CN103663545A - Production method of super-pure titanium sulfate solution - Google Patents
Production method of super-pure titanium sulfate solution Download PDFInfo
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- CN103663545A CN103663545A CN201210335583.4A CN201210335583A CN103663545A CN 103663545 A CN103663545 A CN 103663545A CN 201210335583 A CN201210335583 A CN 201210335583A CN 103663545 A CN103663545 A CN 103663545A
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Abstract
The invention discloses a production method of a super-pure titanium sulfate solution. The production method comprises the steps of settling an acidolysis titanium solution, taking supernatant liquid, and performing pressure filtration on the supernatant liquid through a plate-and-frame filter press; separating the obtained filtrate through ferrous crystals and ferrous iron respectively; performing membrane separation on the obtained titanium solution through an ultrafiltration membrane, thereby obtaining the super-pure titanium sulfate solution. The invention aims to provide the production method of the super-pure titanium sulfate solution, which is short in flow, simple and convenient in operation, saving in water consumption, stable in product quality and high in product purity.
Description
Technical field
The present invention relates to a kind of production method of ultra-pure sulfuric acid titanium liquid.
Background technology
It is ripe production method that sulfate process titanium dioxide is produced, and the raw material of use is ilmenite or titanium slag, sulfuric acid.Sulfate process titanium dioxide is produced and mainly following several operations, to be consisted of: the purification of acidolysis, titanium liquid (comprising the operations such as sedimentation, crystallization, separation, filtration), titanium liquid are concentrated, hydrolysis, washing and rinsing, salt processing, calcining, crushing packing.Wherein, the quality of titanium liquid directly has influence on the operation of follow-up each operation and the quality of the finished product.At present, the indexs such as the total titanium of titanium liquid, iron titanium ratio, F value, titanous can be well controlled, and purify and have fluctuation during stability, purification is to characterize with the solid content in titanium liquid, it has impact to the stability of titanium liquid, the quality that titanium liquid purifies, more directly has influence on the quality of the finished product.Prior art acidolysis titanium liquid, after sedimentation, is got the advanced andante frame of supernatant liquid heat filtering, after filter titanium liquid through ferrous crystallization with ferrous separated after, adopt sheet frame to carry out controlled filter.Plate Filtration is comprised of filter plate, filter cloth and filtration adjuvant etc., after titanium liquid filters, according to the variation of filter pressure, will every now and then filter cloth be cleaned even and be changed, and workload is large, and wash-down water can reduce the concentration of titanium liquid, even if reuse wash water is also the reciprocal of flow process; And have damaged situation during filter cloth, and in titanium liquid, impurity will enter next procedure with titanium liquid, and titanium liquid difficult quality is stable to be controlled.Adopt after prior art controlled filter in titanium liquid foreign matter content more than 20ppm, the total titanium 150g/L of titanium liquid left and right.
Summary of the invention
The object of this invention is to provide the production method that a kind of flow process is short, easy and simple to handle, save water consumption, constant product quality, a kind of ultra-pure sulfuric acid titanium liquid that purity is high.
The production method of a kind of ultra-pure sulfuric acid titanium of the present invention liquid, adopts following steps: acidolysis titanium liquid, after sedimentation, is got to the upper strata stillness of night through plate-and-frame filter press press filtration; By the filtrate of gained respectively through ferrous crystallization with ferrous separated after; The titanium liquid of gained, through ultra-filtration membrane, is carried out to membrane sepn, obtain ultra-pure sulfuric acid titanium liquid.
As a preferred version of technique scheme, described ultra-filtration membrane is hollow fiber ultrafiltration membrane.
Traditional method is that the titanium liquid of gained is filtered through plate and frame, need be periodically filter cloth is cleaned even and be changed, and workload is large, and a large amount of filter cloth washing water can cause the system water cannot balance, and brings pressure to sewage disposal; And if the not tight or filter cloth that filter cloth is installed in this process has breakage, in titanium liquid, impurity will enter next procedure with titanium liquid, titanium liquid difficult quality is stable to be controlled.And employing technique scheme, due to adopt will through ferrous crystallization with ferrous separated after; The titanium liquid of gained, through ultra-filtration membrane, is adopted to ultra-filtration membrane, carry out membrane sepn.Easy and simple to handle, saving water consumes, constant product quality.
In technique scheme, for accelerating subsidence rate, add that volume is that acidolysis titanium liquid is long-pending 2～10% when the sedimentation of acidolysis titanium liquid, concentration is 1～5 ‰ flocculation agent polyacrylamide, sedimentation 4～10h.
In technique scheme, for accelerating filtering rate, add filtration adjuvant getting the upper strata stillness of night before plate-and-frame filter press carries out press filtration, described filtration adjuvant is selected from any one in wood charcoal powder, lignocellulose, diatomite.
In technique scheme, ferrous crystallization adopts vacuum crystallization and freezing and crystallizing, and described crystallization final temperature is controlled at 12～18 ℃.
In sum, the invention has the beneficial effects as follows: adopt that this kind of production method flow process is short, easy and simple to handle, to save water consumption, constant product quality, purity high.
Embodiment
Below in conjunction with embodiment, the present invention will be further described:
Embodiment mono-:
Get acidolysis titanium liquid 100m
3, total titanium 125g/L, 58 ℃ of temperature, add 400m
3subsider, adds 2 m at line mixer simultaneously
3mass concentration be 2 ‰ polyacrylamides, after sedimentation 4h; Get supernatant liquid 250m
2sheet frame carry out heat filtering, flow is 30m
3/ h, before titanium liquid filters first to sheet frame precoating wood charcoal powder drainage layer; Titanium liquid after heat filtering is carried out to vacuum crystallization, and crystallization final temperature is controlled at 13 ℃; Titanium liquid after crystallization is carried out to disk filtration and remove crystalline sulfuric acid ferrous iron; The ferrous titanium liquid of removal crystalline sulfuric acid is filtered with ultra-filtration membrane, obtain titanium liquid 65m
3, total titanium 162g/L, solid content 9mg/L.
Embodiment bis-:
Get acidolysis titanium liquid 100m
3, total titanium 125g/L, 58 ℃ of temperature, add 400m
3subsider, adds 7m at line mixer simultaneously
3mass concentration be 3 ‰ polyacrylamides, after sedimentation 6h; Get supernatant liquid 250m
2sheet frame carry out heat filtering, flow is 40m
3/ h, before titanium liquid filters first to sheet frame precoating lignocellulose drainage layer; Titanium liquid after heat filtering is carried out to vacuum crystallization, and crystallization final temperature is controlled at 16 ℃; Titanium liquid after crystallization is carried out to disk filtration and remove crystalline sulfuric acid ferrous iron; The ferrous titanium liquid of removal crystalline sulfuric acid is filtered with ultra-filtration membrane, obtain titanium liquid 65m
3, total titanium 163g/L, solid content 9.2mg/L.
Embodiment tri-:
Get acidolysis titanium liquid 100m
3, total titanium 125g/L, 58 ℃ of temperature, add 400m
3subsider, adds 10m at line mixer simultaneously
3mass concentration be 5 ‰ polyacrylamides, after sedimentation 10h; Get supernatant liquid 250m
2sheet frame carry out heat filtering, flow is 35m
3/ h, titanium liquid adds super-cell before filtering in titanium liquid; Titanium liquid after heat filtering is carried out to vacuum crystallization, and crystallization final temperature is controlled at 18 ℃; Titanium liquid after crystallization is carried out to disk filtration and remove crystalline sulfuric acid ferrous iron; The ferrous titanium liquid of removal crystalline sulfuric acid is filtered with ultra-filtration membrane, obtain titanium liquid 65m
3, total titanium 161g/L, solid content 9.1mg/L.
Claims (5)
1. a production method for ultra-pure sulfuric acid titanium liquid, its step is as follows: acidolysis titanium liquid, after sedimentation, is got to the upper strata stillness of night through plate-and-frame filter press press filtration; By the filtrate of gained respectively through ferrous crystallization with ferrous separated after; The titanium liquid of gained, through ultra-filtration membrane, is carried out to membrane sepn, obtain ultra-pure sulfuric acid titanium liquid.
2. the production method of a kind of ultra-pure sulfuric acid titanium liquid according to claim 1, is characterized in that described ultra-filtration membrane is hollow fiber ultrafiltration membrane.
3. the production method of a kind of ultra-pure sulfuric acid titanium liquid according to claim 1 and 2, is characterized in that adding when the sedimentation of acidolysis titanium liquid that volume is that acidolysis titanium liquid is long-pending 2～10%, mass concentration is 1～5 ‰ flocculation agent polyacrylamide, sedimentation 4～10h.
4. the production method of a kind of ultra-pure sulfuric acid titanium liquid according to claim 1 and 2, it is characterized in that before plate-and-frame filter press carries out press filtration, adding filtration adjuvant getting the upper strata stillness of night, described filtration adjuvant is any one in wood charcoal powder, lignocellulose, diatomite.
5. the production method of a kind of ultra-pure sulfuric acid titanium liquid according to claim 1 and 2, is characterized in that described ferrous crystallization comprises vacuum crystallization and freezing and crystallizing, and described crystallization final temperature is controlled at 12～18 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210335583.4A CN103663545B (en) | 2012-09-12 | 2012-09-12 | A kind of production method of super-pure titanium sulfate solution |
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| CN201210335583.4A CN103663545B (en) | 2012-09-12 | 2012-09-12 | A kind of production method of super-pure titanium sulfate solution |
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| CN103663545A true CN103663545A (en) | 2014-03-26 |
| CN103663545B CN103663545B (en) | 2015-09-16 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386740A (en) * | 2014-11-21 | 2015-03-04 | 湖南有色湘乡氟化学有限公司 | Preparation method of high-purity calcium hydrofluotitanate |
| CN105439105A (en) * | 2015-12-22 | 2016-03-30 | 江苏久吾高科技股份有限公司 | Integrated membrane treatment and recovery technology and apparatus for waste acid in production process of titanium dioxide |
| CN106809883A (en) * | 2015-11-30 | 2017-06-09 | 南京钛白化工有限责任公司 | Sulfate process titanium dioxide produces the device and method of ferrous sulfate |
| CN106966427A (en) * | 2017-03-14 | 2017-07-21 | 襄阳龙蟒钛业有限公司 | The purification method of a kind of acidolysis titanium liquid and for the filter in method |
| CN107697948A (en) * | 2017-11-21 | 2018-02-16 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of titanium sulfate liquid high-efficient purification |
| CN109319831A (en) * | 2018-11-26 | 2019-02-12 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of purification method of titanium sulfate liquid |
| CN111308021A (en) * | 2020-03-31 | 2020-06-19 | 龙佰四川钛业有限公司 | Method for detecting filtering performance of titanium liquid filter aid |
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- 2012-09-12 CN CN201210335583.4A patent/CN103663545B/en not_active Expired - Fee Related
Patent Citations (5)
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| JPH01153528A (en) * | 1987-12-09 | 1989-06-15 | Asahi Chem Ind Co Ltd | Treatment of dispersion of gel of titanic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386740A (en) * | 2014-11-21 | 2015-03-04 | 湖南有色湘乡氟化学有限公司 | Preparation method of high-purity calcium hydrofluotitanate |
| CN104386740B (en) * | 2014-11-21 | 2016-04-06 | 湖南有色湘乡氟化学有限公司 | A kind of preparation method of high-purity fluorine calcium titanate |
| CN106809883A (en) * | 2015-11-30 | 2017-06-09 | 南京钛白化工有限责任公司 | Sulfate process titanium dioxide produces the device and method of ferrous sulfate |
| CN105439105A (en) * | 2015-12-22 | 2016-03-30 | 江苏久吾高科技股份有限公司 | Integrated membrane treatment and recovery technology and apparatus for waste acid in production process of titanium dioxide |
| CN106966427A (en) * | 2017-03-14 | 2017-07-21 | 襄阳龙蟒钛业有限公司 | The purification method of a kind of acidolysis titanium liquid and for the filter in method |
| CN106966427B (en) * | 2017-03-14 | 2019-10-08 | 襄阳龙蟒钛业有限公司 | The purification method of a kind of acidolysis titanium liquid and for the filter in method |
| CN107697948A (en) * | 2017-11-21 | 2018-02-16 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of titanium sulfate liquid high-efficient purification |
| CN109319831A (en) * | 2018-11-26 | 2019-02-12 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of purification method of titanium sulfate liquid |
| CN111308021A (en) * | 2020-03-31 | 2020-06-19 | 龙佰四川钛业有限公司 | Method for detecting filtering performance of titanium liquid filter aid |
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| CN103663545B (en) | 2015-09-16 |
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