CN107638712B - A kind of device and method for administering ammonium para-tungstate crystal blocking - Google Patents
A kind of device and method for administering ammonium para-tungstate crystal blocking Download PDFInfo
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- CN107638712B CN107638712B CN201710937702.6A CN201710937702A CN107638712B CN 107638712 B CN107638712 B CN 107638712B CN 201710937702 A CN201710937702 A CN 201710937702A CN 107638712 B CN107638712 B CN 107638712B
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Abstract
A kind of device for administering ammonium para-tungstate crystal blocking, including crystallizing evaporator, the bottom of crystallizing evaporator is connect by pipeline with crystallizer, crystallizer outlet is connect by pipeline with cooling cyclone, the bottom and top of cooling cyclone pass through pipeline respectively and connect with vacuum tipping bucket filter and accurate filter, vacuum tipping bucket filter and accurate filter pass through the second conveyance conduit respectively and the first conveyance conduit is connect with mother liquor storage tank, vacuum is equipped with by flow container on second conveyance conduit and the first conveyance conduit, first conveyance conduit, second conveyance conduit and vacuum are by being equipped with steam blast device on flow container, a kind of device and method for administering ammonium para-tungstate crystal blocking of the present invention, it is recrystallized using mother liquor is cooling, magma is classified two sections of essence filterings, the process technology scheme of Dynamic Vapor blowing cleaning, secondary tungsten can effectively be solved Sour crystalline ammonium mother liquor liquid discharging apparatus and pipeline cleaning Crystallization Plugging problem.
Description
Technical field:
The present invention relates to non-ferrous metal field of hydrometallurgy, and in particular to a kind of device for administering ammonium para-tungstate crystal blocking
And method.
Background technique:
The advanced technologies process of current ammonium paratungstate production are as follows: tungsten concentrate -- decomposing leaching -- alkaline extraction-evaporation tungsten,
Molybdenum crude separation-ion exchange depth removes the pure ammonium tungstate evaporative crystallization of molybdenum-, and it is secondary to be especially suitable for high impurity low-grade scheelite production
Ammonium tungstate.
Outstanding problem existing in the prior art are as follows: the knot generated in the unit process of Crystallization Procedure solid-liquor separation
Brilliant mother liquor easily generates Crystallization Plugging phenomenon in equipment and pipe conveying procedure, liquid after especially filtering, and Crystallization Plugging is more prominent
Out.
Blockage phenomenon is since fines material manages the cooling worn under filter, mother liquor temperature decline state in filter progress
Crystallization be precipitated again, equipment pipe and the feed liquid temperature difference it is big caused by particle flash precipitating, inner wall it is rough caused by crystallization wall built-up it is long
Big accumulation effect, the high molybdenum of feed liquid and the physicochemical characteristic of high-carbon acid group, free ammonia evaporation evolution causes mother liquor pH value in evaporation process
It reduces, it is insoluble that solution concentration causes impurity enriched effect, especially carbonate, tungstate radicle to generate under given conditions with impurity element
The result of the reasons combined influences such as property precipitation of salts.
Importantly because flow velocity is too slow causes discharge unsmooth for mother liquor conveying, is detained, leads to crystallization from less to more, by shortcake to
The process of hard qualitative change easily causes APT crystallization to be precipitated and is deposited in pipeline, equipment surface, results in blockage, influences the smooth of technique,
Block clearing is frequent, serious to restrict production.
The method of current common block clearing has following several: 1. mechanical chipping methods, but low efficiency, metal loss are serious；2.
Chemical solvent dissolving method, but easily bring impurity element into, APT production is not particularly suitable for；3. giant jet douche method, but
It will cause liquid expansion, increase energy consumption；4. in-pipe formula method for cleaning installs complicated for operation, bad adaptability；5. ultrasonic wave skill
Art, but invest big, maintenance cost height.
It can be seen that the prior art all Shortcomings, and be the end block clearing operation of the passive type of lag, it is adopted on source of having no way of
The administering method for taking science, cannot cost-effectively solve root problem.
Summary of the invention:
Above-mentioned in order to overcome the shortcomings of, the present invention provides a kind of device and methods of improvement ammonium para-tungstate crystal blocking.
The technical solution adopted by the present invention to solve the technical problems:
A kind of device for administering ammonium para-tungstate crystal blocking, including crystallizing evaporator, the baiting valve of crystallizing evaporator pass through
Pipeline is connect with crystallizer, and crystallizer outlet connect by pipeline with cooling cyclone, the bottom discharge openings of cooling cyclone with
Top overflow port passes through pipeline respectively and connect with vacuum tipping bucket filter and accurate filter, vacuum tipping bucket filter and accurate mistake
Filter passes through the second conveyance conduit respectively and the first conveyance conduit is connect with mother liquor storage tank, the second conveyance conduit and the first delivery pipe
Vacuum is equipped on road by flow container, first conveyance conduit, the second conveyance conduit and vacuum are sprayed by steam is equipped on flow container
Blowing apparatus.
The crystallizer is economic benefits and social benefits vacuum crystallizer or pressure cooler crystallizer.
The steam jet of the steam blast device is inserted into inside the first, second conveyance conduit, and with conveyance conduit length
Direction is installed in parallel, and is spaced 2-5 meters of layouts.
The Discharge outlet end of first, second conveyance conduit is equipped with air mist eliminating and filters in gradually big formula megaphone-shaped
Device.
The steam blast device is controlled by PLC system.
First, second conveyance conduit is equipped with material-gathering device, and material-gathering device is vertically arranged with conveyance conduit.
A method of ammonium para-tungstate crystal blocking is administered, is included the following steps:
A, alkaline extraction strip liquor is put into evaporative crystallization in crystallizing evaporator；
B, crystalline mother solution and magma that initial temperature is 95-103 degree are entered in crystallizer by baiting valve, then is tied
Crystalline substance, the temperature of control mother liquor magma outflow is less than 50 ± 2 degree；
C, after the cooling flowed out in step B crystalline mother solution and magma enter back into cyclone separator realize classification, it is laggard
Two sections of essence filterings of row；
Cyclone separator is equipped with jacketed pipe, and stream has a cooling water in jacketed pipe, and cooling water circular flow is 6-10 cubes/it is small
When, the crystalline mother solution of inflow and magma are further cooled down 2-5 degree, the thick magma of cyclone separator bottom enters skip mistake
Filter, which is realized, to be separated by solid-liquid separation, and liquid is entered in mother liquor storage tank by vacuum by flow container and the second conveyance conduit after filter, cyclone separator
The supernatant of top overflow enters accurate filter, further filters out tiny acicular crystal, and liquid is by vacuum by flow container after filter
Enter in mother liquor storage tank of crystallization with the first conveyance conduit；
D, liquid has one section of discharge interval, during this period the spray of PLC system control steam after entering mother liquor storage tank after filter
Blowing apparatus is carried out steam blast operation by flow container to the first, second conveyance conduit and vacuum, from conveyance conduit starting to end
It is successively blown, interval time 5-10 second, steam pressure 0.4-0.5MPa.
After crystalline mother solution and magma in the step B enter pressure cooler crystallizer, the back extraction for being 25 degree using temperature
Liquid is cooling medium, forces cooling to precipitate crystal indirectly, and forced circulation, which is realized, in local area systems forces cooling；It is stripped flow velocity
It is changed to 5-8 cubic meters/hour of flow；Strip liquor cooling medium enters crystallizing evaporator after potent heat exchange heating pretreatment,
It is operated conducive to the optimization of Crystallization Procedure；Control ammonia evolution rate is 3-6% in heat exchange heating preprocessing process；Carbon dioxide ease
Extracting rate 1-3%, temperature rise 5-8 degree.
Mother liquor magma in the step B, which enters in economic benefits and social benefits vacuum crystallizer, to be recrystallized, wherein an effect vacuum-
0.02-0.05Mpa, 80 ± 2 degree of temperature, two effect vacuum -0.05-0.08Mpa, 50 ± 2 degree of temperature.
Due to the adoption of the technical scheme as described above, the present invention has the following advantages:
A kind of device and method for administering ammonium para-tungstate crystal blocking of the present invention, recrystallized using mother liquor cooling,
Magma is classified the process technology scheme of two sections of essence filterings, Dynamic Vapor blowing cleaning, can effectively solve ammonium para-tungstate crystal mother solution
Liquid discharging apparatus and pipeline cleaning Crystallization Plugging problem.
Detailed description of the invention:
Fig. 1 is structural schematic diagram of the invention；
Fig. 2 is steam blast schematic device.
Specific embodiment:
The present invention can be explained in more detail by following example, the open purpose of the present invention is intended to protect model of the present invention
All interior changes and improvements are enclosed, the invention is not limited to the following examples；
The device of a kind of improvement ammonium para-tungstate crystal blocking with reference to the accompanying drawings, including crystallizing evaporator 1, evaporative crystallization
The baiting valve of device 1 is connect by pipeline with crystallizer 2, and the outlet of crystallizer 2 is connect by pipeline with cooling cyclone 3, cooling rotation
The bottom and top for flowing device 3 pass through pipeline respectively and connect with vacuum tipping bucket filter 5 and accurate filter 4, the filtering of vacuum tipping bucket
Device 5 and accurate filter 4 are connect by the second conveyance conduit 82 and the first conveyance conduit 81 with mother liquor storage tank 6 respectively, and second is defeated
It send and is equipped with vacuum on pipeline 82 and the first conveyance conduit 81 by flow container 7, first conveyance conduit 81, the second conveyance conduit 82
With vacuum by being equipped with steam blast device 10 on flow container 7.
The crystallizer 2 is economic benefits and social benefits vacuum crystallizer or pressure cooler crystallizer.
The steam jet of the steam blast device 10 is inserted into inside the first, second conveyance conduit, and with delivery pipe road length
Degree direction is installed in parallel, and is spaced 2-5 meters of layouts.
The Discharge outlet end of first, second conveyance conduit 81,82 is equipped with air mist eliminating in gradually big formula megaphone-shaped
Filter device.
First, second conveyance conduit 81,82 is equipped with material-gathering device 9, and material-gathering device 9 is vertical with conveyance conduit 8 to be set
It sets.
A method of ammonium para-tungstate crystal blocking is administered, is included the following steps:
A, alkaline extraction strip liquor is put into evaporative crystallization in crystallizing evaporator；
B, crystalline mother solution and magma that initial temperature is 95-103 degree are entered in crystallizer 2 by bottom discharge valve, into
Row recrystallization, the temperature of control mother liquor magma outflow is less than 50 ± 2 degree；
C, the cooling post mother liquor magma flowed out in step B, which enters back into, realizes classification in cyclone separator 3；Two sections are carried out later
Essence filtering；
Cyclone separator is equipped with jacketed pipe, and stream has a cooling water in jacketed pipe, and cooling water circular flow is 6-10 cubes/it is small
When, the crystalline mother solution of inflow and magma are further cooled down 2-5 degree, the thick magma of 3 bottom of cyclone separator enters skip
Filter 5, which is realized, to be separated by solid-liquid separation, and liquid is entered in mother liquor storage tank 6 by vacuum by flow container 7 and the second conveyance conduit 82, eddy flow point
Supernatant from 3 top overflow of device enters accurate filter 4, further filters out tiny acicular crystal, liquid passes through vacuum after filter
Entered in mother liquor storage tank 6 by flow container 7 and the first conveyance conduit 81；
D, liquid has one section of discharge interval after entering mother liquor storage tank 6 after filter, and the control of PLC system 11 during this period is steamed
Vapour blowing device 10 is to the first, second conveyance conduit 81,82(, that is, conveyance conduit 8) and vacuum by flow container 7 carry out steam blast
Operation is originated to end from conveyance conduit 8 and is successively blown, interval time 5-10 second, steam pressure 0.4-0.5MPa.
After crystalline mother solution and magma in the step B enter pressure cooler crystallizer, the back extraction for being 25 degree using temperature
Liquid is cooling medium, forces cooling to precipitate crystal indirectly, and forced circulation, which is realized, in local area systems forces cooling；It is stripped flow quantity
5-8 cubic meters/hour；Strip liquor cooling medium enters crystallizing evaporator after potent heat exchange heating pretreatment, is conducive to crystallization
The optimization of process operates；Control ammonia evolution rate is 3-6% in heat exchange heating preprocessing process；Carbon dioxide evolution rate 1-3%,
Temperature rise 5-8 degree.
Mother liquor magma in the step B, which enters in economic benefits and social benefits vacuum crystallizer, to be recrystallized, wherein an effect vacuum-
0.02-0.05Mpa, 80 ± 2 degree of temperature, two effect vacuum -0.05-0.08Mpa, 50 ± 2 degree of temperature.
Due to the adoption of the technical scheme as described above, the present invention has the following advantages:
1. acicular crystal eduction rate is the principle of 6-10% using crystalline mother solution in cooling stage, relevant art control is taken
System, eliminates mother liquor degree of supersaturation further, realizes the abundant recrystallization of mother liquor.
It especially with economic benefits and social benefits vacuum crystallizer, realizes and is concentrated by evaporation progress synchronous with crystallisation by cooling, reduce mother liquor in postorder
Precipitation crystallization probability, reduce the content of metal of mother liquor；The bigger difference of tungsten solubility product is utilized, simultaneously with ammonium paramolybdate
Molybdenum eduction rate existing for form is extremely low, about 0.5-2%, can remove molybdenum in the further separation of same cooling temperature point realization tungsten
Effect is good.
It, can be real based on the molten rate of ammonia for slightly the returning molten thick APT property unrelated with its crystal morphology and lattice granule size
Now increase the crystallization recovery rate of crude separation process.Percent crystallization in massecuite is greatly improved, energy consumption is reduced, reduces blocking, reduces loss of material, it is excellent
Change work on the spot environment, improves recovery rate of iron.The sieve classification of different grain size rank ammonium paratungstate easy to accomplish.Utilize cooling
Process preheats strip liquor energy conservation and environmental protection, utilizes operation.
2. wearing filter Probability Distribution Principle, in addition to granularity factor influences, quantity of solvent in unit filter area using filtering
Throughput is few, wears filter and loses few principle to realize that mother liquor is classified two sections of secondary filters；Order of ammoniumparatungstate crystal has density big, easy
The characteristic of precipitating realizes efficient solid-liquid separation effect using different filter plants.It wears filter phenomenon to reduce, improves percent crystallization in massecuite, pipe
Road does not block up, easy to operate, and operation rate is high, reduces labor intensity, reduces the physics such as evaporating, emitting, dripping or leaking of liquid or gas caused by failure, mechanical damage
It loses.
3. pyrocaloric effect and strong diffusivity using steam, form pulse high temperature gas flow wave, change layer stream by steam blast
For turbulent flow, the impact cleaning function for acting on equipment and pipeline is reinforced.
The application of preventive block clearing processing technique, fundamentally solves blockage problem.
4. continuous, interval of this technology for ammonium paratungstate evaporate crude separation crystallization and ammonium paratungstate evaporative crystallization,
Versatility, favorable reproducibility.
Not stating part in the above content carefully is the prior art, therefore does not run business into particular one and state.
Claims (8)
1. a kind of device for administering ammonium para-tungstate crystal blocking, it is characterised in that: including crystallizing evaporator, crystallizing evaporator is put
Material valve is connect by pipeline with crystallizer, and crystallizer outlet is connect by pipeline with cooling cyclone, the bottom of cooling cyclone
Discharge port and top overflow port pass through pipeline respectively and connect with vacuum tipping bucket filter and accurate filter, vacuum tipping bucket filter
Pass through the second conveyance conduit respectively with accurate filter and the first conveyance conduit is connect with mother liquor storage tank, the second conveyance conduit and
Vacuum is equipped on one conveyance conduit by flow container, first conveyance conduit, the second conveyance conduit and vacuum in flow container by being all provided with
There is steam blast device；The steam jet of the steam blast device is inserted into inside the first, second conveyance conduit, and and delivery pipe
Road length direction is installed in parallel, and is spaced 2-5 meters of layouts.
2. a kind of device for administering ammonium para-tungstate crystal blocking according to claim 1, it is characterised in that: the crystallizer
It is economic benefits and social benefits vacuum crystallizer or pressure cooler crystallizer.
3. a kind of device for administering ammonium para-tungstate crystal blocking according to claim 1, it is characterised in that: described first,
The Discharge outlet end of second conveyance conduit is equipped with air mist eliminating filter device in gradually big formula megaphone-shaped.
4. a kind of device for administering ammonium para-tungstate crystal blocking according to claim 1, it is characterised in that: the steam spray
Blowing apparatus is controlled by PLC system.
5. a kind of device for administering ammonium para-tungstate crystal blocking according to claim 1, it is characterised in that: described first,
Second conveyance conduit is equipped with material-gathering device, and material-gathering device is vertically arranged with conveyance conduit.
6. a kind of method for administering ammonium para-tungstate crystal blocking using device as described in claim 1, it is characterised in that: including such as
Lower step:
A, alkaline extraction strip liquor is put into evaporative crystallization in crystallizing evaporator；
B, crystalline mother solution and magma that initial temperature is 95-103 degree are entered in crystallizer by baiting valve, are recrystallized,
The temperature of mother liquor magma outflow is controlled less than 50 ± 2 degree；
C, crystalline mother solution and magma enter back into and realize classification in cyclone separator after the cooling flowed out in step B, carry out two later
Section essence filtering；
Cyclone separator is equipped with jacketed pipe, and stream has cooling water in jacketed pipe, and cooling water circular flow is 6-10 cubic meters/hour,
The crystalline mother solution of inflow and magma are further cooled down 2-5 degree, the thick magma of cyclone separator bottom enters skip filtering
Machine, which is realized, to be separated by solid-liquid separation, and liquid is entered in mother liquor storage tank by vacuum by flow container and the second conveyance conduit after filter, on cyclone separator
The supernatant of portion's overflow enters accurate filter, further filters out tiny acicular crystal, after filter liquid by vacuum by flow container and
First conveyance conduit enters in mother liquor storage tank of crystallization；
D, liquid has one section of discharge interval, during this period PLC system control steam blast dress after entering mother liquor storage tank after filter
It sets and steam blast operation is carried out by flow container to the first, second conveyance conduit and vacuum, originated from conveyance conduit to end successively
Blowing, interval time 5-10 second, steam pressure 0.4-0.5MPa.
7. according to the method described in claim 6, it is characterized by: crystalline mother solution and magma in the step B enter pressure
It is cooling medium using the strip liquor that temperature is 25 degree after cooler crystallizer, forces cooling to precipitate crystal indirectly, in local area systems
Interior forced circulation, which is realized, forces cooling；5-8 cubic meters/hour of flow quantity of back extraction；Strip liquor cooling medium passes through potent heat exchange liter
Enter crystallizing evaporator after temperature pretreatment, is operated conducive to the optimization of Crystallization Procedure；It is controlled in heat exchange heating preprocessing process
Ammonia evolution rate is 3-6%；Carbon dioxide evolution rate 1-3%, temperature rise 5-8 degree.
8. according to the method described in claim 6, it is characterized by: the mother liquor magma in the step B enters economic benefits and social benefits vacuum knot
It is recrystallized in brilliant device, wherein an effect vacuum -0.02-0.05Mpa, 80 ± 2 degree of temperature, two imitate vacuum -0.05-0.08Mpa,
50 ± 2 degree of temperature.
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| CN201710937702.6A CN107638712B (en) | 2017-09-30 | 2017-09-30 | A kind of device and method for administering ammonium para-tungstate crystal blocking |
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| CN201710937702.6A CN107638712B (en) | 2017-09-30 | 2017-09-30 | A kind of device and method for administering ammonium para-tungstate crystal blocking |
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607739A (en) * | 2008-11-20 | 2009-12-23 | 厦门钨业股份有限公司 | Closed cycle process for crystalline mother solution of ammonium paratungstate |
| CN204502455U (en) * | 2015-01-09 | 2015-07-29 | 赣州亚泰钨业有限公司 | One utilizes tungsten waste to prepare ammonium paratungstate evaporated crystallization device |
| CN204380311U (en) * | 2015-01-09 | 2015-06-10 | 江西耀升钨业股份有限公司 | A kind of high-purity ammonium paratungstate evaporated crystallization device |
| RU2600045C1 (en) * | 2015-06-09 | 2016-10-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | Method of producing ammonium paratungstate |
| CN205127680U (en) * | 2015-11-06 | 2016-04-06 | 铜陵有色金属集团股份有限公司铜冠冶化分公司 | Prevent organic amine desulfurization desorber of wet process of reboiler crystallization jam |
| CN106395906A (en) * | 2016-10-27 | 2017-02-15 | 江西稀有金属钨业控股集团有限公司 | Method and system for preparing ammonium metatungstate from tungsten oxide waste |
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Effective date of registration: 20211117 Address after: 471500 Heyu town Heyu village, Luanchuan County, Luoyang City, Henan Province Patentee after: Luoyang Luanchuan Molybdenum Group tungsten Co.,Ltd. Address before: 471500 north of Yihe River, huameishan Road, Chengdong new district, Luanchuan County, Luoyang City, Henan Province Patentee before: China Molybdenum Co.,Ltd. |
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