CN109607608A - A kind of production method of non-coating rutile type titanium white - Google Patents
A kind of production method of non-coating rutile type titanium white Download PDFInfo
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- CN109607608A CN109607608A CN201910091764.9A CN201910091764A CN109607608A CN 109607608 A CN109607608 A CN 109607608A CN 201910091764 A CN201910091764 A CN 201910091764A CN 109607608 A CN109607608 A CN 109607608A
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Abstract
The present invention relates to titanium dioxide preparation fields, more particularly to a kind of production method of non-coating rutile type titanium white, this method include (1) selected raw material (2) titanium liquid prepare (3) titanium liquid preheating (4) production crystal seed (5) be added crystal seed (6) hydrolysis (7) rinse (8) washing (9) calcining and etc., titanium liquid in the present invention after acidolysis can be hydrolyzed without concentration, low energy consumption, by the way that crystal type promoting reagent is added when preparing crystal seed, titanium dioxide can be promoted to convert in process of production toward rutile, play stronger transformation of crystal facilitation, and calcination temperature is lower, significantly reduce the damage to equipment, by the way that crystal type promoting reagent is added when preparing crystal seed and keeps the temperature 3 hours the two links after calcining, the titanium dioxide that production can be promoted to obtain is converted toward rutile, rutile high conversion rate, To obtain the non-coating rutile type titanium white of high-rutile content.
Description
Technical field
The present invention relates to titanium dioxide preparation fields, and in particular to a kind of production of non-coating rutile type titanium white
Method.
Background technique
Titanium dioxide (English name: titanium dioxide), main component are the white pigment of titanium dioxide (TiO2),
Titanium dioxide is considered as a kind of current best white pigment of performance in the world, is widely used in coating, plastics, papermaking, printing
The industry such as ink, chemical fibre, rubber, cosmetics.Titanium dioxide is in nature there are three types of crystal habit: rutile-type, anatase titanium dioxide and
Plate titanium-type, rutile-type are the most stable of crystal habits of titanium dioxide, compact structure, have compared with anatase titanium dioxide higher hardness,
Density, dielectric constant and index of refraction have higher covering power and anti-loss of gloss and resistance to chalking, not only have stable physics
Chemical property, but also the pigment performance with excellent optics, electrology characteristic and brilliance, rutile type titanium white are answered extensively
Medicine and other fields are summed it up for coating, plastics, papermaking, printing ink, chemical fibre, rubber, ceramics, cosmetics and food additive.
Currently, the method for domestic production titanium dioxide mainly has sulfuric acid process and chloridising.Chloridising is with TiO2Content 85% with
On high titanium slag (or rutile concentrate) be that raw material through chlorination, purification and oxidation operation obtains rutile titanium dioxide.It should
Method and process process is short, serialization high degree of automation, and " three wastes " discharge amount is few, and product is high-quality, but the disadvantage is that raw material matter
Amount requires height, and research and development technology difficulty is big, only has a few company to grasp technique (Du Pont, U.S. connection chemistry etc.) at present, if
Standby investment cost is high.
Sulfuric acid process is with ilmenite concentrate (TiO2Content 45%~50%) and acid-dissolved titanium slag (TiO275%) content is about raw material, warp
Acidolysis, the preparation of titanium liquid, hydrolysis, calcining and postprocessing working procedures, obtain anatase titanium dioxide or rutile titanium dioxide.Party's law technology at
Ripe, equipment investment expense is low, but process flow is long, and " three wastes " discharge amount is big.After the chilled Crystallization Separation of sulfuric acid process is ferrous
Diluted Ti solution TiO2Concentration generally about 150g/L, for the qualified pigment-level titanium white of preparation, it is necessary to it is dense that this diluted Ti solution is subjected to vacuum
Contracting, until being concentrated to TiO2 200 ± 5g/L(pressurized hydrolysis use) or TiO2215~230g/L(ordinary-pressure hydrolysis use) until, it causes
Process flow is complicated；A large amount of rutile calcining seeds need to be added when furthermore producing rutile titanium dioxide, and are carried out for a long time
High-temperature calcination (950 DEG C of >), energy consumption is high, big to the damage of equipment, and the rutile rate of crystal seed is low, rutile first product product
Matter is not high.
Summary of the invention
The object of the present invention is to provide a kind of production method of non-coating rutile type titanium white, this method technique letters
Single, the titanium liquid after acidolysis can be hydrolyzed without concentration, and low energy consumption, and calcination temperature is low, alleviates the damage to equipment
Wound, and by the way that crystal type promoting reagent is added when preparing crystal seed and keeps the temperature 3 hours the two links after calcining, it can promote to give birth to
It produces obtained titanium dioxide to convert toward rutile, rutile high conversion rate, to obtain the non-coating golden red of high-rutile content
Stone-type titanium dioxide.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of production method of non-coating rutile type titanium white, which comprises the following steps:
(1) selected raw material: P in control titanium ore205Mass percentage is less than 0.05%；
(2) prepared by titanium liquid: routinely sulfuric acid will be added in titanium ore by technique, through acidolysis, sedimentation, freezing, crystallization and ferrous iron
Titanium liquid is obtained after separating technology, titanium liquid is without concentration, and the index of correlation of obtained titanium liquid is as follows: TiO2Concentration: 140 ± 10g/
L, F value: 1.85~2.05；Iron titanium ratio: 0.30~0.45；Clarity: level-one supernatant；Trivalent Ti content: 0.5~1.5g/L；Surely
It is qualitative: >=300；
(3) titanium liquid preheats: preparing by technic index and the titanium liquid measured (by the volume of titanium liquid needed for each hydrolyzer) is thrown into
Foreheater is hydrolyzed, and is passed through steam and is heated (preheating of titanium liquid)；It is measured simultaneously by the 2.2% of every pot of Hydrolysis of Titanium liquid measure volume past
The pre- heat channel of crystal seed titanium liquid squeezes into titanium liquid；Crystal seed preparation vessel squeezes into lye, while crystal type promoting reagent is added, by Hydrolysis of Titanium liquid (m3):
Crystal type promoting reagent (kg)=2.5:1~1.2 ratio is added, and opens stirring；
(4) make crystal seed: when titanium liquid foreheater titanium liquid temperature is raised to 75 DEG C, the starting pre- heat channel of crystal seed titanium liquid stirs and opens steaming
Vapor inlet valve heats up to crystal seed titanium liquid；And steam inlet valve is opened, it heats up to the lye in crystal seed preparation vessel, and keep lye
Temperature is at 84-87 DEG C；When crystal seed titanium liquid is warming up to 84-87 DEG C, the pre- heat channel baiting valve of crystal seed titanium liquid is opened preheated titanium
Liquid is put into crystal seed preparation vessel, controls discharging time 5-8 minutes, continues to heat the material in crystal seed preparation vessel after discharging crystal seed titanium liquid
Stop heating when to 95-97 DEG C, crystal seed is made；
(5) crystal seed is added: the titanium liquid that foreheater is hydrolyzed in crystal seed manufacturing process continues to heat up, and controls at 95-97 DEG C, waits
Crystal seed carries out that (waiting time is not too long, has to that the titanium liquid of foreheater is allowed first to be warming up to 95-97 DEG C, must not first be made to
To crystal seed, equal titaniums liquid is warming up to 95-97 DEG C again), ready-made crystal seed is quickly added in preheated titanium liquid, stirs 10- after adding
15 minutes, hydrolysis foreheater baiting valve is opened, the titanium liquid of hydrolysis foreheater is put into hydrolyzer, while starting hydrolyzer and stirring
It mixes, when titanium liquid touches the heating steam pipe in hydrolyzer, opens small steam and heat up to Hydrolysis of Titanium liquid；
(6) it hydrolyzes: after hydrolyzing foreheater titanium liquid and discharging, increasing steam inlet valve, so that Hydrolysis of Titanium liquid is rapidly achieved boiling and start
Hydrolysis adjusts small steam, prevents transition boiling after the boiling of Hydrolysis of Titanium liquid；It being kept for slight boiling condition 120-150 minutes, hydrolysis terminates,
Turn off steam valve；
(7) it rinses: after blowing, rinsing titanium hydrolysis foreheater, the pre- heat channel of crystal seed titanium liquid and crystal seed preparation vessel well, rush
Washing lotion is discharged into light white sink；Flushing finishes, and closes hydrolysis foreheater and crystal seed production slot baiting valve, each valve restore normal；
(8) it washs: washing the product metatitanic acid after hydrolysis by prior art, wash time is kept for 40-60 minutes, washing
Guarantee filter cake iron content≤0.03% when to terminal；
(9) it calcines: the qualified filter cake of washing is beaten with deionized water, control slurry concentration is 300 ± 20 grams per liters, through filter press
After pressing dry, filter cake weight water content being controlled in 45-55%, is transported to rotary kiln, drying is calcined at 860 DEG C, control falls kiln product sulphur
Material is put into a temperature control after calcining and carries out constant temperature placement 3 hours in 860 DEG C of thermostatic tank by content less than 0.05%
Afterwards, material is continuously entered from tank deck, is continuously discharged from tank bottom, is entered back into cooling kiln and is cooled down, is most crushed, packed afterwards, obtained
To non-coating rutile type titanium white.
In the production method of above-mentioned non-coating rutile type titanium white, the lye is the hydrogen that concentration is 60g/L
Sodium hydroxide solution, the additional amount of lye are the 32~35% of crystal seed titanium liquid measure volume.
The production method of above-mentioned non-coating rutile type titanium white, crystal type promoting reagent used in step (3) are zinc
Salt or pink salt, the esterification for specifically including stannous chloride, zinc sulfate, zinc chloride etc. or stannous chloride, zinc sulfate, zinc chloride are answered
Object, such as zinc abietate are closed, the crystal type promoting reagent can also (address be in Sichuan Province China using Chengdu jump new science and technology research institute
The room 25-1-28-1 of Chengdu high and new technology industrial development zone Tianfu Avenue middle section 177) production entitled " reason is crystal stabilization " product, should
" reason is crystal stabilization " is compound crystal type promoting reagent, is combined for organic matter polyalcohol with inorganic salts.
The production method of the non-coating rutile type titanium white, the non-coating rutile titanium dioxide produced
Rutile content >=90% in powder.And under being met using the non-coating rutile type titanium white that the method for the present invention produces
Every test rating in table 1.
The invention has the benefit that
1, the production method of non-coating rutile type titanium white provided by the invention, this method is in non-coating enamel grade titanium dioxide powder
It carries out producing non-coating rutile type titanium white on the basis of production method, simple process, the titanium liquid after acidolysis is without overrich
Contracting can be hydrolyzed, and low energy consumption, and calcination temperature is low, alleviate the damage to equipment, greatly reduce production cost,
After calcining by by titanium dioxide in heat insulation tank insulation reaction 3 hours, the obtained titanium dioxide of production can be promoted toward rutile
Conversion, rutile high conversion rate, to obtain the non-coating rutile type titanium white of high-rutile content.Using present invention side
Rutile content >=90% in the non-coating rutile type titanium white that method produces, and meet non-coating rutile type titanium
Every test rating of white powder.
2, the present invention can play stronger transformation of crystal facilitation by the way that crystal type promoting reagent is added when preparing crystal seed,
Promote product to convert toward rutile, the correct progress that crystal seed can induce pyrohydrolysis to react is added in hydrolytic process, induces titanium
Liquid is hydrolyzed into the metatitanic acid with the pre- structure of rutile-type；So that titanium dioxide produced, it can be under lower calcination temperature
Transform into rutile type titanium white；And crystal type promoting reagent used in the present invention be it is soluble, will not be to the pure of product
Degree impacts.
3, titanium white production method calcination process all at present does not all keep the temperature this link, so with production enamel titanium
The rutile content that the method for white powder produce resulting titanium dioxide is all very low, is only improved and forges to raising rutile content
Temperature is burnt, and core of the present invention is that addition crystal type promoting reagent and calcining are increased on the basis of producing enamel grade titanium dioxide powder to be terminated
3 hours the two links are kept the temperature, by the improvement of the two processing steps, the titanium dioxide produced has stronger rutile
Conversion trend can produce the non-coating rutile type titanium white for obtaining high-rutile content compared with low energy consumption.This
Invention stablizes the obtained non-coating rutile type titanium white quality of production by changing technique, have with high purity, whiteness is good,
Uniform particle sizes and the characteristics of higher reducing power, compared with traditional conventional products, have production cost low, and it is excellent that quality is stablized etc.
Point, the deep welcome by customers, is suitably applied the industrial departments such as enamel, ceramics, electronics, metallurgy.
Detailed description of the invention
Fig. 1 is the schematic device of calcine technology in the production method of the non-coating rutile type titanium white of the present invention；
Fig. 2 is the structural schematic diagram of thermostatic tank used in the production method of the non-coating rutile type titanium white of the present invention；
The title of figure label is as follows:
1, calcination rotary kiln, 2, thermostatic tank, 3, cooling kiln, 4, thermostatic tank cover, 5, electrode, 6, porcelain tube, 7, constant temperature tank, 8,
Discharge turntable, 9, discharge port, 10, discharging adjustable plate, 11, outlet pipe, 12, material blanking tube, 13, transmission device, 14, rack, 15, turn
Axis, 16, drip tray, 17, cooling jacket, 18, water inlet pipe, 19, receiver, 20, refractory brick, 21 alumina silicate Nomexs.
Specific embodiment
Embodiment 1
A kind of production method of non-coating rutile type titanium white, comprising the following steps:
(1) selected raw material: P in control titanium ore205Mass percentage is less than 0.05%；
(2) prepared by titanium liquid: routinely sulfuric acid will be added in titanium ore by technique, through acidolysis, sedimentation, freezing, crystallization and ferrous iron
Titanium liquid is obtained after separating technology, titanium liquid is without concentration, and the index of correlation of obtained titanium liquid is as follows: TiO2Concentration: 140 ± 10g/
L, F value: 1.85~2.05；Iron titanium ratio: 0.30~0.45；Clarity: level-one supernatant；Trivalent Ti content: 0.5~1.5g/L；Surely
It is qualitative: >=300；
(3) titanium liquid preheats: preparing by technic index and the titanium liquid measured throws hydrolysis foreheater into, and be passed through steam and added
Heat；It measures simultaneously by the 2.2% of every pot of Hydrolysis of Titanium liquid measure volume toward the pre- heat channel of crystal seed titanium liquid and squeezes into titanium liquid；Crystal seed preparation vessel is squeezed into
Lye, the lye are the sodium hydroxide solutions that concentration is 60g/L, and the additional amount of lye is the 32% of crystal seed titanium liquid measure volume；
Crystal type promoting reagent is added simultaneously, by Hydrolysis of Titanium liquid (m3): crystal type promoting reagent (kg)=2.5:1 ratio is added, and opens stirring；Institute
The crystal type promoting reagent stated is stannous chloride；
(4) make crystal seed: when titanium liquid foreheater titanium liquid temperature is raised to 75 DEG C, the starting pre- heat channel of crystal seed titanium liquid is stirred and is opened
Steam inlet valve heats up to crystal seed titanium liquid；And steam inlet valve is opened, it heats up to the lye in crystal seed preparation vessel, and keep alkali
Liquid temperature is at 84 DEG C；When crystal seed titanium liquid is warming up to 84 DEG C, opens the pre- heat channel baiting valve of crystal seed titanium liquid and preheated titanium liquid is put
Enter crystal seed preparation vessel, control discharging time 5 minutes, discharges and continue to heat material in crystal seed preparation vessel after crystal seed titanium liquid to 95 DEG C
When stop heating, be made crystal seed；
(5) crystal seed is added: the titanium liquid that foreheater is hydrolyzed in crystal seed manufacturing process continues to heat up, and controls at 95 DEG C, waits brilliant
Kind is carried out, and ready-made crystal seed is quickly added in preheated titanium liquid, is stirred 10 minutes after adding, and hydrolysis foreheater blowing is opened
Valve is put into the titanium liquid of hydrolysis foreheater in hydrolyzer, while starting hydrolyzer stirring, when titanium liquid touches adding in hydrolyzer
When live steam pipe, opens small steam and heat up to Hydrolysis of Titanium liquid；
(6) it hydrolyzes: after hydrolyzing foreheater titanium liquid and discharging, increasing steam inlet valve, so that Hydrolysis of Titanium liquid is rapidly achieved boiling and start
Hydrolysis adjusts small steam, prevents transition boiling after the boiling of Hydrolysis of Titanium liquid；It is kept for slight boiling condition 120 minutes, hydrolysis terminates, and turns off
Steam valve；
(7) it rinses: after blowing, rinsing titanium hydrolysis foreheater, the pre- heat channel of crystal seed titanium liquid and crystal seed preparation vessel well, rush
Washing lotion is discharged into light white sink；Flushing finishes, and closes hydrolysis foreheater and crystal seed production slot baiting valve, each valve restore normal；
(8) it washs: washing the product metatitanic acid after hydrolysis by prior art, wash time is kept for 40 minutes, and washing is extremely
Guarantee filter cake iron content≤0.03% when terminal；
(9) it calcines: the qualified filter cake of washing is beaten with deionized water, control slurry concentration is 280 grams per liters, is pressed dry through filter press
Afterwards, control filter cake weight water content is transported to rotary kiln 45%, drying is calcined at 860 DEG C, it is small that control falls kiln product sulfur content
Material is put into a temperature control in 860 DEG C of thermostatic tank after progress constant temperature placement 3 hours after 0.05%, calcining, material
It continuously enters from tank deck, is continuously discharged from tank bottom, enter back into cooling kiln and cooled down, most crushed, packed afterwards, obtain non-coating
Use rutile type titanium white；Produce rutile content >=90% in obtained non-coating rutile type titanium white.
Embodiment 2
A kind of production method of non-coating rutile type titanium white, comprising the following steps:
(1) selected raw material: P in control titanium ore205Mass percentage is less than 0.05%；
(2) prepared by titanium liquid: routinely sulfuric acid will be added in titanium ore by technique, through acidolysis, sedimentation, freezing, crystallization and ferrous iron
Titanium liquid is obtained after separating technology, titanium liquid is without concentration, and the index of correlation of obtained titanium liquid is as follows: TiO2Concentration: 140 ± 10g/
L, F value: 1.85~2.05；Iron titanium ratio: 0.30~0.45；Clarity: level-one supernatant；Trivalent Ti content: 0.5~1.5g/L；Surely
It is qualitative: >=300；
(3) titanium liquid preheats: preparing by technic index and the titanium liquid measured throws hydrolysis foreheater into, and be passed through steam and added
Heat；It measures simultaneously by the 2.2% of every pot of Hydrolysis of Titanium liquid measure volume toward the pre- heat channel of crystal seed titanium liquid and squeezes into titanium liquid；Crystal seed preparation vessel is squeezed into
Lye, the lye are the sodium hydroxide solutions that concentration is 60g/L, and the additional amount of lye is the 33% of crystal seed titanium liquid measure volume；
Crystal type promoting reagent is added simultaneously, by Hydrolysis of Titanium liquid (m3): crystal type promoting reagent (kg)=2.5:1.1 ratio is added, and opens stirring；
The crystal type promoting reagent is zinc salt (zinc sulfate or zinc chloride)；
(4) make crystal seed: when titanium liquid foreheater titanium liquid temperature is raised to 75 DEG C, the starting pre- heat channel of crystal seed titanium liquid stirs and opens steaming
Vapor inlet valve heats up to crystal seed titanium liquid；And steam inlet valve is opened, it heats up to the lye in crystal seed preparation vessel, and keep lye
Temperature is at 86 DEG C；When crystal seed titanium liquid is warming up to 86 DEG C, opens the pre- heat channel baiting valve of crystal seed titanium liquid and preheated titanium liquid is put into
Crystal seed preparation vessel controls discharging time 7 minutes, when discharging the material that continues after crystal seed titanium liquid heat in crystal seed preparation vessel to 96 DEG C
Stop heating, crystal seed is made；
(5) crystal seed is added: the titanium liquid that foreheater is hydrolyzed in crystal seed manufacturing process continues to heat up, and controls at 96 DEG C, waits brilliant
Kind is carried out, and ready-made crystal seed is quickly added in preheated titanium liquid, is stirred 12 minutes after adding, and hydrolysis foreheater blowing is opened
Valve is put into the titanium liquid of hydrolysis foreheater in hydrolyzer, while starting hydrolyzer stirring, when titanium liquid touches adding in hydrolyzer
When live steam pipe, opens small steam and heat up to Hydrolysis of Titanium liquid；
(6) it hydrolyzes: after hydrolyzing foreheater titanium liquid and discharging, increasing steam inlet valve, so that Hydrolysis of Titanium liquid is rapidly achieved boiling and start
Hydrolysis adjusts small steam, prevents transition boiling after the boiling of Hydrolysis of Titanium liquid；It is kept for slight boiling condition 140 minutes, hydrolysis terminates, and turns off
Steam valve；
(7) it rinses: after blowing, rinsing titanium hydrolysis foreheater, the pre- heat channel of crystal seed titanium liquid and crystal seed preparation vessel well, rush
Washing lotion is discharged into light white sink；Flushing finishes, and closes hydrolysis foreheater and crystal seed production slot baiting valve, each valve restore normal；
(8) it washs: washing the product metatitanic acid after hydrolysis by prior art, wash time is kept for 50 minutes, and washing is extremely
Guarantee filter cake iron content≤0.03% when terminal；
(9) it calcines: the qualified filter cake of washing is beaten with deionized water, control slurry concentration is 300 grams per liters, is pressed dry through filter press
Afterwards, control filter cake weight water content is transported to rotary kiln 50%, drying is calcined at 860 DEG C, it is small that control falls kiln product sulfur content
Material is put into a temperature control in 860 DEG C of thermostatic tank after progress constant temperature placement 3 hours after 0.05%, calcining, material
It continuously enters from tank deck, is continuously discharged from tank bottom, enter back into cooling kiln and cooled down, most crushed, packed afterwards, obtain non-coating
Use rutile type titanium white；Produce rutile content >=90% in obtained non-coating rutile type titanium white.
Embodiment 3
A kind of production method of non-coating rutile type titanium white, comprising the following steps:
(1) selected raw material: P in control titanium ore205Mass percentage is less than 0.05%；
(2) prepared by titanium liquid: routinely sulfuric acid will be added in titanium ore by technique, through acidolysis, sedimentation, freezing, crystallization and ferrous iron
Titanium liquid is obtained after separating technology, titanium liquid is without concentration, and the index of correlation of obtained titanium liquid is as follows: TiO2Concentration: 140 ± 10g/
L, F value: 1.85~2.05；Iron titanium ratio: 0.30~0.45；Clarity: level-one supernatant；Trivalent Ti content: 0.5~1.5g/L；Surely
It is qualitative: >=300；
(3) titanium liquid preheats: preparing by technic index and the titanium liquid measured throws hydrolysis foreheater into, and be passed through steam and added
Heat；It measures simultaneously by the 2.2% of every pot of Hydrolysis of Titanium liquid measure volume toward the pre- heat channel of crystal seed titanium liquid and squeezes into titanium liquid；Crystal seed preparation vessel is squeezed into
Lye, the lye are the sodium hydroxide solutions that concentration is 60g/L, and the additional amount of lye is the 35% of crystal seed titanium liquid measure volume；
Crystal type promoting reagent is added simultaneously, by Hydrolysis of Titanium liquid (m3): crystal type promoting reagent (kg)=2.5:1.2 ratio is added, and opens stirring；
The crystal type promoting reagent is the product of Chengdu jump new science and technology research entitled " reason is crystal stabilization " produced；
(4) make crystal seed: when titanium liquid foreheater titanium liquid temperature is raised to 75 DEG C, the starting pre- heat channel of crystal seed titanium liquid stirs and opens steaming
Vapor inlet valve heats up to crystal seed titanium liquid；And steam inlet valve is opened, it heats up to the lye in crystal seed preparation vessel, and keep lye
Temperature is at 87 DEG C；When crystal seed titanium liquid is warming up to 87 DEG C, opens the pre- heat channel baiting valve of crystal seed titanium liquid and preheated titanium liquid is put into
Crystal seed preparation vessel controls discharging time 8 minutes, when discharging the material that continues after crystal seed titanium liquid heat in crystal seed preparation vessel to 97 DEG C
Stop heating, crystal seed is made；
(5) crystal seed is added: the titanium liquid that foreheater is hydrolyzed in crystal seed manufacturing process continues to heat up, and controls at 97 DEG C, waits brilliant
Kind is carried out, and ready-made crystal seed is quickly added in preheated titanium liquid, is stirred 15 minutes after adding, and hydrolysis foreheater blowing is opened
Valve is put into the titanium liquid of hydrolysis foreheater in hydrolyzer, while starting hydrolyzer stirring, when titanium liquid touches adding in hydrolyzer
When live steam pipe, opens small steam and heat up to Hydrolysis of Titanium liquid；
(6) it hydrolyzes: after hydrolyzing foreheater titanium liquid and discharging, increasing steam inlet valve, so that Hydrolysis of Titanium liquid is rapidly achieved boiling and start
Hydrolysis adjusts small steam, prevents transition boiling after the boiling of Hydrolysis of Titanium liquid；It is kept for slight boiling condition 150 minutes, hydrolysis terminates, and turns off
Steam valve；
(7) it rinses: after blowing, rinsing titanium hydrolysis foreheater, the pre- heat channel of crystal seed titanium liquid and crystal seed preparation vessel well, rush
Washing lotion is discharged into light white sink；Flushing finishes, and closes hydrolysis foreheater and crystal seed production slot baiting valve, each valve restore normal；
(8) it washs: washing the product metatitanic acid after hydrolysis by prior art, wash time is kept for 60 minutes, and washing is extremely
Guarantee filter cake iron content≤0.03% when terminal；
(9) it calcines: the qualified filter cake of washing is beaten with deionized water, control slurry concentration is 320 grams per liters, is pressed dry through filter press
Afterwards, control filter cake weight water content is transported to rotary kiln (calcining kiln) 55%, and drying is calcined at 860 DEG C, and control falls kiln product
Material is put into the control of temperature after calcining and carries out constant temperature in 860 DEG C of thermostatic tank to place 3 small by sulfur content less than 0.05%
Shi Hou, material are continuously entered from tank deck, are continuously discharged from tank bottom, are entered back into cooling kiln and are cooled down, are most crushed, packed afterwards,
Obtain non-coating rutile type titanium white；Produce rutile content >=90% in obtained non-coating rutile type titanium white.
Schematic device such as Fig. 1 institute of calcine technology in the production method of the non-coating rutile type titanium white of the present invention
Show；It can be seen from figure 1 that the device of calcine technology includes calcination rotary kiln 1, thermostatic tank 2 and cooling kiln 3, the discharging of calcination rotary kiln 1
Mouth is connected with the top feed end of thermostatic tank 2, and the discharge port of 2 bottom of thermostatic tank is connected with the feed inlet of cooling kiln 3；It will be inclined
Metatitanic acid, which is transported in calcination rotary kiln 1, carries out calcining drying, discharge port of the material obtained after calcining is dry from calcination rotary kiln 1
Into the top feed mouth of thermostatic tank 2, after material fills thermostatic tank 2, start to release from the discharge outlet of constant temperature pot bottom, later
Material is constantly continuously entered from 2 tank deck of thermostatic tank, is continuously discharged from tank bottom, lasts 3 hours, material from thermostatic tank 2 discharge after, then
Into being cooled down in cooling kiln 3, is most crushed, packed to get to non-coating rutile type titanium white afterwards.
Wherein the structural schematic diagram of the thermostatic tank 2 is as shown in Fig. 2, the thermostatic tank 2 includes 4 He of thermostatic tank cover
Constant temperature tank 7, the outer surface of constant temperature tank 7 are provided with one layer of refractory brick 20 and one layer of alumina silicate Nomex from the inside to surface
21, the centre of fire brick layer is additionally provided with one layer of electrode 5, thermostatic tank 2 can be made to be maintained at permanent by carrying out electrified regulation to electrode 5
Temperature state, alumina silicate Nomex 21 can play the role of insulation；Its periphery peace of part of the electrode 5 beyond constant temperature tank 7
Equipped with porcelain tube 6, the bottom of constant temperature tank 7 is equipped with discharging turntable 8, and discharge port 9 is equipped with by the turntable 8 that discharges, is installed at discharge port 9
There is discharging adjustable plate 10, discharge port 9 is mounted below receiver 19, and receiver 19 is connected with material blanking tube 12, and rack 14 is mounted on
The lower section of thermostatic tank 2,14 lower part of rack are equipped with transmission device 13, there is the connection of shaft 15 between rack 14 and the bottom of thermostatic tank 2,
Shaft 15 is connected with transmission device 13, drives the operation of shaft 15 to drive discharging turntable 8 to run by transmission device 13, rack
The outside of the shaft connected between 2 bottom of 14 tops and thermostatic tank is equipped with cooling jacket 17, plays cooling effect, cooling jacket
17 top is equipped with water inlet pipe 18, and outside is equipped with drip tray 16, and the lower part of drip tray 16 is equipped with outlet pipe 11, and cooling water is from water inlet
Enter cooling jacket 17 in pipe 18, is discharged from outlet pipe 11.
Claims (5)
1. a kind of production method of non-coating rutile type titanium white, which comprises the following steps:
(1) selected raw material: P in control titanium ore205Mass percentage is less than 0.05%；
(2) prepared by titanium liquid: routinely sulfuric acid will be added in titanium ore by technique, through acidolysis, sedimentation, freezing, crystallization and ferrous iron
Titanium liquid is obtained after separating technology, titanium liquid is without concentration, and the index of correlation of obtained titanium liquid is as follows: TiO2Concentration: 140 ± 10g/
L, F value: 1.85~2.05；Iron titanium ratio: 0.30~0.45；Clarity: level-one supernatant；Trivalent Ti content: 0.5~1.5g/L；Surely
It is qualitative: >=300；
(3) titanium liquid preheats: preparing by technic index and the titanium liquid measured throws hydrolysis foreheater into, and be passed through steam and added
Heat；It measures simultaneously by the 2.2% of every pot of Hydrolysis of Titanium liquid measure volume toward the pre- heat channel of crystal seed titanium liquid and squeezes into titanium liquid；Crystal seed preparation vessel is squeezed into
Lye, while crystal type promoting reagent is added, by Hydrolysis of Titanium liquid (m3): crystal type promoting reagent (kg)=2.5:1~1.2 ratio is added, and opens
Open stirring；
(4) make crystal seed: when titanium liquid foreheater titanium liquid temperature is raised to 75 DEG C, the starting pre- heat channel of crystal seed titanium liquid stirs and opens steaming
Vapor inlet valve heats up to crystal seed titanium liquid；And steam inlet valve is opened, it heats up to the lye in crystal seed preparation vessel, and keep lye
Temperature is at 84-87 DEG C；When crystal seed titanium liquid is warming up to 84-87 DEG C, the pre- heat channel baiting valve of crystal seed titanium liquid is opened preheated titanium
Liquid is put into crystal seed preparation vessel, controls discharging time 5-8 minutes, continues to heat the material in crystal seed preparation vessel after discharging crystal seed titanium liquid
Stop heating when to 95-97 DEG C, crystal seed is made；
(5) crystal seed is added: the titanium liquid that foreheater is hydrolyzed in crystal seed manufacturing process continues to heat up, and controls at 95-97 DEG C, waits
Crystal seed is carried out, and ready-made crystal seed is quickly added in preheated titanium liquid, is stirred 10-15 minutes after adding, and hydrolysis preheating is opened
Pot baiting valve, the titanium liquid of hydrolysis foreheater is put into hydrolyzer, while starting hydrolyzer stirring, when titanium liquid touches hydrolyzer
When interior heating steam pipe, opens small steam and give the heating of Hydrolysis of Titanium liquid；
(6) it hydrolyzes: after hydrolyzing foreheater titanium liquid and discharging, increasing steam inlet valve, so that Hydrolysis of Titanium liquid is rapidly achieved boiling and start
Hydrolysis adjusts small steam, prevents transition boiling after the boiling of Hydrolysis of Titanium liquid；It being kept for slight boiling condition 120-150 minutes, hydrolysis terminates,
Turn off steam valve；
(7) it rinses: after blowing, rinsing titanium hydrolysis foreheater, the pre- heat channel of crystal seed titanium liquid and crystal seed preparation vessel well, rush
Washing lotion is discharged into light white sink；Flushing finishes, and closes hydrolysis foreheater and crystal seed production slot baiting valve, each valve restore normal；
(8) it washs: washing the product metatitanic acid after hydrolysis by prior art, wash time is kept for 40-60 minutes, washing
Guarantee filter cake iron content≤0.03% when to terminal；
(9) it calcines: the qualified filter cake of washing is beaten with deionized water, control slurry concentration is 300 ± 20 grams per liters, through filter press
After pressing dry, filter cake weight water content being controlled in 45-55%, is transported to rotary kiln, drying is calcined at 860 DEG C, control falls kiln product sulphur
Material is put into a temperature control after calcining and carries out constant temperature placement 3 hours in 860 DEG C of thermostatic tank by content less than 0.05%
Afterwards, material is continuously entered from tank deck, is continuously discharged from tank bottom, is entered back into cooling kiln and is cooled down, is most crushed, packed afterwards, obtained
To non-coating rutile type titanium white.
2. the production method of non-coating rutile type titanium white according to claim 1, which is characterized in that the alkali
Liquid is the sodium hydroxide solution that concentration is 60g/L, and the additional amount of lye is the 32~35% of crystal seed titanium liquid measure volume.
3. the production method of non-coating rutile type titanium white according to claim 1, which is characterized in that the crystalline substance
Type promotor is zinc salt or pink salt.
4. the production method of non-coating rutile type titanium white according to claim 1 or 3, which is characterized in that described
Crystal type promoting reagent be Chengdu jump new science and technology research entitled " reason is crystal stabilization " produced product.
5. the production method of non-coating rutile type titanium white according to claim 1, which is characterized in that production obtains
Non- coating rutile type titanium white in rutile content >=90%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112939075A (en) * | 2021-04-21 | 2021-06-11 | 济南裕兴化工有限责任公司 | Novel metatitanic acid calcined rutile crystal form conversion promoter |
| CN114314653A (en) * | 2021-12-28 | 2022-04-12 | 龙佰襄阳钛业有限公司 | Preparation system and method for additional seed crystal index optimization |
| CN114573021A (en) * | 2022-03-14 | 2022-06-03 | 淮安市鸿洋钛业有限公司 | High-purity mixed crystal titanium dioxide and production method thereof |
| CN114772636A (en) * | 2022-05-31 | 2022-07-22 | 龙佰四川钛业有限公司 | Production method for regulating particle size of titanium dioxide |
| CN114853059A (en) * | 2022-05-31 | 2022-08-05 | 龙佰四川钛业有限公司 | Method for regulating and controlling particle size of hydrolysis seed crystal |
| CN115417451A (en) * | 2022-10-24 | 2022-12-02 | 攀钢集团研究院有限公司 | Method for preparing rutile titanium dioxide |
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| CN103880070A (en) * | 2013-12-31 | 2014-06-25 | 江苏泛华化工有限公司 | Production method of titanium dioxide particles |
| CN108545772A (en) * | 2018-05-04 | 2018-09-18 | 广西金茂钛业有限公司 | A kind of preparation method of colorant titanium dioxide additional hydrolyzing seed crystal |
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| CN103880070A (en) * | 2013-12-31 | 2014-06-25 | 江苏泛华化工有限公司 | Production method of titanium dioxide particles |
| CN108545772A (en) * | 2018-05-04 | 2018-09-18 | 广西金茂钛业有限公司 | A kind of preparation method of colorant titanium dioxide additional hydrolyzing seed crystal |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939075A (en) * | 2021-04-21 | 2021-06-11 | 济南裕兴化工有限责任公司 | Novel metatitanic acid calcined rutile crystal form conversion promoter |
| CN114314653A (en) * | 2021-12-28 | 2022-04-12 | 龙佰襄阳钛业有限公司 | Preparation system and method for additional seed crystal index optimization |
| CN114573021A (en) * | 2022-03-14 | 2022-06-03 | 淮安市鸿洋钛业有限公司 | High-purity mixed crystal titanium dioxide and production method thereof |
| CN114772636A (en) * | 2022-05-31 | 2022-07-22 | 龙佰四川钛业有限公司 | Production method for regulating particle size of titanium dioxide |
| CN114853059A (en) * | 2022-05-31 | 2022-08-05 | 龙佰四川钛业有限公司 | Method for regulating and controlling particle size of hydrolysis seed crystal |
| CN114853059B (en) * | 2022-05-31 | 2023-11-14 | 龙佰四川钛业有限公司 | Method for regulating particle size of hydrolysis seed crystal |
| CN114772636B (en) * | 2022-05-31 | 2023-11-14 | 龙佰四川钛业有限公司 | Production method for regulating particle size of titanium dioxide |
| CN115417451A (en) * | 2022-10-24 | 2022-12-02 | 攀钢集团研究院有限公司 | Method for preparing rutile titanium dioxide |
| CN115417451B (en) * | 2022-10-24 | 2023-11-24 | 攀钢集团研究院有限公司 | Process for preparing rutile titanium dioxide |
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