CN212450667U

CN212450667U - Rehenic acid ammonium purification system

Info

Publication number: CN212450667U
Application number: CN202020460639.9U
Authority: CN
Inventors: 杨彦红; 孙元; 周亦胄
Original assignee: Institute of Metal Research of CAS
Current assignee: Institute of Metal Research of CAS
Priority date: 2020-04-01
Filing date: 2020-04-01
Publication date: 2021-02-02
Anticipated expiration: 2030-04-01

Abstract

The utility model provides a rhenate purification system, dissolve the cauldron including the heating, condensation crystallization kettle, the first liquid outlet that the cauldron was dissolved in the heating passes through the optional through connection of filter element with condensation crystallization kettle's first inlet, be equipped with first cooling tube on condensation crystallization kettle's the wall body, the first cooling medium of circulation cools off with the rhenate solution to in the condensation crystallization kettle in the first cooling tube, first cooling medium is the same with the solution of rhenate, pumping unit connects between condensation crystallization kettle's second liquid outlet and the second inlet that the cauldron was dissolved in the heating. According to the utility model discloses a rhenic acid ammonium purification system can the first cooling medium of make full use of absorb the heat exchange heat of solution in the condensation crystallization kettle, effectively reduces the heating energy consumption in the heating dissolving kettle, can reduce the waste to the water resource with the rhenic acid ammonium solution cyclic utilization after the crystallization simultaneously.

Description

Rehenic acid ammonium purification system

Technical Field

The utility model belongs to the technical field of the motor is made, concretely relates to ammonium rhenate purification system.

Background

Ammonium rhenate is a key product for producing a super heat-resistant alloy required by aerospace and nuclear industries and catalyzing Pt-Re alloy for producing lead-free or low-lead gasoline by refining and reforming petroleum. In the petroleum smelting process, the reforming catalyst plays an important role, the traditional single-metal platinum catalyst has low catalytic activity and poor selectivity, and the service life is generally less than two years. In the electronic structure of metallic rhenium, 5 electrons of unsaturated 4d layer are easy to release, 2 electrons of 6s layer are easy to participate to form covalent bond, and the characteristics of larger lattice parameter and the like are added, so rhenium and the compound thereof show excellent catalytic activity. The rhenium element is added to the platinum reforming catalyst taking alumina as a carrier in the oil smelting process, so that the catalyst has better activity, higher stability and aromatic hydrocarbon yield, and the service life of the catalyst is prolonged to 3-4 years. More than 50% of the commercial catalytic processes employ a platinum-rhenium catalyst, wherein the rhenium content is 0.3% of the total amount and the rhenium content in the rhenium petroleum reforming catalyst is as much as 20% of the total demand. At present, ammonium rhenate purification methods have many defects, for example, a solution after purification and crystallization cannot be recycled and is directly subjected to final evaporation and crystallization, so that the efficiency of the purification process is reduced, and water resources are wasted due to evaporation loss of the solution (water); for another example, in the process of condensation and crystallization of the solution, a cooling medium is required to perform heat exchange cooling on the solution, and the heat of the cooling cannot be recycled, so that the energy consumption for heating the solution is large, and the production cost for purification is high.

SUMMERY OF THE UTILITY MODEL

Therefore, the to-be-solved technical problem of the utility model is to provide a rhenate purification system, can the first cooling medium of make full use of absorb the heat exchange heat of solution in the condensation crystallization kettle, effectively reduce the heating energy consumption in the heating dissolution kettle, can reduce the waste to the water resource with the rhenate solution cyclic utilization after the crystallization simultaneously, when promoting purification efficiency.

In order to solve the problem, the utility model provides an ammonium rhenate purification system, including heating dissolving kettle, condensation crystallization kettle, the heating dissolving kettle's first liquid outlet with the first inlet of condensation crystallization kettle passes through the optional through connection of filter element, be equipped with first cooling tube on the wall body of condensation crystallization kettle, flow through first cooling medium in the first cooling tube is in order to right ammonium rhenate solution in the condensation crystallization kettle cools off, first cooling medium is the same with the solution of ammonium rhenate, still includes pumping means, pumping means connect in the second liquid outlet of condensation crystallization kettle with between the second inlet of heating dissolving kettle, in order to be in the solution that the crystallization among the condensation crystallization kettle finishes and first cooling medium pump after the heat transfer in the first cooling tube is sent into in the heating dissolving kettle.

Preferably, the periphery of the condensation crystallization kettle is provided with a first heat preservation layer, and a second heat preservation layer is arranged on a pipeline between the pumping component and the first cooling pipe and a pipeline between the pumping component and the second liquid inlet.

Preferably, the first heat preservation layer is made of heat preservation carbon felt, and/or the second heat preservation layer is made of heat preservation carbon felt.

Preferably, be equipped with elevating system, crystal filter in the condensation crystallization kettle, after the crystallization of ammonium rhenate solution is accomplished, elevating system can drive crystal filter goes up and down between the cauldron bottom and cauldron top.

Preferably, an ultrasonic generator is further arranged in the condensation crystallization kettle and/or the heating dissolution kettle.

Preferably, the ammonium rhenate purification system further comprises a vacuum collection device, wherein the vacuum collection device comprises a collection head and a vacuum generator, and the vacuum generator generates vacuum during operation so as to collect ammonium rhenate crystals crystallized on the crystal filter plate through the collection head.

Preferably, be equipped with the heater block on the wall body of heating dissolving kettle, the heater block centers on the perisporium annular of heating dissolving kettle lays, the wall body of heating dissolving kettle is constructed with crystal heating stoving chamber, heating stoving chamber centers on the heater block is kept away from the periphery side annular of heating dissolving kettle lays, the ammonium rhenate crystal that vacuum collection device collected can be carried to in the heating stoving intracavity.

Preferably, the heating member comprises graphite or an induction coil.

Preferably, a second cooling pipe is further arranged on a wall body of the condensation crystallization kettle, a flow path of the second cooling pipe is independent of a flow path of the first cooling pipe, and a second cooling medium circulates in the second cooling pipe, so that after the temperature of the ammonium rhenate solution is reduced to a first preset temperature by the first cooling pipe, the ammonium rhenate solution is reduced to a second preset temperature from the first preset temperature.

Preferably, the second liquid inlet is also provided with a liquid supplementing port.

The utility model provides an ammonium rhenate purification system, on the one hand through the timely pump of pumping parts with the first cooling medium after the heat transfer send into in the heating dissolves the cauldron, thereby can improve and be in the heating initial temperature in the heating dissolves the cauldron, and then reduced the demand to the required heating energy of solution heating wherein, realize energy-conserving purpose; on the other hand, with solution (tail liquid) after the crystal has been separated out in the condensation crystallization cauldron is pumped once more and is sent into in the heating dissolving cauldron, make the ammonium rhenate purification system need not carry out solitary evaporation crystallization to the tail liquid at every turn as in prior art, this has promoted the work efficiency of purification technology, and the very big reduction of while has saved the purification cost to the demand consumption of volume (for example water).

Drawings

Fig. 1 is a schematic structural diagram of an ammonium rhenate purification system according to an embodiment of the present invention.

The reference numerals are represented as:

1. heating the dissolving kettle; 11. a first liquid outlet; 12. a second liquid inlet; 13. a heating member; 14. a heating drying cavity; 141. a crystal output port; 15. a fluid infusion port; 161. a feed inlet; 162. a material pushing device; 163. A seal member; 2. condensing the crystallization kettle; 21. a first liquid inlet; 22. a second liquid outlet; 23. a first insulating layer; 24. a lifting mechanism; 25. a crystallization filter plate; 261. a first cooling pipe; 262. a second cooling pipe; 3. a filter member; 4. a pumping member; 5. an ultrasonic generator; 6. a vacuum collection device; 61. a collection head; 62. a vacuum generator; 7. an electromagnetic valve.

Detailed Description

Referring to fig. 1, according to an embodiment of the present invention, there is provided an ammonium rhenate purification system, including a heating and dissolving kettle 1, a condensation and crystallization kettle 2, wherein a first liquid outlet 11, a second liquid inlet 12, and a feed inlet 161 are configured on a wall body of the heating and dissolving kettle 1, a material pushing device 162 is disposed in the feed inlet 161, the material pushing device 162 is capable of feeding external ammonium rhenate crystal raw material to be purified into the heating and dissolving kettle 1 through the feed inlet 161, and external solvent (e.g. water) is capable of being fed into the heating and dissolving kettle 1 through the second liquid inlet 12, so as to form an ammonium rhenate solution containing impurities in the heating and dissolving kettle 1, the first liquid outlet 11 of the heating and dissolving kettle 1 and the first liquid inlet 21 of the condensation and crystallization kettle 2 pass through a filter component 3 (the filter material of the filter component 3 may be, for example, gauze, or a filter member made of meltblown or non-woven fabric), a first cooling pipe 261 is disposed on a wall body of the condensation crystallization kettle 2, a first cooling medium flows through the first cooling pipe 261 to cool the ammonium rhenate solution in the condensation crystallization kettle 2, the first cooling medium is the same as the ammonium rhenate solution, the apparatus further comprises a pumping member 4, the pumping member 4 is connected between the second liquid outlet 22 of the condensation crystallization kettle 2 and the second liquid inlet 12 of the heating and dissolving kettle 1 to pump the crystallized solution in the condensation crystallization kettle 2 and the first cooling medium after heat exchange in the first cooling pipe 261 into the heating and dissolving kettle 1, the selectable connection between the first liquid inlet 21 and the first liquid outlet 11 may be implemented by disposing an electromagnetic valve 7 on the corresponding connecting pipe as shown in fig. 1, so as to realize the penetration or the truncation of the heating and dissolving kettle 1 and the condensation and crystallization kettle 2, and also realize the flow control of the ammonium rhenate solution. In the technical scheme, on one hand, the first cooling medium subjected to heat exchange is timely pumped into the heating and dissolving kettle 1 through the pumping part 4, so that the heating initial temperature in the heating and dissolving kettle 1 can be increased, the requirement on heating energy required by heating the solution in the heating and dissolving kettle is further reduced, and the purpose of energy conservation is achieved; on the other hand, the solution (tail liquid) after the crystals in the condensation crystallization kettle 2 are separated out is pumped into the heating and dissolving kettle 1 again, so that the ammonium rhenate purification system does not need to perform separate evaporation crystallization on the tail liquid at every time as in the prior art, the work efficiency of the purification process is improved, the consumption of the volume (such as water) is greatly reduced, and the purification cost is saved.

The feed inlet 161 has a corresponding feed tube, and the pusher 162 has a corresponding feed rod, the feed rod and the feed tube are inserted into each other to ensure that the feed rod can reciprocate along the length direction of the feed tube, and the smaller the gap between the feed rod and the feed tube, the better, the smaller the gap between the feed rod and the feed tube, and the smaller the gap between the feed rod and the feed tube, the smaller the gap. And further, the free end of the feeding pipe and the matching position between the feeding rods are also provided with a sealing element 163 to further improve the sealing property, and the sealing element 163 only needs to adopt a high-temperature resistant rubber ring. Similarly, a sealing member 163 may be disposed at the joint of the filtering component 3 and the pipe fitting matching with the filtering component to improve the sealing performance, and at the same time, the filtering component 3 can be detachably connected to the corresponding pipe fitting to facilitate the replacement of the filtering component 3.

In order to fully utilize the heating heat of the first cooling medium heat exchange and prevent the heat loss in the pumping process, preferably, a first heat preservation layer 23 is arranged on the periphery of the condensation crystallization kettle 2, a second heat preservation layer is arranged on a pipeline between the pumping part 4 and the first cooling pipe 261 and a pipeline between the pumping part 4 and the second liquid inlet 12, and the first heat preservation layer 23 or the second heat preservation layer may be made of the same heat preservation material, for example, agglomerated polyurethane foam is sprayed on the outer side surface of the corresponding part, preferably, the first heat preservation layer 23 is made of a heat preservation carbon felt, and/or the second heat preservation layer is made of a heat preservation carbon felt.

Preferably, be equipped with elevating system 24, crystal filter 25 in condensation crystallization kettle 2, after the crystallization of ammonium rhenate solution finishes, elevating system 24 can drive crystal filter 25 (its preparation filter media can be the same with aforementioned filter component 3) goes up and down between the cauldron bottom and cauldron top, so, when condensation crystallization process finishes, the ammonium rhenate crystal of appearing is in crystal filter 25 is last and quilt elevating system 24 rises above the liquid level of tail liquid, and is close to condensation crystallization kettle 2's cauldron top position to in order to retrieve the crystal after the purification. The lifting mechanism 24 can be implemented in various forms, such as a lifting assembly with the simplest combination of pulleys and ropes, a vertical lifting assembly with motor rotation and worm gear, a reciprocating oil cylinder or an air cylinder which is commonly seen, and the selection of the structural forms can be carried out according to the objective implementation conditions of system construction.

In the prior art, tools such as a doctor blade are used for collecting purified ammonium rhenate crystals, which is a traditional way that wastes time and labor and has extremely low working efficiency, as a preferred embodiment, the ammonium rhenate purification system further comprises a vacuum collection device 6, the vacuum collection device 6 comprises a collection head 61 and a vacuum generator 62, the vacuum generator 62 generates vacuum during operation to collect the ammonium rhenate crystals crystallized on the crystal filter plate 25 through the collection head 61, wherein the vacuum generator 62 is a generator utilizing the venturi effect, namely the venturi effect, and can generate a great vacuum degree under the action of high-pressure air flow, the collection head 61 is installed at the vacuum port of the vacuum generator 62, when the crystal filter plate 25 is lifted to the kettle top position by the lifting mechanism 24, the vacuum generator 62 is operated, at this time, the opening of the collecting head 61 generates a great vacuum suction force, so as to adsorb and collect the precipitated and purified ammonium rhenate crystals attached to the crystal filter plate 25 to a predetermined position, the predetermined position can be, for example, a drying box in the prior art, and preferably, a heating part 13 is arranged on the wall body of the heating and dissolving kettle 1, the heating part 13 is annularly arranged around the peripheral wall of the heating and dissolving kettle 1, the wall body of the heating and dissolving kettle 1 is configured with a crystal heating and drying chamber 14, the heating and drying chamber 14 is annularly arranged around the outer peripheral side of the heating part 13 far away from the heating and dissolving kettle 1, and the ammonium rhenate crystals collected by the vacuum collecting device 6 can be conveyed into the heating and drying chamber 14. Among this technical scheme heating dissolving kettle 1 when realizing the heating to solution in the cauldron, can also drying and heating the crystal that is in its week side and goes up one and separate out purification crystallization cycle and form, make full use of heater block 13 is keeping away from the heat of one side in the heating dissolving kettle 1 cauldron realizes drying process to the ammonium rhenate crystal after the purification when realizing thermal all-round utilization. It is understood that the outer wall of the oven drying chamber 14 is preferably provided with a layer of insulating material, and the oven drying chamber 14 is also provided with a corresponding crystal outlet 141 for collecting the dried purified crystals.

The heating component 13 includes graphite or an induction coil, and it can be understood that the graphite or the induction coil is electrically connected with an external power supply to realize a corresponding heating function, and the graphite or the induction coil can be wound in the wall body of the heating and dissolving kettle 1 at uniform intervals.

In order to realize energy saving by recycling the heat of the first cooling medium and maximally ensure the precipitation of crystals in the solution, preferably, a second cooling pipe 262 is further disposed on the wall of the condensation crystallization kettle 2, the flow paths of the second cooling pipe 262 and the first cooling pipe 261 are independent from each other, and a second cooling medium flows through the second cooling pipe 262, so that after the first cooling pipe 261 reduces the temperature of the ammonium rhenate solution to a first preset temperature (for example, 20 ℃), the ammonium rhenate solution is reduced from the first preset temperature to a second preset temperature (for example, about 0 ℃), in such a way that the first cooling pipe 261 and the second cooling pipe 262 are controlled to reduce the temperature independently, that is, the solution in the kettle is cooled by the first cooling pipe 261 first, and then the second cooling pipe 262 is used to further reduce the temperature, on the one hand, the precipitation efficiency of crystals in the solution can be ensured, and on the other hand, the problem that the temperature difference between the first cooling pipe 261 and the second cooling pipe 262 causes the temperature of the first cooling medium in the first cooling pipe 261 to be too low to achieve the shortage of heat utilization is prevented.

In order to ensure the stability of the amount of the solution in the heating and dissolving tank 1, it is preferable that the second solution inlet 12 is further configured with a solution replenishing port 15 for replenishing the amount of the solution in the tank in time when the amount of the solution in the tank is small. Further, in order to ensure the dissolution and crystallization uniformity and efficiency of the solute and the solvent in the heating and dissolving kettle 1 and the condensation and crystallization kettle 2, preferably, an ultrasonic generator 5 is further disposed in the condensation and crystallization kettle 2 and/or the heating and dissolving kettle 1.

In the aspect of specific application, firstly, the ammonium rhenate crystal raw material to be purified is fed into the heating and dissolving kettle 1 through the feed inlet 161, synchronously, solvent water is introduced through the second liquid inlet 12, the heating element 13 is started to heat water in the kettle so as to ensure that the ammonium rhenate crystal raw material can be efficiently dissolved to form a saturated ammonium rhenate solution, the general control solution temperature is heated to about 100 ℃ (the specific temperature is determined flexibly according to the type of the solvent and should not exceed the boiling point of the corresponding solvent in principle), so as to prevent waste caused by solvent evaporation, after the saturated ammonium rhenate solution (containing impurities) is formed in the heating and dissolving kettle 1, the continuous heating of the heating element 13 is maintained at the moment so as to prevent the solution in the heating and dissolving kettle 1 from being condensed and cooled, synchronously, the electromagnetic valve 7 on a pipeline between the heating and dissolving kettle 1 and the condensation and crystallization kettle 2 is controlled to be, filtering corresponding impurities from a saturated solution in a heating and dissolving kettle 1 by a filter component 3, then feeding the saturated solution into a condensation and crystallization kettle 2, stopping the heating process of a heating component 13 when the solution in the heating and dissolving kettle 1 is exhausted, synchronously conducting a first cooling pipe 261, cooling the solution in the condensation and crystallization kettle 2 by first cooling medium water in a first stage, transferring part of the heat of the solution in the kettle to the first cooling medium, namely the first cooling medium heats up and cools the solution in the kettle at the same time to realize the condensation and crystallization in the first stage, starting a pumping component 4 to make the heated first cooling medium water flow into the heating and dissolving kettle to recycle the heat of the part, when the temperature in the kettle is reduced to 20 ℃, the cooling effect of the first cooling medium at the moment will step into a bottleneck period, and the first stage of the condensation and crystallization is finished, at this time, the first cooling pipe 261 is cut off, the second cooling pipe 262 is synchronously conducted to further cool and crystallize the solution in the kettle by using a second cooling medium, namely, dry ice, so as to ensure the efficiency of crystal precipitation and the precipitation amount, after the precipitation of the crystal meets the requirement, the cooling process is stopped, the electromagnetic valve 7 between the pumping part 4 and the second liquid outlet 22 is conducted to convey the tail liquid back to the heating and dissolving kettle 1 for reuse, the next purification cycle is started, meanwhile, the lifting mechanism 24 is controlled to lift the crystal filter plate 25 attached with the precipitated crystal from the kettle bottom to the kettle top, the vacuum collection device 6 is synchronously started to absorb and collect the precipitated crystal and convey the crystal to the heating and drying cavity 14, further, the precipitated crystal can be dried by using the heating temperature of the heating part 13, and finally the dried crystal is conveyed to a corresponding collection part through the crystal output port 141, and a complete ammonium rhenate crystal purification process is completed, and the process is understood to have each cycle period performed synchronously, and the corresponding production rhythm is reasonably arranged in specific control.

It is readily understood by a person skilled in the art that the advantageous ways described above can be freely combined, superimposed without conflict.

The above description is only exemplary of the present invention and should not be construed as limiting the present invention, and any modifications, equivalents and improvements made within the spirit and principles of the present invention are intended to be included within the scope of the present invention. The above is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims

1. The utility model provides an ammonium rhenate purification system, characterized in that, including heating dissolving kettle (1), condensation crystallization kettle (2), first liquid outlet (11) of heating dissolving kettle (1) with first inlet (21) of condensation crystallization kettle (2) are through filter element (3) selectable through connection, be equipped with first cooling tube (261) on the wall body of condensation crystallization kettle (2), circulate first cooling medium in first cooling tube (261) in order to right ammonium rhenate solution in condensation crystallization kettle (2) cools off, first cooling medium is the same with the solvent of ammonium rhenate, still includes pumping means (4), pumping means (4) connect in second liquid outlet (22) of condensation crystallization kettle (2) with between second inlet (12) of heating dissolving kettle (1), with the solution that will be in crystallization in condensation crystallization kettle (2) finishes and first cold after the heat transfer in first cooling tube (261) The cooling medium is pumped into the heating dissolving kettle (1).

2. The ammonium rhenate purification system of claim 1, wherein a first heat preservation layer (23) is arranged on the periphery of the condensation crystallization kettle (2), and a second heat preservation layer is arranged on a pipeline between the pumping part (4) and the first cooling pipe (261) and a pipeline between the pumping part (4) and the second liquid inlet (12).

3. The ammonium rhenate purification system of claim 2, wherein the first insulation layer (23) is made of insulation carbon felt, and/or the second insulation layer is made of insulation carbon felt.

4. The ammonium rhenate purification system according to any one of claims 1 to 3, wherein a lifting mechanism (24) and a crystal filter plate (25) are arranged in the condensation crystallization kettle (2), and after the ammonium rhenate solution is crystallized, the lifting mechanism (24) can drive the crystal filter plate (25) to lift between the kettle bottom and the kettle top.

5. The ammonium rhenate purification system according to claim 4, wherein an ultrasonic generator (5) is further arranged in the condensation crystallization kettle (2) and/or the heating and dissolving kettle (1).

6. The ammonium rhenate purification system of claim 4, further comprising a vacuum collection device (6), wherein the vacuum collection device (6) comprises a collection head (61), a vacuum generator (62), and the vacuum generator (62) generates vacuum during operation to collect ammonium rhenate crystals crystallized on the crystal filter plate (25) through the collection head (61).

7. The ammonium rhenate purification system of claim 6, wherein a heating element (13) is arranged on a wall body of the heating and dissolving kettle (1), the heating element (13) is annularly arranged around the peripheral wall of the heating and dissolving kettle (1), a crystal heating and drying cavity (14) is formed in the wall body of the heating and dissolving kettle (1), the heating and drying cavity (14) is annularly arranged around the outer peripheral side of the heating element (13) far away from the heating and dissolving kettle (1), and ammonium rhenate crystals collected by the vacuum collection device (6) can be conveyed into the heating and drying cavity (14).

8. The ammonium rhenate purification system of claim 7, characterized in that the heating element (13) comprises graphite or an induction coil.

9. The ammonium rhenate purification system according to any one of claims 1 to 3 and 5 to 8, wherein a second cooling pipe (262) is further arranged on a wall body of the condensation crystallization kettle (2), a flow path of the second cooling pipe (262) is independent from that of the first cooling pipe (261), and a second cooling medium is circulated in the second cooling pipe (262) so as to reduce the temperature of the ammonium rhenate solution from a first preset temperature to a second preset temperature after the first cooling pipe (261) reduces the temperature of the ammonium rhenate solution to the first preset temperature.

10. The ammonium rhenate purification system of claim 1, wherein the second liquid inlet (12) is further provided with a liquid supplementing port (15).