CN206014431U - Molybdenum trisulfide production reaction unit - Google Patents
Molybdenum trisulfide production reaction unit Download PDFInfo
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- CN206014431U CN206014431U CN201620886296.6U CN201620886296U CN206014431U CN 206014431 U CN206014431 U CN 206014431U CN 201620886296 U CN201620886296 U CN 201620886296U CN 206014431 U CN206014431 U CN 206014431U
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Abstract
The utility model discloses a kind of molybdenum trisulfide production reaction unit, including reaction settling basin and waste gas recovering device, reaction settling basin includes reaction tank, concentration basin, located at the supernatant liquid pool between reaction tank and concentration basin, inner fovea part is recessed at the lower bottom part of reaction tank at least, equipped with the permanent magnet induction device for driving solution obliquely flow at inner fovea part, supernatant bottom of pond portion is provided with slurry passage, reaction tank is connected with concentration basin by slurry passage, waste gas recovering device is connected with the top seal of reaction settling basin located at the top of reaction tank, waste gas recovering device.Molybdenum trisulfide production of the present utility model uses reaction unit disposal ability big, can achieve continuous uninterrupted production, MoS3High income, wastage of material is few, MoS3Yield big, meanwhile, the whole production cycle is shorter, and input cost is not substantially increased, and income is than high；In addition, being recycled by waste gas, it is achieved that green production, routinely development potentiality is big.
Description
Technical field
This utility model is related to the production preparation field of nanometer class molybdenum disulfide, and more particularly to a kind of molybdenum trisulfide production is used
Reaction unit.
Background technology
Nano molybdenum disulfide has the physics of uniqueness and chemical property with its special structure, is widely used in oil and adds
The field such as hydrogen desulfurization, Non-aqueous lithium battery, high resiliency new material and its coating and photoelectrochemical cell.At present, nano molybdenum disulfide
Preparation method have a lot, but most of preparation methoies can only be confined to laboratory, can reach the side of industrial scale metaplasia product
But relatively seldom, mostly using chemical synthesiss, thermal decomposition method and oxidizing process etc., thermal decomposition method is generally by pyrolysis MoS for method3
To obtain target product, the preparation process of the method, equipment and simple to operate is not high to producing personnel specialty level requirement, fits
Answering property is stronger, but temperature control is critically important in the preparation due to the method, and temperature is low may to obtain amorphous state MoS2, temperature
Higher crystal then easily grows, while the elemental sulfur for producing is more serious to equipment corrosion, yield cannot often be ensured；Oxidizing process
It is to utilize MoCl3MoS is prepared in autoxidation reaction2, nanometer MoS obtained in oxidizing process2Purity is very high, and particle size is reachable
0.01-0.03 μm, but due to preparation process used in molybdenum carbonyl strong toxicity, while can also produce CO gases, to environment and
The impact of people is larger, thus constrains which and develop；Chemical synthesiss are typically called liquid-phase precipitation method, i.e., using liquid-phase chemical reaction
First synthesize MoS3, finally by MoS3Synthesis nanometer MoS2, course of reaction is simple, and easy to operate, yield is high, and low cost is to apply most
Extensive method.
Nanometer MoS is produced in existing utilization liquid-phase precipitation method2In, waste gas and waste liquid yield larger, raw material and reactant
Consume seriously, due to the long-term continued downturn of molybdenum bisuphide price market, while high consumption, as cost of investment is asked
Topic, below standard waste gas and waste are often directly externally discharged by enterprise, and these problems result in molybdenum bisuphide manufacturing enterprise category
In high pollution enterprise.In addition, the yield of existing molybdenum bisuphide manufacturing enterprise is often relatively low, can have toward contact inside product
Machine solvent（Prior art is using Organic substances such as pyridine, hydrazines as solvent）, production scale is less, it is impossible to realize that high-volume is continuous raw
Produce,, in reaction precipitation technique, often the cycle is longer for which, less efficient.Particularly intermediate product MoS is being prepared3When, production effect
Rate is in reduced levels.
Utility model content
Goal of the invention of the present utility model is：For above-mentioned problem, there is provided a kind of molybdenum trisulfide production is with instead
Device is answered, by optimizing MoS3Production technology and process units, prepare MoS quick3While, realize serialization green production.
The technical solution adopted in the utility model is as follows：A kind of molybdenum trisulfide production reaction unit, including reaction precipitation
Pond and waste gas recovering device, reaction settling basin include reaction tank, concentration basin, the supernatant between reaction tank and concentration basin
Pond, is recessed inner fovea part at the lower bottom part at least of reaction tank, equipped with the permanent magnetism sense for driving solution obliquely flow at inner fovea part
Device, supernatant bottom of pond portion is answered to be provided with slurry passage, reaction tank is connected with concentration basin by slurry passage, and waste gas recovering device sets
In the top of reaction tank, waste gas recovering device is connected with the top seal of reaction settling basin.
Further, reaction tank, supernatant liquid pool and concentration basin are mutually isolated by division board, and the top side of reaction tank is provided with
Material inlet, opposite side are provided with purified liquor outlet A, and the bottom of slurry passage is provided with slurry outlet.
Further, the side of concentration basin top clean solution tank upward is provided with purified liquor outlet B, and supernatant bottom of pond portion passes through division board
With slurry channel separation, and clear liquid mouth is provided with supernatant bottom of pond portion.
Further, portable plate is provided with slurry passage, and slurry passage controls the opening and closing of slurry passage by portable plate.
Further, waste gas recovering device includes the sealing flange located at reaction settling basin top, at the top of sealing flange
Air pump, located at the three-level alkali liquor absorption tower of air pump outfan, sealing flange is provided with reaction material import, three-level alkali liquor absorption tower
Absorbing liquid outfan be connected with the input of vaporizer, the material outfan of vaporizer is connected with reaction material import.
Used as a kind of alternative, reaction settling basin includes reaction tank and concentration basin, at reaction tank lower bottom part at least in
Into inner fovea part, equipped with the permanent magnet induction device for driving solution obliquely flow at inner fovea part, the bottom of concentration basin is provided with slurry to spill
Outlet, reaction tank and concentration basin are isolated by division board, and division board bottom is provided with portable plate, and reaction tank is by portable plate and concentration
Pond connects
Further, permanent magnet induction device includes frame and non-magnetic housing, is rotatably connected to main shaft in housing, and main shaft is by electricity
Motivation drives, and main shaft is provided with yoke, and spaced permanent magnet is housed in yoke, and two adjacent permanent magnet polarities are set on the contrary
Put.
Further, in order to improve magnetic conductivity, toughness and the corrosion resistance of yoke, electromagnetic agitation effect is made to reach most preferably, magnetic
Yoke is made up of iron-base amorphous alloy material, and iron-base amorphous alloy material is consisted of：Fe70Al3Ga2Y1.63V1.37In1
Co10B8Si3, which passes through following steps and is obtained：
Step one, raw material prepare, and it is 99.99% to take purity respectively, and granularity is 40 μm of Fe powder, and purity is 99.5%, granularity
For 80 μm of Al powder, purity is 99%, and granularity is 80 μm of Ga powder, and purity is 99%, and granularity is 75 μm of Y powder, and purity is
99.5%, granularity is 75 μm of V powder, and purity is 97.5%, and granularity is 120 μm of In powder, and purity is 98.5%, and granularity is 75 μm
Co powder, purity are 99.9%, and granularity is that 15 μm of B powder and purity are 99.9%, and granularity is 75 μm of Si powder, by atomic percent
Nominal alloying component is made into, being then placed in together with the sintered carbide ball of a diameter of 8mm in planetary type ball-milling tank carries out ball milling, ball
Before mill, ball grinder want evacuation process, when vacuum reaches 0.5Pa in the ball grinder, is filled with the argon of 1MPa into ball grinder,
During ball milling, drum's speed of rotation is 300r/min, and ball powder mass ratio is 25:1, Ball-milling Time is 150h, obtains iron-based amorphous powder；
Step 2, the iron-based amorphous powder for obtaining be placed in heat-treatment furnace made annealing treatment, annealing temperature is 550 DEG C,
Heating rate is 20 DEG C/min, and annealing time is 1h, the iron-based amorphous powder after being annealed；
Step 3, the iron-based amorphous powder after the annealing for obtaining is placed in thermal conductivity more than 30W/（m·K）Hard alloy
In mould, mould is assembled, then mould is placed in discharging plasma sintering equipment carries out high-pressure sinter, extract before sintering and burn
To 0.5Pa, during sintering, sintering pressure is 500MPa to the indoor vacuum of knot, and sintering temperature is 950 DEG C, heating rate is 90 DEG C/
Min, is incubated 8min, is finally quickly cooled to room temperature and obtains final product.
In sum, as a result of above-mentioned technical proposal, the beneficial effects of the utility model are：
1st, reaction tank is used for the dissolving and reaction of raw material, raw material under the agitation of permanent magnet induction device, reaction thoroughly and
Side reaction is few, a large amount of MoS of production3Be deposited in reaction tank sedimentation after, poured in concentration basin by slurry passage, least a portion of not
Sedimentation MoS3Precipitation is flowed in supernatant liquid pool through purified liquor outlet A, concentration basin MoS then to high concentration3Solution is preserved and is settled, dense
The MoS of contracting pond inner bottom part enrichment3Precipitation water content is few, and being flowed in filter by slurry outlet carries out coarse filtration, big to obtain
Amount water content few ground MoS3, least a portion of do not settle MoS3Precipitation is flowed in supernatant liquid pool, in supernatant liquid pool through purified liquor outlet B
Clear liquid by clear liquid mouth flow into filter in carry out smart filtration, with acquisition MoS as much as possible3, compared to prior art, instead
Answer the disposal ability of sedimentation tank big, can achieve continuous uninterrupted production, MoS3High income, the MoS in waste liquid3Content is few, former
Material wastes few, MoS3Yield big, meanwhile, the whole production cycle is shorter, and input cost is not substantially increased, income ratio
High；
2nd, by arranging permanent magnetism agitating apparatus, the solution in reaction tank is achieved and is at the uniform velocity stirred, the dissolving and dispersion of raw material
Effect reaches most preferably, solves the problems, such as that existing manual stirring or churned mechanically inconvenience and stirring are uneven.
3rd, the setting of waste gas recovering device achieves waste gas recycling, by the H produced in production process2S gases reclaim life
Into Na2S raw materials, and the Na that will be generated2S raw materials are rejoined in reaction tank, have on the one hand both solved problem of environmental pollution, separately
On the one hand realize the recycling of S again, reduce the consumption of raw material, improve yield and yield, whole production system is hardly
Poisonous fume is externally discharged, it is achieved that green production, routinely development potentiality is big；
4th, yoke adopts Fe70Al3Ga2Y1.63V1.37In1Co10B8Si3Iron-base amorphous alloy material, its magnetic conductivity and toughness
Not only be better than the existing silicon steel material for commonly using, compared to the ferrous materials of general high intensity, except manufacturing cost relatively high by one
Point is outer, and the intensity of Fe-based amorphous alloy composite of the present utility model, decay resistance and anti-wear performance are better than typically high-strength
More than 2 times of the ferrous materials of degree, its intensity is up to 1.83GPa, even if yoke is chronically under the working environment of severe corrosive（Three
Produce in molybdenum sulfide production environment and contain a certain amount of H2The deep-etching gas such as S）, its excellent corrosion resistance can guarantee that yoke has
Longer usage cycles, reduce and change number of times and replacement cost, coming into operation for a long time beneficial to enterprise, and better results for input.
Description of the drawings
Fig. 1 is the production system that a kind of molybdenum trisulfide production reaction unit of the present utility model is used for nanometer class molybdenum disulfide
Structural representation during system；
Fig. 2 is molybdenum trisulfide production reaction unit structural representation of the present utility model；
Fig. 3 is permanent magnet induction apparatus structure schematic diagram of the present utility model；
Fig. 4 is another kind of situation of reaction precipitation pool structure of the present utility model.
Labelling in figure：1 is reaction settling basin, and 101 is reaction tank, and 1011 is material inlet, and 1012 is purified liquor outlet A,
1013 is inner fovea part, and 1014 is permanent magnet induction device, and 10141 is frame, and 10142 is housing, and 10143 is main shaft, and 10144 is magnetic
Yoke, 10145 is permanent magnet, and 102 is concentration basin, 1021 purified liquor outlet B, and 103 is supernatant liquid pool, and 1031 is clear liquid mouth, and 1032 are
Slurry passage, 1033 is slurry outlet, and 104 is division board, and 1041 is portable plate, and 2 is cleaning device, and 3 is vacuum drier, 4
For disintegrating machine, 5 is powder crusher, and 6 is gas solid reactor, and 7 is waste gas recovering device, and 701 is sealing flange, and 7011 are reaction
Material import, 702 is air pump, and 703 is three-level alkali liquor absorption tower, and 704 is vaporizer, and 8 is Pulp pump A, and 9 is Pulp pump B, 10 be plus
Pressure filter, 11 is flame filter press, and 12 is membrane separation device, and 13 is quantifier, and 14 is dust-precipitator, and 15 is cleaner unit, and 16 are
Collection device.
Specific embodiment
Below in conjunction with the accompanying drawings, this utility model is described in detail.
In order that the purpose of this utility model, technical scheme and advantage become more apparent, below in conjunction with accompanying drawing and enforcement
Example, is further elaborated to this utility model.It should be appreciated that specific embodiment described herein is only in order to explaining
This utility model, is not used to limit this utility model.
Embodiment one
As shown in Figure 1 to Figure 3, the production system of a kind of nanometer of class molybdenum disulfide, it include that molybdenum trisulfide production is reacted
Device, cleaning device 2, vacuum drier 3, disintegrating machine 4, powder crusher 5 and gas solid reactor 6.
Molybdenum trisulfide production reaction unit, including reaction settling basin 1 and waste gas recovering device 7, reaction settling basin 1, bag
Include reaction tank 101, concentration basin 102, the supernatant liquid pool 103 between reaction tank 101 and concentration basin 102, waste gas recovering device 7
Located at 101 top of reaction tank, reaction settling basin 1 is used for reacting and precipitating intermediate product, as shown in Fig. 2 reaction tank 101, on
Clean solution tank 103 and concentration basin 102 are arranged successively, mutually isolated by division board 104 between them, the top one of reaction tank 101
Side is provided with material inlet 1011, for, in the entrance reaction tank 101 of raw material, opposite side is provided with purified liquor outlet A1012, purified liquor outlet
The position of A1012 suitably can be adjusted as needed, and purified liquor outlet A1012 is used for excluding the clear liquid in reaction tank 101, with
When the solution in reaction tank 101 exceed specified volume when, plussage can enter supernatant liquid pool by purified liquor outlet A1012 overflows
In 103, with the impact of solution excess in elimination reaction pond 101, guarantee safe production.
As shown in Fig. 2 be recessed inner fovea part 1013 at the lower bottom part of reaction tank 101 at least, inner fovea part 1013 cuts
Face is curved, equipped with the permanent magnet induction device 1014 for driving solution obliquely flow, preferably inner fovea part 1013 pairs at inner fovea part 1013
Claim to arrange at two, be separately positioned on 101 liang of diagonal angles of reaction tank, while permanent magnet induction device 1014 is installed at inner fovea part 1013,
By the oblique driving of the permanent magnet induction device 1014 at two ends angle, solution forms oblique convection current in reaction tank, and then makes stirring
More preferably, the chemical reaction in reaction tank carries out more thorough effect.
In figure 3, permanent magnet induction device 1014 includes frame 10141 and non-magnetic housing 10142, rotates in housing 10142
Main shaft 10143 is connected with, main shaft 10143 is driven by motor, main shaft 10143 is provided with yoke 10144, in yoke 10144
Spaced permanent magnet 10145 is housed, adjacent two permanent magnets, 10145 opposite polarity is arranged, after actuating motor, main shaft
10143 rotarily drive yoke 10144 and permanent magnet 10145 is rotated, and magnetic field will be acted in reaction tank 101 in rotation process
Solution and produce continuously induced potential and faradic current, faradic current and the action of a magnetic field produce electromagnetic push, due to
Permanent magnet 10145 rotates, thus its electromagnetic push makes the solution of 101 bottom of reaction tank ramp up simultaneously for tangential thrust
Reach at the top of solution, and then solution is constantly stirred, the solution for constantly stirring makes raw material ammonium molybdate, raw material sodium sulfide, dispersant
It is uniformly dispersed with HCl solution, beneficial to the carrying out of reaction, significantly reduces the generation of side reaction.
103 bottom of supernatant liquid pool is provided with clear liquid mouth 1031 and slurry passage 1032,102 top of concentration basin clean solution tank upward
103 side is provided with purified liquor outlet B1021, and reaction tank 101 is connected with concentration basin 102 by slurry passage 1032, slurry passage
1032 bottom is provided with slurry outlet 1033, and slurry passage 1032 is controlled by slidable portable plate 1041 or switch valve
Solution in reaction tank 101 enters concentration basin 102, and the highly concentrated solution being settled out in reaction tank 101 can be made to be transferred to concentration basin
Continue precipitation in 102, the purpose for so arranging is that one is to reduce the sedimentation time, reduces the impact of solvent, and shortening is obtained
The time of required slurry, two is can to continue through reaction tank to produce more MoS3, i.e., obtained due to one-time reaction
MoS3Precipitation is less, and while can making to be deposited in by way of transfer is precipitated continuation sedimentation, reaction tank 101 can continue to use next life
Produce MoS3Precipitation, reduces the addition of the materials such as solvent, improves the disposal ability of reaction tank 101, reaction precipitation is greatly shortened
Time.When needing to filter the slurry for having precipitated, portable plate 1041 or switch valve need to be only closed, open slurry outlet
1033.In concentration basin 102, the slurry for having precipitated is transferred out of reaction settling basin 1, remaining clear liquid by slurry passage 1032
Then flowed in supernatant liquid pool, in the same manner by purified liquor outlet B1021, the work of the effect of purified liquor outlet B1021 and purified liquor outlet A1012
With the same, contribute to discharge clear liquid and prevent over capacity.
Waste gas recovering device 7, including the sealing flange 701 located at 1 top of reaction settling basin, sealing flange 701 is used for close
Envelope reaction settling basin 1, the H for preventing2S gases are externally discharged, and the top of sealing flange 701 is provided with air pump 702, air pump 702
For conveying the H produced in reaction settling basin 12S gases, and by H2S gases are delivered to three-level alkali liquor absorption tower 703, reaction tank
The sealing flange 701 on 101 positive top is provided with reaction material import 7011, enters in reaction tank 101 for reaction material, three-level alkali
The absorbing liquid outfan on liquid absorption tower 703 is connected with the input of vaporizer 704, the material outfan of vaporizer 704 be located at
Reaction material import 7011 on sealing flange 701 connects, after three-level alkali liquor absorption tower 703 is recycled to waste gas, remaining
Externally can directly discharge after gas is qualified after testing, that is, reach national regulation H2S gases maximum concentration is less than 150mg/m3When,
Externally can directly discharge, otherwise also need to continue cycling through process；Vaporizer 704 is used for concentrating the Na for generating2S solution, concentration
Na afterwards2S solution can be directly used for preparing MoS3, it is achieved that devil liquor recovery is using circulation, and then reduces consuming cost.
The input connection slurry outlet 1033 of Pulp pump A8, for slurry is delivered in pressing filter 10, slurry
The input connection clear liquid mouth 1031 of pump B9, for clear liquid is delivered in flame filter press 11.By pressing filter 10 with
11 common filtration of flame filter press, MoS3The yield of precipitation reaches highest, reduces MoS3The loss of precipitation.
Pressing filter 10, the feeding mouth of pressing filter 10 are connected with Pulp pump A8, the filtering residue mouth of pressing filter 10
It is connected with cleaning device 2, the filtrate (liquid of pressing filter 10 is connected with flame filter press 11；
Flame filter press 11, the feeding mouth of flame filter press 11 are connected with Pulp pump B9, the filtering residue mouth of flame filter press 11
It is connected with cleaning device 2, the filtrate (liquid of flame filter press 11 is connected with membrane separation device 12, the filtrate of membrane separation device 12 goes out
Mouth is connected with reaction material import 7011.
Membrane separation device 12 is used for separating ammonium chloride, reduces the ammonium chloride content in filtrate, to desalinate filtrate, makes filtrate
Used in reaction tank being gone successively to as recycling design, to realize that solvent is recycled, and existing production technology is direct
Solvent is externally discharged, the solvent of high strength ammonium-chloride can also cause severe contamination to environment, and therefore, the recovery of solvent is not only saved
Cost is saved, the pollution to environment has been also reduced, membrane separation device 12 can be membrance separation desalination apparatus.
Cleaning device 2 be used for filtration after MoS3Precipitation is cleaned, it is preferred to use ultrasonic cleaning apparatus.Cleaning dress
Put 2 material outlet to be connected with vacuum drier 3, the material outlet of vacuum drier 3 is connected with quantifier, vacuum drier 3
By MoS3After precipitation vacuum drying, MoS is calculated by quantifier 133Yield, raw material reaction is analyzed by the yield data that obtains
Whether carry out, thoroughly, if yield is relatively low, adjusting S：The mol ratio of Mo and the proportional quantity of HCl solution, until yield is close to or big
Till theoretical yield.
Material in quantifier 13 is delivered in disintegrating machine 4 by conveyer device, the outlet of disintegrating machine 4 and powder crusher
5 connections, the outlet of powder crusher 5 are connected with dust-precipitator 14, and the dust outlet of dust-precipitator 14 is connected with gas solid reactor 6, gas
The waste gas outlet of gas-solids reactors 6 is connected with cleaner unit 15, and the powder body outlet of gas solid reactor 6 is connected with collection device 16, dedusting
The dust outlet of device 15 is connected with collection device 16, and the outlet port of cleaner unit 15 is connected with waste gas recovering device 7.
4 couples of bulk MoS of disintegrating machine3Granulated, with to block MoS3Carry out pretreatment, then by granulating after
MoS3It is put in powder crusher 5 and makes powder, powder MoS3Equably it is layered in gas solid reactor 6, more specifically, gas
Gas-solids reactors 6 be fixed bed gas solid reactor, the MoS after powder3Be conducive to and H2It is fully contacted and reacts, contracts significantly
In the short response time, reduce energy consumption.Dust-precipitator 14 is used for collecting powder MoS3, cleaner unit 15 is used for reclaiming to be taken away by gas
Amount of powder MoS2, furtherly, the three-level alkali liquor absorption tower of the outlet port of cleaner unit 15 and waste gas recovering device 7
703 connections, with the H produced in gas recovery2S gases, now, in the gas of 703 external discharge of three-level alkali liquor absorption tower, its group
Into being N2And H2, also a small amount of unabsorbed H2S gases and a small amount of air, for making waste gas discharge be up to state standards, it is stipulated that
H in the waste gas of the discharge of three-level alkali liquor absorption tower 7032S gas contents have to be lower than 150mg/m3.
In above-described embodiment, the production method of nanometer class molybdenum disulfide is comprised the following steps：
Step 1, cleaning reaction settling basin 1, by material inlet 1011 of the deionized water of design flow by reaction settling basin 1
Add in reaction tank 101, solid material ammonium molybdate and raw material sodium sulfide are pressed S then：Mo mol ratios are 4-5:1 is entered by raw material
Mouth 1011 is added in reaction tanks 101, starts permanent magnet induction device 1014, after solid is thoroughly mixed dissolving, adds proportional quantity
Dispersant is disperseed, then booster air pump 702, and wherein, dispersant can be that the poly- diethanol that mass fraction is 11% is water-soluble
Liquid, 6-7% of the addition for solid material ammonium molybdate mass fraction, the temperature control in reaction tank is at 30-35 DEG C；
After the completion of step 2, step 1, wait reaction tank to be sufficiently stirred for reacting, into reaction tank 101, then add proportional quantity
HCl solution be neutralized reaction, wherein, the mass fraction of HCl solution is 36%-40%, waits reaction tank 101 to be sufficiently stirred for instead
Should, turbid solution is obtained, when the turbidity of solution no longer occurs significant change, permanent magnet induction device 1014 is closed, is made reaction tank
Turbid solution in 101 staticly settles layering；
When being substantially layered occur in step 3, the turbid solution in step 2, slurry passage 1032 is opened, turbid solution bottom is highly concentrated
Degree solution is poured in concentration basin 102, after highly concentrated solution all incorporates concentration basin 102, closes slurry passage 1032, high concentration
Solution in concentration basin 102 continues to staticly settle layering, now, if needing to continue on for raw material hybrid reaction in reaction tank 101
When, then continue to add reaction raw materials to reaction tank 101 and be again started up permanent magnet induction device 1014, if needing not continue to react,
Purified liquor outlet A1012 is then opened, and the solution in reaction tank 101 is flowed in supernatant liquid pool 103；
When being substantially layered occur in step 4, the highly concentrated solution in the concentration basin 102 of step 3, slurry outlet is opened
1033, the slurry for being formed 102 inner bottom part of concentration basin is pumped into by Pulp pump A8 and is filtered in pressing filter 10, to be concentrated
After the slurry of 102 inner bottom part of pond all flows out, purified liquor outlet B9 is opened, surplus solution flows into supernatant liquid pool 103 in concentration basin 102
Interior；
Step 5, the clear liquid mouth 1031 for opening 103 bottom of supernatant liquid pool, the solution in supernatant liquid pool 103 pass through Pulp pump B9
Pump into and filtered in flame filter press 11；
Step 6, pressing filter 10 are filtered to supplied materials after receiving supplied materials, add deionized water to be desalinated during filtration
Filter, the filtering residue for obtaining is entered by filtering residue mouth and cleaned in cleaning device 2, and filtrate then enters sheet frame mistake by filtrate (liquid
Filtered in filter 11 again；
Step 7, flame filter press 11 are filtered to supplied materials after receiving supplied materials, and the filtering residue for obtaining is entered clearly by filtering residue mouth
Cleaned in cleaning device 2, filtrate is then entered by filtrate (liquid and carry out in membrane separation device 12 membrance separation desalt processing, film point
From device 12 by supplied materials desalt processing after, entered in reaction tank 101 by reaction material import and realize cycling utilization of wastewater；
Step 8, cleaning device 2 receive supplied materials after cleaning treatment is carried out to supplied materials, then by cleaning after supplied materials enter very
In empty drying machine 3, vacuum drier 3 carries out vacuum drying treatment to supplied materials, and baking temperature is 80-90 DEG C, after the completion of drying, obtains
To lump material, lump material is delivered to quantifier and is weighed, whether calculated yield, inspection raw material reaction are carried out thoroughly, if
Yield is less than 90%, then adjust S：The mol ratio of Mo and the proportional quantity of HCl solution, until yield near or above theoretical yield is
Only；
After the completion of step 9, step 8, dried material is delivered to carry out in disintegrating machine 4 in small, broken bits, make lump material crush
For granular material, then the granular material for obtaining is delivered in powder crusher 5 and is crushed, powder crusher 5 will
Crushing material is that mean diameter is 0.6-0.8 μm of powder, is then collected by dust-precipitator 14；
Step 10, dust-precipitator 14 enter the powder of collection in gas solid reactor 6, empty the air in gas solid reactor 6,
Under vacuum conditions, it is 4 to be passed through nitrogen and hydrogen volume ratio in 500-900 DEG C:3 mixed gas carry out gas-solid reaction, reaction
Oxygen content in Shi Yange control gases is less than 0.001mL/m3, after reacting completely, cleaner unit 15 will be gentle for the powder that collects
Powder in gas-solids reactors 6 is entered in collection device 16, that is, obtain nano molybdenum disulfide product, and waste gas is then by cleaner unit 15
Outlet port is entered in waste gas recovering device 7；
Step 11, waste gas recovering device 7 receive the waste gas for coming Self-duster 15 and air pump 702, and waste gas is sent into three-level
Carry out alkali liquor absorption in alkali liquor absorption tower 703, to be absorbed completely after, alkali liquor is entered in vaporizer 704 by absorbing liquid outfan
It is evaporated concentration, residual gas qualified rear directly externally discharge after testing；
Step 12, vaporizer 704 receive alkali liquor and carry out evaporation and concentration, and after concentration of lye to be concentrated is qualified, alkali liquor leads to
Cross reaction material import 7011 to enter in reaction tank 101, realize the cyclic utilization of waste.
In step 10, intensification order is that first intensification gas solid reactor 6 then passes to mixed gas to 500-550 DEG C,
Air pressure in detection gas solid reactor 6, when there is significant change in air pressure in the gas solid reactor 6, intensification gas solid reactor 6 to
800 DEG C, continue observation air pressure change, when being decreased obviously occurs in air pressure, 6 to 900 DEG C of intensification gas solid reactor treats stable gas pressure
Afterwards, reduce by 6 temperature of gas solid reactor to be incubated to 800 DEG C, then slow cooling is to room temperature, wherein, when mixed gas are passed through, gaseous mixture
The air inflow of body keeps 70-90ml/min.
In above-described embodiment, in order to improve magnetic conductivity, toughness and the corrosion resistance of yoke, electromagnetic agitation effect is made to reach most
Good, yoke is made up of iron-base amorphous alloy material, and iron-base amorphous alloy material is consisted of：Fe70Al3Ga2Y1.63V1.37In1
Co10B8Si3, which passes through following steps and is obtained：
Step one, raw material prepare, and it is 99.99% to take purity respectively, and granularity is 40 μm of Fe powder, and purity is 99.5%, granularity
For 80 μm of Al powder, purity is 99%, and granularity is 80 μm of Ga powder, and purity is 99%, and granularity is 75 μm of Y powder, and purity is
99.5%, granularity is 75 μm of V powder, and purity is 97.5%, and granularity is 120 μm of In powder, and purity is 98.5%, and granularity is 75 μm
Co powder, purity are 99.9%, and granularity is that 15 μm of B powder and purity are 99.9%, and granularity is 75 μm of Si powder, by atomic percent
Nominal alloying component is made into, being then placed in together with the sintered carbide ball of a diameter of 8mm in planetary type ball-milling tank carries out ball milling, ball
Before mill, ball grinder want evacuation process, when vacuum reaches 0.5Pa in the ball grinder, is filled with the argon of 1MPa into ball grinder,
During ball milling, drum's speed of rotation is 300r/min, and ball powder mass ratio is 25:1, Ball-milling Time is 150h, obtains iron-based amorphous powder；
Step 2, the iron-based amorphous powder for obtaining be placed in heat-treatment furnace made annealing treatment, annealing temperature is 550 DEG C,
Heating rate is 20 DEG C/min, and annealing time is 1h, the iron-based amorphous powder after being annealed；
Step 3, the iron-based amorphous powder after the annealing for obtaining is placed in thermal conductivity more than 30W/（m·K）Hard alloy
In mould, mould is assembled, then mould is placed in discharging plasma sintering equipment carries out high-pressure sinter, extract before sintering and burn
To 0.5Pa, during sintering, sintering pressure is 500MPa to the indoor vacuum of knot, and sintering temperature is 950 DEG C, heating rate is 90 DEG C/
Min, is incubated 8min, is finally quickly cooled to room temperature and obtains final product.
Measure through experiment, Fe70Al3Ga2Y1.63V1.37In1Co10B8Si3The saturation induction of iron-base amorphous alloy material is strong
Spend for 0.85T, coercivity is 6.841A/m, intensity reaches 1.83GPa, and consistency reaches 97.9%.
Embodiment two
Embodiment two is identical with embodiment one, and its difference is, the structure of reaction settling basin 1 is different, such as Fig. 4 institutes
Show, reaction settling basin 1 includes reaction tank 101 and concentration basin 102, is recessed inner fovea part at 101 lower bottom part of reaction tank at least
1013, equipped with the permanent magnet induction device 1014 for driving solution obliquely flow at inner fovea part 1013, the bottom of concentration basin 102 is provided with slurry
Material outlet 1033, reaction tank 101 and concentration basin 102 are isolated by division board 104, and 104 bottom of division board is provided with slidable work
Dynamic plate 1041 or switch valve, reaction tank 101 are connected with concentration basin 102 by portable plate 1041 or switch valve, and slurry goes out
1033 mouthfuls are connected with Pulp pump B9, and the delivery outlet of Pulp pump B9 is connected with flame filter press 11, that is, eliminate pressing filter 10
With Pulp pump A8, its filter effect also can be identical with embodiment one, but than relatively time-consuming, the service life of flame filter press 11 is more real
The flame filter press 11 that applies in example one is short.
Preferred embodiment of the present utility model is the foregoing is only, not in order to limit this utility model, all at this
Any modification, equivalent and improvement that is made within the spirit and principle of utility model etc., should be included in this utility model
Protection domain within.
Claims (7)
1. a kind of molybdenum trisulfide production reaction unit, including reaction settling basin and waste gas recovering device, it is characterised in that reaction
Sedimentation tank includes reaction tank, concentration basin, the supernatant liquid pool between reaction tank and concentration basin, the lower bottom part at least of reaction tank
Place is recessed inner fovea part, and equipped with the permanent magnet induction device for driving solution obliquely flow at inner fovea part, supernatant bottom of pond portion is provided with
Slurry passage, reaction tank are connected with concentration basin by slurry passage, and waste gas recovering device is located at the top of reaction tank, waste gas recovery
Device is connected with the top seal of reaction settling basin.
2. molybdenum trisulfide production reaction unit as claimed in claim 1, it is characterised in that reaction tank, supernatant liquid pool and dense
Contracting pond is mutually isolated by division board, and the top side of reaction tank is provided with material inlet, and opposite side is provided with purified liquor outlet A, slurry
The bottom of passage is provided with slurry outlet.
3. molybdenum trisulfide production reaction unit as claimed in claim 1, it is characterised in that concentration basin top clean solution tank upward
Side be provided with purified liquor outlet B, supernatant bottom of pond portion is by division board and slurry channel separation, and is provided with supernatant bottom of pond portion
Clear liquid mouth.
4. molybdenum trisulfide production reaction unit as claimed in claim 1, it is characterised in that be provided with activity in slurry passage
Plate, slurry passage control the opening and closing of slurry passage by portable plate.
5. molybdenum trisulfide production reaction unit as claimed in claim 1, it is characterised in that waste gas recovering device includes being located at
The sealing flange on reaction settling basin top, the air pump at the top of sealing flange, located at the three-level alkali liquor absorption of air pump outfan
Tower, sealing flange are provided with reaction material import, and the absorbing liquid outfan of three-level alkali liquor absorption tower is connected with the input of vaporizer,
The material outfan of vaporizer is connected with reaction material import.
6. molybdenum trisulfide production reaction unit as claimed in claim 1, it is characterised in that reaction settling basin includes reaction tank
And concentration basin, inner fovea part is recessed at reaction tank lower bottom part at least, at inner fovea part equipped with the obliquely flow of driving solution forever
Magnetic-inductive device, the bottom of concentration basin are provided with slurry outlet, and reaction tank and concentration basin are isolated by division board, and division board bottom sets
There are portable plate, reaction tank to connect with concentration basin by portable plate.
7. molybdenum trisulfide production reaction unit as claimed in claim 1, it is characterised in that permanent magnet induction device includes frame
And non-magnetic housing, main shaft is rotatably connected in housing, main shaft is driven by motor, and main shaft is provided with yoke, is equipped with yoke
Spaced permanent magnet, two adjacent permanent magnet polarities are reversed.
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| CN201620886296.6U CN206014431U (en) | 2016-08-16 | 2016-08-16 | Molybdenum trisulfide production reaction unit |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114699894A (en) * | 2022-03-07 | 2022-07-05 | 中船(邯郸)派瑞特种气体股份有限公司 | Recovery device and method for residual gas of gas-liquid hydrolysis reaction |
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2016
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114699894A (en) * | 2022-03-07 | 2022-07-05 | 中船(邯郸)派瑞特种气体股份有限公司 | Recovery device and method for residual gas of gas-liquid hydrolysis reaction |
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Granted publication date: 20170315 Termination date: 20180816 |