CN101469367A - Method for recycling titanium dioxide acid hydrolysis residue - Google Patents
Method for recycling titanium dioxide acid hydrolysis residue Download PDFInfo
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- CN101469367A CN101469367A CNA2007103048727A CN200710304872A CN101469367A CN 101469367 A CN101469367 A CN 101469367A CN A2007103048727 A CNA2007103048727 A CN A2007103048727A CN 200710304872 A CN200710304872 A CN 200710304872A CN 101469367 A CN101469367 A CN 101469367A
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- titanium dioxide
- acid hydrolysis
- residue
- ilmenite
- dioxide acid
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a novel method for recovering and utilizing acidolysis residue of titanium white, which comprises the following steps: A, the acidolysis residue of the titanium white containing 20 to 40 percent of TiO2, 10 to 20 percent of Fe<3+>, 5 to 8 percent of H2SO4 and other impurities is water scrubbed and filtered to obtain low-acid acidolysis residue of the titanium white with H2SOR4 content lower than 5 percent; B, the low-acid acidolysis residue of the titanium white obtained in step A is smashed and dispersed; C, a product obtained in step B is added with water and is subjected to rough concentration to obtain heavy slag slurry and light slag slurry; D, the heavy slag slurry obtained in step C is subjected to magnetic separation to obtain magnetic ilmenite and the impurities; and E, the magnetic ilmenite obtained in step D is dried to obtain an ilmenite product containing 47 to 49 percent of the TiO2. The method can recover and utilize the TiO2 in residue produced during the acidolysis of the titanium white, improve the yield, and can also reduce environmental pollution.
Description
Technical field
The present invention relates to a kind of titanium dioxide acid hydrolysis residue recovery technology field.
Background technology
Contain many solid residues in the solution in the production process of titanium pigment after the ilmenite powder acidolysis leaching, its main component is unreacted ilmenite powder, and a spot of vitriolic impurity that is insoluble to.Separate through sedimentation, suction filtration, its amount has 500～600 kilograms approximately for one ton of titanium white of every production, and butt is about 160～180 kilograms.Butt contains TiO
220～40%, contain Fe10～20%.Even this residue generally still has certain acid solution through washing and suction filtration, wet basis contains H
2SO
45～8%.If do not handled, will cause the wasting of resources, environmental pollution.
At present the method that generally adopts has three kinds: a kind of is after measuring the residue water content, and the residue that will wet uses as dilution water and sneaks in the reactant, through with the reactant thorough mixing after the initiation reaction of heating again.The 2nd, with the residue cleaning, drying, usefulness again after the grinding can be used with new breeze, also can decompose separately.The 3rd, with the acidolysis of in autoclave pressure, pressurizeing after wet residue and the vitriol oil batching.Above method respectively has shortcoming: use residue to repeat to decompose separately, acidolysis rate is lower, generally is difficult to reach 80%, and the titanium white inferior quality of gained, should not produce the kind that coating titanium white etc. is had relatively high expectations; Use with new breeze, misoperation easily impacts quality product.
Summary of the invention:
The purpose of this invention is to provide a kind of novel method with recovering and utilizing acidolysis residue, it not only can be with the TiO in the titanium dioxide acid hydrolysis process residue
2Recycle, improve productive rate, and can reduce environmental pollution.
Technical scheme of the present invention is: a kind of recovering and utilizing acidolysis residue novel method comprises the steps: that A. will contain TiO
220-40%, Fe
3+10-20%, H
2SO
4The titanium dioxide acid hydrolysis residue washing filtering of 5-8% and other impurity gets H
2SO
4Content is lower than 5% low sour titanium dioxide acid hydrolysis residue; B.The low sour titanium dioxide acid hydrolysis residue of gained in the A step is smashed dispersion; C. B step products obtained therefrom being added water roughly selects to such an extent that the heavy slag is starched and light slag slurry; D. C step gained is got the magnetic separation of heavy slag slurry and get magnetic ilmenite and impurity; E. D step gained magnetic ilmenite drying must be contained TiO
2The ilmenite product of 47-49%.
Above-mentioned recovering and utilizing acidolysis residue novel method, it is that application machine power stirs that described step B smashes dispersion, and stirring velocity is 600-800 rev/min, and churning time is 50-80 minute.
Above-mentioned recovering and utilizing acidolysis residue novel method, the stirring velocity of described step B are 700 rev/mins, and churning time is 60 minutes.
Above-mentioned recovering and utilizing acidolysis residue novel method, described step B and step C can carry out simultaneously.
Beneficial effect of the present invention: not only can be with the TiO in the titanium dioxide acid hydrolysis process residue
2Recycle, improve productive rate, and can reduce environmental pollution.
Products obtained therefrom of the present invention is pulverized, and the recovery ilmenite of pulverizing can carry out acidolysis production separately, also can mix to join with new breeze and carry out acidolysis.Carry out the effect such as the table 1 (adopting the solid phase method acidolysis, the ordinary-pressure hydrolysis flow process) of acidolysis separately
Table 1 is the effect table (adopting the solid phase method acidolysis, the ordinary-pressure hydrolysis flow process) that the ilmenite of recovery carries out acidolysis separately
| Acid ore deposit ratio | Acidolysis rate % | Ti 3+(g/l) | TiO 2(g/l) | The Fe value | Stability |
| 1：1.52 | 94.0 | 1.81 | 128.36 | 1.77 | 340 |
| 1：1.54 | 95.1 | 1.74 | 127.96 | 1.80 | 350 |
| 1：1.56 | 95.5 | 1.85 | 128.55 | 1.85 | 350 |
| 1：1.58 | 96.8 | 1.92 | 126.46 | 1.85 | 350 |
| 1：1.60 | 96.3 | 1.92 | 127.43 | 1.79 | 360 |
| 1：1.62 | 97.01 | 1.84 | 127.93 | 1.94 | 360 |
As can be seen from the above table, sour ore deposit can reach 97.01% than in the 1:1.52-1:1.62 acidolysis rate, minimumly reaches 94.0%, and Ti
3+, TiO
2, F value, stable every index all reach requirement.The ilmenite acidolysis fully separately that this patent reclaims is described, produces qualified titanium liquid.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Specific embodiment
Embodiment 1: will contain TiO
220%, Fe
3+10%, H
2SO
45% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
41.6%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 600 rev/mins, stirred 50 minutes, enter spiral concentrator add water roughly select heavy product, light product is a waste residue, then the gained heavy product is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
247% ilmenite.
Embodiment 2: will contain TiO
225%, Fe
3+12%, H
2SO
46% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
4H
2SO
41.5%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 650 rev/mins, stirred 55 minutes, enter spiral concentrator add water roughly select heavy product, light product is a waste residue, then gained heavy slag liquid is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
247.8% ilmenite.
Embodiment 3: will contain TiO
240%, Fe
3+20%, H
2SO
48% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
4H
2SO
41.4%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 800 rev/mins, stirred 80 minutes, enter spiral concentrator add water roughly select heavy product, light product advances to be waste residue, then gained heavy slag liquid is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
249% ilmenite.
Embodiment 4: will contain TiO
239%, Fe
3+18%, H
2SO
47% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
4H
2SO
41.5%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 750 rev/mins, stirred 80 minutes, enter spiral concentrator add water roughly select heavy product, light product is a waste residue, then gained heavy slag liquid is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
249% ilmenite.
Embodiment 5: will contain TiO
230%, Fe
3+15%, H
2SO
47% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
41.3%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 700 rev/mins, stirred 60 minutes, enter spiral concentrator add water roughly select heavy product, light product is a waste residue, then gained heavy slag liquid is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
248% ilmenite.
Embodiment 6: will contain TiO
220%, Fe
3+20%, H
2SO
48% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
41.4%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 800 rev/mins, stirred 80 minutes, enter spiral concentrator add water roughly select heavy product, light product is a waste residue, then gained heavy slag liquid is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
249% ilmenite.
Embodiment 7: will contain TiO
240%, Fe
3+10%, H
2SO
48% and the titanium dioxide acid hydrolysis residue slurries of impurity inject pressure filter, reclaim filtrate after, water washes residual filter cake, filters to make it contain H
2SO
41.4%; To hang down sour titanium dioxide acid hydrolysis residue then and smash dispersion, owing to contain certain acidity in the residue, its operation can be selected enamel still, stir with brute force, stirring velocity is 800 rev/mins, stirred 80 minutes, enter spiral concentrator add water roughly select heavy product, light product is a waste residue, then gained heavy slag liquid is carried out selected magnetic product and the non-magnetic product of sub-electing of two-stage with wet magnetic separator, magnetic product 98% is an ilmenite, and magnetic product is carried out drying with drying plant, make the ilmenite water content less than 1%, promptly obtain containing TiO
249% ilmenite.
The present invention smashes, disperses and roughly selects step and also can carry out simultaneously, utilizes and carries out antiseptic ball mill, and the residue that will wet adds continuously, water filling continuously simultaneously, and light product overflows from the upper end, and heavy product flows out from the lower end, enters down operation.
Claims (4)
1. the method that titanium dioxide acid hydrolysis residue reclaims comprises the steps: that A. will contain TiO
220-40%, Fe
3+10-20%, H
2SO
4The titanium dioxide acid hydrolysis residue of 5-8% and impurity gets H through washing filtering
2SO
4Content is lower than 5% low sour titanium dioxide acid hydrolysis residue; B. the low acidity titanium dioxide acid hydrolysis residue of gained in the A step is smashed dispersion; C. B step products obtained therefrom being added water roughly selects to such an extent that the heavy slag is starched and light slag slurry; D. the magnetic separation of C step gained heavy slag slurry is got magnetic ilmenite and impurity; E. D step gained magnetic ilmenite drying must be contained TiO
2The ilmenite product of 47-49%.
2. the method that titanium dioxide acid hydrolysis residue according to claim 1 reclaims is characterized in that: it is that application machine power stirs that described step B smashes dispersion, and stirring velocity is 600-800 rev/min, and churning time is 50-80 minute.
3. the method that titanium dioxide acid hydrolysis residue according to claim 2 reclaims, it is characterized in that: the stirring velocity of described step B is 700 rev/mins, churning time is 60 minutes.
4. the method that titanium dioxide acid hydrolysis residue according to claim 2 reclaims, it is characterized in that: described step B and step C carry out simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007103048727A CN101469367B (en) | 2007-12-30 | 2007-12-30 | Method for recycling titanium dioxide acid hydrolysis residue |
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|---|---|---|---|
| CN2007103048727A CN101469367B (en) | 2007-12-30 | 2007-12-30 | Method for recycling titanium dioxide acid hydrolysis residue |
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| CN101469367A true CN101469367A (en) | 2009-07-01 |
| CN101469367B CN101469367B (en) | 2010-10-13 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086491A (en) * | 2010-12-14 | 2011-06-08 | 北京中冶设备研究设计总院有限公司 | Method for recycling ferrotitanium resource by using titanium sludge |
| CN102602990A (en) * | 2012-03-31 | 2012-07-25 | 四川龙蟒钛业股份有限公司 | Recycling method for producing acidolysis slag in titanium dioxide with sulfuric acid method |
| CN103316764A (en) * | 2013-06-27 | 2013-09-25 | 攀钢集团钛业有限责任公司 | Method for recycling titanium dioxide from titanium dioxide acidolysis sludge |
| CN106865606A (en) * | 2017-03-14 | 2017-06-20 | 襄阳龙蟒钛业有限公司 | A kind of production method of titanium dioxide |
| CN107324380A (en) * | 2017-07-11 | 2017-11-07 | 攀钢集团研究院有限公司 | The method that titaniferous material is reclaimed from titanium dioxide acid hydrolysis residue |
| CN108726563A (en) * | 2018-06-08 | 2018-11-02 | 龙蟒佰利联集团股份有限公司 | A kind of method that acidolysis tailing recycles in production process of titanium pigment |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3742838A1 (en) * | 1987-12-17 | 1989-07-13 | Kronos Titan Gmbh | METHOD FOR PRODUCING TITANIUM DIOXIDE PIGMENTS |
| CN1064032C (en) * | 1993-10-09 | 2001-04-04 | 宁甲保 | Method for removing waste acid and waste slag from the titanium dioxide production by sulfuric acid method |
| CN1285743C (en) * | 2000-12-12 | 2006-11-22 | 海威尔德钢铁和钒矿有限公司 | Method for recovering titanium dioxide from titanium dioxide bearing materials like steel making slags |
-
2007
- 2007-12-30 CN CN2007103048727A patent/CN101469367B/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086491A (en) * | 2010-12-14 | 2011-06-08 | 北京中冶设备研究设计总院有限公司 | Method for recycling ferrotitanium resource by using titanium sludge |
| CN102086491B (en) * | 2010-12-14 | 2013-01-02 | 北京中冶设备研究设计总院有限公司 | Method for recycling ferrotitanium resource by using titanium sludge |
| CN102602990A (en) * | 2012-03-31 | 2012-07-25 | 四川龙蟒钛业股份有限公司 | Recycling method for producing acidolysis slag in titanium dioxide with sulfuric acid method |
| WO2013143236A1 (en) * | 2012-03-31 | 2013-10-03 | 四川龙蟒钛业股份有限公司 | Method for recycling acidolysis residue from production of titanium white by sulphuric acid process |
| CN102602990B (en) * | 2012-03-31 | 2014-01-08 | 四川龙蟒钛业股份有限公司 | Recycling method for producing acidolysis slag in titanium dioxide with sulfuric acid method |
| CN103316764A (en) * | 2013-06-27 | 2013-09-25 | 攀钢集团钛业有限责任公司 | Method for recycling titanium dioxide from titanium dioxide acidolysis sludge |
| CN103316764B (en) * | 2013-06-27 | 2016-05-11 | 攀钢集团钛业有限责任公司 | A kind of method that reclaims titanium dioxide from titanium dioxide acid hydrolysis body refuse |
| CN106865606A (en) * | 2017-03-14 | 2017-06-20 | 襄阳龙蟒钛业有限公司 | A kind of production method of titanium dioxide |
| CN107324380A (en) * | 2017-07-11 | 2017-11-07 | 攀钢集团研究院有限公司 | The method that titaniferous material is reclaimed from titanium dioxide acid hydrolysis residue |
| CN108726563A (en) * | 2018-06-08 | 2018-11-02 | 龙蟒佰利联集团股份有限公司 | A kind of method that acidolysis tailing recycles in production process of titanium pigment |
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| CN101469367B (en) | 2010-10-13 |
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Address after: 454191 Jiaozuo District, Henan city Feng Feng Office Patentee after: Longmang group Limited by Share Ltd billions Address before: 454191 Henan Province, Jiaozuo City Station area three km west of lotus road Henan baililian chemical Limited by Share Ltd Patentee before: Henan Baililian Chemical Co., Ltd. |
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Address after: 454191 Fengfeng office, zhongzhan District, Jiaozuo City, Henan Province Patentee after: Longbai Group Co.,Ltd. Address before: 454191 Fengfeng office, zhongzhan District, Jiaozuo City, Henan Province Patentee before: LOMON BILLIONS GROUP Co.,Ltd. |
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