CN108414394A - The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate - Google Patents
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate Download PDFInfo
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- CN108414394A CN108414394A CN201810609621.8A CN201810609621A CN108414394A CN 108414394 A CN108414394 A CN 108414394A CN 201810609621 A CN201810609621 A CN 201810609621A CN 108414394 A CN108414394 A CN 108414394A
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- demarcation strip
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
Abstract
The invention discloses the methods that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：Detect the TiO of ilmenite2Grade；The concentrated sulfuric acid is added into acidolysis pot with after ilmenite, is sufficiently stirred, hydrolysising mother liquid, diluting concentrated sulfuric acid is added later；Solid formation is obtained after acidolysis reaction is complete, and after solid formation curing, leaching liquid leaching acidolysis solid formation is added into acidolysis pot；Iron powder is added into acidolysis pot, carries out reduction reaction；Part leaching liquid after sampling reduction reaction in acidolysis pot, the leaching liquid of taking-up is filtered, obtains titanium liquid and residue, drying to constant weight by residual washing-out, and detects TiO in residue butt2Grade；Measure the total volume of the leaching liquid obtained in acidolysis pot after reduction reaction；Calculate acidolysis rate.The present invention is measured analysis under the actual condition not affected the normal production, easy to operate, and accuracy is high, and stability is good, can be directly used for the acidolysis process parameter in analysis production, strong for production technology directiveness.
Description
Technical field
The present invention relates to ilmenite acidolysis rate detection technique fields.It is more particularly related to which sulfate process titanium dioxide is given birth to
The method that production process measures mixing titanium ore acidolysis rate.
Background technology
In current technology, major part producer of China is all to use Titanium White Production By Sulfuric Acid Process, and ilmenite is titanium dioxide life
The main raw material of production, factory can directly grasp utilization rate of the production technology to raw material titanium resource using the acidolysis rate of ilmenite
Situation.Therefore, acidolysis rate is the important indicator of titanium white production cost control, and accuracy plays ten to plant produced operation
Divide important directiveness effect.
In Producing Titanium Dioxide enterprise, the method for measuring acidolysis rate is typically to be sampled from the leaching liquid on acidolysis pot top, to it
It is filtered washing, the calculating of acidolysis rate is carried out by detecting the titanium amount in titanium liquid and residue respectively.The deficiency of this kind of method
Place is, due to the acidolysis leaching stage of titanium white actual production, to add part titaniums containing dissolving such as hydrolysising mother liquid, production recovered liquid
Waste water, the acidolysis rate measured is more higher than practical acidolysis rate, cannot accurately reflect the practical acidolysis rate of production process, operation instruction
Property is poor.The patent of invention of Publication No. CN102830200A discloses a kind of method of detection titaniferous ore acidolysis rate, this method
The detection utilization for being confined to laboratory is measured, the acidolysis rate situation accurately reflected in actual production process, production can not be stablized
Poor practicability.
Invention content
The object of the present invention is to provide the methods that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, pass through analysis
The TiO of ferrotianium composite ore2Grade, acidolysis, curing, leaching acidolysis solid formation, reduction reaction, leaching liquid sampling, leaching liquid filter
Separating treatment, residue drying and processing and etc., obtain the TiO in the throwing mine amount for calculating acidolysis rate2Quality, in residue butt
TiO2Grade etc., accurately calculate the acidolysis rate of actual production mixing titanium ore.This method is in the reality not affected the normal production
Analysis is measured under the operating mode of border, easy to operate, accuracy is high, and stability is good, can be directly used for the acidolysis work in analysis production
Skill parameter is strong for production technology directiveness.
In order to realize these purposes and other advantages according to the present invention, it is mixed to provide sulfate process titanium dioxide production process measurement
The method for closing titanium ore acidolysis rate, including：
Step 1: the TiO of detection ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 78~85%；Hydrolysising mother liquid is slurry vacuum diaphragm machine upper piece suction filtration in washing after titanium hydrolysis
The liquid separated.
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, reduction reaction is carried out, iron powder is added and constantly surveys the dense of titanous in the process
Degree so that a concentration of 0.5-1.5g/L of titanous of generation；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: measuring the total volume v of the leaching liquid obtained in acidolysis pot after reduction reaction2；
Step 7: calculating acidolysis rate, acidolysis rate=[1- (w2×mc×v2)/(w1×m×v1)] × 100%, wherein w1Table
Show mixing ilmenite TiO2Grade；w2Indicate TiO in residue butt2Grade；M indicates that mixing titanium ore throws mine amount；mcFor residue
Constant weight quality；v1For leaching liquid sampling volume；v2For leaching liquid total volume.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, the step
Two are specially：After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.3~1.6 into acidolysis pot is 98%, adopt
It is persistently stirred with compressed air, is added hydrolysising mother liquid later, the mass concentration of diluting concentrated sulfuric acid to 78~85%.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and hydrolysis is added
Mother liquor, the mass concentration of diluting concentrated sulfuric acid to 80~85%.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, the leaching
Liquid is 1 in mass ratio by production recovered liquid and clear water:1 composition, the additive amount of leaching liquid are set as：The volume and ferrotianium of leaching liquid
The mass ratio of mine is 3.5m3/ t is produced in recovered liquid containing dissolving 5~30g/L of titanium, 10~60g/L of effective acid, ferrous sulfate
100~200g/L.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, the hydrolysis
Contain dissolving 5~10g/L of titanium, 250~300g/L of effective acid, 150~200g/L of ferrous sulfate in mother liquor.Preferably, described
Sulfate process titanium dioxide production process measure mixing titanium ore acidolysis rate method in, in the step 3 curing time of solid formation be
The time of 30~60min, leaching liquid leaching acidolysis solid formation are 4~6h.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 500~
The residual washing-out specific method that drying to constant weight in the step 5, is by 1000mL：
Residue is used to 40~60 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100
DEG C or more drying to constant weight.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, the acidolysis
Pot include：
Pot body；
Compressed air access tube is connected to the bottom of the pot body, and the air opening end of compressed air access tube is set vertically
It sets；
Air sparger, is arranged in the back taper portion of pot body, and the air sparger includes：
Air distribution plate is made of the first plate body of polylith, and the first plate body of polylith be integrally formed, the first plate body of polylith on to
Under set gradually, in addition to the first plate body positioned at the top, other first plate bodys are inner hollow, and top and bottom are opened wide
Truncated cone-shaped, the first plate body for being located at the top is circle, and horizontally disposed；Except the first plate body positioned at the top
Outside, in other two piece of first adjacent plate bodys, the busbar of underlying first plate body and the angle ratio of vertical direction are positioned at upper
Side the first plate body busbar and vertical direction the small 4-8 degree of angle, and the top of underlying first plate body be located at it is upper
The bottom of first plate body of side overlaps, the mother of the length of the busbar of underlying first plate body and the first plate body being located above
The equal length of line；Madial wall positioned at the bottom of the first plate body of bottom and the back taper portion is fixed and is seamlessly connected,
And the busbar of the first plate body positioned at bottom is vertical with the busbar in back taper portion, is located at the outer of the first plate body of the top
The internal diameter at the top of diameter and the first plate body adjacent thereto is equal, is located at the edge of the first plate body of the top and adjacent thereto
The top fixation and seamless connection of first plate body are arranged at intervals with multiple air distribution holes on every piece of first plate body.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, the air
Distributor further includes：
The first demarcation strip of polylith, is arranged at intervals on the lower section of the air distribution plate, in addition to the first plate body positioned at the top,
In other first plate bodys, adjacent two pieces of first plate bodys correspond to one piece of first demarcation strip, and the first demarcation strip is inner hollow, and
The intersection of the open reverse frustoconic in top and bottom, the top of the first demarcation strip and corresponding two pieces of first plate bodys is solid
Fixed and seamless connection, bottom extends in compressed air access tube or is flushed with the bottom in the back taper portion；
Second demarcation strip is the cylinder bodily form, and is arranged in the lower section of the first plate body of the top, the second demarcation strip
It is coaxially disposed with back taper portion, the outer diameter of the second demarcation strip is equal with the outer diameter of the first plate body of the top, the second demarcation strip
Top and the bottom of the first plate body positioned at the top are fixed and are seamlessly connected, bottom extend in compressed air access tube or with
The bottom in the back taper portion flushes.
Preferably, the sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and described first
The bottom of demarcation strip and second demarcation strip is flushed with the bottom in the back taper portion；Three piece of first adjacent demarcation strip
In, it is more than itself and position at a distance from the bottom of the first intermediate demarcation strip is between the bottom of the first demarcation strip on the outside of it
Distance between the bottom of first demarcation strip of side in the inner, the bottom of the side wall in the back taper portion and on the outermost side first
Distance between the bottom of demarcation strip is more than the bottom of the first demarcation strip on the outermost side and the first demarcation strip adjacent thereto
Distance between bottom is less than at a distance from the bottom of innermost first demarcation strip is between the bottom of the second demarcation strip and is located at most
The bottom of first demarcation strip of inside at a distance between the bottom of the first adjacent demarcation strip of innermost first demarcation strip,
And more than the internal diameter of the second demarcation strip.
The present invention includes at least following advantageous effect：
The present invention throws TiO in mine amount by detecting acidolysis2Quality and total leaching liquid residue in TiO2Quality, it is counter to push away
The acidolysis rate for obtaining actual production process is calculated, testing result is accurate, and stability height is a kind of in the item not affected the normal production
Under part, the accurate method for detecting the true acidolysis rate of actual condition, and can reflect the acidolysis process parameter in actual production, it produces
It is guiding strong.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Description of the drawings
Fig. 1 is the structural schematic diagram of acidolysis pot according to an embodiment of the invention；
Fig. 2 is the structural schematic diagram of air distribution plate according to an embodiment of the invention.
Specific implementation mode
With reference to embodiment and legend, the present invention is described in further detail, to enable those skilled in the art's reference
Specification word can be implemented according to this.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained；In the description of the present invention, term " transverse direction ", " vertical
To ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", the instructions such as "outside" side
Position or position relationship are to be based on the orientation or positional relationship shown in the drawings, and are merely for convenience of description of the present invention and simplification of the description,
It is not instruction or implies that signified device or element must have a particular orientation, with specific azimuth configuration and operation, because
This is not considered as limiting the invention.
Embodiment 1
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：
Step 1: ilmenite is carried out to match mine and ball milling, the fineness of the miberal powder after ball milling is 325 mesh, residue on sieve 2%, inspection
Survey the TiO of ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 80%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, and it is lasting to stir, reduction reaction is carried out, iron powder is added and constantly surveys in the process
The concentration of titanous so that a concentration of 0.5g/L of titanous of generation can stop plus iron powder, meets postorder hydrolysis, washing step
Technological requirement；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: measuring the total volume v of the leaching liquid obtained in acidolysis pot after reduction reaction2；
Step 7: calculating acidolysis rate, acidolysis rate=[1- (w2×mc×v2)/(w1×m×v1)] × 100%, wherein m tables
Show that ilmenite throws mineral amount.The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, the step
Two are specially：After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.3 into acidolysis pot is 98%, using compression
Air persistently stirs, and so that material is in the state of mixing substantially uniformity, hydrolysising mother liquid is added later, the quality of diluting concentrated sulfuric acid is dense
It spends to 80%.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the leaching liquid is by producing back
It is 1 to receive liquid and clear water in mass ratio:The additive amount of 1 composition, leaching liquid is 27.811m3, produce in recovered liquid containing dissolving titanium
26.5g/L, effective acid 54.2g/L, ferrous sulfate 176.9g/L and a small amount of soluble metallic salt substance.It is substituted with production recovered liquid
Part clear water can carry out waste utilization to production recovered liquid, economize on resources.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, contains in the hydrolysising mother liquid
Dissolve titanium 6.8g/L, effective acid 260.8g/L, ferrous sulfate 172.9g/L and a small amount of soluble metallic salt substance.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, solid formation in the step 3
Curing time be 30min, the time of leaching liquid leaching acidolysis solid formation is 4h, and remaining solid is in the leaching liquid after leaching
Non- acidolysis ilmenite and insoluble impurities.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 500mL, the step
In five, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 40 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
w2It is 27.37%；mcFor 15.404g；v2For 31.77m3；w1It is 46.21%；M is 7946Kg；v1For 0.5L.
Acidolysis rate=(1- (27.37% × 15.404g × 31.77m346.21% × 7946Kg of)/(× 0.5L)) ×
100%=92.70%
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, as depicted in figs. 1 and 2, institute
Stating acidolysis pot includes：
The structure of pot body 100, pot body 100 is any type in the prior art, and the application only changes air sparger
Structure；
Compressed air access tube 110 is connected to the bottom of the pot body 100, the air outlet of compressed air access tube 110
End is vertically arranged and is flushed with the bottom in the back taper portion of pot body 100 or reverse frustoconic portion, and is fixedly connected, and compressed air is passed through
The air opening end of pipe 110 is overlapped with the vertical projection of the bottom in back taper portion；
Air sparger, is arranged in the back taper portion of pot body 100, and the air sparger includes：
Air distribution plate 120 is made of the first plate body of polylith 121, and the first plate body of polylith 121 is integrally formed, polylith first
Plate body 121 is set gradually from top to bottom, and in addition to the first plate body 121 positioned at the top, other first plate bodys 121 are in inside
Sky, and the open truncated cone-shaped in top and bottom, the first plate body 121 for being located at the top is circle, and horizontally disposed；It removes
Outside the first plate body 121 of the top, in other two piece of first adjacent plate bodys 121, underlying first plate body 121
The angle of busbar and vertical direction 4-8 degree smaller than the angle of the busbar and vertical direction of the first plate body 121 being located above, and position
It is overlapped with the bottom for the first plate body 121 being located above in the top of the first plate body 121 of lower section；Positioned at the first plate of bottom
The madial wall in the bottom of body 121 and the back taper portion is fixed and is seamlessly connected, and the mother of the first plate body 121 positioned at bottom
Line is vertical with the busbar in back taper portion, is located at the outer diameter of the first plate body 121 of the top and the first plate body adjacent thereto
The internal diameter at 121 top is equal, is located at the top at the edge and the first plate body 121 adjacent thereto of the first plate body 121 of the top
Portion fixes and is seamlessly connected, and multiple air distribution holes are arranged at intervals on every piece of first plate body 121.
When in use, air is entered by compressed air access tube 110 in back taper portion, then is distributed by air acidolysis pot
Hole enters reaction zone.Because the busbar of the first plate body 121 and the angle of vertical direction gradually increase from outside to inside, air can react
It is evenly distributed in area, to make acidolysis solid formation be not easy to be formed in 100 inner wall of pot body, and then reduces the shape of acidolysis solid formation
At raising acidolysis efficiency keeps the acidolysis rate measured more acurrate.Because of the busbar and back taper of the first plate body 121 for being located at bottom
The busbar in portion is vertical, can be along back taper portion after compressed air is placed through the air distribution hole on the first plate body 121 of bottom
Generatrix direction reactant is stirred, ensure that the uniformity stirred when acidolysis reaction, keep acidolysis reaction object loose porous,
Leaching is easier to.So as to eliminate the solid phase for remaining in back taper portion and back taper portion and the binding site in middle cylinder portion
Object.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the air sparger also wraps
It includes：
The first demarcation strip of polylith 130, is arranged at intervals on the lower section of the air distribution plate 120, except positioned at the first of the top
Outside plate body 121, in other first plate bodys 121, corresponding one piece of first demarcation strip 130 of adjacent two piece of first plate body 121, first
Demarcation strip 130 is inner hollow, and the open reverse frustoconic in top and bottom, the top of the first demarcation strip 130 and right with it
The intersection for two piece of first plate body 121 answered is fixed and is seamlessly connected, and bottom is extended to be flushed with the bottom in the back taper portion；
Second demarcation strip 140 is the cylinder bodily form, and is arranged in the lower section of the first plate body 121 of the top, and second
Demarcation strip 140 is coaxially disposed with back taper portion, the outer diameter phase of the outer diameter of the second demarcation strip 140 and the first plate body 121 of the top
The bottom of the first plate body 121 Deng, the top of the second demarcation strip 140 and positioned at the top is fixed and is seamlessly connected, bottom and institute
The bottom for stating back taper portion flushes.
When in use, air enters back taper portion and on the outermost side the to acidolysis pot by compressed air access tube 110
Between one demarcation strip 130, between adjacent two piece of first demarcation strip 130, it is located at innermost first demarcation strip 130 and second point
After between partition board 140 and in the second demarcation strip 140, reaction zone is entered by each air distribution hole, can guarantee so each
There are enough compressed airs to pass through in air distribution hole.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, first demarcation strip 130
It is flushed with the bottom in the back taper portion with the bottom of second demarcation strip 140；Three piece of first adjacent demarcation strip 130
In, it is more than at a distance from the bottom of the first intermediate demarcation strip 130 is between the bottom of the first demarcation strip 130 on the outside of it
Its between the bottom of the first demarcation strip 130 on its inside at a distance from, the bottom of the side wall in the back taper portion with positioned at most
Distance between the bottom of first demarcation strip 130 in outside be more than the first demarcation strip 130 on the outermost side bottom and with its phase
Distance between the bottom of the first adjacent demarcation strip 130 is located at bottom and the second demarcation strip of innermost first demarcation strip 130
Distance between 140 bottom is less than positioned at the bottom of innermost first demarcation strip 130 and is located at innermost first demarcation strip
Distance between the bottom of 130 the first adjacent demarcation strips 130, and more than the internal diameter of the second demarcation strip 140.It can guarantee entrance in this way
Compressed air between the side wall in back taper portion and the first demarcation strip 130 on the outermost side is most, in the second demarcation strip 140 most
It is few, in this way under the premise of ensureing that the middle part of reaction zone has enough compressed airs, compressed air can be enhanced to acidolysis pot pot
The stirring dynamics of wall.
Embodiment 2
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：
Step 1: ilmenite is carried out to match mine and ball milling, the fineness of the miberal powder after ball milling is 325 mesh, residue on sieve 3%, inspection
Survey the TiO of ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 82%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, and it is lasting to stir, reduction reaction is carried out, iron powder is added and constantly surveys in the process
The concentration of titanous so that a concentration of 1g/L of titanous of generation can stop plus iron powder, meet postorder hydrolysis, washing step
Technological requirement；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: measuring the total volume v of the leaching liquid obtained in acidolysis pot after reduction reaction2；
Step 7: calculating acidolysis rate, acidolysis rate=[1- (w2×mc×v2)/(w1×m×v1)] × 100%, wherein m tables
Show that ilmenite throws mineral amount.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the step 2 is specially：
After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.4 into acidolysis pot is 98%, continued using compressed air
Stirring makes material be in the state of mixing substantially uniformity, hydrolysising mother liquid is added later, the mass concentration of diluting concentrated sulfuric acid is extremely
82%.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the leaching liquid is by producing back
It is 1 to receive liquid and clear water in mass ratio:The additive amount of 1 composition, leaching liquid is 28.007m3, produce in recovered liquid containing dissolving titanium
28.5g/L, effective acid 56.3g/L, ferrous sulfate 167.2g/L.Part clear water is substituted with production recovered liquid, production can be recycled
Liquid carries out waste utilization, economizes on resources.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, contains in the hydrolysising mother liquid
Dissolve titanium 7.5g/L, effective acid 271.2g/L, ferrous sulfate 183.6g/L.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, solid formation in the step 3
Curing time be 45min, the time of leaching liquid leaching acidolysis solid formation is 5h, and remaining solid is in the leaching liquid after leaching
Non- acidolysis ilmenite and insoluble impurities.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 700mL, the step
In five, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 50 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
w2It is 26.16%；mcFor 21.566g；v2For 31.68m3；w1It is 46.21%；M is 8002Kg；v1For 0.7L.
Acidolysis rate=(1- (26.16% × 21.566g × 31.68m346.21% × 8002Kg of)/(× 0.7L)) ×
100%=93.10%
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, as depicted in figs. 1 and 2, institute
Stating acidolysis pot includes：
The structure of pot body 100, pot body 100 is any type in the prior art, and the application only changes air sparger
Structure；
Compressed air access tube 110 is connected to the bottom of the pot body 100, the air outlet of compressed air access tube 110
End is vertically arranged and is flushed with the bottom in the back taper portion of pot body 100 or reverse frustoconic portion, and is fixedly connected, and compressed air is passed through
The air opening end of pipe 110 is overlapped with the vertical projection of the bottom in back taper portion；
Air sparger, is arranged in the back taper portion of pot body 100, and the air sparger includes：
Air distribution plate 120 is made of the first plate body of polylith 121, and the first plate body of polylith 121 is integrally formed, polylith first
Plate body 121 is set gradually from top to bottom, and in addition to the first plate body 121 positioned at the top, other first plate bodys 121 are in inside
Sky, and the open truncated cone-shaped in top and bottom, the first plate body 121 for being located at the top is circle, and horizontally disposed；It removes
Outside the first plate body 121 of the top, in other two piece of first adjacent plate bodys 121, underlying first plate body 121
The angle of busbar and vertical direction 4-8 degree smaller than the angle of the busbar and vertical direction of the first plate body 121 being located above, and position
It is overlapped with the bottom for the first plate body 121 being located above in the top of the first plate body 121 of lower section；Positioned at the first plate of bottom
The madial wall in the bottom of body 121 and the back taper portion is fixed and is seamlessly connected, and the mother of the first plate body 121 positioned at bottom
Line is vertical with the busbar in back taper portion, is located at the outer diameter of the first plate body 121 of the top and the first plate body adjacent thereto
The internal diameter at 121 top is equal, is located at the top at the edge and the first plate body 121 adjacent thereto of the first plate body 121 of the top
Portion fixes and is seamlessly connected, and multiple air distribution holes are arranged at intervals on every piece of first plate body 121.
When in use, air is entered by compressed air access tube 110 in back taper portion, then is distributed by air acidolysis pot
Hole enters reaction zone.Because the busbar of the first plate body 121 and the angle of vertical direction gradually increase from outside to inside, air can react
It is evenly distributed in area, to make acidolysis solid formation be not easy to be formed in 100 inner wall of pot body, and then reduces the shape of acidolysis solid formation
At raising acidolysis efficiency keeps the acidolysis rate measured more acurrate.Because of the busbar and back taper of the first plate body 121 for being located at bottom
The busbar in portion is vertical, can be along back taper portion after compressed air is placed through the air distribution hole on the first plate body 121 of bottom
Generatrix direction reactant is stirred, ensure that the uniformity stirred when acidolysis reaction, keep acidolysis reaction object loose porous,
Leaching is easier to.So as to eliminate the solid phase for remaining in back taper portion and back taper portion and the binding site in middle cylinder portion
Object.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the air sparger also wraps
It includes：
The first demarcation strip of polylith 130, is arranged at intervals on the lower section of the air distribution plate 120, except positioned at the first of the top
Outside plate body 121, in other first plate bodys 121, corresponding one piece of first demarcation strip 130 of adjacent two piece of first plate body 121, first
Demarcation strip 130 is inner hollow, and the open reverse frustoconic in top and bottom, the top of the first demarcation strip 130 and right with it
The intersection for two piece of first plate body 121 answered is fixed and is seamlessly connected, and bottom is extended to be flushed with the bottom in the back taper portion；
Second demarcation strip 140 is the cylinder bodily form, and is arranged in the lower section of the first plate body 121 of the top, and second
Demarcation strip 140 is coaxially disposed with back taper portion, the outer diameter phase of the outer diameter of the second demarcation strip 140 and the first plate body 121 of the top
The bottom of the first plate body 121 Deng, the top of the second demarcation strip 140 and positioned at the top is fixed and is seamlessly connected, bottom and institute
The bottom for stating back taper portion flushes.
When in use, air enters back taper portion and on the outermost side the to acidolysis pot by compressed air access tube 110
Between one demarcation strip 130, between adjacent two piece of first demarcation strip 130, it is located at innermost first demarcation strip 130 and second point
After between partition board 140 and in the second demarcation strip 140, reaction zone is entered by each air distribution hole, can guarantee so each
There are enough compressed airs to pass through in air distribution hole.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, first demarcation strip 130
It is flushed with the bottom in the back taper portion with the bottom of second demarcation strip 140；Three piece of first adjacent demarcation strip 130
In, it is more than at a distance from the bottom of the first intermediate demarcation strip 130 is between the bottom of the first demarcation strip 130 on the outside of it
Its between the bottom of the first demarcation strip 130 on its inside at a distance from, the bottom of the side wall in the back taper portion with positioned at most
Distance between the bottom of first demarcation strip 130 in outside be more than the first demarcation strip 130 on the outermost side bottom and with its phase
Distance between the bottom of the first adjacent demarcation strip 130 is located at bottom and the second demarcation strip of innermost first demarcation strip 130
Distance between 140 bottom is less than positioned at the bottom of innermost first demarcation strip 130 and is located at innermost first demarcation strip
Distance between the bottom of 130 the first adjacent demarcation strips 130, and more than the internal diameter of the second demarcation strip 140.It can guarantee entrance in this way
Compressed air between the side wall in back taper portion and the first demarcation strip 130 on the outermost side is most, in the second demarcation strip 140 most
It is few, in this way under the premise of ensureing that the middle part of reaction zone has enough compressed airs, compressed air can be enhanced to acidolysis pot pot
The stirring dynamics of wall.
Embodiment 3
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：
Step 1: ilmenite is carried out to match mine and ball milling, the fineness of the miberal powder after ball milling is 325 mesh, residue on sieve 5%, inspection
Survey the TiO of ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 85%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, it is sufficiently stirred, carries out reduction reaction, constantly survey during iron powder is added
The concentration of titanous so that a concentration of 1.5g/L of titanous of generation can stop plus iron powder, meets postorder hydrolysis, washing step
Technological requirement；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: measuring the total volume v of the leaching liquid obtained in acidolysis pot after reduction reaction2；
Step 7: calculating acidolysis rate, acidolysis rate=[1- (w2×mc×v2)/(w1×m×v1)] × 100%, wherein m tables
Show that ilmenite throws mineral amount.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the step 2 is specially：
After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.6 into acidolysis pot is 98%, continued using compressed air
Stirring makes material be in the state of mixing substantially uniformity, hydrolysising mother liquid is added later, the mass concentration of diluting concentrated sulfuric acid is extremely
85%.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the leaching liquid is by producing back
It is 1 to receive liquid and clear water in mass ratio:The additive amount of 1 composition, leaching liquid is 28.437m3, produce in recovered liquid containing dissolving titanium
29.1g/L, effective acid 58.2g/L, ferrous sulfate 181.5g/L.Part clear water is substituted with production recovered liquid, production can be recycled
Liquid carries out waste utilization, economizes on resources.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, contains in the hydrolysising mother liquid
Dissolve titanium 9.1g/L, effective acid 295.6g/L, ferrous sulfate 196.3g/L.The sulfate process titanium dioxide production process measures mixing
In the method for titanium ore acidolysis rate, the curing time of solid formation is 60min in the step 3, leaching liquid leaching acidolysis solid formation
Time is 6h, and remaining solid is non-acidolysis ilmenite and insoluble impurities in the leaching liquid after leaching.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 1000mL, the step
In rapid five, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 60 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
w2It is 25.58%；mcFor 30.629g；v2For 31.36m3；w1It is 46.21%；M is 8125Kg；v1For 1.0L.
Acidolysis rate=(1- (25.58% × 30.629g × 31.36m346.21% × 8125Kg of)/(× 1.0L)) ×
100%=93.46%
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, as depicted in figs. 1 and 2, institute
Stating acidolysis pot includes：
The structure of pot body 100, pot body 100 is any type in the prior art, and the application only changes air sparger
Structure；
Compressed air access tube 110 is connected to the bottom of the pot body 100, the air outlet of compressed air access tube 110
End is vertically arranged and is flushed with the bottom in the back taper portion of pot body 100 or reverse frustoconic portion, and is fixedly connected, and compressed air is passed through
The air opening end of pipe 110 is overlapped with the vertical projection of the bottom in back taper portion；
Air sparger, is arranged in the back taper portion of pot body 100, and the air sparger includes：
Air distribution plate 120 is made of the first plate body of polylith 121, and the first plate body of polylith 121 is integrally formed, polylith first
Plate body 121 is set gradually from top to bottom, and in addition to the first plate body 121 positioned at the top, other first plate bodys 121 are in inside
Sky, and the open truncated cone-shaped in top and bottom, the first plate body 121 for being located at the top is circle, and horizontally disposed；It removes
Outside the first plate body 121 of the top, in other two piece of first adjacent plate bodys 121, underlying first plate body 121
The angle of busbar and vertical direction 4-8 degree smaller than the angle of the busbar and vertical direction of the first plate body 121 being located above, and position
It is overlapped with the bottom for the first plate body 121 being located above in the top of the first plate body 121 of lower section；Positioned at the first plate of bottom
The madial wall in the bottom of body 121 and the back taper portion is fixed and is seamlessly connected, and the mother of the first plate body 121 positioned at bottom
Line is vertical with the busbar in back taper portion, is located at the outer diameter of the first plate body 121 of the top and the first plate body adjacent thereto
The internal diameter at 121 top is equal, is located at the top at the edge and the first plate body 121 adjacent thereto of the first plate body 121 of the top
Portion fixes and is seamlessly connected, and multiple air distribution holes are arranged at intervals on every piece of first plate body 121.
When in use, air is entered by compressed air access tube 110 in back taper portion, then is distributed by air acidolysis pot
Hole enters reaction zone.Because the busbar of the first plate body 121 and the angle of vertical direction gradually increase from outside to inside, air can react
It is evenly distributed in area, to make acidolysis solid formation be not easy to be formed in 100 inner wall of pot body, and then reduces the shape of acidolysis solid formation
At raising acidolysis efficiency keeps the acidolysis rate measured more acurrate.Because of the busbar and back taper of the first plate body 121 for being located at bottom
The busbar in portion is vertical, can be along back taper portion after compressed air is placed through the air distribution hole on the first plate body 121 of bottom
Generatrix direction reactant is stirred, ensure that the uniformity stirred when acidolysis reaction, keep acidolysis reaction object loose porous,
Leaching is easier to.So as to eliminate the solid phase for remaining in back taper portion and back taper portion and the binding site in middle cylinder portion
Object.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the air sparger also wraps
It includes：
The first demarcation strip of polylith 130, is arranged at intervals on the lower section of the air distribution plate 120, except positioned at the first of the top
Outside plate body 121, in other first plate bodys 121, corresponding one piece of first demarcation strip 130 of adjacent two piece of first plate body 121, first
Demarcation strip 130 is inner hollow, and the open reverse frustoconic in top and bottom, the top of the first demarcation strip 130 and right with it
The intersection for two piece of first plate body 121 answered is fixed and is seamlessly connected, and bottom is extended to be flushed with the bottom in the back taper portion；
Second demarcation strip 140 is the cylinder bodily form, and is arranged in the lower section of the first plate body 121 of the top, and second
Demarcation strip 140 is coaxially disposed with back taper portion, the outer diameter phase of the outer diameter of the second demarcation strip 140 and the first plate body 121 of the top
The bottom of the first plate body 121 Deng, the top of the second demarcation strip 140 and positioned at the top is fixed and is seamlessly connected, bottom and institute
The bottom for stating back taper portion flushes.
When in use, air enters back taper portion and on the outermost side the to acidolysis pot by compressed air access tube 110
Between one demarcation strip 130, between adjacent two piece of first demarcation strip 130, it is located at innermost first demarcation strip 130 and second point
After between partition board 140 and in the second demarcation strip 140, reaction zone is entered by each air distribution hole, can guarantee so each
There are enough compressed airs to pass through in air distribution hole.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, first demarcation strip 130
It is flushed with the bottom in the back taper portion with the bottom of second demarcation strip 140；Three piece of first adjacent demarcation strip 130
In, it is more than at a distance from the bottom of the first intermediate demarcation strip 130 is between the bottom of the first demarcation strip 130 on the outside of it
Its between the bottom of the first demarcation strip 130 on its inside at a distance from, the bottom of the side wall in the back taper portion with positioned at most
Distance between the bottom of first demarcation strip 130 in outside be more than the first demarcation strip 130 on the outermost side bottom and with its phase
Distance between the bottom of the first adjacent demarcation strip 130 is located at bottom and the second demarcation strip of innermost first demarcation strip 130
Distance between 140 bottom is less than positioned at the bottom of innermost first demarcation strip 130 and is located at innermost first demarcation strip
Distance between the bottom of 130 the first adjacent demarcation strips 130, and more than the internal diameter of the second demarcation strip 140.It can guarantee entrance in this way
Compressed air between the side wall in back taper portion and the first demarcation strip 130 on the outermost side is most, in the second demarcation strip 140 most
It is few, in this way under the premise of ensureing that the middle part of reaction zone has enough compressed airs, compressed air can be enhanced to acidolysis pot pot
The stirring dynamics of wall.
In Producing Titanium Dioxide enterprise, the method for measuring acidolysis rate is typically to be sampled from the leaching liquid on acidolysis pot top, to it
It is filtered washing, the calculating of acidolysis rate is carried out by detecting the titanium amount in titanium liquid and residue respectively.The deficiency of this kind of method
Place is, due to the acidolysis leaching stage of titanium white actual production, in order to save cost, and is utilized to waste, adds water
The waste water of part titaniums containing dissolving such as hydrolysis mother liquor, production recovered liquid, then under conditions of same leaching liquid volume, obtained titanium liquid is dense
Degree can be higher, and the acidolysis rate measured is more higher than practical acidolysis rate, cannot accurately reflect the practical acidolysis rate of production process.
Comparative example 1
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：
Step 1: ilmenite is carried out to match mine and ball milling, the fineness of the miberal powder after ball milling is 325 mesh, residue on sieve 2%, inspection
Survey the TiO of ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 80%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, and it is lasting to stir, reduction reaction is carried out, iron powder is added and constantly surveys in the process
The concentration of titanous so that a concentration of 0.5g/L of titanous of generation can stop plus iron powder, meets postorder hydrolysis, washing step
Technological requirement；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: the titanium concentration c that detection obtains after filtering1And accurate recording titanium liquid product v3；
Step 7: calculating acidolysis rate, acidolysis rate=(v3×c1)/(w2×mc+v3×c1) × 100%, wherein v3Expression takes
The titanium liquid product that sample leaching liquid filtration washing obtains, c1Indicate its titanium concentration.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the step 2 is specially：
After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.3 into acidolysis pot is 98%, continued using compressed air
Stirring makes material be in the state of mixing substantially uniformity, hydrolysising mother liquid is added later, the mass concentration of diluting concentrated sulfuric acid is extremely
80%.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the leaching liquid is by producing back
It is 1 to receive liquid and clear water in mass ratio:The additive amount of 1 composition, leaching liquid is 27.811m3, produce in recovered liquid containing dissolving titanium
26.5g/L, effective acid 54.2g/L, ferrous sulfate 176.9g/L.Part clear water is substituted with production recovered liquid, production can be recycled
Liquid carries out waste utilization, economizes on resources.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, contains in the hydrolysising mother liquid
Dissolve titanium 6.8g/L, effective acid 260.8g/L, ferrous sulfate 172.9g/L.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, solid formation in the step 3
Curing time be 30min, the time of leaching liquid leaching acidolysis solid formation is 4h, and remaining solid is in the leaching liquid after leaching
Non- acidolysis ilmenite and insoluble impurities.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 500mL, the step
In five, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 40 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
The acidolysis pot that comparative example 1 uses is same as Example 1.
Calculate acidolysis rate, acidolysis rate=(v3×c1)/(w2×mc+v3×c1) × 100%, wherein v3Indicate sampling leaching
The titanium liquid product that liquid filtration washing obtains, c1Indicate its titanium concentration.
Acidolysis rate=(0.773L × 83.86g/L)/(27.37% × 15.404g+0.773L × 83.86g/L) × 100%
=93.89%
Compared with Example 1 compared with the acidolysis rate that conventional method calculates is 1.19 percentage points more higher than actual acidolysis rate.
Comparative example 2
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：
Step 1: ilmenite is carried out to match mine and ball milling, the fineness of the miberal powder after ball milling is 325 mesh, residue on sieve 3%, inspection
Survey the TiO of ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 82%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, and it is lasting to stir, reduction reaction is carried out, iron powder is added and constantly surveys in the process
The concentration of titanous so that a concentration of 1g/L of titanous of generation can stop plus iron powder, meet postorder hydrolysis, washing step
Technological requirement；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: the titanium concentration c that detection obtains after filtering1And accurate recording titanium liquid product v3；
Step 7: calculating acidolysis rate, acidolysis rate=(v3×c1)/(w2×mc+v3×c1) × 100%, wherein v3Expression takes
The titanium liquid product that sample leaching liquid filtration washing obtains, c1Indicate its titanium concentration..
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the step 2 is specially：
After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.4 into acidolysis pot is 98%, continued using compressed air
Stirring makes material be in the state of mixing substantially uniformity, hydrolysising mother liquid is added later, the mass concentration of diluting concentrated sulfuric acid is extremely
82%.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the leaching liquid is by producing back
It is 1 to receive liquid and clear water in mass ratio:The additive amount of 1 composition, leaching liquid is 28.007m3, produce in recovered liquid containing dissolving titanium
28.5g/L, effective acid 56.3g/L, ferrous sulfate 167.2g/L.Part clear water is substituted with production recovered liquid, production can be recycled
Liquid carries out waste utilization, economizes on resources.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, contains in the hydrolysising mother liquid
Dissolve titanium 7.5g/L, effective acid 271.2g/L, ferrous sulfate 183.6g/L.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, solid formation in the step 3
Curing time be 45min, the time of leaching liquid leaching acidolysis solid formation is 5h, and remaining solid is in the leaching liquid after leaching
Non- acidolysis ilmenite and insoluble impurities.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 700mL, the step
In five, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 50 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
The acidolysis pot that comparative example 2 uses is same as Example 2.
Calculate acidolysis rate, acidolysis rate=(v3×c1)/(w2×mc+v3×c1) × 100%, wherein v3Indicate sampling leaching
The titanium liquid product that liquid filtration washing obtains, c1Indicate its titanium concentration.
Acidolysis rate=(1.106L × 85.92g/L)/(26.16% × 21.566g+1.106L × 85.92g/L) × 100%
=94.40%
Compared with Example 2 compared with the acidolysis rate that conventional method calculates is 1.30 percentage points more higher than actual acidolysis rate.
Comparative example 3
The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, including：
Step 1: ilmenite is carried out to match mine and ball milling, the fineness of the miberal powder after ball milling is 325 mesh, residue on sieve 5%, inspection
Survey the TiO of ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute
The mass concentration of the concentrated sulfuric acid is to 85%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, leaching liquid leaching acid is added into acidolysis pot
Solve solid formation；
Step 4: iron powder is added into acidolysis pot, it is sufficiently stirred, carries out reduction reaction, constantly survey during iron powder is added
The concentration of titanous so that a concentration of 1.5g/L of titanous of generation can stop plus iron powder, meets postorder hydrolysis, washing step
Technological requirement；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, is obtained
To titanium liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: the titanium concentration c that detection obtains after filtering1And accurate recording titanium liquid product v3；
Step 7: calculating acidolysis rate, acidolysis rate=(v3×c1)/(w2×mc+v3×c1) × 100%, wherein v3Expression takes
The titanium liquid product that sample leaching liquid filtration washing obtains, c1Indicate its titanium concentration..
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the step 2 is specially：
After the concentrated sulfuric acid and ilmenite that the mass fraction that addition mass ratio is 1.6 into acidolysis pot is 98%, continued using compressed air
Stirring makes material be in the state of mixing substantially uniformity, hydrolysising mother liquid is added later, the mass concentration of diluting concentrated sulfuric acid is extremely
85%.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, and the leaching liquid is by producing back
It is 1 to receive liquid and clear water in mass ratio:The additive amount of 1 composition, leaching liquid is 28.437m3, produce in recovered liquid containing dissolving titanium
29.1g/L, effective acid 58.2g/L, ferrous sulfate 181.5g/L.Part clear water is substituted with production recovered liquid, production can be recycled
Liquid carries out waste utilization, economizes on resources.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, contains in the hydrolysising mother liquid
Dissolve titanium 9.1g/L, effective acid 295.6g/L, ferrous sulfate 196.3g/L.The sulfate process titanium dioxide production process measures mixing
In the method for titanium ore acidolysis rate, the curing time of solid formation is 60min in the step 3, leaching liquid leaching acidolysis solid formation
Time is 6h, and remaining solid is non-acidolysis ilmenite and insoluble impurities in the leaching liquid after leaching.
The sulfate process titanium dioxide production process measures in the method for mixing titanium ore acidolysis rate, v1For 1000mL, the step
In rapid five, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 60 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
The acidolysis pot that comparative example 3 uses is same as Example 3.
Calculate acidolysis rate, acidolysis rate=(v3×c1)/(w2×mc+v3×c1) × 100%, wherein v3Indicate sampling leaching
The titanium liquid product that liquid filtration washing obtains, c1Indicate its titanium concentration.
Acidolysis rate=(1.756L × 87.25g/L)/(25.58% × 30.629g+1.756L × 87.25g/L) × 100%
=95.13%
Compared with Example 3 compared with the acidolysis rate that conventional method calculates is 1.67 percentage points more higher than actual acidolysis rate.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and embodiment shown and described herein and legend.
Claims (10)
1. the method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate, which is characterized in that including：
Step 1: the TiO of detection ilmenite2Grade w1；
Step 2: the concentrated sulfuric acid is added into acidolysis pot with after ilmenite, it is sufficiently stirred, hydrolysising mother liquid is added later, dilute dense sulphur
The mass concentration of acid is to 78~85%；
Step 3: obtaining solid formation after acidolysis reaction is complete, after solid formation curing, it is solid that leaching liquid leaching acidolysis is added into acidolysis pot
Phase object；
Step 4: iron powder is added into acidolysis pot, reduction reaction is carried out；
Step 5: the part leaching liquid v after sampling reduction reaction in acidolysis pot1, the leaching liquid of taking-up is filtered, titanium is obtained
Liquid and residue, by residual washing-out drying to constant weight mc, and detect TiO in residue butt2Grade w2；
Step 6: measuring the total volume v of the leaching liquid obtained in acidolysis pot after reduction reaction2；
Step 7: calculating acidolysis rate, acidolysis rate=[1- (w2×mc×v2)/(w1×m×v1)] × 100%, wherein m indicates titanium
Iron ore throws mineral amount.
2. the method that sulfate process titanium dioxide production process as described in claim 1 measures mixing titanium ore acidolysis rate, which is characterized in that
The step 2 is specially：The concentrated sulfuric acid and ferrotianium that the mass fraction that addition mass ratio is 1.3~1.6 into acidolysis pot is 98%
It after mine, is persistently stirred using compressed air, is added hydrolysising mother liquid later, the mass concentration of diluting concentrated sulfuric acid to 78~85%.
3. the method that sulfate process titanium dioxide production process as claimed in claim 2 measures mixing titanium ore acidolysis rate, which is characterized in that
Hydrolysising mother liquid, the mass concentration of diluting concentrated sulfuric acid to 80~85% is added.
4. the method that sulfate process titanium dioxide production process as described in claim 1 measures mixing titanium ore acidolysis rate, which is characterized in that
The leaching liquid is 1 in mass ratio by production recovered liquid and clear water:1 composition, the additive amount of leaching liquid are set as：The body of leaching liquid
The mass ratio of product and ilmenite is 3.5m3/ t is produced in recovered liquid containing dissolving 5~30g/L of titanium, 10~60g/L of effective acid, sulphur
100~200g/L of sour ferrous iron.
5. the method that sulfate process titanium dioxide production process as claimed in claim 4 measures mixing titanium ore acidolysis rate, which is characterized in that
Contain dissolving 5~10g/L of titanium, 250~300g/L of effective acid, 150~200g/L of ferrous sulfate in the hydrolysising mother liquid.
6. the method that sulfate process titanium dioxide production process as described in claim 1 measures mixing titanium ore acidolysis rate, which is characterized in that
The curing time of solid formation is 30~60min in the step 3, and the time of leaching liquid leaching acidolysis solid formation is 4~6h.
7. the method that sulfate process titanium dioxide production process as described in claim 1 measures mixing titanium ore acidolysis rate, which is characterized in that
v1For 500~1000mL, in the step 5, it is by the residual washing-out specific method that drying to constant weight：
Residue is used into 40~60 DEG C of the abundant washes clean of warm water, after removing the soluble titanium in residue completely, 100 DEG C with
It is upper that drying to constant weight.
8. the method that sulfate process titanium dioxide production process as described in claim 1 measures mixing titanium ore acidolysis rate, which is characterized in that
The acidolysis pot includes：
Pot body；
Compressed air access tube is connected to the bottom of the pot body, and the air opening end of compressed air access tube is vertically arranged；
Air sparger, is arranged in the back taper portion of pot body, and the air sparger includes：
Air distribution plate is made of the first plate body of polylith, and the first plate body of polylith be integrally formed, the first plate body of polylith from top to bottom according to
Secondary setting, in addition to the first plate body positioned at the top, other first plate bodys are inner hollow, and the open circle in top and bottom
Platform shape, the first plate body for being located at the top is circle, and horizontally disposed；In addition to the first plate body positioned at the top,
In his two piece of first adjacent plate body, the busbar of underlying first plate body and the angle of vertical direction than be located above
The busbar of one plate body and the small 4-8 degree of the angle of vertical direction, and the top of underlying first plate body and be located above the
The bottom of one plate body overlaps, the length of the busbar of the length of the busbar of underlying first plate body and the first plate body being located above
It spends equal；Madial wall positioned at the bottom of the first plate body of bottom and the back taper portion is fixed and is seamlessly connected, and is located at
The busbar of first plate body of bottom is vertical with the busbar in back taper portion, be located at the top the first plate body outer diameter and with
The internal diameter at the top of its first adjacent plate body is equal, is located at the edge of the first plate body of the top and the first plate adjacent thereto
The top fixation and seamless connection of body are arranged at intervals with multiple air distribution holes on every piece of first plate body.
9. the method that sulfate process titanium dioxide production process as claimed in claim 8 measures mixing titanium ore acidolysis rate, which is characterized in that
The air sparger further includes：
The first demarcation strip of polylith, is arranged at intervals on the lower section of the air distribution plate, in addition to the first plate body positioned at the top, other
In first plate body, adjacent two pieces of first plate bodys correspond to one piece of first demarcation strip, and the first demarcation strip is inner hollow, and top
With the open reverse frustoconic in bottom, the intersection of the top of the first demarcation strip and corresponding two pieces of first plate bodys fix and
It is seamlessly connected, bottom extends in compressed air access tube or flushed with the bottom in the back taper portion；
Second demarcation strip is the cylinder bodily form, and is arranged in the lower section of the first plate body of the top, the second demarcation strip with fall
Tapered portion is coaxially disposed, and the outer diameter of the second demarcation strip is equal with the outer diameter of the first plate body of the top, the top of the second demarcation strip
Fix and be seamlessly connected with the bottom of the first plate body positioned at the top, bottom extend in compressed air access tube or with it is described
The bottom in back taper portion flushes.
10. the method that sulfate process titanium dioxide production process as claimed in claim 9 measures mixing titanium ore acidolysis rate, feature exist
In the bottom of first demarcation strip and second demarcation strip is flushed with the bottom in the back taper portion；Adjacent three pieces
In first demarcation strip, at a distance from the bottom of the first intermediate demarcation strip is between the bottom of the first demarcation strip on the outside of it
More than its between the bottom of the first demarcation strip on its inside at a distance from, the bottom of the side wall in the back taper portion with positioned at most
Distance between the bottom of first demarcation strip in outside is more than the bottom and adjacent thereto the of the first demarcation strip on the outermost side
Distance between the bottom of one demarcation strip, at a distance from the bottom of innermost first demarcation strip is between the bottom of the second demarcation strip
Less than positioned at the bottom of the bottom of innermost first demarcation strip first demarcation strip adjacent with innermost first demarcation strip is located at
Distance between portion, and more than the internal diameter of the second demarcation strip.
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