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CN208577766U - A kind of continuous production device of metallic potassium - Google Patents

A kind of continuous production device of metallic potassium Download PDF

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Publication number
CN208577766U
CN208577766U CN201820858808.7U CN201820858808U CN208577766U CN 208577766 U CN208577766 U CN 208577766U CN 201820858808 U CN201820858808 U CN 201820858808U CN 208577766 U CN208577766 U CN 208577766U
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China
Prior art keywords
tank
potassium
metallic
condenser
sodium
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CN201820858808.7U
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Inventor
刘湛
刘林学
郝光顺
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Shandong Xi Shangxi New Material Science And Technology Co Ltd
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Shandong Xi Shangxi New Material Science And Technology Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The utility model discloses a kind of continuous production devices of metallic potassium, including reactor, the reactor includes pipe reaction cylinder, conveyor screw is installed in pipe reaction cylinder, is provided in the pipe reaction cylinder and is sequentially connected logical feed stage, preheating section, conversion zone and heat preservation and slags tap section;The described feeder setting is in feed stage, and the rectifying mechanism is arranged in conversion zone, and the receiving mechanism is connected with rectifying mechanism, and the recovering mechanism of slagging tap is arranged slags tap section in heat preservation;The rectifying mechanism includes rectifying column, and rectifier bottoms are provided with the vapor-liquid separation changeover portion being connected with conversion zone, are provided with the first condenser at the top of rectifying column, the bottom of the first condenser is connected with receiving mechanism.It is small to completely eliminate all security risks, equipment investment in production process by quantity-produced technique using potassium chloride, metallic sodium as initial feed using continuous reaction apparatus for the device of the utility model.

Description

A kind of continuous production device of metallic potassium
Technical field
The utility model belongs to chemical field, is related to the production of metallic potassium, and in particular to a kind of continuous production of metallic potassium Device.
Background technique
Metallic potassium and its derived product be chemical industry, space flight, underwater kit oxygen supply, unsafe condition oxygen supply save oneself, the neck such as pharmacy The highly useful raw material in domain.Synthetic method about metallic potassium industrialized can only have a kind of potassium chloride metallic sodium high temperature to set at present Change reaction method.This method reaction condition is harsher, is the reaction temperature for needing 850 DEG C or so first, at these temperatures The material of reactor is required it is relatively high, should high temperature resistant also want corrosion-resistant, equipment input cost is relatively high;Since displacement is reacted It is that reversible reaction will guarantee that the conversion ratio of reaction must under vacuum constantly separate the potassium of generation from system distillation, this is just Need to solve vacuum-packed problem;Due under high temperature metallic potassium, sodium all with oxygen, nitrogen vigorous reaction, this requires system anoxybiotic, Exhausted nitrogen simultaneously carries out under protection of argon gas, this also needs to solve the problems, such as sealing;Since the fusing point of potassium chloride is 770 DEG C, potassium Boiling point is 774 DEG C, and the temperature of reaction necessarily is greater than this temperature, and the potassium generated is very easy to be dissolved in potassium chloride and be not easy Escape, this just needs enough temperature, enough disengagement areas and enough stirring intensities just to can guarantee that reaction constantly carries out, The disengagement area heat transfer problem for increasing reactor is just exposed, and increasing stirring intensity can solve under heat transfer problem but high temperature Stirring vacuum sealing problem can not solve so far, in addition, the reaction is exothermic reaction, the temperature of reaction is controlled after reacting and starting As soon as being a problem again, the excessively high sodium to lead out of temperature is more, and side reaction is also more, and temperature reduces is very easy to occur " stiff pot " now again As causing entirely to react failure, significant loss;Since potassium remaining in byproduct of reaction, sodium have the post-processing of byproduct of reaction Then major safety risks pass through essence so the prior art is all first to be steamed out the potassium of generation and unreacted sodium together again It evaporates to separate again and generates pure potassium, which again increases production costs and equipment investment.
Be designed to small reactor based on the above technical bottleneck prior art, without stirring intermittently operated, in this way heat transfer with The problem of sealing is all right to be solved, but the conversion ratio reacted is not high, reaction it is inefficient, production capacity can not improve, and need every time Will displaced air repeatedly, need to consume a large amount of argon gas, it is often more important that security risk is relatively more, and maximum security risk is When reaction residue is a kind of containing metallic sodium, the potassium chloride of potassium, common salt mixture after reaction, it is necessary under protection of argon gas Reaction mixture is transferred in another container, is then cooled down again, mixture this so just becomes a kind of bulk cannot It directly releases from container, container can only be moved on to otherwise and be dissolved out mixture therein with a large amount of water, this When be very easy to detonation occur, be unable to control, even and if safety disposition to also bigger (the mainly water of the corrosion of equipment The corrosion of system chloride ion), also easily-deformable reuse factor is low for equipment, while it is dilute molten to generate a large amount of chloride containing potassium, common salt Liquid waste water dis posal cost is relatively high.This is also the main reason for metallic potassium cannot be mass produced both at home and abroad, is at high cost.
Therefore, how to eliminate safe hidden trouble, reduce cost, solve Mixing Machine sealing problem, reduce energy consumption, reduce dirt Dye, large-scale production are the problem that metallic potassium and potassium utilize field enterprises pay attention and research all the time.
Summary of the invention
In view of the deficienciess of the prior art, the purpose of the utility model is to provide a kind of continuous productions of metallic potassium Device realizes the serialization large-scale production of metallic potassium preparation process, solves peace present in existing metallic potassium production process It is conflicting between full hidden danger and production efficiency, it is difficult to the technical issues of having both.
In order to solve the above-mentioned technical problem, the utility model adopts the following technical solution is achieved:
A kind of continuous production device of metallic potassium, including reactor further include feeder, rectifying mechanism, receiving mechanism With recovering mechanism of slagging tap;
The reactor includes pipe reaction cylinder, and conveyor screw is equipped in pipe reaction cylinder, and the tubular type is anti- It answers to be provided in cylinder and is sequentially connected logical feed stage, preheating section, conversion zone and heat preservation and slags tap section;The feeder setting In feed stage, the rectifying mechanism is arranged in conversion zone, and the receiving mechanism is connected with rectifying mechanism, and described slags tap back Mechanism setting is received to slag tap section in heat preservation;
The rectifying mechanism includes rectifying column, and rectifier bottoms are provided with the vapor-liquid separation transition being connected with conversion zone Section, rectifying column top are provided with the first condenser, and the bottom of the first condenser is connected with receiving mechanism.
The utility model also has following technical characteristic:
The feeder includes closed potassium chloride temporary storage tank and potassium chloride continuous feed meter, and potassium chloride is temporary It is connected at the top of the bottom of tank and potassium chloride continuous feed meter, the bottom of potassium chloride continuous feed meter and feed stage It is connected;
It further include closed metallic sodium temporary storage tank and metallic sodium continuous feed meter, bottom and the gold of metallic sodium temporary storage tank Belong to and being connected at the top of sodium continuous feed meter, the bottom of metallic sodium continuous feed meter is connected with feed stage;
Bag filter, bag type filtering are provided in the potassium chloride temporary storage tank and potassium chloride continuous feed meter Device is connected with the first vacuum gas-guide tube;The potassium chloride temporary storage tank and potassium chloride continuous feed meter also with the first argon Gas gas source pipe is connected;
The metallic sodium temporary storage tank and metallic sodium continuous feed meter is connected with the second vacuum gas-guide tube;Described Metallic sodium temporary storage tank and metallic sodium continuous feed meter are also connected with the second argon gas gas source pipe;
Potassium chloride temporary storage tank, potassium chloride continuous feed meter, metallic sodium temporary storage tank and the metallic sodium continuous feed Weighing module is provided on meter.
The bottom of the potassium chloride continuous feed meter and the bottom of metallic sodium continuous feed meter are first and double Screw mixer is connected, and twin-screw mixing procedure device is connected with feed stage again.
Heating insulation layer is provided on the outer wall of the metallic sodium temporary storage tank and metallic sodium continuous feed meter.
Phegma deflector, the bottom of phegma deflector are additionally provided in the vapor-liquid separation changeover portion of the rectifying mechanism End is obliquely installed towards conversion zone close to one end of preheating section.
The receiving mechanism includes the receiver that the first condenser bottom is arranged in, the top of receiver and the second condenser Portion is connected, and is connected at the top of the bottom of the second condenser and receiving tank;The bottom of receiving tank and the top of third condenser It is connected, the bottom of third condenser is connected with packaging supply unit;
The top of second condenser is also communicated with one end of U-shaped return pipe, the other end of U-shaped return pipe and installation Backflow distributor at the top of rectifying column is connected;
The receiving tank is connected with third argon gas gas source pipe;
The receiving tank is also connected with third vacuum gas-guide tube, and third vacuum gas-guide tube is connected with vacuum buffer tank Logical, vacuum buffer tank is connected with the 4th vacuum gas-guide tube;
The vacuum buffer tank is also connected at the top of the first condenser.
The recovering mechanism of slagging tap includes the one end of heat preservation residue outlet that section is connected of slagging tap with heat preservation, keeps the temperature residue outlet The other end with condensation scraping blade tank top be connected, condensation scraping blade tank bottom end and the feed inlet phase of the first spiral pusher cooler Connection, the discharge port of the first spiral pusher cooler are connected with the feed inlet of the second spiral pusher cooler, and the second spiral pushes away Expect that the discharge port of cooler is connected with remaining potassium sodium removal tank;
Coldplate is installed in the condensation scraping blade tank, rotatable revolving scraper is installed below coldplate, is rotated The solid for being set in coldplate bottom can be scraped slabbing and removed from coldplate by scraper;
The condensation scraping blade tank is connected with the 4th argon gas gas source pipe, and the condensation scraping blade tank is also led with the 5th vacuum Tracheae is connected;
The first identical, described spiral of the structure of the first spiral pusher cooler and the second spiral pusher cooler Pusher cooler includes tubular type cooling cylinder, is equipped with pushing spiral body in tubular type cooling cartridge body, tubular type cooling cartridge is arranged in vitro There is cooling collet;
The remaining potassium sodium removal tank includes tank body, and cooling jacket is provided on the outer wall of tank body, is equipped in tank body Agitating paddle, top of the tank are equipped with the 4th condenser that circulation cooling circuit can be formed with tank body, the bottom of the 4th condenser Fixed gas blow-down pipe is installed, tank base is connected with sodium chloride and potassium chloride separation and recovery system;
The top of the remaining potassium sodium removal tank is connected with Nitrogen source gases pipe, the top of the remaining potassium sodium removal tank Portion is also added pipe with raw alcohol and is connected.
The utility model compared with prior art, has the following technical effect that
The device of the utility model using potassium chloride, metallic sodium as initial feed, passes through quantity-produced technique when in use All security risks in production process are completely eliminated, equipment investment is small, and production process is easily controllable, high production efficiency, production At low cost, process no longer generates waste water and solid waste, and technical process is simple, is very easy to industrially promotion and implementation, has operation Simply, environmental-friendly, the characteristics of production safety, low energy consumption, it will push metallic potassium industry that revolutionary progress occurs.The device It can be realized the serialization large-scale production of metallic potassium preparation process, the equipment safety hidden danger is low, high production efficiency.
Detailed description of the invention
Fig. 1 is the overall structure diagram of the utility model.
Fig. 2 is the structural schematic diagram of the feeder of the utility model.
Fig. 3 is the structural schematic diagram of the receiving mechanism of the utility model.
Fig. 4 is the structural schematic diagram of the recovering mechanism of slagging tap of the utility model.
The meaning of each label in figure are as follows: 1- reactor, 2- feeder, 3- rectifying mechanism, 4- receiving mechanism, 5- slag tap Recovering mechanism;
11- pipe reaction cylinder, 12- conveyor screw, 13- feed stage, 14- preheating section, 15- conversion zone, 16- heat preservation are slagged tap Section;
21- potassium chloride temporary storage tank, 22- potassium chloride continuous feed meter, 23- metallic sodium temporary storage tank, 24- metallic sodium connect Continuous feed gauge, 25- bag filter, 26- the first vacuum gas-guide tube, 27- the first argon gas gas source pipe, the second vacuum of 28- are led Tracheae, 29- twin-screw mixing procedure device, 210- heating insulation layer, 211- Weighing module, 212- the second argon gas gas source pipe;
31- rectifying column, 32- vapor-liquid separation changeover portion, the first condenser of 33-, 34- phegma deflector;
41- receiver, the second condenser of 42-, 43- receiving tank, 44- third condenser, 45- pack supply unit, 46-U Shape return pipe, 47- third argon gas gas source pipe, 48- third vacuum gas-guide tube, 49- vacuum buffer tank, the 4th vacuum air guide of 410- Pipe, 411- backflow distributor;
51- keeps the temperature residue outlet, and 52- condenses scraping blade tank, 53- the first spiral pusher cooler, the cooling of the second spiral pusher of 54- Device, 55- remnants' potassium sodium remove tank, 56- coldplate, 57- revolving scraper, the 4th argon gas gas source pipe of 58-, the 5th vacuum air guide of 59- Pipe, the 4th condenser of 510-, 511- fixed gas blow-down pipe, 512- sodium chloride and potassium chloride separation and recovery system, 513- Nitrogen source gases Pipe is added in pipe, 514- raw alcohol;531- tubular type cooling cylinder, 532- pushing spiral body, 533- cooling collet;551- tank body, 552- cooling jacket, 553- agitating paddle.
Explanation is further explained in detail to the particular content of the utility model with reference to embodiments.
Specific embodiment
Specific embodiment of the utility model is given below, it should be noted that the utility model is not limited to following tool Body embodiment, all equivalent transformations made on the basis of the technical solutions of the present application each fall within the protection scope of the utility model.
Embodiment 1:
In compliance with the above technical solution, as shown in Figures 1 to 4, the present embodiment provides a kind of continuous production device of metallic potassium, It further include feeder 2, rectifying mechanism 3, receiving mechanism 4 and recovering mechanism 5 of slagging tap including reactor 1;
Reactor 1 includes pipe reaction cylinder 11, is equipped with conveyor screw 12, pipe reaction cylinder in pipe reaction cylinder 11 It is provided in 11 and is sequentially connected logical feed stage 13, preheating section 14, conversion zone 15 and heat preservation and slags tap section 16;Feeder 2 is arranged In feed stage 13, rectifying mechanism 3 is arranged in conversion zone 15, and receiving mechanism 4 is connected with rectifying mechanism 3, recovering mechanism 5 of slagging tap setting It slags tap section 16 in heat preservation;
Rectifying mechanism 3 includes rectifying column 31, and 31 bottom of rectifying column is provided with the vapor-liquid separation mistake being connected with conversion zone 15 Section 32 is crossed, the first condenser 33 is provided at the top of rectifying column 31, the bottom of the first condenser 33 is connected with receiving mechanism 4.
Specifically, feeder 2 includes closed potassium chloride temporary storage tank 21 and potassium chloride continuous feed meter 22, chlorination The bottom of potassium temporary storage tank 21 is connected with the top of potassium chloride continuous feed meter 22, potassium chloride continuous feed meter 22 Bottom is connected with feed stage 13;
It further include closed metallic sodium temporary storage tank 23 and metallic sodium continuous feed meter 24, the bottom of metallic sodium temporary storage tank 23 Portion is connected with the top of metallic sodium continuous feed meter 24, the bottom of metallic sodium continuous feed meter 24 and feed stage 13 It is connected;
Bag filter 25, pocket type mistake are provided in potassium chloride temporary storage tank 21 and potassium chloride continuous feed meter 22 Filter 25 is connected with the first vacuum gas-guide tube 26;
Bag filter 25, bag type filtering are provided in potassium chloride temporary storage tank 21 and potassium chloride continuous feed meter 22 Device 25 is connected with the first vacuum gas-guide tube 26;The potassium chloride temporary storage tank 21 and potassium chloride continuous feed meter 22 is also equal It is connected with the first argon gas gas source pipe 27;
Metallic sodium temporary storage tank 23 and metallic sodium continuous feed meter 24 are connected with the second vacuum gas-guide tube 28;Described Metallic sodium temporary storage tank 23 and metallic sodium continuous feed meter 24 are also connected with the second argon gas gas source pipe 212;
Potassium chloride temporary storage tank 21, potassium chloride continuous feed meter 22, metallic sodium temporary storage tank 23 and metallic sodium continuous feed Weighing module 211 is provided on meter 24.
As a kind of preferred embodiment of the present embodiment, the bottom of potassium chloride continuous feed meter 22 and metallic sodium continuously into Expect that the bottom of meter 24 is first connected with twin-screw mixing procedure device 29, twin-screw mixing procedure device 29 is connected with feed stage 13 again.
As a kind of preferred embodiment of the present embodiment, metallic sodium temporary storage tank 23 and metallic sodium continuous feed meter 24 it is outer Heating insulation layer 210 is provided on wall.
As a kind of preferred embodiment of the present embodiment, phegma is additionally provided in the vapor-liquid separation changeover portion 32 of rectifying mechanism The bottom end of deflector 34, phegma deflector 34 is obliquely installed towards conversion zone 15 close to one end of preheating section 14.
Specifically, receiving mechanism 4 includes the receiver 41 that 33 bottom of the first condenser is arranged in, receiver 41 and second The top of condenser 42 is connected, and the bottom of the second condenser 42 is connected with the top of receiving tank 43;The bottom of receiving tank 43 It is connected with the top of third condenser 44, the bottom of third condenser 44 is connected with packaging supply unit 45;
The top of second condenser 42 is also communicated with one end of U-shaped return pipe 46, the other end of U-shaped return pipe 46 and installation Backflow distributor 411 at 31 top of rectifying column is connected;
Receiving tank 43 is connected with third argon gas gas source pipe 47;
Receiving tank 43 is also connected with third vacuum gas-guide tube 48, and third vacuum gas-guide tube 48 is connected with vacuum buffer tank 49 Logical, vacuum buffer tank 49 is connected with the 4th vacuum gas-guide tube 410;
Vacuum buffer tank 49 is also connected with the top of the first condenser 33.
Packaging supply unit 45 in the present embodiment is using conventional packaging conveying system.
Specifically, recovering mechanism 5 of slagging tap includes the one end of heat preservation residue outlet 51 that section 16 is connected of slagging tap with heat preservation, heat preservation The other end of residue outlet 51 is connected with the top of condensation scraping blade tank 52, and the bottom end and the first spiral pusher for condensing scraping blade tank 52 drop The feed inlet of warm device 53 is connected, the discharge port of the first spiral pusher cooler 53 and the second spiral pusher cooler 54 into Material mouth is connected, and the discharge port of the second spiral pusher cooler 54 is connected with remaining potassium sodium removal tank 55;
Coldplate 56 is installed in condensation scraping blade tank 52, rotatable revolving scraper 57 is installed below coldplate 56, is revolved Turn scraper 57 and the solid for being set in 56 bottom of coldplate can be scraped slabbing to remove from coldplate 56;
Condensation scraping blade tank 52 be connected with the 4th argon gas gas source pipe 58, condense scraping blade tank 52 also with the 5th vacuum gas-guide tube 59 It is connected;
First spiral pusher cooler 53 is identical with the structure of the second spiral pusher cooler 54, the cooling of the first spiral pusher Device 53 includes tubular type cooling cylinder 531, and pushing spiral body 532, tubular type cooling cylinder 531 are equipped in tubular type cooling cylinder 531 It is provided with cooling collet 533 outside;
Remaining potassium sodium removal tank 55 includes tank body 551, is provided with cooling jacket 552, tank body 551 on the outer wall of tank body 551 Agitating paddle 553 is inside installed, the 4th condenser that can form circulation cooling circuit with tank body 551 is installed at the top of tank body 551 510, the bottom of the 4th condenser 510 is equipped with fixed gas blow-down pipe 511, and 551 bottom of tank body separates back with sodium chloride and potassium chloride Receipts system 512 is connected;
The top of remaining potassium sodium removal tank 55 is connected with Nitrogen source gases pipe 513, and the top of remaining potassium sodium removal tank 55 is also Pipe 514 is added with raw alcohol to be connected.
As the preferred embodiment of the present embodiment, reactor 1, the first spiral pusher cooler 53 and the cooling of the second spiral pusher There is heat-insulated cooling section in the both ends machinery rotary seal part of device 54.
In the present embodiment, sodium chloride and potassium chloride separation and recovery system 512 is using conventional sodium chloride and potassium chloride separation and recovery System.
The device of the present embodiment uses continuous reaction apparatus, and material distills while reacting in conversion zone, passes through rectifying Tower separates the metallic potassium of generation and unreacted sodium, and the metallic potassium of generation is condensed into receiving mechanism, received metallic potassium warp It cools down again and keeps liquid condition continuous discharge, molding, encapsulation.Before unreacted metallic sodium returns to tubular reactor conversion zone End.Unreacted potassium chloride and the sodium chloride mixture of generation enter section of vertically slagging tap through level section outflow of slagging tap, and overcome vacuum The scraper for being frozen into solid through distributing device continuous discharge to cooler under normal pressure afterwards, while being rotated is scraped from cooler with sheet Under, the sodium chloride and potassium chloride mixture of sheet are cooled within 60 DEG C through multiple coil stuff pulling cooling unit, then fall into falling property gas The remaining potassium sodium removal tank of body protection makes the metallic potassium wherein contained, metallic sodium react generation sodium alkoxide and alcohol with the alcohol being pre-placed Potassium, mixture are delivered to finishing plant again, decompose sodium alkoxide, potassium alcoholate with hydrochloric acid, then separate alcohol return system and apply, isolate Potassium chloride return system is applied, and the sodium chloride isolated is at by-product sale.
Embodiment 2:
The present embodiment provides a kind of continuous production processes of metallic potassium, which is characterized in that the technique is used such as 1 institute of embodiment The continuous production device for the metallic potassium stated realizes the continuous production of metallic potassium.
The device of the present embodiment is using automatic control and manual both of which.
In the device of the present embodiment, heated part gasket winds flexible graphite sealing pad using 310S.
In the device of the present embodiment, rectifying column uses screen waviness packings, and material 310S, the number of plates of rectifying column is 15 Between~100.
In the device of the present embodiment, the internal diameter of pipe reaction cylinder 11 is 300~1000mm, and 14 length of preheating section is 2000~5000mm, 15 length of conversion zone are 2000~6000mm, keep the temperature the 16 1000~2000mm of length of section that slags tap, keep the temperature out The internal diameter of slag pipe 51 is 50~300mm, and the length of heat preservation residue outlet 51 is greater than 5000mm.
This method specifically includes the following steps:
Step 1, the first vacuum gas-guide tube 26, the second vacuum gas-guide tube 28, the 4th vacuum gas-guide tube 410 and the 5th vacuum Vacuum system of the gas-guide tube 59 with pressure no more than -0.095MPa is connected;First argon gas gas source pipe 27, the second argon gas gas source pipe 212, third argon gas gas source pipe 47 and the 4th argon gas gas source pipe 58 are connected with argon system;Nitrogen source gases pipe 513 and nitrogen system It is connected;
Vacuum system, argon system and nitrogen system are the conventional base system of enterprise;
All terminal valves connecting with normal pressure system for closing the continuous production device of metallic potassium, vacuumize, then cut Disconnected vacuum system inputs argon gas to normal pressure to the continuous production device of metallic potassium, then is vacuumized by vacuum system, then use argon gas Displacement, 3~5 times repeatedly, being finally evacuated to pressure is
- 0.095Mpa or less;
Step 2 closes 21 bottom valve of potassium chloride temporary storage tank and presses raw material potassium chloride vacuum suck potassium chloride temporary storage tank 21 According to step 1 method carry out repeatedly vacuumize-argon gas replacement operator, for removing nitrogen and oxygen, with argon gas formed protect Atmosphere simultaneously makes potassium chloride temporary storage tank 21 keep micro-positive pressure relative to atmospheric pressure by argon gas;
23 bottom valve of metallic sodium temporary storage tank is closed, metallic sodium pressure sodium machine is pressed into metallic sodium temporary storage tank 23, is formed with argon gas Protective atmosphere simultaneously makes metallic sodium temporary storage tank 23 keep micro-positive pressure relative to atmospheric pressure by argon gas;
By the vacuum suck potassium chloride continuous feed meter 22 of the potassium chloride in potassium chloride temporary storage tank 21, then by raw material chlorine Change potassium vacuum suck potassium chloride temporary storage tank 21 is simultaneously spare under protection of argon gas;
By the vacuum suck metallic sodium continuous feed meter 24 of the molten metal sodium in metallic sodium temporary storage tank 23, then will Raw metal sodium pressure sodium machine indentation metallic sodium temporary storage tank 23 is simultaneously spare under protection of argon gas;
Metallic sodium temporary storage tank 23 and the heat preservation of metallic sodium continuous feed meter 24 are at 110 DEG C;
Potassium chloride raw material and metal sodium raw materials are (1.05~3.0) by step 3 in molar ratio: 1 be added reactor 1 to Expect that section 13, the temperature of the preheating section 14 of reactor 1 are maintained at 300~770 DEG C, the temperature of conversion zone 15 is maintained at 770~850 DEG C, raw material carries out rectifying by rectifying mechanism 3 while conversion zone 15 reacts, and distillate starts infinite reflux, until metallic potassium closes It is received again after lattice;
Receiving tank 43 is connected with packaging supply unit 45, controls and receives 43 bottom valve of tank to packaging discharge port pipeline drop and is greater than 1160mm, this is highly enough that vacuum is overcome to use metallic potassium with liquid condition continuous discharge, on continuous baling line under normal pressure Argon gas protection molding, and encapsulated with white oil;
In distillation process, high-temperature molten salt coolant liquid, third condenser 44 are used in the first condenser 33, the second condenser 42 Using conduction oil coolant liquid, controlling cooling temperature makes received metallic potassium be maintained at liquid condition;
During continuous feed unreacted potassium chloride and chlorine can be continuously discharged by keeping the temperature section 16 of slagging tap in reactor 1 By-product is received in change;
The by-product of step 4, step 3 discharge is entered in condensation scraping blade tank 52 by heat preservation residue outlet 51, drops down onto cooling It is frozen into solid when plate 56, while solid being scraped by revolving scraper 57 and falls to tank bottom, drops down onto the slag of tank bottom through the first spiral Pusher cooler 53 and the second spiral pusher cooler 54 are cooled within 60 DEG C, then fall into nitrogen protection be previously added raw material In the remaining potassium sodium removal tank 55 of alcohol;
The metallic potassium and metallic sodium and raw alcohol immediate response contained in slag charge is gone at raw sodium alkoxide and potassium alcoholate in remaining potassium sodium Except obtained mixture is delivered to sodium chloride and potassium chloride separation and recovery system 512 again after reacting in tank 55, with hydrochloric acid decompose sodium alkoxide, Potassium alcoholate, then separate alcohol return system and apply, the potassium chloride return system isolated is applied, and the sodium chloride isolated is at byproduct pin It sells.
High-temperature molten salt is used in the cooling collet 553 of first spiral pusher cooler 53 and the second spiral pusher cooler 54 Coolant liquid;
Cooling water is used in the cooling jacket 552 of remaining potassium sodium removal tank 55.
As a kind of preferred embodiment of the present embodiment, potassium chloride is pure potassium chloride or is 1%~50% chlorine containing mass content Change the potassium chloride of sodium.
As a kind of preferred embodiment of the present embodiment, device material therefor is resistance to potassium chloride, sodium chloride, metallic sodium, metal The metal material of potassium, reactor, rectifying column, discharger are heat resisting steel, preferably 310S heat resisting steel.
As a kind of preferred embodiment of the present embodiment, heating method is induction heating or infrared heating in electric heating.
As a kind of preferred embodiment of the present embodiment, the ingredient of high-temperature molten salt coolant liquid is 43% based on parts by weight NaNO2, 7% NaNO3, 50% KNO3.The operating temperature of high-temperature molten salt coolant liquid is at 200~450 DEG C.Conduction oil coolant liquid Operating temperature in room temperature~400 DEG C.

Claims (7)

1. a kind of continuous production device of metallic potassium, including reactor (1), which is characterized in that further include feeder (2), essence Evaporate mechanism (3), receiving mechanism (4) and recovering mechanism of slagging tap (5);
The reactor (1) includes pipe reaction cylinder (11), is equipped with conveyor screw (12), institute in pipe reaction cylinder (11) It is provided in the pipe reaction cylinder (11) stated and is sequentially connected logical feed stage (13), preheating section (14), conversion zone (15) and protects Temperature slags tap section (16);In feed stage (13), the rectifying mechanism (3) is arranged in conversion zone for feeder (2) setting (15), the receiving mechanism (4) is connected with rectifying mechanism (3), and described recovering mechanism of slagging tap (5) setting is slagged tap section in heat preservation (16);
The rectifying mechanism (3) includes rectifying column (31), and rectifying column (31) bottom is provided with to be connected with conversion zone (15) Vapor-liquid separation changeover portion (32) is provided with the first condenser (33) at the top of rectifying column (31), the bottom of the first condenser (33) with Receiving mechanism (4) is connected.
2. the continuous production device of metallic potassium as described in claim 1, which is characterized in that the feeder (2) includes Closed potassium chloride temporary storage tank (21) and potassium chloride continuous feed meter (22), the bottom of potassium chloride temporary storage tank (21) and chlorination It is connected at the top of potassium continuous feed meter (22), bottom and feed stage (13) phase of potassium chloride continuous feed meter (22) Connection;
It further include closed metallic sodium temporary storage tank (23) and metallic sodium continuous feed meter (24), metallic sodium temporary storage tank (23) Be connected at the top of bottom and metallic sodium continuous feed meter (24), the bottom of metallic sodium continuous feed meter (24) with give Material section (13) is connected;
Bag filter (25) are provided in the potassium chloride temporary storage tank (21) and potassium chloride continuous feed meter (22), Bag filter (25) is connected with the first vacuum gas-guide tube (26);The potassium chloride temporary storage tank (21) and potassium chloride continuously into Material meter (22) is also connected with the first argon gas gas source pipe (27);
The metallic sodium temporary storage tank (23) and metallic sodium continuous feed meter (24) is connected with the second vacuum gas-guide tube (28) It is logical;The metallic sodium temporary storage tank (23) and metallic sodium continuous feed meter (24) also with the second argon gas gas source pipe (212) It is connected;
Potassium chloride temporary storage tank (21), potassium chloride continuous feed meter (22), metallic sodium temporary storage tank (23) and the metallic sodium Weighing module (211) are provided on continuous feed meter (24).
3. the continuous production device of metallic potassium as claimed in claim 2, which is characterized in that the potassium chloride continuous feed meter The bottom of measuring device (22) and the bottom of metallic sodium continuous feed meter (24) are first connected with twin-screw mixing procedure device (29), double Screw mixer (29) is connected with feed stage (13) again.
4. the continuous production device of metallic potassium as claimed in claim 2, which is characterized in that the metallic sodium temporary storage tank (23) Heating insulation layer (210) are provided with on the outer wall of metallic sodium continuous feed meter (24).
5. the continuous production device of metallic potassium as described in claim 1, which is characterized in that the vapour-liquid of the rectifying mechanism point From being additionally provided with phegma deflector (34) in changeover portion (32), the bottom end of phegma deflector (34) is leaned on towards conversion zone (15) One end of nearly preheating section (14) is obliquely installed.
6. the continuous production device of metallic potassium as described in claim 1, which is characterized in that the receiving mechanism (4) includes Receiver (41) in the first condenser (33) bottom is set, is connected at the top of receiver (41) and the second condenser (42), It is connected at the top of the bottom of second condenser (42) and receiving tank (43);The bottom and third condenser (44) of receiving tank (43) Top be connected, the bottom of third condenser (44) is connected with packaging supply unit (45);
The top of second condenser (42) is also communicated with one end of U-shaped return pipe (46), U-shaped return pipe (46) it is another It holds and is connected with the backflow distributor (411) being mounted at the top of rectifying column (31);
The receiving tank (43) is connected with third argon gas gas source pipe (47);
The receiving tank (43) is also connected with third vacuum gas-guide tube (48), third vacuum gas-guide tube (48) and vacuum buffer Tank (49) is connected, and vacuum buffer tank (49) is connected with the 4th vacuum gas-guide tube (410);
The vacuum buffer tank (49) is also connected at the top of the first condenser (33).
7. the continuous production device of metallic potassium as described in claim 1, which is characterized in that the recovering mechanism of slagging tap (5) One end including the heat preservation residue outlet (51) that section (16) is connected of slagging tap with heat preservation keeps the temperature the other end and the condensation of residue outlet (51) The top of scraping blade tank (52) is connected, and the bottom end of condensation scraping blade tank (52) is connected with the feed inlet of the first spiral pusher cooler (53) Logical, the discharge port of the first spiral pusher cooler (53) is connected with the feed inlet of the second spiral pusher cooler (54), and second The discharge port of spiral pusher cooler (54) is connected with remaining potassium sodium removal tank (55);
It is equipped with coldplate (56) in the condensation scraping blade tank (52), rotatable rotation is installed below coldplate (56) and is scraped The solid for being set in coldplate (56) bottom can be scraped slabbing and removed from coldplate (56) by knife (57), revolving scraper (57);
The condensation scraping blade tank (52) is connected with the 4th argon gas gas source pipe (58), and the condensation scraping blade tank (52) is also with Five vacuum gas-guide tubes (59) are connected;
The first spiral pusher cooler (53) is identical with the structure of the second spiral pusher cooler (54), and described first Spiral pusher cooler (53) includes tubular type cooling cylinder (531), is equipped with pushing spiral body in tubular type cooling cylinder (531) (532), cooling collet (533) is provided with outside tubular type cooling cylinder (531);
Remaining potassium sodium removal tank (55) includes tank body (551), is provided with cooling jacket on the outer wall of tank body (551) (552), it is equipped with agitating paddle (553) in tank body (551), circulation can be formed with tank body (551) by being equipped at the top of tank body (551) 4th condenser (510) of cooling circuit, the bottom of the 4th condenser (510) are equipped with fixed gas blow-down pipe (511), tank body (551) bottom is connected with sodium chloride and potassium chloride separation and recovery system (512);
The top of remaining potassium sodium removal tank (55) is connected with Nitrogen source gases pipe (513), the remaining potassium sodium removal The top of tank (55) is also added pipe (514) with raw alcohol and is connected.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950208A (en) * 2018-06-04 2018-12-07 山东习尚喜新材料科技股份有限公司 A kind of continuous production device and technique of metallic potassium
CN112358408A (en) * 2020-11-30 2021-02-12 江苏凯美普瑞工程技术有限公司 Production process and device of glycine

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950208A (en) * 2018-06-04 2018-12-07 山东习尚喜新材料科技股份有限公司 A kind of continuous production device and technique of metallic potassium
CN108950208B (en) * 2018-06-04 2023-09-29 山东习尚喜新材料科技股份有限公司 Continuous production device and process of metal potassium
CN112358408A (en) * 2020-11-30 2021-02-12 江苏凯美普瑞工程技术有限公司 Production process and device of glycine

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