sends into freezing concentrating device, and in setting-up time, complete freeze concentration process, feed liquid is separated into highly concentrated solution and waste water, and the solid content of highly concentrated solution is the highest is no more than 40%; Solution sends into spray chilling tower, and waste water sends into water cooling box, and water cooling box is provided with one-level heat pump; The low-temperature receiver of water cooling box as secondary heat pump and the thermal source of one-level heat pump; Dry run is: the granulation of feed liquid spray chilling, and the temperature of spray chilling granulation controls at-40 DEG C, and under low-temperature condition, the particle that spraying produces is frozen instantaneously, makes freeze-dried powder.
Embodiment 2
A kind of leaves of plants powder process freeze-dry process, it is characterized in that, with 6 years to 10 years growing plants leaves for raw material, reject withered and yellow leaf and field trash, with chitin rinsing, the draining of the deacetylation of D-2.3.5.6-tetrahydroxy-2-hexenoic acid-gamma lactone acid sodium+1% concentration of 5% concentration of preparation, again after vacuum drying at low temperature 35 DEG C of DEG C of temperature, at-8 DEG C of temperature, stored refrigerated is for subsequent use; Open freezing concentrating device, feed liquid sends into freezing concentrating device, and in setting-up time, complete freeze concentration process, feed liquid is separated into highly concentrated solution and waste water, and the solid content of highly concentrated solution is the highest is no more than 40%; Solution sends into spray chilling tower, and waste water sends into water cooling box, and water cooling box is provided with one-level heat pump; The low-temperature receiver of water cooling box as secondary heat pump and the thermal source of one-level heat pump; Dry run is: the granulation of feed liquid spray chilling, and the temperature of spray chilling granulation controls at-60 DEG C, and under low-temperature condition, the particle that spraying produces is frozen instantaneously, makes freeze-dried powder.
Embodiment 3
A kind of leaves of plants powder process freeze-dry process, it is characterized in that, with 6 years to 10 years growing plants leaves for raw material, reject withered and yellow leaf and field trash, with chitin rinsing, the draining of the deacetylation of D-2.3.5.6-tetrahydroxy-2-hexenoic acid-gamma lactone acid sodium+1% concentration of 5% concentration of preparation, again after vacuum drying at low temperature-45 DEG C of temperature, at 8 DEG C of temperature, stored refrigerated is for subsequent use; Open freezing concentrating device, feed liquid sends into freezing concentrating device, and in setting-up time, complete freeze concentration process, feed liquid is separated into highly concentrated solution and waste water, and the solid content of highly concentrated solution is the highest is no more than 40%; Solution sends into spray chilling tower, and waste water sends into water cooling box, and water cooling box is provided with one-level heat pump; The low-temperature receiver of water cooling box as secondary heat pump and the thermal source of one-level heat pump; Dry run is: the granulation of feed liquid spray chilling, and the temperature of spray chilling granulation controls at-60 DEG C, and under low-temperature condition, the particle that spraying produces is frozen instantaneously, makes freeze-dried powder.
Embodiment 4
A kind of leaves of plants powder process freeze-dry process, it is characterized in that, with 6 years to 10 years growing plants leaves for raw material, reject withered and yellow leaf and field trash, with chitin rinsing, the draining of the deacetylation of D-2.3.5.6-tetrahydroxy-2-hexenoic acid-gamma lactone acid sodium+1.5% concentration of 3.5% concentration of preparation, again after vacuum drying at low temperature 10-20 DEG C temperature, at 2-6 degree temperature, stored refrigerated is for subsequent use; Open freezing concentrating device, feed liquid sends into freezing concentrating device, and in setting-up time, complete freeze concentration process, feed liquid is separated into highly concentrated solution and waste water, and the solid content of highly concentrated solution is the highest is no more than 40%; Solution sends into spray chilling tower, and waste water sends into water cooling box, and water cooling box is provided with one-level heat pump; The low-temperature receiver of water cooling box as secondary heat pump and the thermal source of one-level heat pump; Dry run is: the granulation of feed liquid spray chilling, and the temperature of spray chilling granulation controls at-40 ~-60 DEG C, and under low-temperature condition, the particle that spraying produces is frozen instantaneously, makes freeze-dried powder.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And these belong to spirit institute's apparent change of extending out of the present invention or change and are still among protection scope of the present invention.
Claims (1)
1. a leaves of plants powder process freeze-dry process, it is characterized in that, with 6 years to 10 years growing plants leaves for raw material, reject withered and yellow leaf and field trash, with chitin rinsing, the draining of the deacetylation of D-2.3.5.6-tetrahydroxy-2-hexenoic acid-gamma lactone acid sodium+1.5% concentration of 3.5% concentration of preparation, again after vacuum drying at low temperature 10-20 DEG C temperature, at 2-6 degree temperature, stored refrigerated is for subsequent use; Open freezing concentrating device, feed liquid sends into freezing concentrating device, and in setting-up time, complete freeze concentration process, feed liquid is separated into highly concentrated solution and waste water, and the solid content of highly concentrated solution is the highest is no more than 40%; Solution sends into spray chilling tower, and waste water sends into water cooling box, and water cooling box is provided with one-level heat pump; The low-temperature receiver of water cooling box as secondary heat pump and the thermal source of one-level heat pump; Dry run is: the granulation of feed liquid spray chilling, and the temperature of spray chilling granulation controls at-40 ~-60 DEG C, and under low-temperature condition, the particle that spraying produces is frozen instantaneously, makes freeze-dried powder.
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| CN201410618063.3A CN104351171A (en) | 2014-11-05 | 2014-11-05 | Plant leaf flour-milling freezing-drying process |
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| CN201410618063.3A CN104351171A (en) | 2014-11-05 | 2014-11-05 | Plant leaf flour-milling freezing-drying process |
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| CN113546032A (en) * | 2020-04-17 | 2021-10-26 | 常州伟博海泰生物科技有限公司 | Allergy-relieving moisture-preserving freeze-dried preparation, instant freeze-dried product, and preparation method and application thereof |
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