CN209148589U - A kind of low-temperature electrolytic extraction carbide refrigerator - Google Patents

A kind of low-temperature electrolytic extraction carbide refrigerator Download PDF

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Publication number
CN209148589U
CN209148589U CN201822000974.6U CN201822000974U CN209148589U CN 209148589 U CN209148589 U CN 209148589U CN 201822000974 U CN201822000974 U CN 201822000974U CN 209148589 U CN209148589 U CN 209148589U
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China
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carbide
low
refrigerator
refrigeration
electrolytic
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CN201822000974.6U
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邱国兴
齐敏
李宇露
王佳喜
王东伟
屈乐欣
马竞翔
战东平
李长生
张慧书
姜周华
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Northeastern University China
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Northeastern University China
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Abstract

A kind of low-temperature electrolytic extraction carbide refrigerator, it include: electrolytic cell, heat exchange slot, refrigeration unit, sealing unit and control unit, wherein: refrigeration unit includes refrigeration groove, cooling wall, water pump and insulating layer, cooling wall is wrapped in outside the upper end of refrigeration groove, cooling wall is connect with water pump, and insulating layer is wrapped in outside the lower end of refrigeration groove;Inside electrolytic cell insertion heat exchange slot, inside heat exchange slot insertion refrigeration groove, electrolytic cell, heat exchange slot and refrigeration groove are close to;Sealing unit includes sealing cover and relief valve;Control unit includes feedback controller and thermometer.Low-temperature electrolytic provided by the utility model extracts carbide refrigerator, it can be in the electrolyte in stability contorting electrolytic cell in -10~5 DEG C of low temperature environment, avoid electrolyte overheated in electrolytic process volatilization and carbide be oxidized, the efficiency of electrolysis improves 40~50%, the consumption of electrolyte reduces 20~30%, and the carbide degree of purity of electrolysis improves 25~35%.

Description

A kind of low-temperature electrolytic extraction carbide refrigerator
Technical field
The utility model belongs to field of material technology, relates generally to a kind of low-temperature electrolytic extraction carbide refrigerator.
Background technique
In order to improve the mechanical property of steel and be allowed to obtain certain special physics, chemical property, can specially add Enter alloying elements, however some carbide in conjunction with alloying element can be precipitated during heat treatment, in steel.Carbide It is one of the important composition phase in steel, type, quantity, size, shape and the distribution of carbide have the performance of steel epochmaking It influences, therefore particularly important to the detection of carbide composition, quantity and size in steel.
The means of carbide mainly have scanning electron microscope method, transmission beam method and electrolytic extraction method in detection steel at present.First two side The deficiency of method is mainly to be in the surface observation of steel, when polishing steel sample surface, since carbide is too small, is easy to cause surface carbon Compound falls off, and influences detection and result.And electrolysis method can be very good such issues that avoid, electrolysis method can be by carbon tiny in steel Compound electrolytic extraction comes out, and detects for subsequent XRD, can carbide in analysis steel qualitatively and quantitatively.
Electrolytic extraction carbide commonly uses anhydrous alcohols electrolyte, and this kind of electrolyte is volatile when temperature is higher, while carbon Compound easily reacts with oxygen in the higher environment of temperature.Therefore electrolytic extraction carbide needs low temperature and oxygen-free environment, generally Carbide electrolysis temperature is no more than 5 DEG C.
Wherein, patent " a method of extract Super304H austenitic stainless steel in micro carbide " is at -5~5 DEG C It is electrolysed under electrolytic environments, but does not refer to cooling way.Patent " a kind of method of electroextraction and subtle field trash in detection steel " In order to obtain low-temperature electrolytic environment, then it is electrolysed in refrigerator, this causes electrolysis procedure inconvenient, and equipment is various.Above-mentioned electrolysis Method all have the shortcomings that one it is common, that is, to obtain none good approach of low temperature environment.
The technical issues of the utility model mainly solves in the presence of background technique passes through liquefied ammonia and manufactures Cryo Fundamentals, control Electrolyte in electrolytic cell processed is stablized in a low temperature environment less than 5 DEG C, and electrolyte is avoided to overheat in electrolytic process Volatilization and carbide are oxidized, to obtain purer carbide.
Utility model content
The purpose of the utility model is to overcome above-mentioned the shortcomings of the prior art, provide a kind of low-temperature electrolytic extraction carbonization Object refrigerator.
A kind of low-temperature electrolytic extraction carbide refrigerator, comprising: electrolytic cell, heat exchange slot, refrigeration unit, sealing unit and control Unit processed, in which:
The refrigeration unit includes refrigeration groove, cooling wall, water pump and insulating layer, wherein the cooling wall is wrapped in Outside the upper end of refrigeration groove, the cooling wall is connect with water pump, and the insulating layer is wrapped in outside the lower end of refrigeration groove;
Inside the electrolytic cell insertion heat exchange slot, inside the heat exchange slot insertion refrigeration groove, the electrolytic cell is changed Heat channel and refrigeration groove are close to;
The sealing unit includes sealing cover and relief valve, and the sealing cover is arranged above electrolytic cell, described Relief valve is arranged on sealing cover;
The control unit includes feedback controller and thermometer, the feedback controller respectively with water pump and temperature Meter connection.
The electrolytic cell is cylindrical opening container, and the heat exchange slot is U-shaped closed container, and the refrigeration groove is U-shaped closed container.
The recess position of the electrolytic cell insertion heat exchange slot, outer wall material is copper sheet.
The recess position of the heat exchange slot insertion refrigeration groove, outer wall material is copper sheet, and internal heat medium is thermal conductive silicon Rouge.
The refrigeration groove is U-shaped closed container, and outer wall material is copper sheet, and internal cavity is equipped with gas-liquid switching layer, described Gas-liquid switching layer by refrigeration groove be separated into up and down two parts, upper partial lumen be condensation chamber, lower part lumen loading liquefied ammonia, institute The gas-liquid switching layer stated is waveform, and wave crest is embedded in one layer of ventilated membrane, the ammonia of rising can be allowed to pass through, and trough is that hollow out is thin Pipe, can allow the liquefied ammonia of condensation to pass through, and material is low-temperature (low temperature) vessel steel.
The cooling wall is that circular copper pipe is wrapped in outside the upper end of refrigeration groove by way of spiral surrounding, cooling wall One water inlet and a water outlet are set, and the water inlet of cooling wall upper end and the water outlet of water pump connect, cooling wall lower end Water outlet is connect with pump intake.
The power of the water pump is controlled by feedback controller.
The sealing cover is provided with the through-hole of thermometer and conducting wire, pads one layer of rubber in through-hole, avoids air from temperature Gap between meter, conducting wire and sealing cover through-hole enters electrolytic cell.
The relief valve includes venthole, weight steelyard weight and bolt, and venthole is connect with sealing cover, is bolted weight steelyard weight With sealing cover, weight steelyard weight withstands on venthole upper end, moves up and down along the vertical direction.
The information input interface of the feedback controller is connect with thermometer, and information output interface is connect with water pump.
The thermometer is placed in electrolytic cell.
A kind of application method of low-temperature electrolytic extraction carbide refrigerator, comprising the following steps:
Step 1: injecting electrolyte into electrolytic cell, use thermometer measure electrolyte temperature;
Step 2: starting feedback controller, electrolyte temperature are automatically imported feedback controller;
Step 3: feedback controller exports feedback signal feed pump, water pump is according to signal output phase according to electrolyte temperature The cooling water inflow answered, cooling water are passed through cooling wall, cool down to cooling wall;
Step 4: the temperature of electrolyte is -10~5 DEG C, places electrolysis sample, covers sealing cover, electrolysis starts;
Step 5: electrolysis 5min unscrews the bolt on sealing cover, and weight steelyard weight moves up the gas that release electrolysis generates, then weighs Power stone roller decline, blocks venthole;
Step 6: electrolysis terminates, and closes power supply, feedback controller and water pump, takes out electrolytic cell, open under oxygen-free environment Sealing cover takes out residual electrolytic sample, pours out electrolyte, extracts for subsequent electrolysate.
In the step 3, the heat of ammonia, converts ammonia in the cooling wall exchange refrigeration groove top condensation chamber For low-temperature liquid ammonia, liquefied ammonia is dripped due to gravity along refrigeration groove inner wall, flows into system by the hollow out tubule of gas-liquid switching layer The lower lumen of cold trap;The liquefied ammonia of refrigeration groove lower lumen takes away the heat of heat exchange slot, is gasificated into ammonia, and ammonia rises, passes through The ventilated membrane of gas-liquid switching layer rises to the top condensate tank(trap) of refrigeration groove, by the reciprocal conversion of liquefied ammonia and ammonia, reaches refrigeration Effect.
In the step 5, the weight steelyard weight is the cap-shaped structure with quality, mating with venthole, it acts as Weight steelyard weight can be moved up and down with vertical direction, and electrolyte bath is since electrolytic process produces gas, so that the gas in electrolytic cell When pressure is greater than atmospheric pressure, weight steelyard weight, which is jacked up, to be moved up, and the gas in electrolytic cell is discharged by venthole, then under weight steelyard weight Drop, blocks gas outlet, and in electrolytic process, weight steelyard weight pumps, to guarantee in electrolytic cell in oxygen-free environment and pressure It is strong constant.
The utility model has the beneficial effects that
Low-temperature electrolytic provided by the utility model extracts carbide refrigerator, can be with the electrolyte in stability contorting electrolytic cell In -10~5 DEG C of low temperature environment, avoid electrolyte overheated in electrolytic process volatilization and carbide be oxidized, be electrolysed Efficiency improve 40~50%, the consumption of electrolyte reduces 20~30%, and the carbide degree of purity of electrolysis improves 25 ~35%.
Detailed description of the invention
Fig. 1 is that the low-temperature electrolytic of embodiment 1 extracts carbide refrigerator schematic diagram;
Fig. 2 is that the relief valve of embodiment 1 illustrates;
Fig. 3 is that the gas-liquid switching layer of embodiment 1 illustrates;
1- refrigeration groove, 2- cooling wall, 3- insulating layer, 4- water pump, 5- heat exchange slot, 6- feedback controller, 7- thermometer, 8- gas Liquid switching layer, 9- water inlet, 10- water outlet, 11- relief valve, 12- sealing cover, 13- ventilated membrane, 14- hollow out tubule, 15- gravity Stone roller, 16- venthole, 17- bolt, 18- electrolytic cell, 19- power supply.
Specific embodiment
Below with reference to embodiment, the utility model is described in further detail.
Embodiment 1
In conjunction with Fig. 1, a kind of low-temperature electrolytic extraction carbide refrigerator specifically includes that electrolytic cell 18, refrigeration groove 1, cooling wall 2, insulating layer 3, water pump 4, heat exchange slot 5, feedback controller 6, thermometer 7, relief valve 11, sealing cover 12, wherein relief valve 11 wraps Include weight steelyard weight 15 and bolt 17, specific structure diagram such as Fig. 2, wherein include gas-liquid heat exchange layer 8, gas-liquid heat exchange layer in refrigeration groove 1 Including ventilated membrane 13 and hollow out tubule 14, specific structure diagram such as Fig. 3.
A kind of application method of low-temperature electrolytic extraction carbide refrigerator: sealing cover 12 is opened, is injected into electrolytic cell 18 The electrolyte of 3/4 cell capacity, measuring electrolyte temperature using thermometer 7 is 20 DEG C;Start feedback controller 6, electrolyte 20 DEG C of temperature are automatically imported feedback controller 6;Water pump 4 exports cooling water inflow according to signal, and cooling water is passed through cooling wall 2, to cold But wall 2 is cooled down;Cooling wall 2 exchanges the heat of ammonia in 1 top condensation chamber of refrigeration groove, and ammonia is made to be converted into low-temperature liquid ammonia, 1 lower lumen of refrigeration groove is flowed into, the liquefied ammonia of 1 lower lumen of refrigeration groove takes away the heat of heat exchange slot 5, is gasificated into ammonia, on ammonia It is raised to the top condensate tank(trap) of refrigeration groove 1;When the temperature of electrolyte is stablized at 5 DEG C hereinafter, placing the electricity of 10 × 10 × 100mm size Desampling covers sealing cover 12, opens power supply 19, voltage and current is controlled respectively in 10.3V and 2.2A, electrolysis starts;Electrolysis 5min unscrews the bolt 17 on sealing cover 12, and weight steelyard weight 15 is moved up by jack-up, and the gas in electrolytic cell 18 passes through 16 row of venthole Out, then weight steelyard weight 15 declines, and blocks gas outlet;After 10h, electrolysis terminates, and takes out electrolytic cell 18, opens under oxygen-free environment close Envelope 12 takes out residual electrolytic sample, pours out electrolyte, extracts for subsequent electrolysate.
The electrolytic efficiency of low-temperature electrolytic extraction carbide refrigerator provided by the utility model improves 42%, electrolyte Consumption reduces 28%, and the carbide degree of purity of electrolysis improves 30%, substantially increases the accuracy of experimental result.

Claims (9)

1. a kind of low-temperature electrolytic extracts carbide refrigerator characterized by comprising electrolytic cell, heat exchange slot, refrigeration unit, close Seal unit and control unit, in which:
The refrigeration unit includes refrigeration groove, cooling wall, water pump and insulating layer, wherein the cooling wall is wrapped in refrigeration Outside the upper end of slot, the cooling wall is connect with water pump, and the insulating layer is wrapped in outside the lower end of refrigeration groove;
Inside the electrolytic cell insertion heat exchange slot, inside the heat exchange slot insertion refrigeration groove, the electrolytic cell, heat exchange slot It is close to refrigeration groove;
The sealing unit includes sealing cover and relief valve, and the sealing cover is arranged above electrolytic cell, the pressure release Valve is arranged on sealing cover;
The control unit includes feedback controller and thermometer, and the feedback controller connects with water pump and thermometer respectively It connects.
2. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the electrolytic cell is circle Cylindrical openings container, the heat exchange slot are U-shaped closed container, and the refrigeration groove is U-shaped closed container.
3. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the electrolytic cell insertion The recess position of heat exchange slot, outer wall material are copper sheet.
4. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the heat exchange slot insertion The recess position of refrigeration groove, outer wall material are copper sheet, and internal heat medium is heat-conducting silicone grease.
5. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the refrigeration groove is U Type closed container, outer wall material are copper sheet, and internal cavity is equipped with gas-liquid switching layer, and the gas-liquid switching layer separates refrigeration groove At upper and lower two parts, upper partial lumen is condensation chamber, and lower part lumen loading liquefied ammonia, the gas-liquid switching layer is waveform, Wave crest is embedded in one layer of ventilated membrane, and trough is hollow out tubule, and material is low-temperature (low temperature) vessel steel.
6. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the cooling wall is circle Shape copper pipe is wrapped in outside the upper end of refrigeration groove by way of spiral surrounding, and a water inlet and a water outlet is arranged in cooling wall Mouthful, the water inlet of cooling wall upper end and the water outlet of water pump connect, and the water outlet of cooling wall lower end is connect with pump intake.
7. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the sealing cover setting There is the through-hole of thermometer and conducting wire.
8. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the relief valve includes Venthole, weight steelyard weight and bolt, venthole are connect with sealing cover, are bolted weight steelyard weight and sealing cover, and weight steelyard weight withstands on outlet Hole upper end, moves up and down along the vertical direction.
9. low-temperature electrolytic according to claim 1 extracts carbide refrigerator, which is characterized in that the feedback controller Information input interface connect with thermometer, information output interface is connect with water pump;The thermometer is placed in electrolytic cell.
CN201822000974.6U 2018-11-30 2018-11-30 A kind of low-temperature electrolytic extraction carbide refrigerator Active CN209148589U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201822000974.6U CN209148589U (en) 2018-11-30 2018-11-30 A kind of low-temperature electrolytic extraction carbide refrigerator

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201822000974.6U CN209148589U (en) 2018-11-30 2018-11-30 A kind of low-temperature electrolytic extraction carbide refrigerator

Publications (1)

Publication Number Publication Date
CN209148589U true CN209148589U (en) 2019-07-23

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Country Status (1)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109254064A (en) * 2018-11-30 2019-01-22 东北大学 A kind of low-temperature electrolytic extraction carbide refrigerator and its application method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109254064A (en) * 2018-11-30 2019-01-22 东北大学 A kind of low-temperature electrolytic extraction carbide refrigerator and its application method
CN109254064B (en) * 2018-11-30 2023-09-26 东北大学 Low-temperature electrolytic extraction carbide refrigerator and application method thereof

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