CN108502920A - A kind of preparation process of titanium dioxide - Google Patents
A kind of preparation process of titanium dioxide Download PDFInfo
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- CN108502920A CN108502920A CN201810267149.4A CN201810267149A CN108502920A CN 108502920 A CN108502920 A CN 108502920A CN 201810267149 A CN201810267149 A CN 201810267149A CN 108502920 A CN108502920 A CN 108502920A
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- titanium dioxide
- ilmenite
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation processes of titanium dioxide, belong to titanium dioxide preparation field, by ilmenite raw material successively through acidolysis, reduction, sedimentation, crystallisation by cooling, hydrolysis and calcining, first through wet grinding before the ilmenite raw material acidolysis, in wet grinding, ilmenite raw material is added in dilution heat of sulfuric acid, the mixed liquor being mixed to form is sent into ball mill and carries out wet grinding.The beneficial effects of the invention are as follows：By being acidified ilmenite powder in advance before acidolysis, and using the method for wet grinding, the particle diameter of ilmenite is reduced, improve the contact area of ilmenite powder and dilute sulfuric acid, to improve the acidizing degree of ilmenite as much as possible, reduce the use of the later stage concentrated sulfuric acid；And the generation of dust can also be reduced using wet grinding, protect environment.
Description
Technical field
The present invention relates to titanium dioxide preparation field more particularly to a kind of preparation processes of titanium dioxide.
Background technology
Titanium dioxide is a kind of white inorganic pigment, molecular formula TiO2, also referred to as titanium white.With nontoxic, best opaque
Property, best whiteness and brightness, it is considered to be the best a kind of white pigment of performance in the world at present, be widely used in coating,
The industry such as plastics, papermaking, printing ink, chemical fibre, rubber, enamel, ceramics, electronic ceramics, glass, alloy, welding rod, cosmetics.
It has two kinds of structures of rutile-type and anatase titanium dioxide, and rutile crystalline structure is fine and close, and more stable, optical activity is small, thus weather-proof
Property is good, while having higher covering power, reducing power.
The main production process of titanium dioxide has sulfuric acid process and chloridising, and common Production By Sulfuric Acid Process technique is in production, meeting
The a large amount of concentrated sulfuric acid is consumed, concentrated sulfuric acid cost of manufacture is higher, makes difficulty, increases the cost that titanium dioxide entirely produces.
Invention content
To overcome, consumption concentrated sulfuric acid amount is big, manufacturing cost is high, manufacture is tired existing for prior art Titanium White Production By Sulfuric Acid Process
The problems such as difficult, the present invention provides a kind of preparation process of titanium dioxide, by ilmenite raw material successively through acidolysis, reduction, sedimentation, cold
But it crystallizes, hydrolyze and calcines, first through wet grinding before the ilmenite raw material acidolysis, in wet grinding, by ilmenite original
Material is added in dilution heat of sulfuric acid, and the mixed liquor being mixed to form is sent into ball mill and carries out wet grinding.
Preferably, vacuum drying step, the vacuum drying step are added between the wet grinding and the acidolysis
It is dried in vacuo for the mixed liquor after wet grinding to be sent into leadwork reactor.
Preferably, before the wet grinding, first the ilmenite raw material is dried and is roughly ground, titanium after control corase grinding
A diameter of 10~20 mesh of iron ores particle.
Preferably, the hydrolysis step is the concentrated sulfuric acid to be slowly introducing into leadwork reactor, and heated, holding 30~
The reaction time of 45min.
Preferably, the reduction step is that dilute sulfuric acid dilution is passed through in leadwork reactor, and iron is continuously added into dilution
Consider powder to be worth doing, the ferric ion restored in mixed liquor becomes ferrous ion, 11~12 hours reaction time.
Preferably, the precipitation step is the cooling acid hydrolysis solution for completing reduction reaction so that solid inert material and not instead
The raw material residue solution answered all is discharged into from the bottom of acid hydrolysis tank in low level sedimentation basin.
Preferably, the crystallisation by cooling step be by it is described it is heavy remove after solution be cooled to 8~12 DEG C, crystallization, filtering is simultaneously
Recycle green vitriol FeSO47H2O.
Preferably, the hydrolysing step is that the solution after the crystallisation by cooling is heated to 90~114 DEG C, and anti-to leadwork
Device is answered persistently to be vacuumized so that hydrating solution boils, and continues to be added 90~100 DEG C of hot water into leadwork reactor.
Preferably, the calcining step is to be sent into internal combustion type after the sediment after the hydrolysis is filtered, is washed to return
It is calcined in rotary kiln.
Preferably, the titanium dioxide Jing Guo the calcining is crushed and obtains required titanium dioxide with coating.
Preferably, contain 42~60% TiO2 in the ilmenite raw material.
Preferably, in the wet grinding steps dilute sulfuric acid a concentration of 7~9mol/L, the mistake of wet grinding in the S2
The aperture of strainer is 180~200 mesh.
Preferably, the vacuum pump for vacuumizing is installed on the leadwork reactor.
Preferably, temperature is 150~180 DEG C in the hydrolysis step, the sulfuric acid that the concentrated sulfuric acid is a concentration of 85~92%.
Preferably, in the precipitation step, in sedimentation, add people's casein and starch flocculant, by gravitational settling, sink
The drop time is maintained at 8~10 hours.
Preferably, the air pressure inside persistently vacuumized in the hydrolysing step is maintained at less than 21000Pa, passes through steam pair
Solution after the crystallisation by cooling is heated, and is brought rapidly up to 112~114 DEG C.
Preferably, the calcination temperature in the calcining step is 900-1250 DEG C, and the gas needs excluded when calcining are adopted
With activated carbon adsorption, to exclude the TiO2 particles carried secretly in tail gas.
Preferably, use aluminum sulfate and sodium hydroxide for coating agent in the coating step, with chemical precipitation method to titanium white
Powder carries out aluminum oxide coating.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) by being acidified ilmenite powder in advance before acidolysis, and using the method for wet grinding, of ilmenite is reduced
Grain diameter, improves the contact area of ilmenite powder and dilute sulfuric acid, to improve the acidizing degree of ilmenite as much as possible, reduces
The use of the later stage concentrated sulfuric acid, finds to prepare that 1kg titanium dioxides technique than before is few to use 28% using this patent method through experiment
The concentrated sulfuric acid；And the generation of dust can also be reduced using wet grinding, protect environment；
(2) by installing the design of vacuum pump on leadwork reactor, convenient for promoting the rate of drying after wet grinding, and
It when hydrolysis temperature has just reached 90 DEG C, can boil, promote hydrolysis, promote hydrolysis rate；
(3) early period, the later stage was accurate to grinding progress every time by repeatedly grinding using crushing using corase grinding, wet grinding
The division of labor effectively controls titanium dioxide size, improves the uniformity of titanium dioxide size.
Specific implementation mode
With reference to embodiments, the present invention will be described in further detail.It should be appreciated that specific reality described herein
Example is applied only to explain the present invention, is not intended to limit the present invention.
Embodiment one：
The preparation process of titanium dioxide, includes the following steps in the present embodiment：
Step 1：Raw material is roughly ground, and ilmenite raw material is dried, is roughly ground, 10 mesh of coarse abrasive grains diameter, wherein ilmenite
Contain 42% TiO2 in raw material；
Step 2：The ilmenite powder for completing to roughly grind in step 1 is added in dilution heat of sulfuric acid by raw material wet-milling, is mixed
It is sent into ball mill afterwards and carries out wet grinding, the wherein a concentration of 7mol/L of dilute sulfuric acid, the aperture of the filter screen of wet grinding is
180 mesh；
Step 3：The mixed liquor for the wet-milling completed in step 2 is sent into leadwork reactor and carries out vacuum by vacuum drying
It is dry, the vacuum pump for vacuumizing is installed on leadwork reactor；
Step 4：Acidolysis after the completion of drying in step 3, is slowly introducing the concentrated sulfuric acid into leadwork reactor, goes forward side by side
Row heating, is kept for the reaction 30min reaction time, and wherein acidolysis temperature is 150 DEG C, the sulfuric acid that the concentrated sulfuric acid is a concentration of 85%；
Step 5：Reduction is passed through dilute sulfuric acid dilution into leadwork reactor, is continually fed into iron filings powder in dilution, also
Ferric ion in former mixed liquor becomes ferrous ion, 11 hours reaction time；
Step 6：Sedimentation, the cooling acid hydrolysis solution for completing reduction reaction so that solid inert material and unreacted raw material are residual
Excess solution is all discharged into from the bottom of acid hydrolysis tank in low level sedimentation basin；In sedimentation, add people's casein and starch flocculant,
By gravitational settling, the sedimentation time is kept for 8 hours；
Step 7：The solution for completing the precipitation step is cooled to 8 DEG C by crystallisation by cooling, and crystallization filters and recycles green vitriol
FeSO4·7H2O；
Step 8：The solution for completing crystallisation by cooling step is heated to 90 DEG C, and continued to leadwork reactor by hydrolysis
It vacuumizes so that hydrating solution boils, and continues to be added 90 DEG C of hot water into leadwork reactor, wherein what is persistently vacuumized is interior
Portion's air pressure remains 20000Pa, and hydrolysis is heated by steam, and is brought rapidly up to 112 DEG C；
Step 9：Calcining, will complete the sediment of hydrolysis, is sent into internal combustion type rotary kiln and is forged after being filtered, washed
It burns, calcination temperature is 900 DEG C, and the gas excluded when calcining needs to use activated carbon adsorption, excludes the TiO2 carried secretly in tail gas
Particle；
Step 10：Coating is crushed, the titanium dioxide after calcining is crushed, coating is carried out after crushing, completes titanium dioxide
Production, wherein coating uses aluminum sulfate and sodium hydroxide for coating agent, and aluminum oxide packet is carried out to titanium dioxide with chemical precipitation method
Film.
Embodiment two：
The preparation process of titanium dioxide, includes the following steps in the present embodiment：
Step 1：Raw material is roughly ground, and ilmenite raw material is dried, is roughly ground, 20 mesh of coarse abrasive grains diameter, wherein ilmenite
Contain 60% TiO2 in raw material；
Step 2：The ilmenite powder for completing to roughly grind in step 1 is added in dilution heat of sulfuric acid by raw material wet-milling, is mixed
It is sent into ball mill afterwards and carries out wet grinding, the wherein a concentration of 9mol/L of dilute sulfuric acid, the aperture of the filter screen of wet grinding is
200 mesh；
Step 3：The mixed liquor for the wet-milling completed in step 2 is sent into leadwork reactor and carries out vacuum by vacuum drying
It is dry, the vacuum pump for vacuumizing is installed on leadwork reactor；
Step 4：Acidolysis after the completion of drying in step 3, is slowly introducing the concentrated sulfuric acid into leadwork reactor, goes forward side by side
Row heating, is kept for the reaction 45min reaction time, and wherein acidolysis temperature is 180 DEG C, the sulfuric acid that the concentrated sulfuric acid is a concentration of 92%；
Step 5：Reduction is passed through dilute sulfuric acid dilution into leadwork reactor, is continually fed into iron filings powder in dilution, also
Ferric ion in former mixed liquor becomes ferrous ion, 12 hours reaction time；
Step 6：Sedimentation, the cooling acid hydrolysis solution for completing reduction reaction so that solid inert material and unreacted raw material are residual
Excess solution is all discharged into from the bottom of acid hydrolysis tank in low level sedimentation basin；In sedimentation, add people's casein and starch flocculant,
By gravitational settling, the sedimentation time is kept for 10 hours；
Step 7：The solution for completing the precipitation step is cooled to 8 DEG C by crystallisation by cooling, and crystallization filters and recycles green vitriol
FeSO4·7H2O；
Step 8：The solution for completing crystallisation by cooling step is heated to 114 DEG C, and is held to leadwork reactor by hydrolysis
It is continuous to vacuumize so that hydrating solution boils, and continues to be added 100 DEG C of hot water into leadwork reactor, wherein persistently vacuumizing
Air pressure inside remain 20000Pa, hydrolysis is brought rapidly up by steam heating to 114 DEG C；
Step 9：Calcining, will complete the sediment of hydrolysis, is sent into internal combustion type rotary kiln and is forged after being filtered, washed
It burns, calcination temperature is 1250 DEG C, and the gas excluded when calcining needs to use activated carbon adsorption, excludes the TiO2 carried secretly in tail gas
Particle；
Step 10：Coating is crushed, the titanium dioxide after calcining is crushed, coating is carried out after crushing, completes titanium dioxide
Production, wherein coating uses aluminum sulfate and sodium hydroxide for coating agent, and aluminum oxide packet is carried out to titanium dioxide with chemical precipitation method
Film.
Embodiment three：
The preparation process of titanium dioxide, includes the following steps in the present embodiment：
Step 1：Raw material is roughly ground, and ilmenite raw material is dried, is roughly ground, 15 mesh of coarse abrasive grains diameter, wherein ilmenite
Contain 51% TiO2 in raw material；
Step 2：The ilmenite powder for completing to roughly grind in step 1 is added in dilution heat of sulfuric acid by raw material wet-milling, is mixed
It is sent into ball mill afterwards and carries out wet grinding, the wherein a concentration of 8mol/L of dilute sulfuric acid, the aperture of the filter screen of wet grinding is
190 mesh；
Step 3：The mixed liquor for the wet-milling completed in step 2 is sent into leadwork reactor and carries out vacuum by vacuum drying
It is dry, the vacuum pump for vacuumizing is installed on leadwork reactor；
Step 4：Acidolysis after the completion of drying in step 3, is slowly introducing the concentrated sulfuric acid into leadwork reactor, goes forward side by side
Row heating, is kept for the reaction 40min reaction time, and wherein acidolysis temperature is 165 DEG C, the sulfuric acid that the concentrated sulfuric acid is a concentration of 88%；
Step 5：Reduction is passed through dilute sulfuric acid dilution into leadwork reactor, is continually fed into iron filings powder in dilution, also
Ferric ion in former mixed liquor becomes ferrous ion, 11 hours reaction time；
Step 6：Sedimentation, the cooling acid hydrolysis solution for completing reduction reaction so that solid inert material and unreacted raw material are residual
Excess solution is all discharged into from the bottom of acid hydrolysis tank in low level sedimentation basin；In sedimentation, add people's casein and starch flocculant,
By gravitational settling, the sedimentation time is kept for 9 hours；
Step 7：The solution for completing the precipitation step is cooled to 10 DEG C by crystallisation by cooling, and crystallization is filtered and recycled green
Alum FeSO47H2O；
Step 8：The solution for completing crystallisation by cooling step is heated to 108 DEG C, and is held to leadwork reactor by hydrolysis
It is continuous to vacuumize so that hydrating solution boils, and continues to be added 96 DEG C of hot water into leadwork reactor, wherein persistently vacuumize
Air pressure inside remains 20000Pa, and hydrolysis is heated by steam, and is brought rapidly up to 112 DEG C；
Step 9：Calcining, will complete the sediment of hydrolysis, is sent into internal combustion type rotary kiln and is forged after being filtered, washed
It burns, calcination temperature is 1100 DEG C, and the gas excluded when calcining needs to use activated carbon adsorption, excludes the TiO2 carried secretly in tail gas
Particle；
Step 10：Coating is crushed, the titanium dioxide after calcining is crushed, coating is carried out after crushing, completes titanium dioxide
Production, wherein coating uses aluminum sulfate and sodium hydroxide for coating agent, and aluminum oxide packet is carried out to titanium dioxide with chemical precipitation method
Film.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as excluding other embodiments, and can be used for various other combinations, modification and
Environment, and can be changed by the above teachings or related fields of technology or knowledge in the scope of the invention is set forth herein
It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention
In scope of the claims.
Claims (10)
1. a kind of preparation process of titanium dioxide, by ilmenite raw material successively through acidolysis, reduction, sedimentation, crystallisation by cooling, hydrolyze and forge
Burn, which is characterized in that first through wet grinding before the ilmenite raw material acidolysis, in wet grinding, by ilmenite raw material plus
Enter into dilution heat of sulfuric acid, the mixed liquor being mixed to form is sent into ball mill and carries out wet grinding.
2. a kind of preparation process of titanium dioxide according to claim 1, which is characterized in that the wet grinding with it is described
Vacuum drying step is added between acidolysis, the vacuum drying step is that the mixed liquor after wet grinding is sent into leadwork reactor
In be dried in vacuo.
3. a kind of preparation process of titanium dioxide according to claim 2, which is characterized in that before the wet grinding, first
The ilmenite raw material is dried and is roughly ground, a diameter of 10 ~ 20 mesh of ilmenite particle after control corase grinding.
4. a kind of preparation process of titanium dioxide according to claim 3, which is characterized in that the hydrolysis step is to leadwork
It is slowly introducing the concentrated sulfuric acid in reactor, and is heated, is kept for the reaction time of 30 ~ 45min.
5. a kind of preparation process of titanium dioxide according to claim 4, which is characterized in that the reduction step is that leadwork is anti-
It answers and is passed through dilute sulfuric acid dilution in device, iron filings powder is continuously added into dilution, the ferric ion restored in mixed liquor becomes two
Valence iron ion, 11 ~ 12 hours reaction time.
6. a kind of preparation process of titanium dioxide according to claim 5, which is characterized in that the precipitation step is to have cooled down
At the acid hydrolysis solution of reduction reaction so that solid inert material and unreacted raw material residue solution are whole from the bottom of acid hydrolysis tank
It is discharged into low level sedimentation basin.
7. a kind of preparation process of titanium dioxide according to claim 6, which is characterized in that the crystallisation by cooling step is will
It is described it is heavy remove after solution be cooled to 8 ~ 12 DEG C, crystallization filters and recycles green vitriol FeSO47H2O.
8. a kind of preparation process of titanium dioxide according to claim 7, which is characterized in that the hydrolysing step is will be described
Solution after crystallisation by cooling is heated to 90 ~ 114 DEG C, and is persistently vacuumized to leadwork reactor so that and hydrating solution boils,
And continue the hot water of 90 ~ 100 DEG C of the addition into leadwork reactor.
9. a kind of preparation process of titanium dioxide according to claim 8, which is characterized in that the calcining step is will be described
Sediment after hydrolysis is filtered, wash after be sent into internal combustion type rotary kiln and calcined.
10. a kind of preparation process of titanium dioxide according to claim 9, which is characterized in that by the titanium Jing Guo the calcining
White powder is crushed obtains required titanium dioxide with coating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114074955A (en) * | 2020-08-18 | 2022-02-22 | 徐州钛白化工有限责任公司 | Preparation method for high-fluidity rutile titanium dioxide |
| CN114074954A (en) * | 2020-08-18 | 2022-02-22 | 徐州钛白化工有限责任公司 | Preparation method of anatase titanium dioxide with high water covering power |
| CN114162857A (en) * | 2021-12-10 | 2022-03-11 | 长沙华希新材料有限公司 | Titanium dioxide for hard alloy and preparation method thereof |
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| CN104071835A (en) * | 2014-06-30 | 2014-10-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of titanium dioxide |
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- 2018-03-28 CN CN201810267149.4A patent/CN108502920A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104071835A (en) * | 2014-06-30 | 2014-10-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of titanium dioxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114074955A (en) * | 2020-08-18 | 2022-02-22 | 徐州钛白化工有限责任公司 | Preparation method for high-fluidity rutile titanium dioxide |
| CN114074954A (en) * | 2020-08-18 | 2022-02-22 | 徐州钛白化工有限责任公司 | Preparation method of anatase titanium dioxide with high water covering power |
| CN114162857A (en) * | 2021-12-10 | 2022-03-11 | 长沙华希新材料有限公司 | Titanium dioxide for hard alloy and preparation method thereof |
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Application publication date: 20180907 |