CN109916141A - A kind of low temperature dewatering processing method for metallurgical alloy powder - Google Patents
A kind of low temperature dewatering processing method for metallurgical alloy powder Download PDFInfo
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- CN109916141A CN109916141A CN201910095672.8A CN201910095672A CN109916141A CN 109916141 A CN109916141 A CN 109916141A CN 201910095672 A CN201910095672 A CN 201910095672A CN 109916141 A CN109916141 A CN 109916141A
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Abstract
The invention discloses a kind of low temperature dewatering processing methods for metallurgical alloy powder, pass through Vacuum Freezing & Drying Technology, moisture content is lower than 0.5% after the freeze-drying of alloyed powder cryogenic vacuum, and alloyed powder non-oxidation browning phenomenon in drying process, without adhesion or agglomeration between powder granule after drying, good dispersion influences the performance of alloyed powder smaller；And entire drying process carries out at low temperature, avoids in high-temperature drying procedures, the safety accidents such as oxidation, combustion explosion occur for alloyed powder, and easy to operate, are freeze-dried time-consuming shorter, the dehydration suitable for high-volume alloyed powder sample.
Description
Technical field
The present invention relates to technical field of drying, and in particular to a kind of low temperature dewatering processing method for metallurgical alloy powder.
Background technique
Aluminium, magnesium chemical property are active, and the alloyed powders such as magnesium powder, magnalium are produced, store, used due to large specific surface area
Journey be easy to slowly in air oxygen and moisture react, cause effective active to reduce, influence using effect, be easy
Various security risks are induced because of exothermic heat of reaction.
Existing magnesium powder, Al-Mg alloy powder drying process have the disadvantage that 1, drying process need be heated at high temperature and it is lazy
Property gas shield, it is high to the tight requirements of equipment, otherwise easily cause the safety accident of alloyed powder oxidation, combustion explosion；2, make
It is undesirable with cheap nitrogen protection effect, and use other inert gases at high cost.
Vacuum freeze drying is the distillation performance being lauched using cryogenic conditions, and low-temperature material is made to be dehydrated and reach drying purpose
A kind of drying means；Wet stock is freezed under its freezing point temperature first, obtains stable solid skeletal, then in suitable vacuum
It heats up under degree, so that ice is directly distilled is vapor, recycles the condenser of vacuum system by Water vapor condensation, to obtain
Dry products；Freeze Drying Technique can preferably keep exterior quality, color, the smell of material, and thoroughly, keeping quality is good for dehydration,
Make the decomposition of effective component simultaneously and scatter and disappear to be reduced to minimum limit, keeps the activity of material effective component.
Vacuum freeze drying is the optimal dewatering type of drying quality generally acknowledged at present, is widely used in food and pharmacy row
Industry, in freezing dry process, temperature setting is too low, and water sublimed is slower, and freeze-drying needs the time elongated, and efficiency reduces, simultaneously
Cause energy waste；Temperature setting is higher, and sample oxidation can be made rotten, and the purpose of vacuum freeze drying is not achieved；At present
Freeze Drying Technique in terms of apply and report all it is more (Zhou Guoyan etc., 2010；Pan Qingfang and Zhou Guoyan,
2011；Pond Chun-shan Mountain, 2010), have no that its related process studies the report in terms of emtallurgy research alloyed powder sample dehydration.
Therefore, it is necessary to establish a kind of freeze drying process of alloyed powder, reduces the water content in alloyed powder and closed with improving
The quality of bronze；Meanwhile under the premise of meeting freeze-drying purpose, freeze-drying efficiency is improved as far as possible, saves the energy.
Summary of the invention
In response to the problems existing in the prior art, the purpose of the present invention is to provide a kind of low temperature dewaterings for metallurgical alloy powder
Processing method is at low temperature controlled the water content in alloyed powder below 0.5% by Vacuum Freezing & Drying Technology.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of low temperature dewatering processing method for metallurgical alloy powder, which comprises the steps of:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located at 0.5~1h
It is interior that temperature in freeze drying equipment is down to -20 DEG C, and maintain 0.5~1h；
S2, freeze: after heat release, being located in 0.5~1.0h and temperature in lyophilizer is down to -40 DEG C hereinafter, then
The pressure in freeze drying equipment is controlled to 10Pa or less and maintains 2~8h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, 1~3h of heat preservation；So
Adjustment vacuum degree is 50 ± 30Pa afterwards, and temperature in freeze drying equipment is maintained to continue 2~4h of heat preservation at -5 DEG C；
S4, parsing: after distillation, if in freeze drying equipment temperature be 28~35 DEG C, and adjust vacuum degree be 10~
20Pa maintains 1~4h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After freezing the vacuum degree recovery 10Pa or less in drying equipment and 1~2h of holding, packaging.
In the above method of the present invention, the alloyed powder can be bought or be prepared by a conventional method by commercially available, described
Alloyed powder is oxidizable, explosive when being heated at high temperature dry, and cryogenic vacuum freeze-drying method can be at low temperature through the invention
The moisture content in alloyed powder is set to be reduced to 0.5% or less.
Wherein, after heretofore described heat release refers to that the water in alloyed powder is subcooled to freezing point, after interior generation nucleus, from
By water just can crystallized in the form of ice, while releasing crystallization heat makes its temperature rise to freezing point, releases the process of crystallization heat
It is exactly exothermic process.
The control method of the step S3 and S4: when adjustment vacuum degree, by opening air inlet from exhaust outlet opposite tank wall,
So that steam in case is obtained external force promotion, accelerates steam discharge, to improve rate of drying, in this operating process, not exclusively
Destroy vacuum.
It is gaseous that the distillation refers to that the moisture content in alloyed powder is directly translated into from solid-state without liquid in the present invention
Process.
Preferably, it is located in step S1 in 0.75h and temperature in freeze drying equipment is down to -20 DEG C, and maintain 0.75h.
Preferably, it is located in step S2 in 0.8h and temperature in freeze drying equipment is down to -40 DEG C or less；Then it controls cold
Freeze the pressure in drying equipment to 10Pa hereinafter, and maintaining 6h.
Preferably, the test method of vacuum degree described in step S5 is that pressure rises method of testing: being closed interval valve 120 seconds, observation
Pressure in freeze drying equipment, rises above 1Pa in 120 seconds, then confirms substantially anhydrous point of product evaporation, shuts down.
Preferably, the alloyed powder moisture content after drying is lower than 0.5%.
Compared with prior art, the beneficial effects of the present invention are:
(1) alloyed powder is freeze-dried by cryogenic vacuum of the present invention, and the moisture content of the alloyed powder after drying is lower than 0.5%,
Non-oxidation browning phenomenon without adhesion or agglomeration, good dispersion between powder granule, and influences the performance of alloyed powder smaller.
(2) after temperature of charge reaches set temperature, delay freeze-drying is carried out to product using low temperature pressure maintaining mode, further really
Protect the degree of drying of product.
(3) entire drying process carries out at low temperature, avoids in high-temperature drying procedures, and oxidation, combustion occur for alloyed powder
The fried safety accident of decrepitate.
(4) it is suitble to the processing of batch samples, and easy to operate, after program setting, one key operation of general staff can be complete
At freezing dry process.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated；It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention；Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method
And equipment.
Embodiment 1
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, starts compressor, it is located at 0.3~
Temperature in freeze drying equipment is down to -20 DEG C in 1.2h, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different temperature fall times carry out low temperature dewatering processing to alloyed powder in step S1, the alloyed powder obtained after dry it is aqueous
Rate the result is as follows:
| Temperature fall time (h) | Moisture content (%) |
| 0.3 | 0.8 |
| 0.5 | 0.28 |
| 0.75 | 0.1 |
| 1 | 0.4 |
| 1.2 | 1.0 |
By upper table result it is found that changing the step temperature fall time in S1, moisture content of the alloyed powder after dry can be generated larger
Influence, and when temperature in freeze drying equipment being down to -20 DEG C in 0.75h, the dehydration efficiency of alloyed powder is best, alloyed powder
Moisture content be down to 0.1%.
Embodiment 2
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.3~1.2h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different soaking times carry out low temperature dewatering processing to alloyed powder in step S1, the alloyed powder obtained after dry it is aqueous
Rate the result is as follows:
| Soaking time (h) | Moisture content (%) |
| 0.3 | 0.6 |
| 0.5 | 0.38 |
| 0.75 | 0.1 |
| 1 | 0.25 |
| 1.2 | 0.8 |
By upper table result it is found that changing the step soaking time in S1, moisture content of the alloyed powder after dry can be generated larger
Influence, and by freeze drying equipment temperature maintain -20 DEG C of 0.75h when, the dehydration efficiency of alloyed powder is best, and alloyed powder contains
Water rate is down to 0.1%.
Embodiment 3
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.2~1.2h and temperature in lyophilizer is down to -40 DEG C hereinafter, then
Pressure in control freeze drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different temperature fall times carry out low temperature dewatering processing to alloyed powder in step S2, the alloyed powder obtained after dry it is aqueous
Rate the result is as follows:
| Temperature fall time (h) | Moisture content (%) |
| 0.2 | 0.7 |
| 0.5 | 0.25 |
| 0.8 | 0.1 |
| 1 | 0.45 |
| 1.2 | 0.7 |
By upper table result it is found that changing the step temperature fall time in S2, moisture content of the alloyed powder after dry can be generated larger
Influence, and when temperature in freeze drying equipment being down to -40 DEG C in 0.8h, the dehydration efficiency of alloyed powder is best, alloyed powder
Moisture content be down to 0.1%.
Embodiment 4
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment is to 10Pa or less and maintains 1~10h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different soaking times carry out low temperature dewatering processing to alloyed powder in step S2, the alloyed powder obtained after dry it is aqueous
Rate the result is as follows:
| Soaking time (h) | Moisture content (%) |
| 1 | 0.7 |
| 2 | 0.45 |
| 3 | 0.35 |
| 4 | 0.28 |
| 5 | 0.2 |
| 6 | 0.1 |
| 7 | 0.08 |
| 8 | 0.07 |
| 10 | 0.06 |
By upper table result it is found that changing the step soaking time in S2, moisture content of the alloyed powder after dry can be generated larger
Influence, with holding time, the drying effect of alloyed powder is gradually promoted, but keep the temperature 6h after, the drying effect of alloyed powder
Variation is smaller, from the aspect of saving cost, selects heat preservation 6h as best.
Embodiment 5
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50 ± 30Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different vacuum degrees carry out low temperature dewatering processing, the moisture content of the alloyed powder obtained after dry to alloyed powder in step S3
The result is as follows:
By upper table result it is found that changing the step vacuum degree in S3, moisture content of the alloyed powder after dry can be generated larger
Influence, as vacuum strength increases, after the drying effect of alloyed powder is gradually promoted, but vacuum degree reaches 50Pa, alloyed powder
Drying effect variation it is smaller, from save cost from the aspect of, select vacuum degree be 50Pa conduct most preferably.
Embodiment 6
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, 0.5~4h of heat preservation；
Then adjustment vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different soaking times carry out low temperature dewatering processing to alloyed powder in step S3, the alloyed powder obtained after dry it is aqueous
Rate the result is as follows:
| Soaking time (h) | Moisture content (%) |
| 0.5 | 0.5 |
| 1 | 0.28 |
| 2 | 0.1 |
| 3 | 0.08 |
| 4 | 0.07 |
By upper table result it is found that changing the step soaking time in S3, moisture content of the alloyed powder after dry can be generated larger
Influence, with holding time, the drying effect of alloyed powder is gradually promoted, but keep the temperature 2h after, the drying effect of alloyed powder
Variation is smaller, from the aspect of saving cost, selects heat preservation 2h as best.
Embodiment 7
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue 1~5h of heat preservation at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different continuation soaking times carry out low temperature dewatering processing to alloyed powder in step S3, the alloyed powder obtained after dry
Moisture content the result is as follows:
| Soaking time (h) | Moisture content (%) |
| 1 | 0.6 |
| 2 | 0.3 |
| 3 | 0.1 |
| 4 | 0.07 |
| 5 | 0.06 |
By upper table result it is found that changing the step S3 relays continuous soaking time, moisture content of the alloyed powder after dry can be generated
Large effect, with holding time is continued, the drying effect of alloyed powder is gradually promoted, and after keeping the temperature 3h, alloyed powder is done
Dry effect variation is smaller, from the aspect of saving cost, selects to continue to keep the temperature 3h as best.
Embodiment 8
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 25~40 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa,
Maintain 2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different temperatures carries out low temperature dewatering processing, the moisture content knot of the alloyed powder obtained after dry to alloyed powder in step S4
Fruit is as follows:
| Temperature (DEG C) | Moisture content (%) |
| 25 | 0.5 |
| 28 | 0.32 |
| 32 | 0.1 |
| 35 | 0.08 |
| 40 | 0.07 |
By upper table result it is found that changing the step temperature in S4, biggish shadow can be generated to moisture content of the alloyed powder after dry
It rings, as temperature increases, the drying effect of alloyed powder is gradually promoted, and after temperature reaches 32 DEG C, the drying effect of alloyed powder becomes
Change it is smaller, comprehensively consider select control drying equipment in temperature be 32 DEG C.
Embodiment 9
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 5~25Pa,
Maintain 2h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different vacuum degrees carry out low temperature dewatering processing, the moisture content of the alloyed powder obtained after dry to alloyed powder in step S4
The result is as follows:
| Vacuum degree (Pa) | Moisture content (%) |
| 5 | 0.07 |
| 10 | 0.08 |
| 15 | 0.1 |
| 20 | 0.28 |
| 25 | 0.54 |
By upper table result it is found that changing the step vacuum degree in S4, moisture content of the alloyed powder after dry can be generated larger
Influence, as vacuum strength increases, after the drying effect of alloyed powder is gradually promoted, but vacuum degree reaches 15Pa, alloyed powder
Drying effect variation it is smaller, therefore select control vacuum degree be 15Pa.
Embodiment 10
The present embodiment provides a kind of low temperature dewatering processing methods for metallurgical alloy powder, include the following steps:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, is started compressor, is located in 0.75h
Temperature in freeze drying equipment is down to -20 DEG C, and maintains 0.75h；
S2, freeze: after heat release, being located in 0.8h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling cold
The pressure frozen in drying equipment to 10Pa or less and maintains 6h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, heat preservation 2h；Then it adjusts
Whole vacuum degree is 50Pa, and temperature in freeze drying equipment is maintained to continue to keep the temperature 3h at -5 DEG C；
S4, parsing: after distillation, if temperature is 32 DEG C in freeze drying equipment, and adjusting vacuum degree is 15Pa, is maintained
0.5~5h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, will be cold
After the vacuum degree frozen in drying equipment restores 10Pa or less and keeps 1.5h, carries out pressure and rises test, close interval valve 120 seconds,
Pressure in freeze drying equipment is observed, 1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down, packet
Dress.
Different vacuum degrees carry out low temperature dewatering processing, the moisture content of the alloyed powder obtained after dry to alloyed powder in step S4
The result is as follows:
| Soaking time (h) | Moisture content (%) |
| 0.5 | 0.6 |
| 1 | 0.3 |
| 2 | 0.1 |
| 3 | 0.08 |
| 4 | 0.07 |
| 5 | 0.06 |
By upper table result it is found that changing the step soaking time in S4, moisture content of the alloyed powder after dry can be generated larger
Influence, with holding time, the drying effect of alloyed powder is gradually promoted, and after keeping the temperature 2h, the drying effect of alloyed powder becomes
Change is smaller, from the aspect of saving cost, selects to continue to keep the temperature 2h as best.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes
It also should be regarded as protection scope of the present invention into supplement；All those skilled in the art, do not depart from spirit of that invention and
In the case where range, using the equivalent variations of a little change, modification and differentiation that disclosed above technology contents are made, it is
Equivalent embodiment of the invention；Meanwhile any equivalent variations that all substantial technologicals according to the present invention do above-described embodiment
Change, modification and differentiation, still fall within protection scope of the present invention.
Claims (5)
1. a kind of low temperature dewatering processing method for metallurgical alloy powder, which comprises the steps of:
S1, pre-freeze: the alloyed powder of processing to be drained off is put into freeze drying equipment, starts compressor, and being located in 0.5~1h will
Temperature is down to -20 DEG C in freeze drying equipment, and maintains 0.5~1h；
S2, freeze: after heat release, being located in 0.5~1.0h and temperature in lyophilizer is down to -40 DEG C hereinafter, then controlling
Pressure in freeze drying equipment to 10Pa or less and maintains 2~8h；
S3, distillation: setting in freeze drying equipment temperature as -5 DEG C, and vacuum maintains 10Pa hereinafter, 1~3h of heat preservation；Then it adjusts
Whole vacuum degree is 50 ± 30Pa, and temperature in freeze drying equipment is maintained to continue 2~4h of heat preservation at -5 DEG C；
S4, parsing: after distillation, if temperature is 28~35 DEG C in freeze drying equipment, and adjusting vacuum degree is 10~20Pa,
Maintain 1~4h；
S5, after temperature reaches 35 DEG C and at least two product temperatures probe more than 25 DEG C in freeze drying equipment, freezing is done
After vacuum degree in dry equipment restores 10Pa or less and keeps 1~2h, packaging.
2. a kind of low temperature dewatering processing method for metallurgical alloy powder according to claim 1, which is characterized in that step
It is located in S1 in 0.75h and temperature in freeze drying equipment is down to -20 DEG C, and maintain 0.75h.
3. a kind of low temperature dewatering processing method for metallurgical alloy powder according to claim 1, which is characterized in that step
It is located in S2 in 0.8h and temperature in freeze drying equipment is down to -40 DEG C hereinafter, then controlling the pressure in freeze drying equipment
To 10Pa hereinafter, and maintaining 6h.
4. a kind of low temperature dewatering processing method for metallurgical alloy powder according to claim 1, which is characterized in that step
The test method of vacuum degree described in S5 is that pressure rises method of testing: it closes interval valve 120 seconds, observes pressure in freeze drying equipment,
1Pa is risen above in 120 seconds, then confirms substantially anhydrous point of product evaporation, is shut down.
5. a kind of low temperature dewatering processing method for metallurgical alloy powder according to claim 1, which is characterized in that dry
Alloyed powder moisture content afterwards is lower than 0.5%.
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