CN106986380A - The method that metatitanic acid calcines production titanium dioxide base-material without sulphur - Google Patents
The method that metatitanic acid calcines production titanium dioxide base-material without sulphur Download PDFInfo
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- CN106986380A CN106986380A CN201710272495.7A CN201710272495A CN106986380A CN 106986380 A CN106986380 A CN 106986380A CN 201710272495 A CN201710272495 A CN 201710272495A CN 106986380 A CN106986380 A CN 106986380A
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- metatitanic acid
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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
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention relates to a kind of production method of sulfuric acid method titanium pigment, a kind of method that metatitanic acid calcines production titanium dioxide base-material without sulphur is specifically disclosed, is comprised the following steps：A, with alkaline reagent and washing qualified metatitanic acid；B, filtering, wash filter cake；C, salt treatment, phosphorus source salt treatment agent used select phosphoric acid, and aluminium, potassium resource salt treatment agent select potassium metaaluminate reagent, and zinc, potassium resource salt treatment agent select inclined potassium zincate reagent；D, calcining obtain titanium dioxide base-material.It is an advantage of the invention that：1) new approaches that a kind of metatitanic acid calcines vent gas treatment are proposed：Without sulphur calcining, so that being produced without sulfur-containing tail gas；2) cause the waste heat of calcining tail gas to reuse as feasible reality, be easy to recycle waste heat from tail gas；3) tail gas produced after calcining, which need not carry out any processing, directly to be discharged, with economic and environment-friendly double benefit.
Description
Technical field
The present invention relates to a kind of titanium white production technique, especially a kind of sulfuric acid method titanium pigment production technology.
Background technology
Titanium dioxide chemical property is stable, is not reacted with most of material in general.The dioxy in nature
Changing titanium has three kinds of crystallizations：Plate titanium-type, rutile titania and rutile-type.Plate titanium-type is unstable crystal formation, no industrial utility value, rutile titania
Type (Anatase) abbreviation A types, and rutile-type (Rutile) abbreviation R types, are important white face all with stable lattice
Material and porcelain glaze, being compared with other Chinese whites has superior whiteness, tinting strength, tinting power, covering power, weatherability, heat resistance and changes
Stability is learned, particularly no toxicity is a kind of current best Chinese white of performance in the world, is widely used in coating, modeling
The industry such as material, papermaking, printing-ink, chemical fibre, rubber, cosmetics.
Typical sulfuric acid method titanium pigment production technology comprises the following steps：
(1) acidolysis reaction is carried out with sulfuric acid with ilmenite concentrate or acid-dissolved titanium slag, obtains titanyl sulfate solution；
(2) hydrolysing titanyl sulfate solution obtains thick metatitanic acid slurry；
(3) thick metatitanic acid slurry is bleached, washed, obtain washing qualified metatitanic acid；
(4) wash qualified metatitanic acid and carry out salt treatment, obtain pretreatment metatitanic acid；
(5) calcine：Pretreatment metatitanic acid feeding rotary kiln calcining obtains titanium dioxide base-material；
(6) titanium dioxide product is made by postprocessing working procedures in titanium dioxide base-material.
The primary operational process of wherein step (5) calcination process is：Pretreatment metatitanic acid after salt treatment is sent into tool
The kiln body tail end (cylinder high-end) for having constant slope and slowly turning round, while the burning mixing of kiln hood direction (low side of cylinder)
Clean flame and hot blast are blown into kiln by room to be dehydrated to filter cake, is calcined.It is dehydrated, is calcined through 1000 DEG C of high temperature above
Hydrolyzed titanium dioxide filter cake afterwards had not only along the circumferential direction rolled but also vertically (from high-end to low side) by inclined revolution kiln body
It is mobile, constantly complete dehydration.Enter cooler eventually through the Double-hydraulic turnover panel discharge valve of kiln head cover bottom, through cooling, screening
Material afterwards is titanium dioxide base-material.
The side of gas consumption about 240 of ton product in whole calcination process, by being dehydrated to rotary kiln, desulfurization, radiation loss
Calculating, 95% heat takes away eventually through rotary kiln kiln tail tail gas, has many methods on reclaiming heat in the tail gas, such as
Waste acid concentration, heating water etc., but be that low value is reclaimed, also paid pilot production uses tail with the mode directly or indirectly exchanged heat
Gas produces steam, generate electricity etc., but be due to a large amount of sulfur trioxides of content, water, sulfur dioxide, heat recovering process in calcining tail gas
In when temperature is less than 330 DEG C, a large amount of acid mists are formed so that equipment material corrodes, and device scraps.Simultaneously because in calcination process
Substantial amounts of sulfuric acid gas is produced, for tail gas qualified discharge, it is necessary to increase such as Water spray, the environmental protection facility such as alkali spray, no
Only device is complicated, and operating cost is high, and can not accomplish zero-emission.
The content of the invention
To solve the intractable problem of tail gas in titanium dioxide base-material production process, the invention provides a kind of metatitanic acid without sulphur
The method of calcining production titanium dioxide base-material.
The technical solution adopted in the present invention is：The method that metatitanic acid calcines production titanium dioxide base-material without sulphur, including it is following
Step：
A, water intaking are washed after qualified metatitanic acid is beaten, and are added into slurry and are measured alkaline reagent and neutralized, fully stirred
Mix, cure, obtain neutralizing slurry；
B, filtering neutralize slurry and obtain filter cake, and washing filter cake is to remove wherein salinity, filter cake after being washed；
C, to after washing filter cake carry out salt treatment, wherein phosphorus source salt treatment agent used selects phosphoric acid, aluminium, potassium resource salt treatment agent
From potassium metaaluminate reagent, zinc, potassium resource salt treatment agent select inclined potassium zincate reagent；Metatitanic acid must be pre-processed after salt treatment；
D, pretreatment metatitanic acid calcine and obtain titanium dioxide base-material.
Inventor proposes in the present invention：The processing method of tail gas is calcined with its Improvement, not as being prevented on source
The generation of tail gas, is studied metatitanic acid calcination process for this imagination inventor.
Inventor proposes that the sulphur in tail gas is necessarily derived from metatitanic acid, and the sulphur in metatitanic acid mainly has two under study for action
Source：1st, the sulfate radical of metatitanic acid itself absorption, mainly in titanyl sulfate solution hydrolytic process, the sulfuric acid oxygen of non-complete hydrolysis
Titanium, this part of sulfuric acid root is to be combined with chemical bond form with metatitanic acid, and release is decomposed at high temperature；2nd, most titanium powder plants
In order to improve the mellowness and pigment performance of calcined product, generally handled using salt treatment agent, wherein being typically represented as
Phosphoric acid, potassium sulfate, aluminum sulfate, zinc sulfate system, therefore sulfate radical in salt treatment agent is another source of sulphur in calcining.In advance
Handle in metatitanic acid calcination process, when temperature is higher than 350 DEG C, the sulfate radical in metatitanic acid will progressively be decomposed, discharged, and work as temperature
Degree is higher than 950 DEG C, and the well-behaved solution of the sulphate groups in metatitanic acid terminates, and ton metatitanic acid point sulfur content (in terms of sulfur dioxide) is about
70kg。
Inventor devises the method for the present invention to prevent the generation of sulfur-containing tail gas accordingly：By alkaline reagent to metatitanic acid
Desulfurization is carried out, and without sulfosalt inorganic agent, (phosphorus source salt treatment agent uses phosphoric acid, and aluminium and potassium resource are substituted using potassium metaaluminate system for combination
Aluminum sulfate/potassium sulfate system, zinc and potassium resource using inclined potassium zincate system substitute zinc sulfate/sulphation potassium system) use, prevent
Sulphur is mixed into pretreatment metatitanic acid, and then is realized without sulphur calcining.It is demonstrated experimentally that being operated by above-mentioned two step, metatitanic acid is pre-processed
In hardly sulfur-bearing (pretreatment metatitanic acid total sulfur content reduction by more than 99%) so that the waste heat of calcining tail gas, which is reused, to be turned into
Feasible reality, calcining tail gas need not carry out environmental protection treatment can qualified discharge, with economic and environment-friendly double benefit.
As a further improvement on the present invention, the alkaline reagent described in step A is selected from the carbonate of alkali metal, alkali metal
Hydroxide, the bicarbonate of alkali metal, one kind or any several mixture in ammoniacal liquor.These alkaline reagents are neutralized
Will not be produced after reaction can not be by washing the precipitation class impurity removed, and the impurity produced is soluble-salt, can be by follow-up
Step B washing procedures are removed, and do not interfere with the quality of final products.
More preferably, the one kind or any several of the alkaline reagent in potassium carbonate, potassium hydroxide, saleratus.
During step C salt treatment, generally it is required for adding potassium resource salt treatment agent, so if being used as step using above sylvite reagent
Rapid A alkaline reagent is neutralized, and the washing procedure load that can substantially reduce step B (because salt treatment agent contains potassium in itself, therefore is washed
The potassium for washing residual minim in rear filter cake does not interfere with product salt treatment formula and quality, without the electrical conductivity of washing lotion is controlled
In lower value).
As a further improvement on the present invention, in step A, gained neutralizes pH=6~8 of slurry liquid phase.To ensure absorption
Sulfuric acid generates soluble-salt by abundant neutralize, while being added without excessive alkaline reagent again, it is to avoid led because neutralization reaction is not in place
The desulfurization of cause thoroughly or caused by a large amount of excess of alkaline reagent does not wash difficult.More preferably, gained neutralizes the pH of slurry liquid phase
=6.5~7.5.
As a further improvement on the present invention, step B washing terminal is：Sulfate radical-free in the wash water produced is washed to examine
Go out.To ensure that sulfate radical content is sufficiently low in filter cake after obtained washing.
The beneficial effects of the invention are as follows：1) new approaches that a kind of metatitanic acid calcines vent gas treatment are proposed：Calcined without sulphur, from
And to produce without sulfur-containing tail gas；2) due to tail gas not sulfur-bearing so that the waste heat of calcining tail gas is reused to be showed as feasible
It is real, it is easy to recycle waste heat from tail gas；3) tail gas produced after method of the invention calcining need not carry out any processing
Can directly it discharge, with economic and environment-friendly double benefit.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment one：
Qualified metatitanic acid is washed with water according to following steps and prepares titanium dioxide base-material：
(1) qualified metatitanic acid is washed in water intaking, is added water and is beaten to TiO2=300g/l (Fe=28ppm in butt), into slurry
Add potassium hydroxide solution (KOH concentration is 100g/l) control addition and cause slurry pH=6.5, be sufficiently stirred for post curing
120min, obtains neutralizing slurry；
(2) slurry will be neutralized and directly carry out suction filtration, washing filter cake sulfate radical-free into the wash water produced is detected, washed
Filter cake afterwards；
(3) toward addition salt treatment agent phosphoric acid in filter cake after washing, potassium metaaluminate, control addition causes P in slurry2O5/
TiO2=0.20%；K2O/TiO2=0.26；Al2O3/TiO2=0.26, filter cake sulfur content is detected, filter cake is dried, must be pre-processed
Metatitanic acid；
(4) pretreatment metatitanic acid is by laboratory calcination condition：First pass through 30min and be warming up to 600 DEG C, then with 0.5 DEG C/
When min speed is warming up to base-material rutile conversion ratio=98.5%, record calcining outlet temperature, and surveyed using exhaust analyzer
Determine tail gas sulfur content, then titanium dioxide base-material is obtained after cooling, screening.
(5) the dry powder L of titanium dioxide base-material is detected, black wash b values, brightness, 20 ° of gloss of oiliness, testing result is shown in Table 1.
Embodiment two：
Qualified metatitanic acid is washed with water according to following steps and prepares titanium dioxide base-material：
(1) qualified metatitanic acid is washed in water intaking, is added water and is beaten to TiO2=300g/l (Fe=28ppm in butt), into slurry
Add sodium bicarbonate solution (NaHCO3Concentration is 100g/l) control addition to cause slurry pH=7.8, it is sufficiently stirred for post curing
120min, obtains neutralizing slurry；
(2) slurry will be neutralized and directly carry out suction filtration, washing filter cake sulfate radical-free into the wash water produced is detected, washed
Filter cake afterwards；
(3) toward addition salt treatment agent phosphoric acid in filter cake after washing, inclined potassium zincate, control addition causes P in slurry2O5/
TiO2=0.20%；K2O/TiO2=0.26；ZnO/TiO2=0.10, filter cake sulfur content is detected, filter cake is dried, must be pre-processed
Metatitanic acid；
(4) pretreatment metatitanic acid is by laboratory calcination condition：First pass through 30min and be warming up to 600 DEG C, then with 0.5 DEG C/
When min speed is warming up to base-material rutile conversion ratio=98.5%, record calcining outlet temperature, and surveyed using exhaust analyzer
Determine tail gas sulfur content, then titanium dioxide base-material is obtained after cooling, screening.
(5) the dry powder L of titanium dioxide base-material is detected, black wash b values, brightness, 20 ° of gloss of oiliness, testing result is shown in Table 1.
Embodiment three：
Qualified metatitanic acid is washed with water according to following steps and prepares titanium dioxide base-material：
(1) qualified metatitanic acid is washed in water intaking, is added water and is beaten to TiO2=300g/l (Fe=28ppm in butt), into slurry
Add ammoniacal liquor (NH3Concentration is 100g/l) control addition to cause slurry pH=7.1, post curing 120min is sufficiently stirred for, is obtained
Neutralize slurry；
(2) slurry will be neutralized and directly carry out suction filtration, washing filter cake sulfate radical-free into the wash water produced is detected, washed
Filter cake afterwards；
(3) toward addition salt treatment agent phosphoric acid in filter cake after washing, inclined potassium zincate, control addition causes P in slurry2O5/
TiO2=0.20%；K2O/TiO2=0.26；ZnO/TiO2=0.10, filter cake sulfur content is detected, filter cake is dried, must be pre-processed
Metatitanic acid；
(4) pretreatment metatitanic acid is by laboratory calcination condition：First pass through 30min and be warming up to 600 DEG C, then with 0.5 DEG C/
When min speed is warming up to base-material rutile conversion ratio=98.5%, record calcining outlet temperature, and surveyed using exhaust analyzer
Determine tail gas sulfur content, then titanium dioxide base-material is obtained after cooling, screening.
(5) the dry powder L of titanium dioxide base-material is detected, black wash b values, brightness, 20 ° of gloss of oiliness, testing result is shown in Table 1.
Comparative example four：
(1) qualified metatitanic acid is washed in water intaking, is added water and is beaten to TiO2=300g/l (Fe=28ppm in butt)；Toward the washing
P in salt treatment agent phosphoric acid, potassium hydroxide, aluminum sulfate, control addition adjustment slurry is added in qualified metatitanic acid slurry2O5/TiO2
=0.20%；K2O/TiO2=0.26；Al2O3/TiO2=0.26, filter cake sulfur content is detected, filter cake is dried, inclined titanium must be pre-processed
Acid；
(2) pretreatment metatitanic acid is by laboratory calcination condition：First pass through 30min and be warming up to 600 DEG C, then with 0.5 DEG C/
When min speed is warming up to base-material rutile conversion ratio=98.5%, record calcining outlet temperature, and surveyed using exhaust analyzer
Determine tail gas sulfur content, then titanium dioxide base-material is obtained after cooling, screening.
(3) the dry powder L of titanium dioxide base-material is detected, black wash b values, brightness, 20 ° of gloss of oiliness, testing result is shown in Table 1.
Comparative example five：
(1) qualified metatitanic acid is washed in water intaking, is added water and is beaten to TiO2=300g/l (Fe=28ppm in butt)；Toward the washing
P in salt treatment agent phosphoric acid, potassium hydroxide, zinc sulfate, control addition adjustment slurry is added in qualified metatitanic acid slurry2O5/TiO2
=0.20%；K2O/TiO2=0.26；ZnO/TiO2=0.10, filter cake sulfur content is detected, filter cake is dried, inclined titanium must be pre-processed
Acid；
(2) pretreatment metatitanic acid is by laboratory calcination condition：First pass through 30min and be warming up to 600 DEG C, then with 0.5 DEG C/
When min speed is warming up to base-material rutile conversion ratio=98.5%, record calcining outlet temperature, and surveyed using exhaust analyzer
Determine tail gas sulfur content, then titanium dioxide base-material is obtained after cooling, screening.
(3) the dry powder L of titanium dioxide base-material is detected, black wash b values, brightness, 20 ° of gloss of oiliness, testing result is shown in Table 1.
Table 1：Each embodiment titanium dioxide base pigment performance test results table
The sulfur content for the calcining tail gas that the present invention is produced is almost 0 as can be seen from Table 1, and this method not only will not be right
The pigment performance of gained titanium dioxide base-material has any impact, after being used on the contrary because of metatitanic acid without sulphur calcine technology, metatitanic acid
Calcining outlet temperature reduce about 40 DEG C (absorption sulfuric acid be rutile conversion and strong inhibitor of growing up, therefore calcining mistake
Journey is not only the process for pre-processing metatitanic acid dehydration, while being also the process of desulfurization, it is necessary to slough absorption sulfuric acid by high temperature
Afterwards, rutile particle could grow up and convert well, and this directly results in the generation of calcining high temperature), the reduction product of calcining heat
Pole improves the sintering of particle, therefore particle is easy to grinding, and lattice defect is less, the absorption to light is less, therefore pigment
It can be improved with dispersive property, this is also undoubtedly another big advantage of the present invention.
Claims (5)
1. the method that metatitanic acid calcines production titanium dioxide base-material without sulphur, comprises the following steps：
A, water intaking are washed after qualified metatitanic acid is beaten, and are added into slurry and are measured alkaline reagent and neutralized, are sufficiently stirred for, ripe
Change, obtain neutralizing slurry；
B, filtering neutralize slurry and obtain filter cake, and washing filter cake is to remove wherein soluble-salt, filter cake after being washed；
C, salt treatment is carried out to filter cake after washing, wherein phosphorus source salt treatment agent used selects phosphoric acid, aluminium, potassium resource salt treatment agent are selected
Potassium metaaluminate reagent, zinc, potassium resource salt treatment agent select inclined potassium zincate reagent；Metatitanic acid must be pre-processed after salt treatment；
D, pretreatment metatitanic acid calcine and obtain titanium dioxide base-material.
2. the method that metatitanic acid according to claim 1 calcines production titanium dioxide base-material without sulphur, it is characterised in that：Step A
Described in alkaline reagent be selected from the carbonate of alkali metal, the hydroxide of alkali metal, the bicarbonate of alkali metal, in ammoniacal liquor
It is a kind of or any several.
3. the method that metatitanic acid according to claim 1 calcines production titanium dioxide base-material without sulphur, it is characterised in that：Step A
Described in one kind in potassium carbonate, potassium hydroxide, saleratus of alkaline reagent or any several.
4. the method that the metatitanic acid according to any claim in claims 1 to 3 calcines production titanium dioxide base-material without sulphur,
It is characterized in that：In step A, gained neutralizes pH=6~8 of slurry liquid phase.
5. the method that the metatitanic acid according to any claim in claims 1 to 3 calcines production titanium dioxide base-material without sulphur,
It is characterized in that：Step B washing terminal is：Sulfate radical-free in the wash water produced is washed to detect.
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| CN108299863A (en) * | 2018-01-31 | 2018-07-20 | 攀枝花学院 | A kind of clean preparation method of titanium white |
| CN113044879A (en) * | 2021-03-22 | 2021-06-29 | 龙蟒佰利联集团股份有限公司 | Method for improving quality of sulfuric acid process titanium dioxide |
| CN115521061A (en) * | 2022-08-25 | 2022-12-27 | 广西金茂钛业有限公司 | Method for preparing titanium dioxide for reflective glass |
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| CN108299863A (en) * | 2018-01-31 | 2018-07-20 | 攀枝花学院 | A kind of clean preparation method of titanium white |
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| CN115521061A (en) * | 2022-08-25 | 2022-12-27 | 广西金茂钛业有限公司 | Method for preparing titanium dioxide for reflective glass |
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Application publication date: 20170728 |