CN103900353A - Method for freezing and vacuum-drying micro-nanopowder slurry - Google Patents
Method for freezing and vacuum-drying micro-nanopowder slurry Download PDFInfo
- Publication number
- CN103900353A CN103900353A CN201210578693.3A CN201210578693A CN103900353A CN 103900353 A CN103900353 A CN 103900353A CN 201210578693 A CN201210578693 A CN 201210578693A CN 103900353 A CN103900353 A CN 103900353A
- Authority
- CN
- China
- Prior art keywords
- micro
- nano powder
- powder slurry
- cavity
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention relates to a method for freezing and vacuum-drying micro-nanopowder slurry. The method for freezing and vacuum-drying the micro-nanopowder slurry comprises the steps of primary cooling, wherein the slurry is placed in a cavity and is cooled; secondary cooling, wherein the cavity is vacuumized to enable the slurry to be cooled again; low temperature and constant temperature maintaining, wherein the slurry is maintained at a low temperature; primary warming, wherein the slurry is warmed stage by stage; secondary warming, wherein the slurry is warmed stage by stage again; high temperature and constant temperature maintaining, wherein the slurry is maintained at a high temperature; material taking, wherein micro-nanopowder is taken out of the cavity. According to the method for freezing and vacuum-drying the micro-nanopowder slurry, the phenomenon of agglomeration of dried micro-nanopowder can be avoided, and compared with a learning method, the particle size distribution range of the dried powder is narrowed.
Description
Technical field
The present invention relates to a kind of drying means, refer to especially a kind of by the method for micro-nano powder slurry vacuum freezedrying.
Background technology
Bamboo charcoal or activated carbon are because having splendid absorption, decolouring, the effects such as deodorization, be widely used in air cleaning, sewage disposal, the fields such as weaving, particularly in field of textiles, for bamboo charcoal or activated carbon can evenly be mixed in the plastic master batch of manufacturing fibres for fabrics, need first bamboo charcoal or activated carbon to be made the powder of micron or nano-scale, be mixed to form master batch with plastic raw materials again, take bamboo charcoal as example, conventional practice is the powder that bamboo charcoal is ground to form to the about 10nm to 1000nm of particle diameter (micro-nano) with wet type physics ball-milling method, because the product that adopts wet ball-milling method is the slurry that comprises powder and liquid, therefore need further make it dry.
Commonly use the method for micro-nano powder slurry drying, mainly first micro-nano powder de-watering of slurries to be become to pasty slurry, heating, drying becomes block micro-nano siccative afterwards, recycles special high speed disintegrator, with per minute 25,000 speed that turn, micro-nano siccative is ground into powder.But, utilize this drying means that agglomeration easily occurs, cause dried particle size were to distribute wide, the little nanometer of counting, greatly the even hundreds of microns of tens of microns, make it be unfavorable for the application of subsequent product.
Summary of the invention
For the problems referred to above, main purpose of the present invention is to provide a kind of method of vacuum freeze drying of micro-nano powder slurry, it can effectively avoid dried micro-nano powder to occur agglomeration, and dwindles the particle size distribution range of dry rear powder with respect to prior art method.
For achieving the above object, the method for vacuum freeze drying of a kind of micro-nano powder slurry provided by the present invention, includes the following step:
The first cooling step: have the disk body of the micro-nano powder slurry of a solid content 20wt% to 30wt% to insert in the cavity of a sealing bearing, and this micro-nano powder slurry is cooled to-11 ℃ to-13 ℃, it is dispersant and the wetting agent of 1: 1 that this micro-nano powder pulp bales contains weight ratio, this cavity internal gas pressure is 1atm, and in this micro-nano powder slurry, the average grain diameter of powder is 10nm to 1000nm;
The second cooling step: this cavity is evacuated to this inside cavity air pressure and reaches 120Pa to 140Pa, make this micro-nano powder slurry be cooled to-30 ℃ to-31 ℃;
Cryogenic thermostat step: the temperature of this micro-nano powder slurry is remained on to-30 ℃ to-31 ℃ and maintain 6 to 10 hours;
The first heating step: make the air pressure of this inside cavity be maintained at 120Pa to 140Pa, and be warming up to 40 ℃ to 45 ℃ by stage this micro-nano powder slurry;
The second heating step: make the air pressure of this inside cavity be reduced to 60Pa to 110Pa, and be warming up to 55 ℃ to 60 ℃ by stage this micro-nano powder slurry;
High temperature constant temperature step: make the air pressure of this inside cavity further be reduced to 15Pa, and the temperature of this micro-nano powder slurry is remained on to 52 ℃ to 55 ℃ and maintain 6 to 10 hours;
Material step: the air pressure of this inside cavity is increased to after 1atm, opens cavity and take out dry micro-nano powder.
In the technical scheme of the invention described above, in this first cooling step, the thickness of this micro-nano powder slurry on this disk body is less than or equal to 4cm.
In this first cooling step, this dispersant is polycarboxylate compounds, organic sulfonic acid salt compounds or ethoxylation polymer class compound, and this wetting agent is organic sulfonic acid salt compounds.
In this first cooling step, the total content of this dispersant and wetting agent accounts for the 10wt% to 30wt% of slurry weight.
In this second cooling step, for utilizing an aspiration pump to bleed to this cavity, in the time that this cavity internal gas pressure drops to 120Pa to 140Pa gradually, nitrogen is poured in this cavity and no longer declined so that the air pressure in this cavity is maintained at 120Pa to 140Pa.
This cryogenic thermostat step is for maintaining 8 hours.
In this first heating step, for utilizing an aspiration pump to bleed to this cavity, nitrogen is poured in this cavity simultaneously, make the air pressure in this cavity be maintained at 120Pa to 140Pa.
In this first heating step, first open the required power supply that heats up this micro-nano powder slurry is warming up to 35 ℃, close again the required power supply that heats up, in the time that this micro-nano powder slurry is cooled to 30 ℃, open again the required power supply that heats up this micro-nano powder slurry is warming up to 45 ℃, close the required power supply that heats up, this micro-nano powder slurry can be cooled to 40 ℃ more afterwards again.
In this second heating step, stop nitrogen being poured in this cavity but not stopping aspiration pump, make the air pressure in this cavity be reduced to gradually 60Pa to 110Pa.
In this second heating step, for opening the required power supply that heats up, this micro-nano powder slurry is warming up to 52 ℃, close again the required power supply that heats up, in the time that this micro-nano powder slurry is cooled to 47 ℃, open again the required power supply that heats up this micro-nano powder slurry is warming up to 60 ℃, close the required power supply that heats up, this micro-nano powder slurry can be cooled to 55 ℃ more afterwards again.
This high temperature constant temperature step is for maintaining 8 hours.
In this material step, for stopping this aspiration pump and nitrogen being poured in this cavity so that this cavity internal gas pressure is increased to 1atm.
This micro-nano powder is bamboo carbon powder, activated carbon powder, coffee carbon powder or coconut palm carbon powder.
Adopt technique scheme, due to method of vacuum freeze drying of the present invention be first by freezing micro-nano powder slurry become solid-state after, and heat up in environment under low pressure, impel liquid in solid-state micro-nano powder slurry as the directly distillation and being removed of water and other solvents, compared to the drying means of commonly using, method of vacuum freeze drying of the present invention can avoid dried micro-nano powder to occur agglomeration effectively, and dwindles the particle size distribution range of dry rear powder.
Accompanying drawing explanation
Fig. 1 utilizes radium-shine particle size analyzer to detect the particle diameter distribution map of the powder in micro-nano powder slurry;
Fig. 2 utilizes radium-shine particle size analyzer to detect the particle diameter distribution map via the dried micro-nano powder of method of the present invention.
The specific embodiment
Now lift following examples and by reference to the accompanying drawings structure of the present invention and effect be elaborated.But, should be understood that, the present invention is not limited to content what follows, does not allly violate various modifications and the variation under spirit of the present invention or category, done, all belongs to scope of the present invention.
The method of vacuum freeze drying of micro-nano powder slurry provided by the present invention, mainly includes the following step, and wherein this micro-nano powder can be but be not limited to bamboo carbon powder, activated carbon powder, coffee carbon powder or coconut palm carbon powder:
The first cooling step: it is that the disk body of the micro-nano powder slurry of 20wt% to 30wt% is inserted in the cavity of a sealing that a bearing is had to a solid content, and this micro-nano powder slurry is cooled to-11 ℃ to-13 ℃, it is dispersant and the wetting agent of 1: 1 that this micro-nano powder pulp bales contains weight ratio, and this cavity internal pressure is 1atm, the average grain diameter of the powder in this micro-nano powder slurry is 10nm to 1000nm;
The second cooling step: this cavity is evacuated to this inside cavity air pressure and reaches 120Pa to 140Pa, make this micro-nano powder slurry be cooled to-30 ℃ to-31 ℃;
Cryogenic thermostat step: the temperature of this micro-nano powder slurry is remained on to-30 ℃ under the temperature conditions of-31 ℃ 6 to 10 hours;
The first heating step: make the air pressure of this inside cavity be maintained at 120Pa to 140Pa, and be warming up to 40 ℃ to 45 ℃ by stage this micro-nano powder slurry;
The second heating step: make the air pressure of this inside cavity be reduced to 60Pa to 110Pa, and be warming up to 55 ℃ to 60 ℃ by stage this micro-nano powder slurry;
High temperature constant temperature step: make the pressure of this inside cavity further be reduced to 15Pa, and the temperature of this micro-nano powder slurry is remained under the temperature conditions of 52 ℃ to 55 ℃ to 6 to 10 hours;
Material step: the pressure of this inside cavity is increased to after 1atm, opens cavity and take out dry micro-nano powder.
Wherein, this micro-nano powder is bamboo carbon powder or activated carbon powder.
In this first cooling step, the thickness of this micro-nano powder slurry on this disk body should be less than or equal to 4cm, so, in the time that this micro-nano powder slurry carries out follow-up low pressure heating step, solid water or other solvents in this micro-nano powder slurry can comparatively fast distil.Secondly, in the present invention, this dispersant can use (but being not limited to) polycarboxylate class (polycarboxylate), organic sulfonic acid salt (organic sulfonic acid) or ethoxylation polymer class (ethoxylated polymer) compound, and this wetting agent can use (but being not limited to) organic sulfonic acid salt (organicsulfonic acid) compound.Moreover the total content of this dispersant and wetting agent accounts for the 10wt% to 30wt% of slurry weight, so that the powder in this micro-nano powder slurry can disperse.
In this second cooling step, to utilize an aspiration pump to bleed to this cavity, in the time that this cavity internal gas pressure drops to 120Pa to 140Pa gradually, appropriate nitrogen is poured in this cavity and no longer declined so that the air pressure in cavity is maintained at 120Pa to 140Pa, but also can pour into air or other inert gases as argon gas, if even adopt the bleed pump of power of capable of regulating, without maintaining air pressure in 120Pa to 140Pa in the mode that pours into gas.
In this cryogenic thermostat step, the air pressure in this cavity should be maintained at lower 8 hours of the condition of 120Pa to 140Pa, so that the temperature of the micro-nano powder slurry in this disk body is maintained at-30 ℃ to-31 ℃ equably.
In this first heating step, utilize this pumping of bleeding to continue this cavity to bleed, appropriate nitrogen is poured in this cavity simultaneously, make the air pressure in this cavity be maintained at 120Pa to 140Pa, as previously mentioned, nitrogen can other gas instead, or adopt the bleed pump of power of capable of regulating.Secondly, by the stage intensification of this micro-nano powder slurry, for first opening the required power supply that heats up, this micro-nano powder slurry is warming up to 35 ℃, close afterwards the required power supply that heats up, in the time that this micro-nano powder slurry is cooled to 30 ℃, open again the required power supply that heats up, this micro-nano powder slurry is warming up to 45 ℃, the last required power supply that heats up of closing again, the solid water in this micro-nano powder slurry or other solvents make this micro-nano powder slurry be cooled to 40 ℃, so that can distil in environment under low pressure.But the height of temperature can be adjusted according to need in every one-phase, not necessarily need to meet completely said temperature value.
In this second heating step, for stopping nitrogen being poured in this cavity but do not stop aspiration pump, make the air pressure in this cavity be down to gradually 60Pa to 110Pa.Secondly, by the stage intensification of this micro-nano powder slurry, for opening the required power supply that heats up, this micro-nano powder slurry that is cooled to 40 ℃ in the first heating step is warming up to 52 ℃, close afterwards the required power supply that heats up, in the time that this micro-nano powder slurry is cooled to 47 ℃, open again the required power supply that heats up, this micro-nano powder slurry is warming up to 60 ℃, the last required power supply that heats up of closing again, make this micro-nano powder slurry be cooled to 55 ℃, so that the solid water in this micro-nano powder slurry or other solvents can further distillations in environment under low pressure.Similarly, in every one-phase, the height of temperature can be adjusted according to need, not necessarily needs to meet completely said temperature value.
In this high temperature constant temperature step, should be by this micro-nano powder slurry constant temperature in the condition of 52 ℃ to 55 ℃ lower 8 hours, so that the solid water or other solvents that residue in this micro-nano powder slurry can distil completely in environment under low pressure, make this micro-nano powder slurry become siccative.
In this material step, for stopping this aspiration pump, simultaneously by nitrogen or air or other inert gases as argon gas etc. pours in this cavity, make this cavity internal gas pressure be increased to 1atm, consistent with ambient pressure.Secondly,, in order to make the unlikely variation of air pressure in this cavity too fierce, the process of aforementioned filling nitrogen should continue 15 minutes.
Carry out more at large to illustrate milling method of the present invention by an embodiment below.But the following example is just used for illustrating the present invention, is not used for limiting the scope of the invention.
The preparation of micro-nano powder slurry
First, in ancestor's bamboo charcoal, adding weight ratio in the Meng to be ground is that (Qi Jia chemical company is for selling for the dispersant of 1: 1, model 2146, composition is polycarboxylate compounds) and wetting agent (Qi Jia chemical company is for selling, model 2150, composition is organic sulfonic acid salt compounds), utilize wet ball-milling method (Wet-Ball-Milling Method) by the Meng ancestor's bamboo charcoal be ground to after required particle diameter, by bamboo carbon powder together with water, dispersant, the slurry that wetting agent and other solvents are mixed to form is inserted suspention in non-woven bag and is drained, till being about 25wt% to solid content in this slurry, now this dispersant and this wetting agent account for the approximately 16wt% of this slurry altogether, in this slurry, the particle diameter of powder is by radium-shine particle size analyzer (Particle size distribution analyzer, Horiba company is for selling, model LA-920) detect, result as shown in Figure 1, minimum grain size is 51nm, maximum particle diameter is 226nm, belong to the slurry of micro-nano powder.
Dry run
First, pour above-mentioned micro-nano powder slurry into a disk body, and this micro-nano powder slurry is evenly struck off, make its thickness be about 3 centimeters, afterwards this disk body is inserted in the cavity of a sealing, and this micro-nano powder slurry was cooled to-11 ℃ to-13 ℃ in 2 hours, now this cavity internal gas pressure is 1atm (i.e. 1.013 × 105Pa).
Afterwards, utilize an aspiration pump to bleed 30 minutes to this cavity, make this inside cavity air pressure drop to gradually 130Pa, in this process, this micro-nano powder slurry can be cooled to-30 ℃ to-31 ℃.Afterwards, start appropriate nitrogen to pour in this cavity, make the vacuum in this cavity be maintained at 130Pa, avoid the temperature of this micro-nano powder slurry to continue to reduce, this process approximately continues 8 hours.Thereafter, continuing to bleed and pouring into appropriate nitrogen makes this inside cavity air pressure be maintained at 130Pa, open the required power supply that heats up simultaneously, this micro-nano powder slurry is warming up to 35 ℃ (this process approximately needs 45 minutes), close afterwards this power supply, after 10 minutes, this micro-nano powder slurry is cooled to 30 ℃, opens afterwards this power supply heating 30 minutes again, and this micro-nano powder slurry is warming up to 45 ℃, powered-down is waited for 10 minutes again, while making it be cooled to 40 ℃.Then, stop pouring into nitrogen but continue to open this aspiration pump, so that the air pressure in this cavity is reduced to 60Pa gradually, in this process, then open heat up required power supply this micro-nano powder slurry was warming up to 52 ℃ in approximately 32 minutes, close afterwards this power supply, wait for and within 12 minutes, make this micro-nano powder slurry be cooled to 47 ℃, again open this power supply and this micro-nano powder slurry was warming up to 60 ℃ in approximately 20 minutes, finally close again this power supply, wait for and within 15 minutes, make this micro-nano powder slurry be cooled to 55 ℃ thereafter.
Because aspiration pump continues running and nitrogen do not poured in cavity, air pressure in this cavity will further be reduced to 15Pa, and the temperature of this micro-nano powder slurry is maintained to lower 8 hours of the temperature conditions of 52 ℃ to 55 ℃, so that the residual solid water in this micro-nano powder slurry or other solvents distil completely.
Finally, stop this aspiration pump and again nitrogen slowly poured in this cavity, making the air pressure in this cavity be increased to gradually 1atm, dry micro-nano powder can be taken out.
Particle diameter detects
Dried micro-nano powder is detected with above-mentioned radium-shine particle size analyzer, result as shown in Figure 2, minimum grain size be respectively 51nm and 226nm same with maximum particle diameter, and particle diameter distributes almost identical with Fig. 1, show the phenomenon that method of vacuum freeze drying of the present invention can effectively avoid dried micro-nano powder appearance to reunite, dry forward and backward ancestor's bamboo carbon powder particle diameter in the Meng is consistent, this dried micro-nano powder can evenly mix in plastic raw materials, makes plastic raw materials master batch and carries out following process.
In sum, due to method of vacuum freeze drying of the present invention be first by freezing micro-nano powder slurry become solid-state after, again by heating step impel solid water in the micro-nano powder slurry after freezing or other solvents directly distillation remove, therefore compared to the drying means of commonly using, the present invention can avoid dried micro-nano powder to occur agglomeration effectively, and dwindles the particle size distribution range of dry rear powder with respect to prior art method.
Claims (13)
1. a method of vacuum freeze drying for micro-nano powder slurry, includes the following step:
The first cooling step: have the disk body of the micro-nano powder slurry of a solid content 20wt% to 30wt% to insert in the cavity of a sealing bearing, and this micro-nano powder slurry is cooled to-11 ℃ to-13 ℃, it is dispersant and the wetting agent of 1: 1 that this micro-nano powder pulp bales contains weight ratio, this cavity internal gas pressure is 1atm, and in this micro-nano powder slurry, the average grain diameter of powder is 10nm to 1000nm;
The second cooling step: this cavity is evacuated to this inside cavity air pressure and reaches 120Pa to 140Pa, make this micro-nano powder slurry be cooled to-30 ℃ to-31 ℃;
Cryogenic thermostat step: the temperature of this micro-nano powder slurry is remained on to-30 ℃ to-31 ℃ and maintain 6 to 10 hours;
The first heating step: make the air pressure of this inside cavity be maintained at 120Pa to 140Pa, and be warming up to 40 ℃ to 45 ℃ by stage this micro-nano powder slurry;
The second heating step: make the air pressure of this inside cavity be reduced to 60Pa to 110Pa, and be warming up to 55 ℃ to 60 ℃ by stage this micro-nano powder slurry;
High temperature constant temperature step: make the air pressure of this inside cavity further be reduced to 15Pa, and the temperature of this micro-nano powder slurry is remained on to 52 ℃ to 55 ℃ and maintain 6 to 10 hours;
Material step: the air pressure of this inside cavity is increased to after 1atm, opens cavity and take out dry micro-nano powder.
2. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, is characterized in that: in this first cooling step, the thickness of this micro-nano powder slurry on this disk body is less than or equal to 4cm.
3. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, it is characterized in that: in this first cooling step, this dispersant is polycarboxylate compounds, organic sulfonic acid salt compounds or ethoxylation polymer class compound, and this wetting agent is organic sulfonic acid salt compounds.
4. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, is characterized in that: in this first cooling step, the total content of this dispersant and wetting agent accounts for the 10wt% to 30wt% of slurry weight.
5. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, it is characterized in that: in this second cooling step, for utilizing an aspiration pump, this cavity is bled, in the time that this cavity internal gas pressure drops to 120Pa to 140Pa gradually, nitrogen is poured in this cavity and no longer declined so that the air pressure in this cavity is maintained at 120Pa to 140Pa.
6. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, is characterized in that: this cryogenic thermostat step is for maintaining 8 hours.
7. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, it is characterized in that: in this first heating step, for utilizing an aspiration pump to bleed to this cavity, nitrogen is poured in this cavity simultaneously, make the air pressure in this cavity be maintained at 120Pa to 140Pa.
8. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, it is characterized in that: in this first heating step, first open the required power supply that heats up this micro-nano powder slurry is warming up to 35 ℃, close again the required power supply that heats up, in the time that this micro-nano powder slurry is cooled to 30 ℃, open the required power supply that heats up again this micro-nano powder slurry is warming up to 45 ℃, then close the required power supply that heats up, this micro-nano powder slurry can be cooled to 40 ℃ more afterwards.
9. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 7, is characterized in that: in this second heating step, stop nitrogen being poured in this cavity but not stopping aspiration pump, make the air pressure in this cavity be reduced to gradually 60Pa to 110Pa.
10. the method for vacuum freeze drying of micro-nano powder slurry as claimed in claim 1, it is characterized in that: in this second heating step, for opening the required power supply that heats up, this micro-nano powder slurry is warming up to 52 ℃, close again the required power supply that heats up, in the time that this micro-nano powder slurry is cooled to 47 ℃, open the required power supply that heats up again this micro-nano powder slurry is warming up to 60 ℃, then close the required power supply that heats up, this micro-nano powder slurry can be cooled to 55 ℃ more afterwards.
11. method of vacuum freeze dryings of micro-nano powder slurry as claimed in claim 1, is characterized in that: this high temperature constant temperature step is for maintaining 8 hours.
12. method of vacuum freeze dryings of micro-nano powder slurry as claimed in claim 9, is characterized in that: in this material step, for stopping this aspiration pump and nitrogen being poured in this cavity so that this cavity internal gas pressure is increased to 1atm.
13. method of vacuum freeze dryings of micro-nano powder slurry as claimed in claim 1, is characterized in that: this micro-nano powder is bamboo carbon powder, activated carbon powder, coffee carbon powder or coconut palm carbon powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210578693.3A CN103900353B (en) | 2012-12-27 | 2012-12-27 | The method of vacuum freeze drying of micro-nano powder slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210578693.3A CN103900353B (en) | 2012-12-27 | 2012-12-27 | The method of vacuum freeze drying of micro-nano powder slurry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103900353A true CN103900353A (en) | 2014-07-02 |
| CN103900353B CN103900353B (en) | 2016-03-02 |
Family
ID=50991831
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210578693.3A Active CN103900353B (en) | 2012-12-27 | 2012-12-27 | The method of vacuum freeze drying of micro-nano powder slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103900353B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106311230A (en) * | 2015-06-30 | 2017-01-11 | 中国石油化工股份有限公司 | Preparation method of silver catalyst used for alkene epoxidation, catalyst and application thereof |
| CN106955700A (en) * | 2016-01-08 | 2017-07-18 | 中国石油化工股份有限公司 | A kind of preparation method and applications of silver catalyst for alkene epoxidation |
| CN109916141A (en) * | 2019-01-31 | 2019-06-21 | 武汉科技大学 | A kind of low temperature dewatering processing method for metallurgical alloy powder |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02298790A (en) * | 1989-05-12 | 1990-12-11 | Kyowa Shinku Gijutsu Kk | Device and method for freeze drying |
| CN1266171A (en) * | 1999-03-05 | 2000-09-13 | 煜丰企业有限公司 | Freezing low-temp. drying treatment method |
| CN101050128A (en) * | 2007-04-13 | 2007-10-10 | 中国科学院上海硅酸盐研究所 | Modified freeze dehydration method for preparing porous material |
| US20080142166A1 (en) * | 2004-05-01 | 2008-06-19 | James Kenneth Carson | Drying Process and Apparatus |
| CN101403561A (en) * | 2008-11-07 | 2009-04-08 | 中国林业科学研究院林产化学工业研究所 | Method and apparatus for atomizing, freezing and drying for powder production by using low-temperature low-dew point gas |
| CN101518494A (en) * | 2009-03-23 | 2009-09-02 | 上海东富龙科技股份有限公司 | Full-automatic refrigeration control method |
| CN102173775A (en) * | 2011-02-23 | 2011-09-07 | 山东大学 | Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying |
-
2012
- 2012-12-27 CN CN201210578693.3A patent/CN103900353B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02298790A (en) * | 1989-05-12 | 1990-12-11 | Kyowa Shinku Gijutsu Kk | Device and method for freeze drying |
| CN1266171A (en) * | 1999-03-05 | 2000-09-13 | 煜丰企业有限公司 | Freezing low-temp. drying treatment method |
| US20080142166A1 (en) * | 2004-05-01 | 2008-06-19 | James Kenneth Carson | Drying Process and Apparatus |
| CN101050128A (en) * | 2007-04-13 | 2007-10-10 | 中国科学院上海硅酸盐研究所 | Modified freeze dehydration method for preparing porous material |
| CN101403561A (en) * | 2008-11-07 | 2009-04-08 | 中国林业科学研究院林产化学工业研究所 | Method and apparatus for atomizing, freezing and drying for powder production by using low-temperature low-dew point gas |
| CN101518494A (en) * | 2009-03-23 | 2009-09-02 | 上海东富龙科技股份有限公司 | Full-automatic refrigeration control method |
| CN102173775A (en) * | 2011-02-23 | 2011-09-07 | 山东大学 | Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106311230A (en) * | 2015-06-30 | 2017-01-11 | 中国石油化工股份有限公司 | Preparation method of silver catalyst used for alkene epoxidation, catalyst and application thereof |
| CN106311230B (en) * | 2015-06-30 | 2019-05-31 | 中国石油化工股份有限公司 | Preparation method, catalyst and the application of silver catalyst for alkene epoxidation |
| CN106955700A (en) * | 2016-01-08 | 2017-07-18 | 中国石油化工股份有限公司 | A kind of preparation method and applications of silver catalyst for alkene epoxidation |
| CN106955700B (en) * | 2016-01-08 | 2019-08-20 | 中国石油化工股份有限公司 | A kind of preparation method and applications of the silver catalyst for alkene epoxidation |
| CN109916141A (en) * | 2019-01-31 | 2019-06-21 | 武汉科技大学 | A kind of low temperature dewatering processing method for metallurgical alloy powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103900353B (en) | 2016-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107403698B (en) | A kind of application preparing the method for activated carbon and its active carbon of preparation using biomass | |
| CN103900353B (en) | The method of vacuum freeze drying of micro-nano powder slurry | |
| CN107604634A (en) | A kind of re-compounded aeroge fibrofelt and preparation method thereof | |
| CN105218836A (en) | A kind of emulsifying agent assists biological enzyme to prepare the method for size tunable type starch nanometer granule | |
| CN101358158A (en) | Method for preparing fresh aromatic essential oil | |
| CN104711121A (en) | Method for extracting chrysanthemum indicum essential oil in ultrasonic-assisted solvent-free microwave extraction manner | |
| CN105802589A (en) | High-strength heat-conducting film and preparation method thereof | |
| CN104229783A (en) | Preparation method of graphene film with high thermal conductivity | |
| CN103074109B (en) | Method for removing resin substance from lignite wax | |
| CN104892970A (en) | Method for directly preparing membrane through wood fiber | |
| CN104891485A (en) | Method for preparing nano graphite sheet | |
| CN203694633U (en) | MVR (mechanical vapor recompression) evaporator | |
| CN104860804A (en) | Environment-friendly extracting and purifying method of natural cinnamyl aldehyde | |
| CN105968080A (en) | Method for extracting anthocyanidin from black chokeberries | |
| CN103725418A (en) | Method for extracting jack fruit aromatherapy oil from ionic liquid | |
| CN106272817A (en) | A kind of wicker plaiting article is with wear-resisting anti-corruption inorganic agent | |
| CN204569879U (en) | A kind of Rose drying machine condensate recycling device | |
| CN110395978A (en) | A method of filtering molding machine and preparation ITO planar targets | |
| CN105060894A (en) | Method for preparing zirconium carbide wood ceramic | |
| CN103966878A (en) | Method for preparing microcrystalline cellulose by ionic liquid | |
| CN210150734U (en) | Nano silicon preparation solvent circulation recovery system | |
| CN209348152U (en) | A kind of purifying plant of organic solvent | |
| CN208846869U (en) | A kind of Chinese medicine production peony flower tea drying equipment | |
| CN203373553U (en) | Textile fabric printing and dyeing equipment | |
| CN203494226U (en) | Rapid vacuum supply assisting device for toothpaste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Gui Inventor after: Wang Wankai Inventor after: Wang Wanjie Inventor before: Wang Gui Inventor before: Wang Wanxian Inventor before: Wang Wanjie |
|
| CB03 | Change of inventor or designer information | ||
| CP01 | Change in the name or title of a patent holder |
Address after: No. 1156, No. 14, Zhonghua Road, toufenli Town, Miaoli County, Taiwan, China Patentee after: Wang Gui Patentee after: Wang Wankai Patentee after: Wang Wanjie Address before: No. 1156, No. 14, Zhonghua Road, toufenli Town, Miaoli County, Taiwan, China Patentee before: Wang Gui Patentee before: Wang Wanxian Patentee before: Wang Wanjie |
|
| CP01 | Change in the name or title of a patent holder | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201103 Address after: No.1, Huoju 6th Road, Gongqing City, Jiujiang City, Jiangxi Province Patentee after: Jiangxi zhushengfu Nano Technology Co., Ltd Address before: No. 1156, No. 14, Zhonghua Road, toufenli Town, Miaoli County, Taiwan, China Patentee before: Wang Gui Patentee before: Wang Wankai Patentee before: Wang Wanjie |
|
| TR01 | Transfer of patent right |