CN109082709A - A method of utilizing sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers - Google Patents
A method of utilizing sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers Download PDFInfo
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- CN109082709A CN109082709A CN201811009007.4A CN201811009007A CN109082709A CN 109082709 A CN109082709 A CN 109082709A CN 201811009007 A CN201811009007 A CN 201811009007A CN 109082709 A CN109082709 A CN 109082709A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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Abstract
The invention discloses a kind of methods using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers, belong to resource reclaim reutilization technology field.The present invention is by pretreated Desulphurization and MgCl2Slurries are made after stirring in solution, and saturation Ca (OH) is added dropwise in slurries2, the range of the pH value of slurries is adjusted between 8~9, then slurries are transferred in autoclave and carries out hydrothermal synthesis and obtains calcium sulfate crystal whiskers.The present invention is using sintering flue gas desulfurization ash as raw material, using hydrothermal system oxidation coordinate system for calcium sulfate crystal whiskers, realizes that sintering flue gas desulfurization ash oxidation coordinate system for calcium sulfate crystal whiskers, solves CaSO3It is difficult to quickly oxidation and the longer problem of calcium sulfate crystal whiskers preparation process flow, the recovery utilization rate of Desulphurization is improved, improves the quality of calcium sulfate crystal whiskers.
Description
Technical field
The present invention relates to resource reclaims to recycle field, utilizes sintering flue gas desulfurization ash one more specifically to a kind of
The method of footwork synthesis calcium sulfate crystal whiskers.
Background technique
As country is to SO2The reinforcement of the reinforcement of contamination control and China environmental protection consciousness, sinter flue gas desulfurization ash
Comprehensive utilization in terms of research be gradually concerned by people, and the utilization of sinter flue gas desulfurization ash can be reduced because of heap
Consumed fund, land occupation and environmental pollution are put, reduces the dosage of the natural gypsum, and then reduce the exploitation of the natural gypsum
Amount, preserves the ecological environment.Therefore, many colleges and universities and enterprise have carried out sinter flue gas desulfurization ash comprehensive utilization aspect a large amount of
Research, such as sulfuric acid, cement retarder, gypsum building material and calcium sulfate crystal whiskers are prepared using sintering flue gas desulfurization ash.Wherein,
Calcium sulfate crystal whiskers added value with higher is prepared using sintering flue gas desulfurization ash, calcium sulfate crystal whiskers are grown with single crystal form
A kind of staple fiber, it has uniform cross section, complete shape and the perfect internal structure of height, with glass fibre phase
Than advantage is that it has high intensity, and subtle size is easier to and the organic high molecular compounds such as resin, rubber, plastics
In conjunction with, and the presentation quality of product is excellent.Desulfurization stone can not only be reduced by preparing calcium sulfate crystal whiskers as raw material using desulfurized gypsum
Pollution of the cream to environment can also save natural gypsum resource, and open new way for the high value added utilization of desulfurized gypsum
Diameter, but the method that existing Desulphurization prepares calcium sulfate crystal whiskers is not perfect, so that calcium sulfate crystal whiskers is second-rate, seriously
Limit the high efficient resourcing application of Desulphurization.
Through patent retrieval, the Shi Peiyang of Northeastern University has also carried out correlative study, and has applied for related patents, utilizes sintering
Mine flue gas desulfurization byproduct prepares the method (application number: 201010545829.1 of calcium sulfate crystal whiskers；The applying date: 2010.11.16)
With the method (application number: 200810011193.5 for preparing calcium sulfate crystal whiskers using desulfurized gesso of flue gas；The applying date:
2008.04.25), this method provides a kind of approach for the recycling application of desulfurizing byproduct.But existing method production
Obtained calcium sulfate crystal whiskers are second-rate, limit the value added applications of desulfurizing byproduct.In addition, the title of innovation and creation
Are as follows: the processing unit (number of patent application: CN201610076883.3, data of publication of application: 2016.05.04) of semi-dry desulphurization ash,
The processing unit is by being arranged adsorption tower in the top of heating furnace, and the flue gas that heating semi-dry desulphurization ash generates is in inlet air stack
It enters back into after being cooled down by the cold wind that air-introduced machine is blown out into lower adsorption chamber, the activated coke in lower adsorption chamber is to the SO in flue gas2Into
Row adsorbs for the first time, and then flue gas is entered in upper adsorption chamber by transition flue duct, and the activated coke in upper adsorption chamber is in flue gas
SO2It carries out second to adsorb, then flue gas enters after outlet flue by being discharged in chimney.It has been achieved rapidly to half-dried
Method Desulphurization carries out desulfurization process, solves the problems, such as the secondary pollution of semi-dry desulphurization ash, but still without solving to Desulphurization
Utilization again the technical issues of.In addition, the title of innovation and creation are as follows: the processing unit and processing method of a kind of Desulphurization are (specially
Sharp application number: CN201610344246.X, data of publication of application: 2016.10.12), the processing by the way that a kind of Desulphurization is arranged fills
It sets, comprising: Vertical Mill, dust-precipitator, hot-blast stove, a hot air pipe and second heat air hose；The slag of slag entrance is offered on Vertical Mill
Entrance；Dust-precipitator is connect with the Vertical Mill；The junction of hot air pipe and second heat air hose offers mixed wind entrance.Passing through will
Desulphurization oxidation modification in hot wind so that the slag powders product setting time formed greatly shortens, and has been saved low temperature and has been forged
Equipment investment and process cost are burnt, efficiently solving Desulphurization processing mode in the prior art causes processing cost to increase and formed
The technical issues of new pollution sources, but still the separation problem without solving iron powder in Desulphurization.
Summary of the invention
1. technical problems to be solved by the inivention
The present invention prepares the second-rate problem of calcium sulfate crystal whiskers for Desulphurization in the prior art, provides a kind of benefit
With the method for sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers, the present invention carries out except iron Desulphurization, and uses hydro-thermal
System oxidation coordinate system improves the quality of calcium sulfate crystal whiskers for calcium sulfate crystal whiskers, and can reduce Desulphurization in preparation process
Pollution to environment.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention are as follows:
A kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers of the invention, including
Step 1: Desulphurization pretreatment
Iron powder in Desulphurization is separated with Desulphurization, the bulky grain insoluble matter in Desulphurization is weeded out, obtains pretreated
Desulphurization；
Step 2: calcium sulfate crystal whiskers are prepared
By pretreated Desulphurization and MgCl2Solution is mixed to get slurries, then slurries are transferred to the high pressure of reaction unit
In reaction kettle, and oxygen is passed through into autoclave, the pressure for adjusting in autoclave is 1~2MPA, temperature be 120~
180℃；To the hydrothermal synthesis calcium sulfate crystal whiskers in autoclave.
Preferably, the step of step 2 are as follows:
(1) MgCl that compound concentration is 2%2Solution serves as medium crystallization agent, to MgCl2Solution is added pretreated Desulphurization and stirs
It mixes and uniformly obtains slurries, the solid-to-liquid ratio for controlling slurries is 1/15~1/20；
(2) Ca (OH) of saturation is added dropwise into slurries2Solution, the pH for adjusting slurries is 8~9；
(3) slurries are added in autoclave, are filled with oxygen into autoclave after closing autoclave top cover
Gas, and the slurries in autoclave are stirred, stirring intensity is 400~600r/min, and the reaction time is 2~3h, from
And the hydrothermal synthesis calcium sulfate crystal whiskers in autoclave.
Preferably, the step of step 1 are as follows: Desulphurization is added in Desulphurization iron powder separator and separates iron powder, desulfurization
Desulphurization is blown to iron powder reclaiming chamber body by the blast pass that the blast pipe of grey iron powder separator generates, and electromagnet generates magnetic
Power is by the iron powder adsorption in Desulphurization in the surface of cotton sleeve；The desulfurization after iron powder is separated after closing the blast pass of blast pipe
Ash is drop in accumulator tank under the effect of gravity；The Desulphurization for taking out separation iron powder from accumulator tank is mixed with water, weeds out Desulphurization
In bulky grain insoluble matter, then the Desulphurization for weeding out bulky grain insoluble matter is filtered by vacuum, obtains pretreated Desulphurization.
Preferably, reaction unit includes oxygen cylinder and autoclave, and oxygen cylinder passes through pipeline and autoclave top
Air inlet be connected, oxygen valve is provided on air inlet, is provided with relief valve on the pipeline between air inlet and autoclave,
It is provided with air gauge on the autoclave, is provided with stirring blade in autoclave.
Preferably, step 1: the pretreated specific steps of Desulphurization are as follows:
(1) Desulphurization is added in iron powder recyclable device Desulphurization iron powder separator, opens electromagnet, opens simultaneously
The air valve of blowback gas tank, the blowback air in blowback gas tank flow through pipeline enter electromagnet core cylinder it is intracardiac, then blowback air-flow
It is overflowed from the venthole on iron core surface to electromagnet exterior；
(2) air blast blower is opened, the blast pass that air blast blower generates is recycled through the penetrating iron powder of blast pipe from bottom to top
In cavity；
(3) Desulphurization is delivered in blast pipe by desulfurization ash-pit；
(4) Desulphurization is blown to iron powder reclaiming chamber body by the blast pass of blast pipe, and the iron powder in Desulphurization is adsorbed
In the surface of cotton sleeve；
(5) blast pass of blast pipe is closed, the Desulphurization after separating iron powder is drop in accumulator tank under the effect of gravity；
(6) it goes the Desulphurization of iron power removing to mix with water from accumulator tank taking-up, weeds out bulky grain insoluble matter, then big will be weeded out
The Desulphurization of grain insoluble matter, which is placed in Suction filtration device, to be filtered by vacuum, and pretreated Desulphurization is obtained.
Preferably, the blowback air stream in step 1 (1) in blowback gas tank respectively enters the first air-flow branch by air-flow supervisor
Pipe and the second airflow manifold, and the flow of the first back-flushing valve and the second back-flushing valve is controlled simultaneously.
Preferably, Desulphurization is added to desulfurization ash-pit in step 1 (3), opens the air valve of pressurized gas, pressurized gas
It pressurizes to desulfurization ash-pit, then opens Material valve, Desulphurization is delivered in blast pipe through delivery pipe in desulfurization ash-pit.
Preferably, Desulphurization is blown to iron powder reclaiming chamber body by the blast pass of blast pipe in step 1 (4), is being blown
Desulphurization is blowed to around electromagnet under the action of air-flow, and the iron powder in Desulphurization is adsorbed in cotton sleeve by electromagnet
Surface, blowback air stream is overflowed outward by the venthole on electromagnet core surface at the same time, and Desulphurization is avoided to penetrate into cotton set
In cylinder.
Preferably, iron powder recyclable device Desulphurization iron powder separator includes blast pipe, iron powder recycling cavity, top cover and anti-
Air blowing tank；Electromagnet and cotton sleeve are provided in iron powder reclaiming chamber body, the cotton sleeve is wrapped in the outside of electromagnet, electricity
Magnet includes conducting wire and iron core, and wherein conducting wire is wound in the outside of iron core, and the surface of iron core offers venthole, the venthole with
The cylinder heart of iron core is connected；Top cover is set to the top of iron powder recycling cavity, which is internally provided with filter layer；Blast pipe
It is set to the bottom of iron powder recycling cavity, Desulphurization is entered in iron powder reclaiming chamber body by blast pipe；Above-mentioned blowback gas tank passes through
Gas pipeline is connected with the cylinder heart of iron core, and air inlet bottom of the tube is provided with accumulator tank.
3. beneficial effect
Using technical solution provided by the invention, compared with existing well-known technique, there is following remarkable result:
(1) a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers of the invention, by Desulphurization
In iron powder separated with Desulphurization, remove Desulphurization in bulky grain insoluble matter, obtain pretreated Desulphurization, will be pretreated
Desulphurization and MgCl2Solution stirs to obtain slurries, then by slurries be transferred in the autoclave of reaction unit into
Row hydrothermal synthesis obtains calcium sulfate crystal whiskers；It, can be to avoid being entrained in Desulphurization by the way that the iron powder in Desulphurization is separated removal
Iron powder in hydrothermal system with the CaSO in Desulphurization3The oxygen dissolved in contention slurries, and prevent the iron in Desulphurization
Powder becomes the crystallization attachment point of newborn calcium sulfate, thus leads to a large amount of forming cores of calcium sulfate crystal whiskers, hinders the growth of calcium sulfate crystal whiskers
Process, while coordinate system is aoxidized using hydrothermal system, the quality of calcium sulfate crystal whiskers can be improved for calcium sulfate crystal whiskers；
(2) a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers of the invention, blast pipe
Desulphurization is blown to iron powder reclaiming chamber body by blast pass, and electromagnet generates magnetic force for the iron powder adsorption in Desulphurization in cotton
The surface of sleeve, cotton sleeve improve iron powder and the ironing surface frictional force of electromagnetism, avoid the iron powder quilt of electromagnet adsorption
Wind is fallen, and promotes absorption of the electromagnet to iron powder；Electromagnet is opened, opens simultaneously the air valve of blowback gas tank, in blowback gas tank
Blowback air flow through pipeline enter electromagnet core cylinder it is intracardiac, then blowback air-flow is from the venthole on iron core surface to outside electromagnet
Portion is overflowed, and prevents Desulphurization from penetrated into the gap of cotton sleeve under the action of blast pass, and then promotes Desulphurization and iron powder
Separation；
(3) a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers of the invention, will be from recycling
The Desulphurization of the separation iron powder taken out in slot is uniformly mixed to obtain Desulphurization aqueous solution with water, then moves into Desulphurization aqueous solution
In filter device, the bulky grain insoluble matter in Desulphurization is weeded out by strainer, Desulphurization aqueous solution through the hole on filter screen into
Enter the filter in filter device, Desulphurization aqueous solution enters the filtering outlet of filter bottom under the effect of gravity, and along mistake
It filters out mouth to flow into Buchner funnel, vacuum pump using circulatory water carries out vacuumizing operation at this time, obtains pretreated Desulphurization, will locate in advance
The Desulphurization of reason, which moves into progress hydrothermal synthesis in reaction unit, can be obtained calcium sulfate crystal whiskers.It can be removed using vacuum pump suction filtration de-
Bulky grain insoluble matter in sulphur ash improves the quality of the calcium sulfate crystal whiskers using Desulphurization preparation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the reaction unit of embodiment 1；
Fig. 2 is the SEM figure of the calcium sulfate crystal whiskers of embodiment 1；
Fig. 3 is embodiment 1 not except the SEM figure of the calcium sulfate crystal whiskers of iron；
Fig. 4 is the structural schematic diagram of the Suction filtration device of embodiment 2；
Fig. 5 is the structural schematic diagram of the filter of embodiment 2；
Fig. 6 is the structural schematic diagram of the device of iron powder in a kind of separation Desulphurization of embodiment 2；
Fig. 7 is the schematic top plan view of the top cover of embodiment 2；
Fig. 8 is the structural schematic diagram of the device of iron powder in the separation Desulphurization of embodiment 4；
Fig. 9 is the structural schematic diagram of the device of iron powder in the separation Desulphurization of embodiment 5；
Figure 10 is a kind of flow chart of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers.
Label declaration in schematic diagram:
100, blast pipe；110, the first blast pipe；120, the second blast pipe；130, air hose junction；131, bellows；
140, accumulator tank；150, air blast blower；101, desulfurization ash-pit；102, delivery pipe；103, pressurized gas；104, Material valve；
200, iron powder recycles cavity；201, energization head；202, conducting wire；203, cotton sleeve；204, venthole；205, iron
Core；210, the first electromagnet；220, the second electromagnet；230, third electromagnet；231, left electromagnet；232, right electromagnet；
240, cavity contraction section；
310, top cover；320, filter layer；
410, blowback gas tank；420, air-flow is responsible for；421, the first airflow manifold；422, the second airflow manifold；423, first
Back-flushing valve；424, the second back-flushing valve；
520, autoclave；521, relief valve；522, air gauge；523, air inlet；524, gas heater；525, it stirs
Mix blade；526, insulating layer；527, thermometer；528, oxygen valve；
601, unit is filtered；602, filter；610, Buchner funnel；620, bleeding point；630, vacuum suction bottle；640, rubber
Hose；650, vacuum pump using circulatory water；
710, strainer；720, filtering outlet.
Specific embodiment
Hereafter detailed description of the present invention and example embodiment are more fully understood in combination with attached drawing, wherein of the invention
Element and feature are identified by appended drawing reference.
Structure depicted in this specification attached drawing, ratio, size etc., only to cooperate the revealed content of specification,
So that those skilled in the art understands and reads, enforceable qualifications are not intended to limit the invention, therefore do not have technology
On essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size can be generated not influencing the present invention
The effect of and the purpose that can reach under, should all still fall in the range of disclosed technology contents obtain and can cover.Together
When, cited such as "upper", "lower", "left", "right", " centre " term in this specification are merely convenient to the clear of narration,
Rather than to limit enforceable range, relativeness is altered or modified, under the content of no substantial changes in technology, when also regarding
For the enforceable scope of the present invention；In addition to this, it is not independent from each other between each embodiment of the invention, but can be with
It is combined.
Embodiment 1
As shown in Figure 1, a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers of the invention, this
The Desulphurization that embodiment refers to is sintering flue gas desulfurization ash.
Step 1: Desulphurization pretreatment
Iron powder in Desulphurization is separated with Desulphurization, the bulky grain insoluble matter in Desulphurization is removed, obtains pretreated
Desulphurization；Detailed step are as follows:
(1) Desulphurization is added in Desulphurization iron powder separator, opens electromagnet, opens simultaneously blowback gas tank 410
Air valve, the blowback air in blowback gas tank 410 flow through pipeline enter electromagnet core 205 cylinder it is intracardiac, then blowback air-flow by
The venthole 204 on 205 surface of iron core is overflowed to electromagnet exterior；
Blowback air stream in blowback gas tank 410 respectively enters the first airflow manifold 421 and the second gas by air-flow supervisor 420
Branch pipe 422 is flowed, and controls the flow of the first back-flushing valve 423 and the second back-flushing valve 424 simultaneously；
(2) air blast blower 150, penetrating of the blast pass that air blast blower 150 generates through blast pipe 100 from bottom to top are opened
Iron powder recycles in cavity 200；
(3) Desulphurization is delivered in blast pipe 100 by desulfurization ash-pit 101；
Desulphurization is added to desulfurization ash-pit 101, opens the air valve of pressurized gas 103, pressurized gas 103 is to desulfurization ash-pit
101 pressurize, and then open Material valve 104, Desulphurization is delivered to blast pipe 100 through delivery pipe 102 in desulfurization ash-pit 101
It is interior；
(4) Desulphurization is blown to iron powder recycling cavity 200 by the blast pass of blast pipe 100, the iron powder in Desulphurization
It is adsorbed on the surface of cotton sleeve 203；
Desulphurization is blown to iron powder recycling cavity 200 by the blast pass of blast pipe 100, under the action of blast pass
Desulphurization is blowed to around electromagnet, and the iron powder in Desulphurization is adsorbed in the surface of cotton sleeve 203 by electromagnet, with this
Blowback air stream is overflowed outward by the venthole 204 on 205 surface of electromagnet core simultaneously, and Desulphurization is avoided to penetrate into cotton sleeve
In 203；
(5) Desulphurization after separating iron powder after the blast pass of closing blast pipe 100 drop to recycling under the effect of gravity
In slot 140；
(6) it goes the Desulphurization of iron power removing to mix with water from the taking-up of accumulator tank 140, weeds out bulky grain insoluble matter, then will weed out
The Desulphurization of bulky grain insoluble matter is placed in Buchner funnel 610 and is filtered by vacuum, and obtains pretreated Desulphurization；
Step 2: calcium sulfate crystal whiskers are prepared
By pretreated Desulphurization and MgCl2Solution is mixed to get slurries, then slurries are transferred to the high pressure of reaction unit
In reaction kettle 520, and oxygen is passed through into autoclave 520, adjust autoclave 520 in pressure be 1~2MPA,
Temperature is 120~180 DEG C, and the temperature of the present embodiment is 180 DEG C；To which hydrothermal synthesis calcium sulfate is brilliant in autoclave 520
Palpus；Specific steps are as follows:
(1) MgCl that compound concentration is 2%2Solution serves as medium crystallization agent, to MgCl2Pretreated Desulphurization is added in solution
Slurries are uniformly mixing to obtain, the solid-to-liquid ratio for controlling slurries is 1/15~1/20；
(2) Ca (OH) of saturation is added dropwise into slurries2Solution, the pH for adjusting slurries is 8~9；
(3) slurries are added in autoclave 520, to autoclave 520 after closing 520 top cover of autoclave
In be filled with oxygen, and the slurries in autoclave 520 are stirred, stirring intensity is 400~600r/min, reaction time
For 2~3h, thus the hydrothermal synthesis calcium sulfate crystal whiskers in autoclave 520；High pressure oxygen is the oxidant of oxidation stage, chlorine
Change magnesium as medium crystallization agent, in conjunction with crystallization theory, three processes are protected in specific crystallization:
1) oxidation process is dissolved
Thinner granularity makes Desulphurization have large specific surface area, while hydrothermal system temperature with higher and pressure
Power can promote CaSO3·0.5H2The dissolution of O.The SO generated after dissolution3 2-Rapid oxidation is at SO4 2-, oxidation reaction is incessantly
It carries out, CaSO in Desulphurization3·0.5H2O constantly dissolves.
2) crystallization process
As dissolution oxidation process persistently carries out, the Ca in solution2+、SO4 2-Concentration be continuously increased, as the Ca in solution2 +、 SO4 2-When reaching hypersaturated state at this temperature, the phenomenon that crystallization is precipitated just is had.Experiment shows reaction condition difference,
Corresponding reaction product also can difference, specific reaction equation it is as follows:
Ca2++SO4 2-=CaSO4(threadiness)
Ca2++SO4 2-+1/2H2O=CaSO4·1/2H2O (threadiness)
Ca2++SO4 2-+2H2O=CaSO4·2H2O (threadiness)
3) whisker growth process
Ca after crystal nucleation, in solution2+、SO4 2-It is still in hypersaturated state, is still constantly precipitated in the form of crystal.
Under the conditions of 180 DEG C, CaSO4Solubility is lower than CaSO4·0.5H2O and CaSO4·2H2O, CaSO4It will be centered on nucleus
Quickly cohesion；Simultaneously according to the oriented growth characteristic of calcium sulfate crystal whiskers and under the action of medium crystallization agent, crystal meeting sustainable growth, most
End form is at acicular calcium sulfate crystal whiskers.It is as shown in Figure 2 using the SEM picture of calcium sulfate crystal whiskers manufactured in the present embodiment.
Comparative example 1
The basic content of this comparative example 1 with embodiment 1, the difference is that: in step 1: Desulphurization pretreatment in, do not have
Have the iron powder separation in Desulphurization, but directlys adopt the Desulphurization with iron powder and prepare whisker.It is prepared using this comparative example
Calcium sulfate crystal whiskers SEM picture it is as shown in Figure 3.
Shown in comparison diagram 2 and Fig. 3, the calcium sulfate crystal whiskers production prepared using embodiment 1 is relatively orderly, and calcium sulfate crystal whiskers
What is prepared is relatively fast.Its reason may be: comparative example 1 contains in Desulphurization during using calcium sulfate crystal whiskers are prepared
A large amount of CaSO3, it is not available strong acid and cleans, therefore the present embodiment introduces physical dedoping step, is removed using electromagnet
Iron powder in Desulphurization, if directly carrying out hydro-thermal reaction synthesis calcium sulfate crystal whiskers, iron powder using the Desulphurization for not separating iron powder
Meeting and CaSO in hydrothermal system3The oxygen dissolved in contention slurries, while iron powder becomes the crystallization attachment point of newborn calcium sulfate,
Cause a large amount of forming cores of calcium sulfate crystal whiskers, but slow growth, therefore remove the life that the iron powder in Desulphurization is conducive to calcium sulfate crystal whiskers
Growth process.And the iron powder in Desulphurization is carried out physical removal of impurities during preparing calcium sulfate crystal whiskers by embodiment 1, effectively
Ground removes the iron powder in Desulphurization, to improve the preparation quality of calcium sulfate crystal whiskers.
It is worth noting that the MgCl that compound concentration is 2%2Solution serves as medium crystallization agent, to MgCl2Pretreatment is added in solution
Desulphurization afterwards is uniformly mixing to obtain slurries, and the solid-to-liquid ratio for controlling slurries is 1/15~1/20, can be to avoid Desulphurization in slurries
Agglomeration, while thinner granularity is but also Desulphurization obtains specific surface area with larger；The slurries stirred are added to
In autoclave 520, oxygen is filled with into autoclave 520 after closing 520 top cover of autoclave, and it is anti-to control high pressure
Answering the stirring intensity in kettle 520 is 400~600r/min, and the reaction time is 2~3h, so that hydrothermal system temperature with higher
Degree and pressure, can promote the CaSO in Desulphurization3·0.5H2The dissolution of O, the SO generated after dissolution3 2-Rapid oxidation is at SO4 2-,
Oxidation reaction carries out incessantly, CaSO in Desulphurization3·0.5H2O constantly dissolves, Ca in solution2+、SO4 2-Always in satiety
And state, power is provided for the crystallization and growth of calcium sulfate crystal whiskers, realizes sintering flue gas desulfurization ash oxidation coordinate system for calcium sulfate
Whisker solves CaSO3It is difficult to quickly oxidation and the longer problem of calcium sulfate crystal whiskers preparation process flow, is sintering flue gas desulfurization
Grey high added value resource utilization provides theoretical foundation.
Embodiment 2
The basic content of the present embodiment is with embodiment 1, as shown in Figures 4 and 5, the difference is that: Desulphurization is added to
In Desulphurization iron powder separator, when Desulphurization moves to the lower part of iron powder recycling cavity 200, Desulphurization moves to the first electromagnetism
Around iron 210 and the second electromagnet 220, the iron powder in Desulphurization is adsorbed by the first electromagnet 210 and the second electromagnet 220
In the surface of cotton sleeve 203；Then Desulphurization continues up under the action of blast pass, when Desulphurization moves to
When three 230 surroundings of electromagnet, the iron powder adsorption in Desulphurization is in the surface of third electromagnet 230；Desulphurization is in blast pass
Under effect, through the gap between the first electromagnet 210 and the second electromagnet 220, left electromagnet 231 and right electromagnet are moved to
Junction between 232, and it is adsorbed on the surface of junction, the separating effect of iron powder in Desulphurization is improved, when blowing gas
After stream stops blowing, the Desulphurization after separating iron powder is drop under the effect of gravity in accumulator tank 140, convenient for collecting Desulphurization.
Further, the Desulphurization droping in accumulator tank 140 is collected and is moved into Suction filtration device, Suction filtration device includes
Filter 602, vacuum pump using circulatory water 650 and suction filtration unit 601, vacuum pump using circulatory water 650 is by rubber leather hose 640 and filters single
The bleeding point 620 of member 601 is connected；Filtering unit 601 includes Buchner funnel 610, bleeding point 620 and vacuum suction bottle 630, cloth
The top of vacuum suction bottle 630 is arranged in family name's funnel 610, and the side of vacuum suction bottle 630 is provided with bleeding point 620, bleeding point
620 are connected by rubber leather hose 640 with vacuum pump using circulatory water 650, and the top of Buchner funnel 610 is arranged in filter 602；Filtering
The middle part of device 602 is provided with strainer 710, and the diameter that the pore size filter of strainer 710 is less than bulky grain insoluble matter is simultaneously greater than desulfurization
The diameter of ash, the bottom of filter 602 are provided with filtering outlet 720, and the upper of Buchner funnel 610 is arranged in filtering outlet 720
Portion.After Desulphurization removes iron power removing, it is moved into filter 602 after mixing with distilled water, in the strainer of filter 602
Under 710 effects, the bulky grain insoluble matter in Desulphurization aqueous solution is blocked on the upper surface of strainer 710, can remove Desulphurization
In bulky grain insoluble matter, hole of the Desulphurization aqueous solution of remainder in strainer 710 flow to the bottom of filter 602,
The Desulphurization aqueous solution for flowing into 602 bottom of filter under gravity, continues to the filtering that 602 bottom of filter is arranged in
720 flowing of outlet, then flows into the suction filtration unit 601 being arranged in below filtering outlet 720.
Further, it after Desulphurization aqueous solution flows to Suction filtration device, filters unit 601 and Desulphurization aqueous solution is taken out
The power supply of vacuum pump using circulatory water 650 is first opened in filter, and Desulphurization aqueous solution flows into Buchner funnel 610 under the effect of gravity, circulation
Water vacuum pump 650 is connected by rubber leather hose 640 with the bleeding point 620 that 630 side of vacuum suction bottle is arranged in, and rubber skin is passed through
The Desulphurization aqueous solution that pipe 640 acts in Buchner funnel 610 starts to vacuumize operation, obtains after vacuum filtration pretreated de-
Sulphur ash, weeds out the bulky grain insoluble matter in Desulphurization, improves the purity of Desulphurization, and then improve the sulfuric acid using Desulphurization preparation
The quality of calcium pyroborate, then by pretreated Desulphurization and MgCl2Solution mixing then moves to hydro-thermal in autoclave 520 and closes
At calcium sulfate crystal whiskers.
A kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers of the present embodiment, reaction unit packet
Include oxygen cylinder 510 and autoclave 520,523 phase of air inlet that oxygen cylinder 510 passes through pipeline and 520 top of autoclave
Even, it is provided with oxygen valve 528 on air inlet 523, is provided with pressure release on the pipeline between air inlet 523 and autoclave 520
Valve 521 is provided with air gauge 522 on the autoclave 520, stirring blade 525 is provided in autoclave 520.It will
The slurries stirred adjust the range of pH value between 8~9, are then added in autoclave 520, and it is anti-to close high pressure
Oxygen is filled with into autoclave 520 after answering 520 top cover of kettle, and controlling the stirring intensity in autoclave 520 is 400-
600r/min, reaction time are 2~3h, carry out hydrothermal synthesis and obtain calcium sulfate crystal whiskers.Control the stirring in autoclave 520
Intensity and reaction time can make hydrothermal system temperature and pressure with higher, can promote in Desulphurization
CaSO3·0.5H2The continuous dissolution of O, the SO generated after dissolution3 2-Rapid oxidation is at SO4 2-, so that Ca in solution2+、SO4 2-Always
In hypersaturated state, simultaneous oxidation reaction carries out incessantly, provides power for the crystallization and growth of calcium sulfate crystal whiskers, realizes
Sintering flue gas desulfurization ash oxidation coordinate system further, solves CaSO for calcium sulfate crystal whiskers3It is difficult to quickly oxidation and sulfuric acid
The longer problem of calcium pyroborate preparation process flow.
In the present embodiment, Desulphurization is blown to iron powder recycling cavity 200 by the blast pass of blast pipe 100, electromagnet
Generate magnetic force by the iron powder adsorption in Desulphurization in the surface of cotton sleeve 203, cotton sleeve 203 improve electromagnetism iron surface with
The frictional force of iron powder avoids the iron powder of electromagnet adsorption from being blowed air-flow and blows off；Electromagnet includes conducting wire 202 and iron core
205, wherein conducting wire 202 is wound in the outside of iron core 205, and the surface of iron core 205 offers venthole 204, venthole 204 and iron
The cylinder heart of core 205 is connected, and then blowback gas tank 410 can convey blowback air-flow to the cylinder heart of iron core 205 by gas pipeline；
In addition, the diameter of venthole 204 is greater than the diameter of conducting wire 202, when so that conducting wire 202 passing through the outer surface of venthole 204, enter
The blowback air-flow of iron core 205 can also be flowed out from the gap of 204 surrounding of venthole, then pass through cotton sleeve 203 to outside
Diffusion can avoid Desulphurization from entering in cotton sleeve 203 under the action of blast pass to the blowback air-flow of external diffusion, thus
Achieve the effect that separate iron powder in Desulphurization.
The top cover 310 of the present embodiment is set to the top of iron powder recycling cavity 200, which was internally provided with
Filtering layer 320；Blast pipe 100 is set to the bottom of iron powder recycling cavity 200, and the blast pass in blast pipe 100 is used for desulfurization
In ash blowing to iron powder recycling cavity 200, recycled in cavity 200 so that Desulphurization enters iron powder by blast pipe 100；From air inlet
Pipe 100 enters the blast pass that iron powder receives cavity 200, flows out iron powder by filter layer 320 and receives cavity 200, balance iron powder recycling
Pressure and extraneous pressure in cavity 200, guarantee going on smoothly for separation process.
It is worth noting that electromagnet includes the first electromagnet 210, the second electromagnet 220 and third electromagnet 230,
In the first electromagnet 210 and the second electromagnet 220 be set side by side, be provided between the first electromagnet 210 and the second electromagnet 220
Gap, third electromagnet 230 are set to the top of the first electromagnet 210 and the second electromagnet 220, and third electromagnet 230 with
Above-mentioned gap is correspondingly arranged.The mode of being arranged above and below of electromagnet allow different location, different levels electromagnet with it is de-
Sulphur ash comes into full contact with, to make the iron powder of different location in electromagnet adsorption recovery cavity 200, and then improves in the unit time
The separative efficiency of iron powder.
The third electromagnet 230 of the present embodiment includes left electromagnet 231 and right electromagnet 232, left electromagnet 231 and right electricity
The junction of magnet 232 is located at the surface in gap；The angle of 232 junction of left electromagnet 231 and right electromagnet is β, β value
Range is 120~150 °, and the preferred β value of the present embodiment is 120 °, and the setting of above-mentioned angle β increases third electromagnet
The adsorption area of 230 pairs of iron powders, while enhancing the electromagnetic force of junction, so third electromagnet 230 generate it is stronger
Iron powder in magnetic-adsorption Desulphurization reaches preferable separating effect.
As shown in Figure 6 and Figure 7, top cover 310 is set to the top of iron powder recycling cavity 200, and iron powder recycles the top of cavity 200
Portion is internally provided with internal screw thread, is provided with the external screw thread matched with above-mentioned internal screw thread on 310 lateral wall of top cover, so that iron powder returns
It receives and is connected between cavity 200 and top cover 310 by screw thread, installation effectiveness can be improved in the mode of threaded connection；In addition, the top
Lid 310 is internally provided with filter layer 320, is provided with through-hole on filter layer 320, and the through-hole and above-mentioned energization head 201 match
It closes, energization head 201 is disposed through on filter layer 320 by through-hole, and energization head 201 passes through filter layer 320 and extends to top cover 310
Outside, energization head 201 is electrically connected to a power source.Above-mentioned filter layer 320 is gauze or filled layer with gap or removes
Dirt cloth bag, gas can be flowed out by filter layer 320 in iron powder removal process, and filter layer 320 can will that treated be de-
Sulphur ash is limited in iron powder recycling cavity 200, so that the Desulphurization after processed concentrates in iron powder recycling cavity 200, thus
While carrying out safe and efficient separation to the iron powder in Desulphurization, avoids Desulphurization and overflow iron powder recycling cavity 200
Outside.
Embodiment 3
The basic content of the present embodiment with embodiment 1, the difference is that: be connected on blowback gas tank 410 air-flow supervisor
420, air-flow is responsible on 420 and is connected with the first airflow manifold 421 and the second airflow manifold 422, the first airflow manifold 421 and third
205 both ends of iron core of electromagnet 230 are connected, it should be noted that: the first airflow manifold 421 is connected with the cylinder heart of iron core 205
Logical, the cylinder heart is hollow passageway, and the cylinder heart is connected with the venthole 204 on 205 surface of iron core, and the first airflow manifold 421 connects with the cylinder heart
The position connect is equipped with sealing ring, and blowback air-flow is avoided to reveal from the both ends of 205 hearts of iron core；Second airflow manifold 422 is divided
It is not connected with the iron core 205 of the first electromagnet 210 and the second electromagnet 220, i.e., in the second airflow manifold 422 and iron core 205
The cylinder heart be connected, same second airflow manifold 422 is equipped with sealing ring with cylinder heart link position.Second airflow manifold 422 into
Port includes left port and right output port, and wherein left port is connected with the left end of the iron core 205 of the first electromagnet 210, right output port with
The right end of the iron core 205 of second electromagnet 220 is connected.The air-flow that blowback gas tank 410 generates respectively enters the by gas pipeline
One airflow manifold 421 and the second airflow manifold 422；The first back-flushing valve 423, the second air-flow are provided in first airflow manifold 421
The second back-flushing valve 424 is provided on branch pipe 422；First back-flushing valve 423 is used to control the gas stream in the first airflow manifold 421
Amount, the second back-flushing valve 424 are used to control the gas flow in the second airflow manifold 422.First electromagnet 210 and the second electromagnet
220 are located proximate to blast pipe 100, and power supply provides electric energy to electromagnet by energization head 201, and then electromagnet passes through electromagnetism sense
Magnetic force should be generated, on the one hand, because what the first electromagnet 210 and the second electromagnet 220 at this were contacted with iron powder in Desulphurization
Probability is larger, can suitably increase the number of turns of the first electromagnet 210 and the conducting wire 202 on the second electromagnet 220, and then can increase
Electromagnetism intensity at strong first electromagnet 210 and the second electromagnet 220；On the other hand, third electromagnet 230 is compared to first
Electromagnet 210 and the second electromagnet 220, positional distance blast pipe 100 farther out, so in third electromagnet 230 and Desulphurization
The probability of iron powder contact is lower, needs suitably to increase in the identical situation of electric current the circle of the conducting wire 202 on third electromagnet 230
Number enhances the electromagnetism intensity at third electromagnet 230, recycles cavity iron powder to iron powder is blasted to improve third electromagnet 230
The absorption of the iron powder on 200 tops, and then can be blown off and heavy to avoid the iron powder on 203 surface of adsorption cotton matter sleeve by blowback air-flow
It newly falls into Desulphurization, reduces the purity of Desulphurization separation.
It should be noted that Desulphurization can penetrate into cotton sleeve 203 under the action of 100 blast pass of blast pipe, make
Obtaining in cotton sleeve 203 has Desulphurization residual, causes the separating effect of iron powder poor, at this time can be by adjusting the second back-flushing valve
424 control the gas flow in the second airflow manifold 422, so that blowback air-flow is from the inner surface of cotton sleeve 203 to appearance
Surface current is dynamic, and Desulphurization is avoided to be attached in the fiber holes of cotton sleeve 203.Iron powder in Desulphurization is inhaled under the action of electromagnetic force
It is attached to 203 surface of cotton sleeve, moves to the Desulphurization near electromagnet under the action of the blowback air-flow of venthole 204, instead
It to cotton sleeve 203 is moved away from, promotes Desulphurization and is separated with iron powder, improve the separating effect of iron powder in Desulphurization.Third
Electromagnet 230 is far from blast pipe 100, when Desulphurization moves near third electromagnet 230, suffered by gas impact compared with
It is small at first electromagnet 210 and the second electromagnet 220, so in the present embodiment first can be controlled by the first back-flushing valve 423
Gas flow in airflow manifold 421, so that the gas flow of the first airflow manifold 421 is less than in the second airflow manifold 422
Gas flow.
Further, since blast pass in blast pipe 100 has certain air pressure, Desulphurization is by cannot be by itself weight
Power is entered in blast pipe 100 by delivery pipe 102, therefore seal closure, pressurization is arranged at the top of desulfurization ash-pit 101 in the present embodiment
Gas tank 103 is connected by pipeline with desulfurization ash-pit 101；Pressurized gas 103 be sealing desulfurization ash-pit 101 air pressure is provided, thus
Stream pressure in balance air inlet pipe 100, so that the effect of air pressure and self gravity that Desulphurization is provided in pressurized gas 103
Under, it is delivered in blast pipe 100 by delivery pipe 102, blast pass is by Desulphurization along the pipe of blast pipe 100 in blast pipe 100
Road direction is blown upward in iron powder recycling cavity 200, and then the progress in iron powder recycling cavity 200 to the iron powder in Desulphurization
Separation.
Embodiment 4
The basic content of the present embodiment with embodiment 1, as shown in figure 8, the difference is that: blast pipe 100 include first
Blast pipe 110 and the second blast pipe 120, and the first blast pipe 110 and the second blast pipe 120 are correspondingly arranged, the first blast pipe 110
And the second angle between blast pipe 120 is a, 90~120 ° of the range of a, the first blast pipe 110 and the second blast pipe 120 can
It is generated with the bottom in iron powder recycling cavity 200 to the blast pass blown, is come so that Desulphurization better disperses, and desulfurization
Ash is blowed by the bottom of iron powder recycling cavity 200 to top under the action of blast pass, avoids Desulphurization in self gravity
Lower fall of effect and be piled up in iron powder recycling 200 bottom of cavity, and then promote sufficiently connecing for iron-containing Desulphurization and electromagnet
Touching, improves electromagnet to the separative efficiency of iron powder.
Further, the first blast pipe 110 is provided with desulfurization ash-pit 101 far from the side of the second blast pipe 120；The desulfurization
The bottom of ash-pit 101 is connected by delivery pipe 102 with the first blast pipe 110；Second blast pipe 120 is far from the first blast pipe 110
Side be provided with desulfurization ash-pit 101；The bottom of the desulfurization ash-pit 101 is connected by delivery pipe 102 with the second blast pipe 120；
Desulphurization in desulfurization ash-pit 101 is added separately in the first blast pipe 110 and the second blast pipe 120 by delivery pipe 102, just
In Desulphurization to be added directly into blast pipe 100 along delivery pipe 102, the online separation of iron powder in Desulphurization is realized, is improved
Actual production efficiency.Blast pipe 100 is provided with air blast blower 150, air blast blower far from one end of iron powder recycling cavity 200
150 for blasting air-flow to blast pipe 100.Since the air-flow in blast pipe 100 has certain air pressure, when air pressure is larger, take off
Sulphur ash will cannot enter in blast pipe 100 along delivery pipe 102 from desulfurization ash-pit 101 by the gravity of itself, therefore the present embodiment
The top of desulfurization ash-pit 101 is provided with seal closure, pressurized gas 103 is connected by pipeline with desulfurization ash-pit 101.Pressurized gas
103 be that the desulfurization ash-pit 101 of sealing provides air pressure, thus the stream pressure in balance air inlet pipe 100, so that Desulphurization is being pressurized
Under the action of air pressure and self gravity that gas tank 103 provides, it is delivered in blast pipe 100 by delivery pipe 102, blast pipe 100
In the air-flow that constantly blasts Desulphurization is blown upward in iron powder recycling cavity 200 along the duct orientation of blast pipe 100, and
Iron powder recycles the iron powder in cavity 200 in separation Desulphurization.
Meanwhile the bottom of iron powder recycling cavity 200 is provided with cavity contraction section 240, blast pipe 100 and cavity contraction section
240 bottom is connected；Blast pipe 100 is connected by cavity contraction section 240 with the bottom that iron powder recycles cavity 200, the first air inlet
Air hose junction 130, air hose junction 130 and the first electromagnet 210 and are provided between pipe 110 and the second blast pipe 120
Gap between two electromagnet 220 is correspondingly arranged, and air hose junction 130 extends to above cavity into cavity contraction section 240
The bottom of contraction section 240.The blast pass that blast pipe 100 generates is respectively along the side of the first blast pipe 110 and the second blast pipe 120
To moving upwards, blast pass collects in air hose junction 130 and enters cavity contraction section 240, the bottom of cavity contraction section 240
Design is shunk, is moved upwards so that blast pass is gathered, so that the blast pass that blast pipe 100 is blown into is in cavity contraction section 240
Opposite aggregation is conducive to Desulphurization and is blowed by the bottom of iron powder recycling cavity 200 to top under the action of blast pass, avoided
Desulphurization is deposited on iron powder recycling 200 bottom of cavity because unbalance stress falls under the effect of gravity, and then causes to take off
The separating effect of sulphur ash is poor.It is provided with Material valve 104 in delivery pipe 102, can according to need and be turned on or off Material valve
104；The bottom sidewall of first blast pipe 110 and the second blast pipe 120 is connected by pipeline with air blast blower 150, which sets
It is equipped with air blast valve, air blast valve is used to control the gas flow of the pipeline；The bottom of first blast pipe 110 and the second blast pipe 120
Underface is provided with accumulator tank 140, which is used to collect the Desulphurization after separation iron powder.
As shown in figure 9,240 upper end of cavity contraction section is connected by bellows 131 with the bottom that iron powder recycles cavity 200,
240 lower end of cavity contraction section is connected by bellows 131 with the top of blast pipe 100, and vibration is provided on cavity contraction section 240
Mechanism, the percussion mechanism is for driving cavity contraction section 240 to be vibrated, so that the Desulphurization accumulated on cavity contraction section 240
Accumulator tank 140 is fallen to by the first blast pipe 110 and the second blast pipe 120, convenient for sufficiently collecting the desulfurization of separated iron powder
The yield of the calcium sulfate crystal whiskers using Desulphurization preparation can be improved in ash.
The present invention is described in detail above in conjunction with specific exemplary embodiment.It is understood, however, that can not take off
It is carry out various modifications in the case where from the scope of the present invention being defined by the following claims and modification.Detailed description and drawings
Should be to be considered only as it is illustrative and not restrictive, if there is any such modifications and variations, then they all will
It falls into the scope of the present invention described herein.In addition, Development Status and meaning that background technique is intended in order to illustrate this technology,
It is not intended to limit the present invention or the application and application field of the invention.
Claims (9)
1. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers, it is characterised in that:
Step 1: Desulphurization pretreatment
Iron powder in Desulphurization is separated with Desulphurization, the bulky grain insoluble matter in Desulphurization is weeded out, obtains pretreated desulfurization
Ash；
Step 2: calcium sulfate crystal whiskers are prepared
By pretreated Desulphurization and MgCl2Solution is mixed to get slurries, then slurries are transferred to the autoclave of reaction unit
(520) in, and oxygen is passed through in autoclave (520), adjusting the pressure in autoclave (520) is 1~2MPA, temperature
Degree is 120~180 DEG C；To in the interior hydrothermal synthesis calcium sulfate crystal whiskers of autoclave (520).
2. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 1,
It is characterized in that: the step of step 2 are as follows:
(1) MgCl that compound concentration is 2%2Solution serves as medium crystallization agent, to MgCl2It is equal that pretreated Desulphurization stirring is added in solution
Even to obtain slurries, the solid-to-liquid ratio for controlling slurries is 1/15~1/20；
(2) Ca (OH) of saturation is added dropwise into slurries2Solution, the pH for adjusting slurries is 8~9；
(3) slurries are added in autoclave (520), to autoclave after closing autoclave (520) top cover
(520) it is filled with oxygen in, and the slurries in autoclave (520) are stirred, stirring intensity is 400~600r/min,
Reaction time is 2~3h, thus in the interior hydrothermal synthesis calcium sulfate crystal whiskers of autoclave (520).
3. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 1,
It is characterized in that: the step of step 1 are as follows: Desulphurization is added in Desulphurization iron powder separator and separates iron powder, Desulphurization iron powder
Desulphurization is blown to iron powder recycling cavity (200) by the blast pass that the blast pipe (100) of separator generates, and electromagnet produces
Magnetisation power is by the iron powder adsorption in Desulphurization in the surface of cotton sleeve (203)；Divide after closing the blast pass of blast pipe (100)
It is drop in accumulator tank (140) under the effect of gravity from the Desulphurization after iron powder；Iron powder is separated from taking out in accumulator tank (140)
Desulphurization is mixed with water, weeds out the bulky grain insoluble matter in Desulphurization, then is carried out to the Desulphurization for weeding out bulky grain insoluble matter true
Empty pump filter, obtains pretreated Desulphurization.
4. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 1,
Be characterized in that: reaction unit includes oxygen cylinder (510) and autoclave (520), and oxygen cylinder (510) is anti-by pipeline and high pressure
It answers the air inlet (523) at the top of kettle (520) to be connected, is provided on air inlet (523) oxygen valve (528), air inlet (523) and height
It is provided with relief valve (521) on pipeline between pressure reaction kettle (520), is provided with air gauge on the autoclave (520)
(522), stirring blade (525) are provided in autoclave (520).
5. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 3,
It is characterized in that: step 1: the pretreated specific steps of Desulphurization are as follows:
(1) Desulphurization is added in iron powder recyclable device Desulphurization iron powder separator, opens electromagnet, opens simultaneously blowback
The air valve of gas tank (410), the blowback air in blowback gas tank (410) flow through pipeline enter electromagnet core (205) cylinder it is intracardiac, and
Blowback air-flow is overflowed from the venthole (204) on iron core (205) surface to electromagnet exterior afterwards；
(2) air blast blower (150) are opened, spray of the blast pass that air blast blower (150) generates through blast pipe (100) from bottom to top
Enter in iron powder recycling cavity (200)；
(3) Desulphurization is delivered in blast pipe (100) by desulfurization ash-pit (101)；
(4) Desulphurization is blown to iron powder recycling cavity (200) by the blast pass of blast pipe (100), the iron powder in Desulphurization
It is adsorbed on the surface of cotton sleeve (203)；
(5) blast pass of blast pipe (100) is closed, the Desulphurization after separating iron powder drop to accumulator tank under the effect of gravity
(140) in；
(6) taking out from accumulator tank (140) goes the Desulphurization of iron power removing to mix with water, weeds out bulky grain insoluble matter, then will weed out big
The Desulphurization of particle insoluble matter, which is placed in Suction filtration device, to be filtered by vacuum, and pretreated Desulphurization is obtained.
6. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 5,
Be characterized in that: the blowback air stream in step 1 (1) in blowback gas tank (410) respectively enters the first gas by air-flow supervisor (420)
Branch pipe (421) and the second airflow manifold (422) are flowed, and controls the stream of the first back-flushing valve (423) and the second back-flushing valve (424) simultaneously
Amount.
7. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 5,
It is characterized in that: being added to Desulphurization desulfurization ash-pit (101) in step 1 (3), open the air valve of pressurized gas (103), pressurization
Gas tank (103) pressurizes to desulfurization ash-pit (101), then opens Material valve (104), the interior Desulphurization warp of desulfurization ash-pit (101)
Delivery pipe (102) is delivered in blast pipe (100).
8. a kind of method using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 5,
Be characterized in that: Desulphurization is blown to iron powder recycling cavity (200) by the blast pass of blast pipe (100) in step 1 (4),
Desulphurization is blowed to around electromagnet under the action of blast pass, and the iron powder in Desulphurization is adsorbed in cotton set by electromagnet
The surface of cylinder (203), blowback air stream is overflowed outward by the venthole (204) on electromagnet core (205) surface at the same time, is kept away
Exempt from Desulphurization to penetrate into cotton sleeve (203).
9. described in any item a kind of using sintering flue gas desulfurization ash one-step synthesis method calcium sulfate crystal whiskers according to claim 5-8
Method, it is characterised in that: iron powder recyclable device Desulphurization iron powder separator includes blast pipe (100), iron powder recycling cavity
(200), top cover (310) and blowback gas tank (410)；Electromagnet and cotton sleeve are provided in iron powder recycling cavity (200)
(203), the cotton sleeve (203) is wrapped in the outside of electromagnet, and electromagnet includes conducting wire (202) and iron core (205), wherein
Conducting wire (202) is wound in the outside of iron core (205), and the surface of iron core (205) offers venthole (204), the venthole (204)
It is connected with the cylinder heart of iron core (205)；Top cover (310) is set to the top of iron powder recycling cavity (200), the top cover (310)
It is internally provided with filter layer (320)；Blast pipe (100) is set to the bottom of iron powder recycling cavity (200), and Desulphurization passes through air inlet
(100) are managed to enter in iron powder recycling cavity (200)；Above-mentioned blowback gas tank (410) passes through the cylinder heart of gas pipeline and iron core (205)
It is connected, blast pipe (100) bottom is provided with accumulator tank (140).
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| CN109520302A (en) * | 2018-12-29 | 2019-03-26 | 广州薪光合环保技术有限公司 | Sintering furnace |
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