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CN111850322A - Process and device for producing potassium metal - Google Patents

Process and device for producing potassium metal Download PDF

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Publication number
CN111850322A
CN111850322A CN202010760124.5A CN202010760124A CN111850322A CN 111850322 A CN111850322 A CN 111850322A CN 202010760124 A CN202010760124 A CN 202010760124A CN 111850322 A CN111850322 A CN 111850322A
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China
Prior art keywords
potassium
metal
sodium
rectifying tower
temperature
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CN202010760124.5A
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Chinese (zh)
Inventor
徐海峰
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Zibo Titan Electronic Technology Co Ltd
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Zibo Titan Electronic Technology Co Ltd
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Priority to CN202010760124.5A priority Critical patent/CN111850322A/en
Publication of CN111850322A publication Critical patent/CN111850322A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A production process and a device of metal potassium, belonging to the technical field of metal potassium production process. At present, the metal potassium is generally produced by taking metal sodium and potassium chloride as raw materials and performing reactive distillation by utilizing the difference of the boiling points of the metal potassium and the metal sodium, and the reaction equation is as follows: KCl + Na → K + NaCl, and it is widely believed that other low temperature manufacturing methods are not considered due to the temperature of potassium evaporation necessarily above 700 ℃. The reaction of metal sodium and potassium hydroxide is selected, the temperature required by the reaction is reduced, the method is that potassium steam in the tower top gas is accurately evaporated into the collecting pipeline through the cooperation of pressure, reaction temperature and the temperature of the top of the rectifying tower, and sodium steam flows back, so that the purpose of screening metal potassium is achieved, and the energy consumption and the equipment loss are obviously reduced.

Description

Process and device for producing potassium metal
Technical Field
A production process and a device of metal potassium, belonging to the technical field of metal potassium production process.
Background
The metal potassium is an active alkali metal and is mainly used in the fields of chemical oxygen generators, medical intermediates, electronic industry, potassium-sodium alloy and the like.
The production of the metal potassium generally adopts the metal sodium and the potassium chloride as raw materials, and the metal potassium and the metal sodium are produced by reaction and rectification by utilizing the difference of the boiling points of the metal potassium and the metal sodium, and the reaction equation is as follows: KCl + Na → K + NaCl. Because the melting point of potassium chloride is 772 ℃ and the melting point of sodium chloride is 808 ℃, the reaction needs to be carried out in a material molten state, the by-product sodium chloride needs to be kept in a molten state so as to be discharged, and the manufacturing temperature is often as high as 850 ℃. Therefore, the energy consumption is high, the service life of the equipment is short, and the reaction kettle needs to be replaced after about 4 months.
In the conventional concept, the boiling point of the potassium simple substance is 770 ℃, and in order to realize the distillation of the potassium simple substance after the metal potassium is replaced, the temperature of the whole reaction system is basically increased to the melting points of potassium chloride and sodium chloride, that is, the energy consumption is high and the equipment use period is short, so the current default of the whole industry is that the cost is required for the production of the metal potassium.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a process and a device for producing the metal potassium at low temperature and low energy consumption.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a production process of metal potassium is characterized in that: and simultaneously adding potassium hydroxide and sodium metal in a molten state into a reactor with the upper end being a rectifying tower according to the weight ratio of 2.5-3: 1, controlling the reaction temperature to be 380-420 ℃, controlling the pressure to be-60 to-80 kPa, and controlling the tower top temperature to be 340-360 ℃ by using a rectifying tower top heating wire and a rectifying tower top temperature sensor.
Rectifying the potassium metal obtained from the molten liquid to a receiver with a vacuum pump to be collected, and discharging and collecting the byproduct sodium hydroxide from a byproduct outlet at the lower part of the reactor after the potassium metal is not rectified.
Wherein, the sodium content in the metal sodium is not less than 99 percent; the content of potassium hydroxide is not less than 98%.
The chemical formula of the reaction is: KOH + Na → K + NaOH;
the invention greatly reduces the evaporation difficulty of the metal potassium by controlling the internal pressure of the reactor to be-60 to-80 kPa; then, a heating wire at the top of the rectifying tower is arranged at the top of the rectifying tower to control the temperature of the top of the rectifying tower to be 340-360 ℃, the top gas of the rectifying tower mainly comprises sodium vapor and potassium vapor, the potassium vapor is accurately controlled in the temperature range to accelerate distillation, the potassium vapor is forced to flow into a collecting pipeline, and the sodium vapor is left in the rectifying tower; meanwhile, the partial pressure of the potassium vapor is reduced, so that the potassium vapor from the reactor is promoted to continuously diffuse towards the top of the tower until the products in the receiver are not increased any more, and the reaction is finished.
Preferably, the reaction temperature is 400-420 ℃. If the content is too low, the potassium steam can not be evaporated; if the sodium content is too high, sodium can be evaporated too much, so that the purity of the product is influenced; while affecting the precise control of the overhead temperature.
Preferably, the tower top temperature is 345-355 ℃. If the concentration is too high, sodium vapor can be evaporated out, so that the purity is influenced; if the content is too low, the evaporation speed of potassium steam is slow, and the rectification efficiency is influenced.
Preferably, the pressure is-70 kPa. The lower the pressure, the greater the evaporation amount of sodium vapor, and the higher the pressure, the higher the temperature in the reactor needs to be, resulting in the temperature rise of the top gas of the column, the influence of the heating at the top of the column on the screening of the vapor is weakened, and the accurate control of the evaporation of the potassium vapor alone is difficult.
Preferably, the reactor is heated electrically. The efficiency is higher.
The utility model provides a potassium metal's apparatus for producing which characterized in that: comprises a reactor, a rectifying tower, a vacuum pump, a receiver, a heating wire at the top of the rectifying tower, a sodium melting tank, a potassium hydroxide melting tank and a temperature sensor at the top of the rectifying tower;
the sodium melting tank and the potassium hydroxide melting tank are converged into a main pipeline and then connected to the reactor, the rectifying tower is arranged above the reactor, a rectifying tower top heating wire and a rectifying tower top temperature sensor are arranged on the top of the rectifying tower, the top of the rectifying tower is connected to a receiver through a collecting pipeline, and a vacuum pump is arranged on the receiver.
Preferably, the heating wire at the top of the rectifying tower is coiled on the top of the rectifying tower for multiple circles. The heating area can be effectively enlarged by the multi-coil coiling mode, the steaming temperature of the potassium steam can be accurately controlled in a larger range, and the rectification efficiency is accelerated.
Compared with the prior art, the invention has the beneficial effects that: by utilizing the matching of the reaction pressure, the reaction temperature and the tower top temperature, the technical prejudice that the potassium metal can not be evaporated by the low-temperature reaction of potassium hydroxide and sodium in the traditional method is overcome, the production temperature of the potassium metal is reduced, and the energy consumption and the equipment loss are greatly reduced.
Drawings
FIG. 1 is a schematic view of a potassium metal production apparatus of the present application.
The system comprises a reactor 1, a rectifying tower 2, a vacuum pump 3, a receiver 4, a rectifying tower top heating wire 5, a sodium melting tank 6, a potassium hydroxide melting tank 7 and a rectifying tower top temperature sensor 8.
Detailed Description
Example 1 is the best embodiment of the present invention, and the present invention will be further described with reference to the following examples.
The following examples:
metal sodium: inner Mongolian orchid sodium industry, Inc.;
potassium hydroxide: inner Mongolia Ruidataifeng chemical company Limited liability.
The content of the performance test part is the purity of the metal potassium simple substance in the product metal potassium, and the operation method is as follows:
a dry evaporating dish, paraffin oil which can submerge the sample is put into the evaporating dish, and the sample is put into the evaporating dish; heating and melting completely by an electric furnace, inserting a thermometer, gradually cooling, stopping cooling when the temperature is reduced to a certain temperature, continuing to cool after two minutes, and obtaining the purity of the metal potassium by using a corresponding relation formula of the metal potassium melting point and the purity, wherein the temperature when the cooling is stopped is a metal potassium melting point:
the corresponding relation between the melting point and the purity of the metal potassium is as follows: k% = (0.259 t + 83.50)%;
wherein K% is the content of the metal potassium, and t is the melting point of the metal potassium.
Example 1
Referring to fig. 1: an apparatus for producing potassium metal, comprising: the device comprises a reactor 1, a rectifying tower 2, a rectifying tower top heating wire 5, a receiver 4, a sodium melting tank 6, a potassium hydroxide melting tank 7 and a rectifying tower top temperature sensor 8.
The sodium melting tank 6 and the potassium hydroxide melting tank 7 are connected to a main pipeline and then connected to the reactor 1, the rectifying tower 2 is arranged above the reactor 1, a rectifying tower top heating wire 5 and a rectifying tower top temperature sensor 8 are arranged on the top of the rectifying tower 2, the rectifying tower top heating wire 5 is coiled on the top of the rectifying tower 2, the rectifying tower top is connected to the receiver 4 through a collecting pipeline, and the receiver 4 is provided with the vacuum pump 3.
A production process of metal potassium; 500g of potassium hydroxide and 200g of metal sodium are respectively added into a potassium hydroxide melting tank 7 and a sodium melting tank 6 to be melted and then flow into a reactor 1, the reactor 1 is electrically heated to 410 ℃ in advance, and the pressure is set to-70 kPa; the heating temperature of the heating wire 5 at the top of the rectifying tower is set to be 350 ℃.
The rectified potassium steam enters a collecting pipe, flows into a receiver 4 after being cooled through the pipe wall, and is in balance with the pressure in the reactor 1, and the receiver 4 is provided with a vacuum pump 3 to keep the pressure the same as that in the reactor 1.
The temperature at the top of the tower is basically unchanged in the reaction process and is changed within the range of 345-355 ℃, and the set temperature of the heating wire 5 at the top of the rectifying tower does not need to be changed.
When the reaction proceeded for 120 hours, the weight of the receiver increased by less than 1g in 1 minute, and the reaction was completed. To obtain
The content of the metal potassium in the product is 331 g and 99.7 percent. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
Example 2
The pressure in the reactor was set at-60 kPa, the reaction temperature was set at 420 ℃ and the other conditions were the same as in example 1.
In the reaction process, the temperature of the tower top is measured and observed once every minute, and the heating of the tower top is closed for a plurality of times, so that the sodium vapor is prevented from flowing out after overtemperature.
When the reaction proceeded for 120 minutes, the weight of the receiver increased less than 1g in 1 minute, and the reaction was completed. The obtained product has 335 g of metal potassium and the content of 98.1 percent. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
Example 3
The reaction temperature was set at 380 ℃. The heating wire 5 at the top of the rectifying tower is set to be 360 ℃, and other conditions are the same as those of the embodiment 1.
When the reaction proceeded for 100 minutes, the weight of the receiver increased by less than 1g in 1 minute, and the reaction was completed. The obtained product has 326.5 g of metal potassium and the content of 98.1 percent. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
Example 4
The pressure in the reactor was set at-80 kPa, and the other conditions were the same as in example 3.
The temperature at the top of the tower is measured and observed once per minute in the reaction process, the variation range of the temperature at the top of the tower is controlled not to exceed 3 ℃, and the metal sodium is more sensitive to the temperature and is easier to evaporate.
When the reaction proceeded for 120 minutes, the weight of the receiver increased less than 1g in 1 minute, and the reaction was completed. The obtained product has 328.2 g of metal potassium and the content of 99.3 percent. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
Comparative example 1
The reaction pressure was set to-55 kPa, and the other conditions were the same as in example 2.
When the reaction proceeded for 140 minutes, the weight of the receiver increased less than 1g in 1 minute, and the reaction was completed. The obtained product has 325 g of metal potassium and the content of 90.2 percent. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
The purity of the potassium metal is too low. And the reaction time is too long, the energy consumption is increased, and the efficiency is low.
Comparative example 2
The reaction pressure was set to-85 kPa, the reaction temperature was set to 370 ℃ and the heating wire 5 at the top of the rectifying tower was set to 360 ℃ under the same conditions as in example 1.
The temperature at the top of the tower is accurately controlled to be 360 +/-3 ℃.
When the reaction proceeded for 140 minutes, the weight of the receiver increased less than 1g in 1 minute, and the reaction was completed. The obtained product has 335 g of metal potassium and the content of the metal potassium is 94.0 percent. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
Comparative example 3
The reaction pressure was set to-70 kPa, the reaction temperature was set to 370 ℃ and the heating wire 5 at the top of the rectifying column was set to 370 ℃ under the same conditions as in example 1.
The temperature at the top of the tower is accurately controlled to 370 +/-3 ℃.
When the reaction proceeded for 140 minutes, the weight of the receiver increased less than 1g in 1 minute, and the reaction was completed. The obtained product contains 340 g of metal potassium and 90.1 percent of metal potassium. The sodium hydroxide as a by-product is discharged from the lower part of the reactor 1 and collected.
When the reaction temperature is too high, the sodium vapor output can be increased even if the tower top temperature is reduced; when the reaction temperature is too low, the sodium evaporation amount can be increased and the potassium evaporation speed cannot be increased even if the tower top temperature is increased; when the reaction pressure is increased, the metal sodium is more sensitive to the evaporation temperature, the steam contents of potassium and sodium in the overhead gas are increased, and the sodium is easier to evaporate, so the requirement on the overhead temperature is more strict, and the product purity is greatly influenced.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (6)

1. A production process of metal potassium is characterized in that: adding potassium hydroxide and metal sodium into a reactor (1) respectively in a molten state according to a weight ratio of 2.5-3: 1, and controlling the reaction temperature to be 380-420 ℃ and the pressure to be-60-80 kPa;
rectifying the metal potassium obtained from the molten liquid by a rectifying tower (2) to a receiver (4) with a vacuum pump (3) to be collected, controlling the temperature at the top of the tower to be 340-360 ℃, and discharging and collecting a byproduct sodium hydroxide from an outlet at the lower part of the reactor after the metal potassium is not rectified in the reactor (1);
wherein, the sodium content in the metal sodium is more than 99 percent;
the purity of the potassium hydroxide is not less than 98%.
2. The process for producing potassium metal according to claim 1, wherein: the reaction temperature is 400-420 ℃.
3. The process for producing potassium metal according to claim 1, wherein: the tower top temperature is 345-355 ℃.
4. The process for producing potassium metal according to claim 1, wherein: the pressure is-70 kPa.
5. A production apparatus for a potassium metal production process according to claim 1, characterized in that: comprises a reactor (1), a rectifying tower (2), a vacuum pump (3), a receiver (4), a rectifying tower top heating wire (5), a sodium melting tank (6), a potassium hydroxide melting tank (7) and a rectifying tower top temperature sensor (8);
the sodium melting tank (6) and the potassium hydroxide melting tank (7) are connected to a main pipeline and then connected to the reactor (1), the rectifying tower (2) is arranged above the reactor (1), a rectifying tower top heating wire (5) and a rectifying tower top temperature sensor (8) are arranged on the top of the rectifying tower (2), the top of the rectifying tower (2) is connected to the receiver (4) through a collecting pipeline, and the vacuum pump (3) is arranged on the receiver (4).
6. The production device according to claim 5, wherein: the rectifying tower top heating wire (5) is coiled on the top of the rectifying tower (2) for a plurality of circles.
CN202010760124.5A 2020-07-31 2020-07-31 Process and device for producing potassium metal Pending CN111850322A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115805044A (en) * 2023-01-31 2023-03-17 昌邑荣信化工有限公司 Quantitative feeding equipment is used in potassium metal production

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1311228A (en) * 1961-09-22 1962-12-07 Penarroya Miniere Metall Manufacturing process of lead, potassium and sodium alloys
NL7009290A (en) * 1969-06-25 1970-12-29
WO2009141672A1 (en) * 2008-05-20 2009-11-26 La Perla Srl Method for manufacturing caustic soda or potash and hydrochloric acid, and apparatus therefor
CN110423887A (en) * 2019-07-24 2019-11-08 山东习尚喜新材料科技股份有限公司 A kind of device and technique using potassium hydroxide continuous treatment old metal sodium
CN210420095U (en) * 2019-07-24 2020-04-28 山东习尚喜新材料科技股份有限公司 Utilize potassium hydroxide serialization to handle device of useless metal sodium

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1311228A (en) * 1961-09-22 1962-12-07 Penarroya Miniere Metall Manufacturing process of lead, potassium and sodium alloys
NL7009290A (en) * 1969-06-25 1970-12-29
WO2009141672A1 (en) * 2008-05-20 2009-11-26 La Perla Srl Method for manufacturing caustic soda or potash and hydrochloric acid, and apparatus therefor
CN110423887A (en) * 2019-07-24 2019-11-08 山东习尚喜新材料科技股份有限公司 A kind of device and technique using potassium hydroxide continuous treatment old metal sodium
CN210420095U (en) * 2019-07-24 2020-04-28 山东习尚喜新材料科技股份有限公司 Utilize potassium hydroxide serialization to handle device of useless metal sodium

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115805044A (en) * 2023-01-31 2023-03-17 昌邑荣信化工有限公司 Quantitative feeding equipment is used in potassium metal production

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