CN111249761A - Molten salt distillation purification method and equipment - Google Patents

Molten salt distillation purification method and equipment Download PDF

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Publication number
CN111249761A
CN111249761A CN202010143955.8A CN202010143955A CN111249761A CN 111249761 A CN111249761 A CN 111249761A CN 202010143955 A CN202010143955 A CN 202010143955A CN 111249761 A CN111249761 A CN 111249761A
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molten salt
distillation
condenser
equipment
evaporator
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CN111249761B (en
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窦强
付海英
耿俊霞
罗艳
许璐
李晴暖
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Shanghai Institute of Applied Physics of CAS
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Shanghai Institute of Applied Physics of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/10Vacuum distillation
    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21CNUCLEAR REACTORS
    • G21C3/00Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
    • G21C3/42Selection of substances for use as reactor fuel
    • G21C3/44Fluid or fluent reactor fuel
    • G21C3/54Fused salt, oxide or hydroxide compositions
    • 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
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

Abstract

The invention discloses a method and equipment for distilling and purifying molten salt. The equipment comprises: the system comprises a molten salt storage device, a molten salt distillation device, a molten salt collecting device, a molten salt conveying pipeline and a molten salt collecting pipeline; the molten salt storage equipment comprises a sealed cavity, an air inlet flow meter, pressure measuring equipment, heating equipment and a molten salt lifting barrel; the molten salt distillation equipment comprises a sealed distillation cavity, an evaporator, an electric heater and a condenser; the evaporator, the electric heater and the condenser are all arranged in the sealed distillation cavity; the evaporator, the condenser and the exhaust pipe are connected in sequence. The device uses the equipment, adopts the air pressure difference method to convey the molten salt, and can accurately control the molten salt conveying speed and the molten salt evaporation speed. The method adopts a reduced pressure distillation method to separate and purify the molten salt, realizes effective removal of the hard-to-volatilize impurities in the molten salt, has simple process operation, can improve the purification efficiency of the molten salt, realizes high impurity removal rate, has no by-product, has low energy consumption and can realize continuous distillation.

Description

Molten salt distillation purification method and equipment
Technical Field
The invention relates to a molten salt purification technology, belongs to high-temperature distillation and refining and purification technologies, and particularly relates to a molten salt distillation purification method and equipment.
Background
Molten Salt Reactors (MSR) are a reactor system using liquid fuel, known as a breeder reactor with a better thorium-uranium cycle, whose fuel salt is a high temperature villaumite, which produces a large number of fission products during the operation of the reactor, most of which, especially rare earth, alkaline earth and alkali metal fission products, dissolve in the fuel salt, and the continuous accumulation of fission products in the fuel salt seriously affects the neutron economy in the reactor. Therefore, it is necessary to periodically treat the fuel salt to separate fission products and recover expensive carrier salt, thereby improving the operating efficiency of the reactor and reducing the cost.
In the prior art, the fission product in the carrier molten salt and the purification and recovery of the carrier salt can be realized by adopting a molten salt distillation technology. However, when the technology is used for molten salt purification, for example, patent CN106621429B, the equipment needs to be stopped, and the feeding of molten salt or the collection of purified molten salt is performed. In addition, at present, the feeding of the molten salt is generally to directly add the molten salt to the highest temperature part of the distiller, and the temperature is increased again after the temperature is reduced for each feeding, so that the time and the power are wasted, the production efficiency is low, the continuous production cannot be realized, and the service life of evaporator materials can be damaged due to frequent temperature rise and fall. Therefore, the existing process has the defects of difficult continuous treatment, low purification production efficiency, complex equipment operation and the like, and the process requirements of effectively recovering carrier salt and removing fission products in the fuel treatment process of the molten salt reactor are difficult to meet.
Disclosure of Invention
The invention provides a method and equipment for distilling and purifying molten salt, aiming at overcoming the defects of difficult continuous treatment, low purification efficiency, complex process flow and the like of the existing molten salt separation technology. The method provided by the invention has the advantages that the purification and recovery of the molten salt, effective removal of impurities and no by-product are ensured, meanwhile, the continuous distillation is realized, the purification efficiency of the molten salt is improved, the equipment operation is simplified, and the cost is reduced.
The present invention solves the above technical problems by the following technical solutions.
The invention provides a molten salt distillation and purification device which is characterized by comprising a molten salt storage device, a molten salt distillation device, a molten salt collection device, a molten salt conveying pipeline and a molten salt collection pipeline;
the molten salt storage equipment comprises a first sealed cavity, an air inlet flow meter, pressure measuring equipment, heating equipment and a first molten salt pail; the first molten salt lifting bucket and the heating equipment are both arranged inside the first sealed cavity; the heating equipment is used for heating the first molten salt lifting barrel; the first sealed cavity is provided with an air inlet, a first exhaust port and a first outlet; the intake flowmeter is arranged at the end part of the air inlet; the pressure measuring equipment is arranged on the outer wall of the first sealed cavity and used for measuring the pressure in the first sealed cavity;
the molten salt distillation equipment comprises a sealed distillation cavity, an evaporator, a first electric heater, a second electric heater and a condenser; the sealed distillation cavity is provided with a first inlet, a second outlet, a second exhaust port and an exhaust pipe; the evaporator, the first electric heater, the second electric heater and the condenser are all arranged in the sealed distillation cavity; the evaporator, the condenser and the exhaust pipe are connected in sequence; one end of the exhaust pipe opposite to the condenser extends to the outside of the molten salt distillation equipment through a second exhaust port of the sealed distillation cavity; the first electric heater is used for heating the evaporator; the second electric heater is used for heating the condenser;
the molten salt collecting device comprises a second sealed cavity; the second sealed cavity further comprises a second inlet;
one end of the molten salt conveying pipeline extends to the bottom of the first molten salt lifting barrel through a first outlet of the first sealed cavity, and the other end of the molten salt conveying pipeline extends to the evaporator through a first inlet of the sealed distillation cavity;
one end of the molten salt collecting pipeline extends to the bottom of the condenser through a second outlet of the sealed distillation cavity, and the other end of the molten salt collecting pipeline extends to the inside of the second sealed cavity through a second inlet of the second sealed cavity.
In the present invention, the molten salt treated by the molten salt distillation apparatus is a molten salt capable of obtaining a molten state (i.e., a molten salt having a decomposition temperature higher than a boiling point temperature), such as a fluoride molten salt and/or a chloride molten salt. Preferably, the working state of the molten salt in the molten salt distillation equipment is liquid state and gaseous state.
In the invention, the molten salt storage equipment is conventional molten salt storage equipment in the field. In the molten salt storage equipment, adjusting the internal air pressure of the molten salt storage equipment to form an air pressure difference between the inside of the molten salt storage equipment and the inside of the molten salt distillation equipment, conveying the molten salt in the molten salt storage equipment to the evaporator, and controlling the molten salt conveying speed by monitoring the air inlet flow meter and the pressure measurement equipment, thereby realizing uniform and quantitative feeding of the molten salt.
Preferably, the molten salt storage equipment further comprises a first weighing unit; the first weighing unit is arranged in the first sealed cavity. Preferably, the first molten salt pail is connected with the first weighing unit arranged above the first molten salt pail through a first hanger rod.
Preferably, the air inlet is connected with an external air supply system, and the first exhaust port is connected with an external vacuum system.
Preferably, the gas supply system is used for introducing inert gas into the molten salt storage equipment. The inert gas is a gas that does not react with the material during the use of the device, and is not limited to the rare gas conventionally referred to, and may be, for example, nitrogen.
Preferably, a plurality of infrared reflecting layers are arranged inside the first sealed cavity; the first weighing unit is arranged above the infrared reflecting layer, and the first molten salt pail is arranged below the infrared reflecting layer. The infrared reflecting layer is used for blocking heat radiation of high-temperature molten salt in the first molten salt pail.
Preferably, the plurality of infrared reflecting layers are attached to the inner wall of the side surface of the first sealed cavity; the infrared reflecting layers are further sleeved on the first hanging rod.
Preferably, a first vacuum protection cover is additionally arranged at the top of the first sealed cavity, and the first weighing unit is placed in the first vacuum protection cover.
Preferably, the pressure measuring equipment can measure the internal pressure of the whole first seal cavity at any time, so that the internal pressure can be adjusted more accurately, and the pressure difference between the inside of the first seal cavity and the inside of the molten salt distillation equipment is kept at 10 DEG3-105Pa。
Preferably, the molten salt storage equipment is further provided with a thermocouple for measuring the temperature of the molten salt in the first sealed cavity.
In the invention, under a vacuum environment, the evaporator in the molten salt distillation equipment is heated to the evaporation temperature of molten salt to generate molten salt steam; and condensing the molten salt steam in the condenser to form liquid molten salt, and collecting.
Preferably, the evaporator, the condenser and the exhaust pipe are connected in sequence to form an inner-layer sealing structure.
Preferably, the evaporator comprises an evaporation body, and an evaporation surface of the evaporation body is in a step shape and used for increasing the surface area of the molten salt distillation treatment and improving the efficiency of the molten salt distillation treatment.
Preferably, at least one ceramic protective bracket is sleeved outside the evaporator, and the first heater surrounds the protective bracket.
Preferably, the second electric heater surrounds the condenser.
Preferably, at least one thermocouple is arranged in the evaporator.
Preferably, the condenser comprises a plurality of baffles; the partition plate is arranged in the condenser and divides the condenser into a plurality of condensing parts; the area of the baffle is smaller than the cross section of the condenser.
Preferably, the gaps are formed between the partition plates and the condenser, and the positions of the gaps between the adjacent partition plates are opposite, so that the gas channel with the S-shaped trend is formed in the condenser.
Preferably, through holes are formed in one end, close to the bottom of the condenser, of the partition plate connected with the bottom of the condenser. When the purified molten salt is collected through the molten salt collecting pipeline, the liquid molten salt condensed in the condensing parts can be converged to the molten salt collecting pipeline opening through the through holes.
More preferably, the plurality of partition plates are disposed in parallel with each other inside the condenser.
Preferably, at least one thermocouple is arranged in the condenser.
Preferably, the second exhaust port is connected to an external vacuum system.
In the invention, the molten salt collecting device is a conventional molten salt collecting device in the field.
Preferably, the molten salt collecting device further comprises a second weighing unit and a second molten salt pail, and the second weighing unit and the second molten salt pail are both arranged inside the second sealed cavity; the second molten salt lifting bucket is connected with the second weighing unit arranged above the second molten salt lifting bucket through a second suspender; the second molten salt pail is used for collecting the purified molten salt.
Preferably, the capacity of the first molten salt pail is equal to the capacity of the second molten salt pail.
Preferably, a second vacuum protection cover is additionally arranged at the top of the second sealed cavity, and the second weighing unit is placed in the second vacuum protection cover.
Preferably, the outer wall of the second seal cavity is provided with a water cooling jacket.
Preferably, the other end of the molten salt delivery conduit extends through the first inlet of the sealed distillation chamber to an end of the evaporator opposite the condenser.
Preferably, the molten salt collecting device further comprises a third exhaust port, and the third exhaust port can be used for adjusting the air pressure of the molten salt collecting device.
In a preferred embodiment, the molten salt collecting apparatus further comprises a sampling port.
In a preferred embodiment, in order to realize online sampling and monitor the composition and purity change of the liquid molten salt in real time, the purpose of separating and purifying the molten salt is achieved, and the molten salt distillation and purification equipment further comprises an online sampler; the online sampler is connected with a sampling port of the molten salt collecting device.
Wherein the in-line sampler is conventional in the art.
The invention also provides a molten salt distillation and purification method, which applies the molten salt distillation and purification equipment and specifically comprises the following steps:
s1, adjusting the internal air pressure of the molten salt storage equipment to enable the inside of the molten salt storage equipment and the inside of the molten salt distillation equipment to form an air pressure difference, and conveying the molten salt in the molten salt storage equipment to the evaporator;
s2, heating the evaporator to the evaporation temperature of molten salt in the molten salt distillation equipment under a vacuum environment to generate molten salt steam; and condensing the molten salt steam in the condenser to form liquid molten salt, and collecting by using the molten salt collecting equipment.
According to the invention, the internal air pressure of the molten salt storage equipment is adjusted to form an air pressure difference between the inside of the molten salt storage equipment and the inside of the molten salt distillation equipment, the molten salt in the molten salt storage equipment is conveyed to the evaporator, and the molten salt conveying speed is controlled by monitoring the air inlet flow meter and the pressure measuring equipment, wherein the molten salt conveying speed can be a stable and uniform conveying speed or a pulse conveying speed. And simultaneously controlling the vacuum degree in the molten salt distillation equipment and the heating temperature of the evaporator to realize continuous treatment of molten salt distillation.
Preferably, the molten salt evaporation rate of step S2 is a uniform rate.
More preferably, the molten salt delivery rate in step S1 is equal to the molten salt evaporation rate in step S2.
Preferably, the vacuum degree in the molten salt evaporation equipment is 1-1000 Pa.
Wherein, the evaporation temperature of the molten salt is known to those skilled in the art, and the evaporation temperature of the specific molten salt has a direct relationship with the kind of the specific treated molten salt, and is preferably 300-1300 ℃.
For example, when the molten salt is a fluoride molten salt, the evaporation temperature of the molten salt is 500-. For another example, when the molten salt is a chloride molten salt, the evaporation temperature of the molten salt is 300-. For another example, when the molten salt is FLiNaK, the evaporation temperature of the molten salt is 900-1100 ℃.
Wherein, the condensation temperature of the fused salt steam is known to those skilled in the art, and the specific condensation temperature has a direct relation with the specific treated fused salt type. Preferably, the condensation temperature of the molten salt steam is 80-120 ℃ lower than the evaporation temperature of the molten salt, but the condensation temperature of the molten salt steam must be at least 50 ℃ higher than the melting point of the molten salt.
In the invention, in order to realize online sampling and monitor the composition and the purity change of the liquid molten salt in real time to achieve the aim of separating and purifying the molten salt, an online sampler can be arranged at a sampling port of the molten salt collecting equipment for real-time monitoring.
In the present invention, the above-mentioned preferred conditions can be arbitrarily combined on the basis of common knowledge in the field, so as to obtain each preferred embodiment of the present invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
the invention adopts the air pressure difference method to convey the molten salt and can accurately control the molten salt conveying speed and the molten salt evaporation speed. The method adopts a reduced pressure distillation method to separate and purify the molten salt, realizes effective removal of the hard-to-volatilize impurities in the molten salt, has simple process operation, can improve the purification efficiency of the molten salt, realizes high impurity removal rate, has no by-product, has low energy consumption and can realize continuous distillation.
In a preferred embodiment, the molten salt delivery rate and the molten salt evaporation rate are controlled to be equal, and continuous and stable production is realized. An evaporator and a condenser in the molten salt distillation equipment respectively adopt a step-shaped evaporation surface and an S-shaped gas channel, so that the distillation treatment efficiency is improved. And the purified molten salt can be sampled on line, the composition change of the molten salt can be mastered in real time, and the quality control is realized.
The method can realize that the average impurity removal rate in the molten salt material reaches more than 99 percent and the continuous distillation recovery rate of the molten salt can reach more than 95 percent.
Drawings
Fig. 1 is a schematic structural view of a molten salt distillation purification apparatus of example 1.
Fig. 2 is a schematic structural view of the molten salt storage apparatus of embodiment 1.
Description of the reference numerals
Molten salt storage facility 100
Molten salt distillation apparatus 200
Molten salt collecting apparatus 300
Fused salt delivery conduit 400
Fused salt collecting pipe 500
First sealed chamber 101
Heating device 102
First molten salt pail 103
Air inlet 104
First exhaust port 105
First outlet 106
Pressure measurement device interface 107
First weighing cell 108
First boom 109
Infrared reflecting layer 110
First vacuum protection cover 111
Sealed distillation chamber 201
Evaporator 202
First electric heater 203
Second electric heater 204
Condenser 205
First inlet 206
Second outlet 207
Second exhaust port 208
Exhaust pipe 209
Evaporator 210
Protective bracket 211
Partition 212
Notch 213
Second sealed cavity 301
Second inlet 302
Second weighing cell 303
Second molten salt pail 304
Second boom 305
Second vacuum protection cover 306
Water cooling jacket 307
Sampling port 308
In-line sampler 309
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The present invention will be more clearly and completely described below with reference to the accompanying drawings.
Example 1
The invention provides a molten salt distillation and purification device, which comprises a molten salt storage device 100, a molten salt distillation device 200, a molten salt collecting device 300, a molten salt conveying pipeline 400 and a molten salt collecting pipeline 500, as shown in figures 1-2.
The molten salt storage device 100 comprises a first sealed cavity 101, an air inlet flow meter, a pressure measuring device, a heating device 102 and a first molten salt pail 103; the first molten salt pail 103 and the heating device 102 are both arranged inside the first sealed cavity 101; the heating device 102 is used for heating the first molten salt lifting barrel 103; the first sealed chamber 101 is provided with an air inlet 104, a first air outlet 105 and a first outlet 106; the air inlet flow meter is arranged at the end part of the air inlet 104; the pressure measuring device is disposed on the outer wall of the first sealed chamber 101 through a pressure measuring device interface 107, and is used for measuring the pressure in the first sealed chamber 101.
The molten salt distillation equipment 200 comprises a sealed distillation cavity 201, an evaporator 202, a first electric heater 203, a second electric heater 204 and a condenser 205; the sealed distillation chamber 201 is provided with a first inlet 206, a second outlet 207, a second exhaust port 208 and an exhaust pipe 209; the evaporator 202, the first electric heater 203, the second electric heater 204 and the condenser 205 are all arranged in the sealed distillation cavity 201; the evaporator 202, the condenser 205 and the exhaust pipe 209 are connected in sequence; one end of the exhaust pipe 209 opposite to the condenser 205 extends to the outside of the molten salt distillation apparatus 200 through the second exhaust port 208 of the sealed distillation cavity 201; the first electric heater 203 is used for heating the evaporator 202; the second electric heater 204 is used to heat the condenser 205.
The molten salt collecting device 300 comprises a second sealed cavity 301; the second sealed housing 301 also includes a second inlet 302.
One end of the molten salt delivery pipe 400 extends to the bottom of the first molten salt pail 103 through the first outlet 106 of the first sealed cavity 101, and the other end extends to the evaporator 202 through the first inlet 206 of the sealed distillation cavity 201.
One end of the molten salt collecting pipe 500 extends to the bottom of the condenser 205 through the second outlet 207 of the sealed distillation cavity 201, and the other end extends to the inside of the second sealed cavity 301 through the second inlet 302 of the second sealed cavity 301.
The working state of the molten salt in the molten salt distillation apparatus 200 is liquid and gas.
In the molten salt storage equipment 100, the internal air pressure of the molten salt storage equipment 100 is adjusted to form an air pressure difference between the inside of the molten salt storage equipment 100 and the inside of the molten salt distillation equipment 200, molten salt in the molten salt storage equipment 100 is conveyed to the evaporator 202, and the molten salt conveying speed is controlled by monitoring the air inlet flow meter and the pressure measurement equipment, so that uniform and quantitative feeding of the molten salt is realized.
The molten salt storage facility 100 further comprises a first weighing unit 108; the first weighing unit 108 is disposed inside the first hermetically sealed chamber 101. Preferably, the first molten salt pail 103 is connected to a first weighing unit 108 disposed above the first molten salt pail 103 by a first hanger rod 109.
The air inlet 104 is connected to an external air supply system, and the first exhaust 105 is connected to an external vacuum system.
The gas supply system is used for introducing nitrogen into the molten salt storage device 100.
A plurality of infrared reflecting layers 110 are arranged in the first sealed cavity 101; the first weighing unit 108 is arranged above the infrared reflecting layer 110, and the first molten salt pail 103 is arranged below the infrared reflecting layer 110. The infrared reflecting layer 110 is used for blocking heat radiation of high-temperature molten salt in the first molten salt pail 103.
The plurality of infrared reflecting layers 110 are attached to the inner wall of the side surface of the first sealed cavity 101; a plurality of infrared reflective layers 110 are also provided around the first hanger bar 109.
A first vacuum protection cover 111 is additionally arranged on the top of the first sealed cavity 101, and the first weighing unit 108 is placed inside the first vacuum protection cover 111.
The pressure measuring equipment can measure the internal pressure of the whole first seal cavity 101 at any time, so that the internal pressure can be adjusted more accurately, and the pressure difference between the inside of the first seal cavity 101 and the inside of the fused salt distillation equipment 200 is kept at 10 DEG3-105Pa。
The molten salt storage apparatus 100 is also provided with a thermocouple for measuring the temperature of the molten salt inside the first capsule 101.
Heating an evaporator 202 in the molten salt distillation apparatus 200 to the evaporation temperature of the molten salt in a vacuum environment to generate molten salt steam; the molten salt vapor is condensed in the condenser 205 to form a liquid molten salt, which is collected.
The evaporator 202, the condenser 205 and the exhaust pipe 209 are connected in sequence to form an inner-layer sealing structure.
The evaporator 202 comprises an evaporator body 210, and the evaporation surface of the evaporator body 210 is in a step shape and is used for increasing the surface area of the molten salt distillation treatment and improving the efficiency of the molten salt distillation treatment.
At least one ceramic protective bracket 211 is sleeved outside the evaporator 202, and the first heater is surrounded on the protective bracket 211.
The second electric heater 204 surrounds the condenser 205.
At least one thermocouple is disposed within the evaporator 202.
The condenser 205 comprises a plurality of baffles 212; a partition 212 disposed inside the condenser 205 and dividing the condenser 205 into a plurality of condensing portions; the area of the partition 212 is smaller than the cross-section of the condenser 205. The notches 213 formed between the partitions 212 and the condenser 205 are opposite in position to the notches 213 between adjacent partitions 212, and form gas passages in the condenser 205 in an "S" shape.
The partition 212 connected to the bottom of the condenser 205 has through holes at one end thereof near the bottom of the condenser 205. When the purified molten salt is collected through the molten salt collecting pipeline 500, the liquid molten salt condensed in the plurality of condensing parts can be converged to the opening of the molten salt collecting pipeline 500 through the through hole.
A plurality of baffles 212 are disposed in parallel with each other inside the condenser 205.
At least one thermocouple is disposed within the condenser 205.
The second exhaust port 208 is connected to an external vacuum system.
The molten salt collecting device 300 further comprises a second weighing unit 303 and a second molten salt pail 304, wherein the second weighing unit 303 and the second molten salt pail 304 are both arranged inside the second sealed cavity 301; the second molten salt pail 304 is connected with a second weighing unit 303 arranged above the second molten salt pail 304 through a second hanger rod 305; the second molten salt pail 304 is used to collect the purified molten salt.
The capacity of the first molten salt pail 103 is equal to the capacity of the second molten salt pail 304.
A second vacuum protection cover 306 is additionally arranged on the top of the second sealed cavity 301, and the second weighing unit 303 is placed inside the second vacuum protection cover 306.
The outer wall of the second sealed cavity 301 is provided with a water cooling jacket 307.
The other end of the molten salt delivery conduit 400 extends into the evaporator 202 through the first inlet 206 of the sealed distillation chamber 201 opposite the end of the condenser 205.
A molten salt collection apparatus 300 also includes a sampling port 308.
In order to realize online sampling and monitor the composition and purity change of liquid molten salt in real time, and achieve the purpose of separating and purifying the molten salt, the molten salt distillation and purification equipment further comprises an online sampler 309; the in-line sampler 309 is connected to a sampling port 308 of the molten salt collecting apparatus 300.
The invention also provides a molten salt distillation and purification method, which applies the molten salt distillation and purification equipment and specifically comprises the following steps:
s1, adjusting the internal air pressure of the molten salt storage equipment 100 to enable the inside of the molten salt storage equipment 100 and the inside of the molten salt distillation equipment 200 to form an air pressure difference, and conveying the molten salt in the molten salt storage equipment 100 to an evaporator 202; wherein, the intake air flow meter and the pressure measuring device are respectively used for measuring and controlling the air pressure inside the molten salt storage device 100;
s2, heating the evaporator 202 to the evaporation temperature of the molten salt in the molten salt distillation equipment 200 in a vacuum environment to generate molten salt steam; the molten salt vapor is condensed in the condenser 205 to form a liquid molten salt, which is collected using the molten salt collection apparatus 300.
By adjusting the internal air pressure of the molten salt storage device 100, an air pressure difference is formed between the inside of the molten salt storage device 100 and the inside of the molten salt distillation device 200, molten salt in the molten salt storage device 100 is conveyed to the evaporator 202, the molten salt conveying speed is controlled by monitoring the air inlet flow meter and the pressure measuring device, and meanwhile, the vacuum degree in the molten salt distillation device 200 and the heating temperature of the evaporator 202 are controlled, so that the continuous treatment of molten salt distillation is realized.
The molten salt evaporation rate of step S2 is a uniform rate. The molten salt conveyance rate in step S1 is equal to the molten salt evaporation rate in step S2.
In order to realize online sampling and monitor the composition and purity change of the liquid molten salt in real time to achieve the purpose of separating and purifying the molten salt, an online sampler 309 can be arranged at a sampling port 308 of the molten salt collecting device 300 for real-time monitoring.
In the embodiment, the outer diameter of the molten salt storage equipment reaches 60cm, and the height of the molten salt storage equipment is about 180 cm; the outer diameter of the fused salt distillation equipment reaches 80cm, the length of the fused salt distillation equipment is about 230cm, and the fused salt distillation equipment is a horizontal distillation device. The operating parameters for using the apparatus are listed in table 1. When the device is used for molten salt purification treatment, the treatment capacity can reach 8 kg/h, and the daily treatment capacity can reach 192 kg/day. As will be appreciated by those skilled in the art upon reading the teachings of the present invention, the daily throughput is multiplied if the device size is increased.
Table 1 operating parameters of example 1
Figure BDA0002400070010000121
Figure BDA0002400070010000131
The above-mentioned preferred conditions can be arbitrarily combined on the basis of the common knowledge in the field, so as to obtain the preferred embodiments of the invention.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and scope of the invention, and these changes and modifications are within the scope of the invention.

Claims (10)

1. A fused salt distillation and purification device is characterized by comprising a fused salt storage device, a fused salt distillation device, a fused salt collecting device, a fused salt conveying pipeline and a fused salt collecting pipeline;
the molten salt storage equipment comprises a first sealed cavity, an air inlet flow meter, pressure measuring equipment, heating equipment and a first molten salt pail; the first molten salt lifting bucket and the heating equipment are both arranged inside the first sealed cavity; the heating equipment is used for heating the first molten salt lifting barrel; the first sealed cavity is provided with an air inlet, a first exhaust port and a first outlet; the air inlet flowmeter is arranged at the end part of the air inlet; the pressure measuring equipment is arranged on the outer wall of the first sealed cavity and used for measuring the pressure in the first sealed cavity;
the molten salt distillation equipment comprises a sealed distillation cavity, an evaporator, a first electric heater, a second electric heater and a condenser; the sealed distillation cavity is provided with a first inlet, a second outlet, a second exhaust port and an exhaust pipe; the evaporator, the first electric heater, the second electric heater and the condenser are all arranged in the sealed distillation cavity; the evaporator, the condenser and the exhaust pipe are connected in sequence; one end of the exhaust pipe opposite to the condenser extends to the outside of the molten salt distillation equipment through a second exhaust port of the sealed distillation cavity; the first electric heater is used for heating the evaporator; the second electric heater is used for heating the condenser;
the molten salt collecting device comprises a second sealed cavity; the second sealed cavity further comprises a second inlet;
one end of the molten salt conveying pipeline extends to the bottom of the first molten salt lifting barrel through a first outlet of the first sealed cavity, and the other end of the molten salt conveying pipeline extends to the evaporator through a first inlet of the sealed distillation cavity;
one end of the molten salt collecting pipeline extends to the bottom of the condenser through a second outlet of the sealed distillation cavity, and the other end of the molten salt collecting pipeline extends to the inside of the second sealed cavity through a second inlet of the second sealed cavity.
2. The molten salt distillation purification apparatus as claimed in claim 1, wherein the molten salt storage apparatus further comprises a first weighing unit; the first weighing unit is arranged in the first sealed cavity;
the first molten salt lifting bucket is connected with the first weighing unit arranged above the first molten salt lifting bucket through a first suspender;
the air inlet is connected with an external air supply system, and the first exhaust port is connected with an external vacuum system;
the gas supply system is used for introducing inert gas into the molten salt storage equipment;
a plurality of infrared reflecting layers are arranged inside the first sealed cavity; the first weighing unit is arranged above the infrared reflecting layer, and the first molten salt pail is arranged below the infrared reflecting layer;
the infrared reflecting layers are attached to the inner wall of the side face of the first sealed cavity; the infrared reflecting layers are further sleeved on the first hanging rod;
a first vacuum protection cover is additionally arranged at the top of the first sealing cavity, and the first weighing unit is placed in the first vacuum protection cover;
the pressure measuring equipment measures the pressure in the whole first sealed cavity at any time, and the pressure difference between the inside of the first sealed cavity and the inside of the molten salt distillation equipment is adjusted to be kept at 103-105Pa;
The molten salt storage equipment is also provided with a thermocouple.
3. The molten salt distillation purification apparatus of claim 1, the evaporator comprising an evaporation body having an evaporation surface that is stepped.
4. The molten salt distillation purification apparatus of claim 1, the condenser comprising a number of baffles; the partition plate is arranged in the condenser and divides the condenser into a plurality of condensing parts; the area of the baffle plate is smaller than the cross section of the condenser;
preferably, the gaps formed between the partition plates and the condenser are opposite in position, and an S-shaped gas channel is formed in the condenser;
preferably, through holes are formed in one end, close to the bottom of the condenser, of the partition plate connected with the bottom of the condenser;
more preferably, the plurality of partition plates are disposed in parallel with each other inside the condenser.
5. The molten salt distillation purification apparatus of claim 1, wherein the evaporator, the condenser and the vent pipe are connected in sequence to form an inner seal structure.
6. The molten salt distillation purification apparatus as claimed in claim 1, wherein at least one ceramic protective bracket is sleeved outside the evaporator, and the first electric heater surrounds the protective bracket;
the second electric heater surrounds the periphery of the condenser;
at least one thermocouple is arranged in the evaporator;
at least one thermocouple is arranged in the condenser;
the second exhaust port is connected with an external vacuum system.
7. The molten salt distillation purification apparatus as claimed in claim 1, wherein the molten salt collection apparatus further comprises a second weighing unit and a second molten salt pail, both of which are disposed inside the second sealed cavity; the second molten salt lifting bucket is connected with the second weighing unit arranged above the second molten salt lifting bucket through a second suspender; the second molten salt lifting bucket is used for collecting the purified molten salt;
a second vacuum protection cover is additionally arranged at the top of the second sealed cavity, and the second weighing unit is placed in the second vacuum protection cover;
the outer wall of the second sealed cavity is provided with a water cooling jacket;
the other end of the molten salt conveying pipeline extends to one end of the evaporator opposite to the condenser through the first inlet of the sealed distillation cavity;
the molten salt collecting device also comprises a third exhaust port;
preferably, the molten salt distillation and purification equipment further comprises an online sampler; the molten salt collecting device also comprises a sampling port; the online sampler is connected with the sampling port;
preferably, the capacity of the first molten salt pail is equal to the capacity of the second molten salt pail.
8. A molten salt distillation purification method applying the molten salt distillation purification equipment as claimed in any one of claims 1 to 7, comprising the following steps:
s1, adjusting the internal air pressure of the molten salt storage equipment to enable the inside of the molten salt storage equipment and the inside of the molten salt distillation equipment to form an air pressure difference, and conveying the molten salt in the molten salt storage equipment to the evaporator;
s2, heating the evaporator to the evaporation temperature of molten salt in the molten salt distillation equipment under a vacuum environment to generate molten salt steam; and condensing the molten salt steam in the condenser to form liquid molten salt, and collecting by using the molten salt collecting equipment.
9. The method of claim 8, the molten salt evaporation rate of step S2 being a uniform rate;
preferably, the vacuum degree in the molten salt evaporation equipment is 1-1000 Pa;
preferably, the evaporation temperature of the molten salt is 300-1300 ℃;
preferably, the condensation temperature of the molten salt steam is 80-120 ℃ lower than the evaporation temperature of the molten salt, but the condensation temperature of the molten salt steam must be at least 50 ℃ higher than the melting point of the molten salt.
10. The method of claim 9, the molten salt delivery rate in step S1 being equal to the molten salt evaporation rate in step S2.
CN202010143955.8A 2020-03-04 2020-03-04 Molten salt distillation purification method and equipment Active CN111249761B (en)

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