CN103920303A - Airflow heating defrosting method for cold trap - Google Patents
Airflow heating defrosting method for cold trap Download PDFInfo
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- CN103920303A CN103920303A CN201410165699.7A CN201410165699A CN103920303A CN 103920303 A CN103920303 A CN 103920303A CN 201410165699 A CN201410165699 A CN 201410165699A CN 103920303 A CN103920303 A CN 103920303A
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Abstract
The invention discloses an airflow heating defrosting method for a cold trap. An inertia airflow heating method is adopted, hot airflows and solid solidified inside the cold trap are directly contacted to melt the solid, an air inlet/outlet of the cold trap is connected with an air-blowing heating device, and when defrosting is required, the air-blowing heating device is connected with the cold trap, and other loops are cut off to perform defrosting. According to the method, as the airflow heating method has the advantages of large contact area, small thermal inertia, high flowing speed and the like, the defrosting method is simple and rapid, and compared with the traditional method, the method can save 30% of energy consumption and has short defrosting time.
Description
Technical field
The invention belongs to the Defrost method field of cold-trap, be specifically related to a kind of air-flow heating Defrost method of cold-trap.
Background technology
Cold-trap claims again condense trap, is to utilize low temperature cold wall to trap a kind of cryogenic condensation trap of coercibility steam.Cold-trap is widely used in, in high vacuum and ultra-high vacuum system, being arranged on the pipeline between main pump inlet and vacuum chamber.Cold-trap can not only trap backflow steam and the part lysate from steam flow pump effectively, but also can extract from the coercibility steam in vacuum chamber.The application of cold-trap mainly contains two aspects, on the one hand the application in vacuum freezing drying device; Be on the other hand the trapping to processing medium condensable gas under medicine and chemical field high vacuum condition.
Under high vacuum, the steam that backflows can directly be sublimated at the cold wall surface of cold-trap, condenses into frost.And along with the cold-trap continuous prolongation of running time, the frost of cold wall surface can be more long-pending thicker, envelopes the cold wall of cold-trap completely, and due to medium, to form white thermal conductivity much lower compared with metal material, can cause cold-trap supplementary set efficiency sharply to decline, affect vavuum pump and system vacuum.In addition, because frosting is too much, also can cause cold-trap to stop up, cause system vacuum to decline, affect normal technique, even because high pressure is caused danger.According to the difference of cold-trap range of application, institute's frosting physicochemical properties also differ widely, in the cold-trap of freeze drier, the composition of frost is mainly the ice that water is formed, and in field of medicine and chemical technology, the composition of frost varies, and comprises the raw material of organic solvent, industrial chemicals and some thermal sensitivity.And the fusing point gap of these materials is very large, from-100 DEG C～200 DEG C not etc., therefore brought very large trouble to defrosting.In addition, be generally intermittently operated in vacuum freeze drying field, therefore the working method of cold-trap is not had to strict requirement; And at medicine and chemical field, major part is the technique that can not be interrupted, require cold-trap to there is the characteristic of continued operation, this Defrost method to cold-trap has proposed new requirement-simple and fast, and consuming time short, the preparatory period is short.
At present there are two kinds for the method defrosting, one is to adopt low-pressure steam defrosting, in defrosting workshop section, in cold-trap, keep certain vacuum, material in heating cold-trap, it is under low pressure seethed with excitement, by steam and the solid material transmission of heat by contact condensing on the cold wall of cold-trap of this material, frost is melted; Another kind method is that the refrigerant of cold-trap is closed, and passes into heating agent, by the cold wall heating of cold-trap, material is melted.First method is applicable to lower boiling material, as water, organic solvent, liquefied ammonia etc., but cannot be competent at for the material of higher boiling or thermal sensitivity.And second method goes for high boiling material, but because cold and hot medium alternately passes into, the thermal inertia of cold and hot matchmaker's back-mixing and equipment itself, cause energy consumption very high, in addition, because cold and hot matchmaker is alternately switched, equipment by cold state to hot state, self need heating, and thermal resistance two reasons of equipment self, make equipment reach time of predetermined temperature long, defrosting efficiency is low, after defrosting, the time of cooling is long again, and the effective time is short.
Summary of the invention
The air-flow heating Defrost method that the object of this invention is to provide a kind of cold-trap, it is thermal sensitivity, high boiling material that the method is applicable to white composition, the method energy consumption is low simultaneously, speed is fast, defrosting efficiency is high.
The air-flow heating Defrost method that the invention provides a kind of cold-trap, the method comprises:
Step 1: the first cold-trap, air blowing heating device and the second cold-trap are connected in parallel, and described air blowing heating device is the device of air blast and electric heater unit series connection, and vavuum pump is all connected with the first cold-trap and the second cold-trap respectively with system;
Step 2: close imported valve and outlet valve that air blowing heating device is connected with the first cold-trap, the inlet valve that the inlet valve that the system of opening is connected with the first cold-trap and vavuum pump are connected with the first cold-trap, open refrigerant imported valve, refrigerant exit valve, the refrigerant imported valve of chuck and the refrigerant exit valve of chuck in the first cold-trap, close the heating agent imported valve of the chuck in the first cold-trap and the heating agent outlet valve of chuck, the first cold-trap is normally worked;
Step 3: when needs defrost processing to the first cold-trap, the inlet valve that the inlet valve that shutdown system is connected with the first cold-trap and vavuum pump are connected with the first cold-trap, the inlet valve that the inlet valve that the system of opening is connected with the second cold-trap and vavuum pump are connected with the second cold-trap, switches to the second cold-trap by vavuum pump and system;
Step 4: open the inlet valve that inert gas installation is connected with the first cold-trap, imported valve and outlet valve that air blowing heating device is connected with the first cold-trap, make to be full of inert gas in the first cold-trap, close refrigerant imported valve in the first cold-trap and the refrigerant imported valve of chuck, open air blast, open again electric heater unit, inert gas is through the first cold-trap and air blast, after being heated by electric heater unit, flow into again circulating-heating in the first cold-trap, when temperature reaches after the fusing point of material, material starts to melt, liquid flow in the stock chest in the first cold-trap, defrost process finishes.
Preferably, described air blast comprises pressure fan, axial flow blower, centrifugal blower or roots blower.
Preferably, described electric heater unit comprises electric heater, steam heater, hot oil heater or combustion furnace heater.
Preferably, described inert gas comprises helium, neon, argon gas, xenon, nitrogen, air or oxygen.
Beneficial effect of the present invention
1, the air-flow of a kind of cold-trap of the present invention heating Defrost method, is using air-flow as heat carrier, has density little, the feature that specific heat is little, and firing rate and programming rate are all very fast, and the unwanted heat that heat hot carrier consumes is few; In the method, thermal current can directly contact with material, and heat transfer area is large, and heat transfer efficiency is high, and the frost of forming in cold-trap can melt and flow away very soon because of contact thermal current, can flow in stock chest with deflection plate; Meanwhile, thermal current flows in cold-trap, and heat transfer type is close to convection heat transfer' heat-transfer by convection, and heat transfer coefficient is large;
2, backflow under flow trace in cold-trap and vacuum state by the thermal current flow trace of steam of method of the present invention is quite similar, in the cold wall of cold-trap, hang the thermal current flowing through in the thick place of frost many, defrosting institute calorific requirement just matches with the flow of thermal current, and heat utilization ratio is high;
3, method of the present invention flows in cold-trap by thermal current, dead volume is few, in prior art, the inwall of cold-trap passes in the Defrost method of heating agent, because the cold wall of cold-trap becomes hot wall, can make first to melt with the material of cold-trap surface contact portion, along with constantly carrying out of melting, liquid material flows away gradually, and remainder solid material does not directly contact with heated wall, can fall by Action of Gravity Field on the deflection plate of cold-trap, because material does not directly contact with heated wall, heat transfer can only be by heat conduction and the radiant heat transfer of gas medium in cold-trap, thermal conductivity factor is very low, and deflection plate self-temperature is lower, can not provide enough heats that material is melted, therefore this kind of method can form dead volume, defrosting efficiency is very low, and the present invention utilizes thermal current can bump with deflection plate in flow process, cause the change of flow direction, deflection plate is under the heating of thermal current, and temperature is higher, faster to the heating material speed on it, and therefore air-flow heating dead volume is little,
4, method of the present invention is by the mode of thermal current, gentleer to equipment heating, can reduce the heat fatigue problem that equipment causes because of low suddenly cold and hot, the service life of extension device;
5, method of the present invention directly adds thermal material by air-flow, and the cold wall in cold-trap is without intensification, and after defrosting, temperature is lower, has reduced heating load and follow-up cooling load, saves energy consumption.It is thermal sensitivity, high boiling material that while method of the present invention is applicable to white composition, as naphthalene, bisphenol-A, organic acid, lactide, glycolide etc.
Brief description of the drawings
Fig. 1 is the structural representation of realizing cold-trap Defrost method of the present invention.
In figure, 1, the first cold-trap, 2, the second cold-trap, 3, air blast, 4, electric heater unit, 5, vavuum pump, 6, system, 7, inert gas installation, 8, inert gas installation, 9, discharging opening, 10, reservoir, V1, the inlet valve that inert gas installation is connected with the first cold-trap, V2, the inlet valve that system is connected with the first cold-trap, V3, the outlet valve that air blowing heating device is connected with the first cold-trap, V4, the inlet valve that air blowing heating device is connected with the first cold-trap, V5, the inlet valve that vavuum pump is connected with the first cold-trap, V6, refrigerant imported valve, V7, refrigerant exit valve, V8, the refrigerant imported valve of chuck, V9, the refrigerant exit valve of chuck, V10, the heating agent imported valve of chuck, V11, the heating agent outlet valve of chuck, V12, the outlet valve that air blowing heating device is connected with the second cold-trap, V13, the inlet valve that system is connected with the second cold-trap, V14, the inlet valve that air blowing heating device is connected with the second cold-trap, V15, the inlet valve that vavuum pump is connected with the second cold-trap, V16, the inlet valve that inert gas installation is connected with the second cold-trap, T1, liquidus temperature, T2, hot blast temperature, P1, system internal pressure.
Detailed description of the invention
The air-flow heating Defrost method that the invention provides a kind of cold-trap, as shown in Figure 1, the method comprises:
The first cold-trap 1, air blowing heating device and the second cold-trap 2 are connected in parallel, and described air blowing heating device is the device that air blast 3 and electric heater unit 4 are connected, and vavuum pump 5 is all connected with the first cold-trap 1 and the second cold-trap 2 respectively with system 6;
Close imported valve V4 and outlet valve V3 that air blowing heating device is connected with the first cold-trap 1, air blowing heating device is isolated by valve and vavuum pump 5 and system 6, the inlet valve V5 that the inlet valve V2 that the system of opening is connected with the first cold-trap and vavuum pump are connected with the first cold-trap, open the refrigerant imported valve V6 in the first cold-trap, refrigerant exit valve V7, the refrigerant exit valve V9 of the refrigerant imported valve V8 of chuck and chuck, close the heating agent imported valve V10 of the chuck in the first cold-trap 1 and the heating agent outlet valve V11 of chuck, vavuum pump 5, system 6 and the first cold-trap are normally worked,
Along with constantly carrying out of technique, the devaporation of backflowing is constantly thickeied to the frost layer of the first cold-trap 1 cold wall, when frost thickness acquires a certain degree, need to defrost processing to the first cold-trap 1 time, the inlet valve V5 that the inlet valve V2 that shutdown system 6 is connected with the first cold-trap 1 and vavuum pump 5 are connected with the first cold-trap 1, open the inlet valve V15 that inlet valve V13 that system 6 is connected with the second cold-trap 2 and vavuum pump 5 are connected with the second cold-trap 2, vavuum pump 5 and system 6 are switched to the second cold-trap 2;
Open the inlet valve V1 that inert gas installation 7 is connected with the first cold-trap 1, the imported valve V4 that air blowing heating device is connected with the first cold-trap and outlet valve V3, make to be full of inert gas in the first cold-trap 1, close refrigerant imported valve V6 in the first cold-trap 1 and the refrigerant imported valve V8 of chuck, the refrigerant exit valve V9 of the refrigerant exit valve V7 in the first cold-trap 1 and chuck is in open mode, to prevent causing because the interior temperature of the first cold-trap 1 raises the hypertonia that expansion of liquids causes, open air blast 3, open again electric heater unit 4, inert gas is through the first cold-trap 1 and air blast 3, after being heated by electric heater unit 4, flow into again the interior circulating-heating of the first cold-trap 1, controlled wind speed, in order to avoid carried secretly by the too fast drop causing of wind speed, also will control hot blast temperature simultaneously, ensure defrosting speed faster on the one hand, prevent on the other hand that heating-up temperature is too high and cause sex change or the decomposition of heat sensitive material, the setting of wind speed and temperature need to decide according to different material, when temperature reaches after the fusing point of material, when temperature reaches after the fusing point of material, material starts to melt, and liquid flow in the stock chest 10 in the first cold-trap 1, and defrost process finishes.
After frosting is removed totally, stop electric heater unit 4, air blast 3 continues operation, opens the refrigerant imported valve V8 of refrigerant imported valve V6 and chuck simultaneously, and equipment is cooling.Air blast 3 continues operation until be reduced to room temperature; object is to promote the circulation of inert gas in the first cold-trap 1; a little material steam of carrying secretly in air-flow is condensed to the Leng Bichu of the first cold-trap 1; avoid in air blowing heating device material residual; air blast 3 continues to move the waste heat that can also take away heater simultaneously, reaches the object of protection electric heater unit 4.The first cold-trap 1 returns to after normal temperature, close imported valve V4 and outlet valve V3 that air blowing heating device is connected with the first cold-trap 1, refrigerant continues to pass into, until the first cold-trap 1 normal operating temperature, slowly open again vavuum pump 5 and the valve V5 that the first cold-trap 1 is connected, can continue to come into operation after reaching the vacuum of technological requirement.
When after repeatedly defrosting, stock chest 10 in the first cold-trap 1 reaches after certain liquid level, in defrosting, the refrigerant imported valve V8 of chuck and outlet valve V9 are closed, the heating agent imported valve V10 and the outlet valve V11 that open chuck, heating agent passes into stock chest 10, the material in stock chest is all melted with heating agent, concentrate and be discharged into assigned address, discharge through discharging opening 9.After cooling, the first cold-trap 1 returns to again original state, can move at any time again.
System of the present invention is to treat the general name of vacuumized part, contain processing medium, the first cold-trap 1 of the present invention, the second cold-trap 2, air blast 3 and electric heater unit 4 are all prior aries, the first described cold-trap 1 and the second cold-trap 2 are the identical device of structure, the described inert gas installation 7 connecting with the first cold-trap 1 and the inert gas installation 8 being connected with the second cold-trap 2 can be other devices of two identical inertia, also can be provided with the same device that simultaneously connects the first cold-trap 1 and the second cold-trap 2.Described air blast comprises various ways, preferably includes negative-pressure air fan, axial flow blower, centrifugal blower or roots blower; Described electric heater unit also comprises various ways, comprises electric heater, steam heater, hot oil heater or combustion furnace heater; Inert gas of the present invention is also not particularly limited, inertia is for the composition of " frost ", only otherwise the gas reacting with heated medium is all called inert gas, preferably include helium, neon, argon gas, xenon, nitrogen, air or oxygen etc.
Be example taking material in cold-trap as lactide below, illustrate method of the present invention.
Lactide freezing point is 97 DEG C, and atmospheric boiling point is 264 DEG C, therefore cannot defrost by the way of low-pressure steam, can only be by passing into thermal medium or adopting two kinds of method defrostings of thermal current.
Embodiment 1
The first cold-trap 1, air blowing heating device and the second cold-trap 2 are connected in parallel, and described air blowing heating device is the device that air blast 3 and electric heater unit 4 are connected, and vavuum pump 5 is all connected with the first cold-trap 1 and the second cold-trap 2 respectively with system 6;
Close imported valve V4 and outlet valve V3 that air blowing heating device is connected with the first cold-trap 1, air blowing heating device is isolated by valve and vavuum pump 5 and system 6, the inlet valve V5 that the inlet valve V2 that the system of opening is connected with the first cold-trap and vavuum pump are connected with the first cold-trap, open the refrigerant imported valve V6 in the first cold-trap, refrigerant exit valve V7, the refrigerant exit valve V9 of the refrigerant imported valve V8 of chuck and chuck, close the heating agent imported valve V10 of the chuck in the first cold-trap 1 and the heating agent outlet valve V11 of chuck, vavuum pump 5, system 6 and the first cold-trap are normally worked,
Along with constantly carrying out of technique, the devaporation of backflowing is constantly thickeied to the frost layer of the first cold-trap 1 cold wall, when frost thickness acquires a certain degree, need to defrost processing to the first cold-trap 1 time, the inlet valve V5 that the inlet valve V2 that shutdown system 6 is connected with the first cold-trap 1 and vavuum pump 5 are connected with the first cold-trap 1, open the inlet valve V15 that inlet valve V13 that system 6 is connected with the second cold-trap 2 and vavuum pump 5 are connected with the second cold-trap 2, vavuum pump 5 and system 6 are switched to the second cold-trap 2;
Open the inlet valve V1 that inert gas installation 7 is connected with the first cold-trap 1, the imported valve V4 that air blowing heating device is connected with the first cold-trap and outlet valve V3, make to be full of inert gas in the first cold-trap 1, close refrigerant imported valve V6 in the first cold-trap 1 and the refrigerant imported valve V8 of chuck, the refrigerant exit valve V9 of the refrigerant exit valve V7 in the first cold-trap 1 and chuck is in open mode, open air blast 3, open again electric heater unit 4, inert gas is through the first cold-trap 1 and air blast 3, after being heated by electric heater unit 4, flow into again the interior circulating-heating of the first cold-trap 1, when temperature reaches after the fusing point of material, when temperature reaches after the fusing point of material, material starts to melt, liquid flow in the stock chest 10 in the first cold-trap 1, defrost process finishes.
The technical parameter of air-flow defrosting cold-trap: the weight of cold-trap 1 and cold-trap 2 is all 1000kg, air blowing heating device 100kg, refrigerant temperature :-10 DEG C, inert gas adopts nitrogen; Air-flow defrosting temperature: 120 DEG C, coolant media: 30% ethylene glycol solution, the amount 150kg of cold-trap 1 interior refrigerant, wherein inner coil pipe water storage 100kg, chuck 50kg.When defrosting finishes, 90 DEG C of device temperatures, 70 DEG C of the interior heat medium temperatures of cold-trap 1, need be cooled to-10 DEG C again while again operation.
Comparative example
Pass into the technical parameter of heating agent defrosting cold-trap: weight of equipment 1000kg, refrigerant temperature :-10 DEG C; Heating agent defrosting temperature: 130 DEG C, coolant media: 30% ethylene glycol solution, thermal medium: 30% ethylene glycol solution, the amount 150kg of refrigerant in cold-trap, wherein inner coil pipe water storage 100kg, chuck 50kg.When defrosting finishes, 125 DEG C of device temperatures, in cold-trap, 130 DEG C of heat medium temperatures, need be cooled to-10 DEG C again while again operation.
Experimental result shows: from providing heat aspect to calculate, (be simplification process, the temperature that both defrostings finish rear lactide is identical, and in practical operation, the former lactide temperature will be higher than the latter, and the temperature difference is ignored here.) through an operation cycle, the heat that Defrost method in comparative example need to provide is the heat of 142530kJ, coolingly need to provide identical refrigerating capacity 142530kJ, and the heat that Defrost method of the present invention need to provide is 97940kJ, the heat of cooling needs is all 97940kJ, and the energy consumption of application air-flow heating defrosting is only 69% of heating agent defrosting.(note: stainless specific heat is got 0.502kJ/kg DEG C, 30% aqueous solution specific heat is got 3.56kJ/kg DEG C)
Calculate from time cost, the advantage of air-flow defrosting is more obvious, and air-flow is raised to 120 DEG C of needs 5min from normal temperature, and completing whole material required time only needs 40 minutes.And conventional method heating agent passes into the cold wall of rear cold-trap and is heated to 120 DEG C of needs one hour, finish to need 4 hours completely to defrosting.
The air-flow heating Defrost method of cold-trap of the present invention is not limited to cold-trap, anyly relates to the operation of melting the solid material in process system with the inert gas heating, and is all applicable to this method.
Claims (4)
1. the air-flow of a cold-trap heating Defrost method, is characterized in that, the method comprises:
Step 1: the first cold-trap (1), air blowing heating device and the second cold-trap (2) are connected in parallel, described air blowing heating device is the device of air blast (3) and electric heater unit (4) series connection, and vavuum pump (5) is all connected with the first cold-trap (1) and the second cold-trap (2) respectively with system (6);
Step 2: close imported valve (V4) and outlet valve (V3) that air blowing heating device is connected with the first cold-trap (1), open the inlet valve (V5) that inlet valve (V2) that system (6) is connected with the first cold-trap (1) and vavuum pump are connected with the first cold-trap, open the refrigerant imported valve (V6) in the first cold-trap, refrigerant exit valve (V7), the refrigerant imported valve (V8) of chuck and the refrigerant exit valve (V9) of chuck, close the heating agent imported valve (V10) of chuck in the first cold-trap and the heating agent outlet valve (V11) of chuck, the first cold-trap (1) is normally worked,
Step 3: when needs defrost processing to the first cold-trap (1), the inlet valve (V5) that the inlet valve (V2) that shutdown system (6) is connected with the first cold-trap (1) and vavuum pump are connected with the first cold-trap, open the inlet valve (V15) that inlet valve (V13) that system (6) is connected with the second cold-trap (2) and vavuum pump (5) are connected with the second cold-trap (2), vavuum pump (5) and system (6) are switched to the second cold-trap (2);
Step 4: open the inlet valve (V1) that inert gas installation (7) is connected with the first cold-trap (1), the imported valve (V4) that air blowing heating device is connected with the first cold-trap (1) and outlet valve (V3), make to be full of inert gas in the first cold-trap (1), close refrigerant imported valve (V6) in the first cold-trap (1) and the refrigerant imported valve (V8) of chuck, open air blast (3), open again electric heater unit (4), inert gas is through the first cold-trap (1) and air blast (3), after electric heater unit (4) heating, flowed into again the interior circulating-heating of the first cold-trap (1), when temperature reaches after the fusing point of material, material starts to melt, liquid flow in the stock chest in the first cold-trap (1), defrost process finishes.
2. the air-flow of a kind of cold-trap according to claim 1 heating Defrost method, is characterized in that, described air blast (3) comprises pressure fan, axial flow blower, centrifugal blower or roots blower.
3. the air-flow of a kind of cold-trap according to claim 1 heating Defrost method, is characterized in that, described electric heater unit (4) comprises electric heater, steam heater, hot oil heater or combustion furnace heater.
4. the air-flow of a kind of cold-trap according to claim 1 heating Defrost method, is characterized in that, described inert gas comprises helium, neon, argon gas, xenon, nitrogen, air or oxygen.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410165699.7A CN103920303A (en) | 2014-04-22 | 2014-04-22 | Airflow heating defrosting method for cold trap |
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| CN201410165699.7A CN103920303A (en) | 2014-04-22 | 2014-04-22 | Airflow heating defrosting method for cold trap |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104930819A (en) * | 2015-06-28 | 2015-09-23 | 浙江大学 | Vacuum freeze-drying equipment based on closed moisture absorption solution regeneration and method |
| CN107648878A (en) * | 2017-10-24 | 2018-02-02 | 广州美晨科技实业有限公司 | A kind of manufacture system of single, double fatty acid glyceride |
| CN111939589A (en) * | 2019-05-14 | 2020-11-17 | 广东聚航新材料研究院有限公司 | High-efficient vacuum cold trap |
| US11846575B2 (en) | 2018-12-31 | 2023-12-19 | Teknologian Tutkimuskeskus Vtt Oy | Sampling arrangement |
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| CN2903855Y (en) * | 2006-04-21 | 2007-05-23 | 北美冻干技术股份公司 | Plate type cold trap for freeze drier |
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Application publication date: 20140716 |