CN103663545B - A kind of production method of super-pure titanium sulfate solution - Google Patents
A kind of production method of super-pure titanium sulfate solution Download PDFInfo
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- CN103663545B CN103663545B CN201210335583.4A CN201210335583A CN103663545B CN 103663545 B CN103663545 B CN 103663545B CN 201210335583 A CN201210335583 A CN 201210335583A CN 103663545 B CN103663545 B CN 103663545B
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Abstract
The invention discloses a kind of production method of super-pure titanium sulfate solution, by acidolysis titanium liquid after sedimentation, get supernatant through plate-and-frame filter press press filtration; By the filtrate of gained respectively after ferrous crystallization is separated with ferrous iron; By the titanium liquid of gained through ultra-filtration membrane, carry out membrane sepn, obtain super-pure titanium sulfate solution.Aim 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 super-pure titanium sulfate solution that purity is high.
Description
Technical field
The present invention relates to a kind of production method of super-pure titanium sulfate solution.
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 primarily of following several operation composition: purification (comprising the operations such as sedimentation, crystallization, separation, filtration), the titanium liquid of acidolysis, titanium liquid are concentrated, hydrolysis, washing and rinsing, Ficus caricaL, calcining, crushing packing.Wherein, the quality of titanium liquid directly has influence on the follow-up operation of each operation and the quality of the finished product.At present, in titanium liquid titanium liquid, the index such as mass content, iron titanium ratio, F value, titanous of titanium dioxide can be well controlled, and have fluctuation when purification and stability, purification characterizes with the solid content in titanium liquid, it has impact to the stability of titanium liquid, the quality of titanium liquid purification, more directly has influence on the quality of the finished product.Prior art acidolysis titanium liquid is after sedimentation, and get supernatant liquid advanced andante frame heat filtering, after filter, titanium liquid is after ferrous crystallization is separated with ferrous iron, adopts sheet frame to carry out controlled filter.Plate Filtration is made up of filter plate, filter cloth and filtration adjuvant etc., and titanium liquid will clean filter cloth every now and then according to the change of filter pressure and even change after filtering, 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 during filter cloth, having breakage, in titanium liquid, impurity will enter next procedure with titanium liquid, titanium liquid difficult quality stability contorting.To adopt after prior art controlled filter in titanium liquid foreign matter content at more than 20ppm, about the mass content 150g/L of titanium dioxide in titanium liquid titanium liquid.
Summary of the invention
The object of this invention is to provide a kind of flow process short, easy and simple to handle, save water consumption, constant product quality,
The production method of a kind of super-pure titanium sulfate solution that purity is high.
The production method of a kind of super-pure titanium sulfate solution of the present invention, adopts following steps: by acidolysis titanium liquid after sedimentation, get supernatant through plate-and-frame filter press press filtration; By the filtrate of gained respectively after ferrous crystallization is separated with ferrous iron; By the titanium liquid of gained through ultra-filtration membrane, carry out membrane sepn, obtain super-pure titanium sulfate solution.
As a preferred version of technique scheme, described ultra-filtration membrane is hollow fiber ultrafiltration membrane.
Traditional method is filtered through plate and frame by the titanium liquid of gained, periodically need clean filter cloth and even change, and workload is large, and a large amount of filter cloth washing water can cause system water to balance, and brings pressure to sewage disposal; And if the not tight or filter cloth that filter cloth is installed in the process has breakage, in titanium liquid, impurity will enter next procedure with titanium liquid, titanium liquid difficult quality stability contorting.And adopt technique scheme, will after ferrous crystallization be separated with ferrous iron owing to adopting; By the titanium liquid of gained through ultra-filtration membrane, adopt ultra-filtration membrane, carry out membrane sepn.Easy and simple to handle, saving water consumption, constant product quality.
In technique scheme, in order to accelerate subsidence rate, to add volume when the liquid sedimentation of acidolysis titanium be the flocculation agent polyacrylamide that acidolysis titanium liquid amasss 2 ~ 10%, concentration is 1 ~ 5 ‰, sedimentation 4 ~ 10h.
In technique scheme, before plate-and-frame filter press carries out press filtration, add filtration adjuvant for accelerating filtering rate getting supernatant, described filtration adjuvant be selected from wood charcoal powder, lignocellulose, diatomite any one.
In technique scheme, ferrous crystallization adopts vacuum crystallization and freezing and crystallizing, and described crystallization final temperature controls at 12 ~ 18 DEG C.
In sum, the invention has the beneficial effects as follows: production method flow process is short, easy and simple to handle, saving water consumption, constant product quality, purity are high to adopt this kind.
Embodiment
Below in conjunction with embodiment, the present invention will be further described:
Embodiment one:
Get acidolysis titanium liquid 100m3, the mass content 125g/L of titanium dioxide in titanium liquid, temperature 58 DEG C, adds 400m3 subsider, and the mass concentration simultaneously adding 2 m3 at line mixer is 2 ‰ polyacrylamides, after sedimentation 4h; The sheet frame getting supernatant liquid 250m2 carries out heat filtering, and flow is 30m3/h, first to sheet frame precoating wood charcoal powder drainage layer before titanium liquid filters; Titanium liquid after heat filtering is carried out vacuum crystallization, and crystallization final temperature controls at 13 DEG C; Titanium liquid after crystallization is carried out disk filtration and remove crystalline sulfuric acid ferrous iron; Ferrous for removal crystalline sulfuric acid titanium liquid is filtered with ultra-filtration membrane, obtains titanium liquid 65m3, the mass content 162g/L of titanium dioxide in titanium liquid, solid content 9mg/L.
Embodiment two:
Get acidolysis titanium liquid 100m3, the mass content 125g/L of titanium dioxide in titanium liquid, temperature 58 DEG C, adds 400m3 subsider, and the mass concentration simultaneously adding 7m3 at line mixer is 3 ‰ polyacrylamides, after sedimentation 6h; The sheet frame getting supernatant liquid 250m2 carries out heat filtering, and flow is 40m3/h, first to sheet frame precoating lignocellulose drainage layer before titanium liquid filters; Titanium liquid after heat filtering is carried out vacuum crystallization, and crystallization final temperature controls at 16 DEG C; Titanium liquid after crystallization is carried out disk filtration and remove crystalline sulfuric acid ferrous iron; Removal crystalline sulfuric acid ferrous titanium liquid ultra-filtration membrane is filtered, obtains titanium liquid 65m3, the mass content 163g/L of titanium dioxide in titanium liquid, solid content 9.2mg/L.
Embodiment three:
Get acidolysis titanium liquid 100m3, the mass content 125g/L of titanium dioxide in titanium liquid, temperature 58 DEG C, adds 400m3 subsider, and the mass concentration simultaneously adding 10m3 at line mixer is 5 ‰ polyacrylamides, after sedimentation 10h; The sheet frame getting supernatant liquid 250m2 carries out heat filtering, and flow is 35m3/h, and titanium liquid adds super-cell before filtering in titanium liquid; Titanium liquid after heat filtering is carried out vacuum crystallization, and crystallization final temperature controls at 18 DEG C; Titanium liquid after crystallization is carried out disk filtration and remove crystalline sulfuric acid ferrous iron; Removal crystalline sulfuric acid ferrous titanium liquid ultra-filtration membrane is filtered, obtains titanium liquid 65m3, the mass content 161g/L of titanium dioxide in titanium liquid, solid content 9.1mg/L.
Claims (1)
1. a production method for super-pure titanium sulfate solution, is characterized in that: get acidolysis titanium liquid 100m
3, in titanium liquid, the mass content of titanium dioxide is 125g/L, and temperature 58 DEG C, adds 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, first to sheet frame precoating lignocellulose drainage layer before titanium liquid filters; Titanium liquid after heat filtering is carried out vacuum crystallization, and crystallization final temperature controls at 16 DEG C; Titanium liquid after crystallization is carried out disk filtration and remove crystalline sulfuric acid ferrous iron; Removal crystalline sulfuric acid ferrous titanium liquid ultra-filtration membrane is filtered, obtains titanium liquid 65m
3, in titanium liquid, the mass content of titanium dioxide is 163g/L, solid content 9.2mg/L.
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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 CN103663545A (en) | 2014-03-26 |
| CN103663545B true CN103663545B (en) | 2015-09-16 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN106809883B (en) * | 2015-11-30 | 2018-03-02 | 南京钛白化工有限责任公司 | Sulfate process titanium dioxide produces the device and method of ferrous sulfate |
| CN105439105B (en) * | 2015-12-22 | 2017-10-10 | 江苏久吾高科技股份有限公司 | The integrated processing recovery process of spent acid film and device in a kind of production process of titanium pigment |
| 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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| CN1541944A (en) * | 2003-04-28 | 2004-11-03 | 镇江泛宇钛白粉厂 | Producing method for granular titanium dioxide |
| CN101857269A (en) * | 2010-06-25 | 2010-10-13 | 四川龙蟒钛业股份有限公司 | Method for preparing titanium pigment from novel-process-flow titanium slag and titanium concentrated ore through mixed acidolysis |
| CN101898791A (en) * | 2010-06-25 | 2010-12-01 | 四川龙蟒钛业股份有限公司 | Method for preparing rutile titanium dioxide from new process titanium slag |
| CN102557128A (en) * | 2010-12-07 | 2012-07-11 | 河南佰利联化学股份有限公司 | Novel production process of titanium dioxide powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1541944A (en) * | 2003-04-28 | 2004-11-03 | 镇江泛宇钛白粉厂 | Producing method for granular titanium dioxide |
| CN101857269A (en) * | 2010-06-25 | 2010-10-13 | 四川龙蟒钛业股份有限公司 | Method for preparing titanium pigment from novel-process-flow titanium slag and titanium concentrated ore through mixed acidolysis |
| CN101898791A (en) * | 2010-06-25 | 2010-12-01 | 四川龙蟒钛业股份有限公司 | Method for preparing rutile titanium dioxide from new process titanium slag |
| CN102557128A (en) * | 2010-12-07 | 2012-07-11 | 河南佰利联化学股份有限公司 | Novel production process of titanium dioxide powder |
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