CN108332512A - A kind of freeze-drying method of liquid material - Google Patents
A kind of freeze-drying method of liquid material Download PDFInfo
- Publication number
- CN108332512A CN108332512A CN201810183170.6A CN201810183170A CN108332512A CN 108332512 A CN108332512 A CN 108332512A CN 201810183170 A CN201810183170 A CN 201810183170A CN 108332512 A CN108332512 A CN 108332512A
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- China
- Prior art keywords
- liquid
- precooling
- freeze
- method described
- siccative
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B1/00—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Freezing, Cooling And Drying Of Foods (AREA)
- Drying Of Solid Materials (AREA)
Abstract
The present invention provides a kind of freeze-drying methods of liquid material, characterized in that includes the following steps：（1）Compound additive with emulsification and stabilization is dispersed in liquid material, is prepared into and waits for siccative liquid；（2）Under stiring, it will wait for that siccative liquid carries out precooling at a temperature of 5 DEG C~0 DEG C, be allowed to become to have the precooling material of initial hole；（3）Precooling material is freezed at a temperature of 20 DEG C~50 DEG C, solidification process is completed, obtains the frozen materials with initial hole；（4）Frozen materials are freeze-dried, final products are obtained.The present invention has the characteristics that simple for process, rate is fast and low energy consumption, is suitable for the freeze-drying of food, drug and biological products etc..
Description
Technical field
The invention belongs to the freeze-drying processing technique fields of food, drug and biological products etc., in particular to one
The freeze-drying method of kind liquid material.
Background technology
In all dry technologies, the product quality of freeze-drying is best.Freeze-drying is in food, drug and biological products
There is irreplaceable role in the dehydration of equal heat sensitive materials, but the problem of its process high energy consumption is not found yet so far
Effective solution method.Freeze-drying is mainly by four kinds of material freezing, maintenance system vacuum, lyophilization and steam condensation operations
Composition, the energy consumption of wherein lyophilization account for about the half of whole process total energy consumption.The lyophilization time is long, low rate is that freezing is dry
Where the bottleneck of dry process high energy consumption.The time for shortening lyophilization process, it then also can correspondingly shorten maintenance system vacuum
With distillation vapor condensation process time, thus be the key that improve rates for freeze-drying, reduce total energy consumption.
Invention content
It is an object of the present invention to provide a kind of freeze-drying methods of liquid material simple for process, rate is fast and low energy consumption.
The freeze-drying method of the liquid material of the present invention includes the following steps：It will be with emulsification and stabilization
Compound additive is dispersed in liquid material, is prepared into and is waited for siccative liquid；Under stiring, siccative liquid will be waited for -5 DEG C~0
Precooling is carried out at a temperature of DEG C, is allowed to become to have the precooling material of initial hole；By precooling material -20 DEG C~-
It is freezed at a temperature of 50 DEG C, completes solidification process, obtain the frozen materials with initial hole；Frozen materials are carried out cold
It is lyophilized dry, obtains final products.
The compound additive can be selected from skimmed milk power, gelatin, carragheen, Arabic gum, guar gum, locust bean
In glue, sodium carboxymethylcellulose, mono-stearin, sodium alginate, xanthans, sucrose ester, soybean lecithin, glyceryl laurate ester
1 kind or 2 kinds or more, such as it is 0.05~0.15 that can select the mass ratio of sodium carboxymethylcellulose and skimmed milk power：
1 mixture.Mass fraction of the compound additive in waiting for siccative liquid is generally 1%~3%.
In addition, when the ice fishing amount of freezing dry process is in 3kg/24h or less, the precooling preferably holds in heat preservation
It in device, is carried out while stirring to waiting for liquid nitrogen is added in siccative liquid, liquid nitrogen and waits for the volume ratio of siccative liquid at this time
Generally
It is 1~2：1.And when the ice fishing amount of freezing dry process is more than 3kg/24h, the precooling is preferably being incited somebody to action
Temperature controls in -5 DEG C~0 DEG C of precooling device, is mixed into air while stirring and carries out.The frozen materials
Initial porosity be generally 30%~90%.
The invention is particularly suited to the dehydrations of the liquid material containing food, drug or biological products.The biography of freeze-drying
It passs resistance and mostlys come from the solid skeletal that steam leaves after ice crystal distillation during lyophilization and be formed by porous dry
The migration in area.And the pore structure of solid skeletal depends on the freezing stage of material.Conventional liquid material freezing dry process
It is that will wait for siccative liquid directly freezed, obtains the saturation frozen materials of no initial hole, be unfavorable for the migration of steam.
Relative to conventional freeze-drying method, the present invention has simple for process, fast (the drying time shortening 10% of rate
~40%) the features such as and low energy consumption.
Description of the drawings
Fig. 1 is the process flow diagram of the embodiment of the present invention 1.
Specific implementation mode
The freeze-drying method of the liquid material of the present invention includes the following steps：It will be with emulsification and stabilization
Compound additive is dispersed in liquid material, is prepared into and is waited for siccative liquid；Under stiring, siccative liquid will be waited for -5 DEG C~0
Precooling is carried out at a temperature of DEG C, is allowed to become to have the precooling material of initial hole；By precooling material -20 DEG C~
It is freezed at a temperature of -50 DEG C, completes solidification process, obtain the frozen materials with initial hole；Frozen materials are carried out
Freeze-drying, obtains final products.
Compared with conventional liquid material Freeze Drying Technique, present invention additionally encompasses freezing steps before curing (1)
(2).Specifically, conventional liquid material freezing dry process is to cure liquid material directly freezed, almost do not had
There are " saturation " frozen materials of initial hole, this is unfavorable for the migration of steam in later sublimation drying process.And the present invention passes through
Liquid material precooling is imaged " unsaturation " with initial hole as " ice cream " with (2) by step (1) first
Then frozen materials carry out final freezing solidification process again.Initial pore structure constructed by precooling process will be follow-up
Migration of the steam inside material is greatly promoted during lyophilization to carry to improve the rates for freeze-drying of liquid material
High-energy utilization rate.Moreover, present invention process is simple, operation is easy, there is very high practical value and vast market prospect.
In step (1), the compound additive with emulsification and stabilization used is not particularly limited, it can
It is suitably selected according to the type of liquid material and using purpose etc..Can be from defatted milk as the compound additive
Powder, gelatin, carragheen, Arabic gum, guar gum, locust bean gum, sodium carboxymethylcellulose, mono-stearin, sodium alginate xanthan
1 kind selected in glue, sucrose ester, soybean lecithin and glyceryl laurate ester etc. or 2 kinds or more, carboxymethyl can be used for example
The mass ratio of sodium cellulosate and skimmed milk power is 0.05~0.15：1 mixture is as compound additive.Compound addition
The effect of agent is to construct stable solid matrix material in subsequent precooling step (2) and freezing step (3),
The good shape-retaining ability of frozen materials is assigned, to ensure being smoothed out for freezing dry process.The dosage of additive is not to influence
Liquid material nature is advisable, and the mass fraction in waiting for siccative liquid is generally 1%~3%.
The mass fraction of material can suitably be adjusted according to parameters such as the viscosity of liquid material in liquid material, generally
10%~40% (mass fraction herein refers to the mass fraction in liquid shared by the material of dispersion and dissolving).
Step (2) is to make gas with atomic small by stirring gradual entrained gas while precooling waits for siccative liquid
Bubble regime be uniformly distributed in precooling material process (i.e. formed with initial hole precooling material).In advance
Cryogenic temperature is generally -5 DEG C~0 DEG C, and mixing speed is generally 100r/min~500r/min, and mixing time is generally
5min~
15min, mixed gas can be air, oxygen, nitrogen, helium etc., preferably cheap air.
The method of precooling is not particularly limited, for example, can in cool-bag, with while stirring to waiting doing
The mode that liquid nitrogen is added in feed liquid carries out, and wherein liquid nitrogen and waits for that the volume ratio of siccative liquid is generally 1~2：1.Liquid nitrogen can fill
It treats siccative liquid with dividing and carries out precooling, generate gaseous nitrogen additionally, due to liquid nitrogen gasification, there is no need in addition import gas.This side
Method is easy, operation is easy, but cost is higher, applies in general to the smaller situation of production scale (such as freezing dry process
Ice fishing amount is in 3kg/24h hereinafter, but not limited to this).When production scale is larger (such as freezing dry process
Ice fishing amount is more than 3kg/24h, and but not limited to this), then generally preferably in the precooling by temperature control at -5 DEG C~0 DEG C
Freeze in device (such as being used to prepare the precooling device of ice cream), in a manner of being mixed into air while stirring into
Row.This method is suitable for large-scale industrial production due to the use of cheap air.
Step (3) is to carry out freezing cured process to material, and cooling time is generally 3h~6h.The step will
Precooling
The initial hole frozen in material remains behind, to obtain the frozen materials with initial hole.And conventional freezing
The frozen materials that drying process obtains do not have initial hole then.
The initial porosity of the frozen materials obtained by above-mentioned steps (1)~(3) is generally 30%~90%, this
Sample can obtain preferably freeze-drying effect.Initial porosity can be fitted by controlling mixed gas flow, mixing speed etc.
Work as adjustment.The computational methods of initial porosity are as follows：By the volume for the frozen materials that step of the present invention (1)~(3) obtain
(V1) and under identical cryogenic temperature same amount of liquid material is directly carried out to the volume (V0) of the material of freezing acquisition
Difference divided by by step of the present invention (1)~(3) obtain frozen materials volume (V1), i.e.,：Initial porosity (%)
=100% × (V1-V0)/V1.
Step (4) is that the frozen materials with initial hole that will be had been cured are freeze-dried to obtain final products
Process, can carry out according to a conventional method, the absolute pressure of the process is generally 10Pa~50Pa.
The invention is particularly suited to heat sensitive material or the dehydrations for having bioactivity to require material, such as contain food (example
Such as instant coffee, sea cucumber preparation), drug (such as Chinese herbal medicine extract, American ginseng extract) or biological products (example
Such as enzyme, cell, pharmaceutical protein) liquid material dehydration.
Embodiment
With reference to embodiment, the present invention will be described in detail, but the following examples are only the preferable embodiment of the present invention,
Embodiment 1
As shown in Fig. 1, with sodium carboxymethylcellulose and skimmed milk power mass ratio for 0.1：1 solid mixture is as multiple
Additive is closed, additive is dispersed at 30 DEG C in the coffee liquid that coffee mass fraction is 12%, is prepared into and waits doing
Feed liquid, mass fraction of the additive in waiting for siccative liquid are 1.5%；It will wait for that siccative liquid is transferred in cool-bag, press and feed liquid
Volume ratio 1.5：1 is added liquid nitrogen, while stirring 10min with the rotating speed of 400r/min, obtains having the pre- of initial hole
Frozen materials；Precooling material is freezed into 4h at -35 DEG C, completes solidification process, it is 66.7% to obtain initial porosity
Frozen materials (the saturation frozen materials i.e. relative to not initial hole, the freezing with initial hole prepared under the conditions of this
The volume of material increases 2 times)；By the frozen materials with initial hole in absolute pressure 23Pa~24Pa, radiation
It is freeze-dried 3.5h at 30 DEG C of temperature, obtains the dry products powder 0.307g that moisture content is 1%.
Comparative example 1
By be 12% with 1 same amount of solid masses number of embodiment coffee liquid that 4h is freezed directly at -35 DEG C is complete
After solidification process, it is freeze-dried 5h at absolute pressure 23Pa~24Pa, 30 DEG C of radiation temperature, obtaining moisture content is
4% dry products powder 0.316g.
From the above results, the present invention is compared with conventional freeze-drying method, and drying time reduces 30%, and
And
The moisture content for the dry products that the present invention obtains is less than conventional freeze-drying method.
Claims (8)
1. a kind of freeze-drying method of liquid material, characterized in that include the following steps：
(1) compound additive with emulsification and stabilization is dispersed in liquid material, is prepared into and waits for siccative
Liquid；
(2) under stiring, it will wait for that siccative liquid carries out precooling at a temperature of -5 DEG C~0 DEG C, be allowed to become with initial apertures
The precooling material of gap；The initial porosity of the precooling material is 30%~90%；
(3) precooling material is freezed at a temperature of -20 DEG C~-50 DEG C, completes solidification process, obtain having just
The frozen materials of beginning hole；
(4) frozen materials are freeze-dried, obtain final products.
2. according to the method described in claim 1, characterized in that the compound additive is selected from skimmed milk power, gelatin, OK a karaoke club
It is glue, Arabic gum, guar gum, locust bean gum, sodium carboxymethylcellulose, mono-stearin, sodium alginate, xanthans, sucrose ester, big
1 kind or 2 kinds or more in Fabaceous Lecithin, glyceryl laurate ester.
3. according to the method described in claim 2, characterized in that the compound additive is sodium carboxymethylcellulose and degreasing
The mass ratio of milk powder is 0.05~0.15：1 mixture.
4. according to the method described in claim 1, characterized in that mass fraction of the compound additive in waiting for siccative liquid
It is 1%~3%.
5. according to the method described in claim 1, characterized in that when freezing dry process ice fishing amount 3kg/24h with
When lower, the precooling be in cool-bag, while stirring to wait in siccative liquid be added liquid nitrogen and carry out.
6. according to the method described in claim 5, characterized in that liquid nitrogen is 1~2 with the volume ratio for waiting for siccative liquid：1.
7. according to the method described in claim 1, characterized in that when the ice fishing amount of freezing dry process is more than 3kg/24h
When, the precooling be temperature control in -5 DEG C~0 DEG C of precooling device, is mixed into air while stirring and
It carries out.
8. according to the method described in any one of claim 1-7, characterized in that the liquid material be containing food or
The liquid material of drug.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810183170.6A CN108332512A (en) | 2018-03-06 | 2018-03-06 | A kind of freeze-drying method of liquid material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810183170.6A CN108332512A (en) | 2018-03-06 | 2018-03-06 | A kind of freeze-drying method of liquid material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108332512A true CN108332512A (en) | 2018-07-27 |
Family
ID=62930439
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810183170.6A Withdrawn CN108332512A (en) | 2018-03-06 | 2018-03-06 | A kind of freeze-drying method of liquid material |
Country Status (1)
| Country | Link |
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| CN (1) | CN108332512A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111351318A (en) * | 2020-03-07 | 2020-06-30 | 苏州德沃生物技术有限公司 | Freeze-drying method of antibody coupling latex |
| CN112146363A (en) * | 2020-09-10 | 2020-12-29 | 天津华龛生物科技有限公司 | Pre-freezing drying system and method for microcarrier |
-
2018
- 2018-03-06 CN CN201810183170.6A patent/CN108332512A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111351318A (en) * | 2020-03-07 | 2020-06-30 | 苏州德沃生物技术有限公司 | Freeze-drying method of antibody coupling latex |
| CN112146363A (en) * | 2020-09-10 | 2020-12-29 | 天津华龛生物科技有限公司 | Pre-freezing drying system and method for microcarrier |
| CN112146363B (en) * | 2020-09-10 | 2021-09-21 | 天津华龛生物科技有限公司 | Pre-freezing drying system and method for microcarrier |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180727 |
|
| WW01 | Invention patent application withdrawn after publication |