CN106629838A - Method for preventing scaling of controlled filtration equipment in titanium dioxide production process - Google Patents
Method for preventing scaling of controlled filtration equipment in titanium dioxide production process Download PDFInfo
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- CN106629838A CN106629838A CN201610854595.6A CN201610854595A CN106629838A CN 106629838 A CN106629838 A CN 106629838A CN 201610854595 A CN201610854595 A CN 201610854595A CN 106629838 A CN106629838 A CN 106629838A
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- filtrate
- titanium dioxide
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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
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for controlled filtration in titanium dioxide production via sulfuric acid method, in particular to a method for preventing scaling of controlled filtration equipment in titanium dioxide production process; the method comprises the steps of (1) preheating post-crystallization filtrate, obtained by removing iron sulfate heptahydrate crystal via crystallization, to a temperature above extracting temperature of solid matter to be extracted to obtain pre-heated filtrate, wherein the solid matter to be extracted is obtained by acidolysis of ilmenite; (2) performing controlled filtration on the preheated filtrate. The method has the advantages that the problem that a filter plate is blocked due to scaling during controlled filtration can be thoroughly solve; production efficiency of the whole titanium dioxide production process is improved; the method is simple and is easy to popularize.
Description
Technical field
The present invention relates in a kind of sulfate process titanium dioxide powder producing method, especially a kind of sulfuric acid method titanium pigment production process
Control filter method.
Background technology
Titanium dioxide scientific name titanium dioxide (TiO2) there is optimal opacity, optimal whiteness and brightness, it is considered as
It is current performance Chinese white the most excellent in the world.Be widely used in coating, plastics, papermaking, printing-ink, chemical fibre,
The industry such as rubber, ceramics, cosmetics, food and medicine, its main production method is domestic at present by chloridising and sulfuric acid process
Main production is mainly sulfuric acid process.
The technique of Titanium White Production By Sulfuric Acid Process is as follows：
A, acidolysis ilmenite：With ilmenite as raw material, with sulfuric acid solution TiOSO is obtained4With treating for the composition of ferrous sulfate
Leaching solid formation；
B, leaching：After curing, cooling, water extraction is added in solid formation to be leached, separate solid phase impurity, obtain leaching titanium
Liquid；
C, flocculating setting：Add flocculant to be settled toward leaching titanium liquid, remove most of insoluble impurities therein,
Obtain settling clear liquid；
D, except ferrous sulfate heptahydrate：Vacuum crystallization, separation of solid and liquid removing FeSO are carried out to settling clear liquid4·7H2O crystal, obtains
The filtrate to after crystallization；
E, control are filtered：Filtrate is filtered through control and removes insoluble impurities again after the crystallization for obtaining, then it is concentrated after
Pyrohydrolysis, is obtained metatitanic acid；
F, metatitanic acid is washed, removing is bleached and soluble sulphate and is filtered dry, Jing calcined dehydrations desulfurization conversion is two
Titanium oxide；
G, obtain Jing after dry grinding anatase titanium dioxide product or add accelerator to carry out transformation of crystal in calcining obtaining non-coating gold
Red stone-type first product or product.The rutile-type product of higher gears is such as produced, first product pulp, Jing wet-millings depolymerization classification must also be entered
The salinity in material is washed away after row inorganic surface treatment, after being dried ultramicro grinding and organic process are carried out again.
Calcium oxide due to usually containing mass fraction 1.5～2.5% in ilmenite concentrate, the sulphur in the acid hemolysis process of step A
There is chemical reaction in acid, generate calcium sulphate solid with calcium oxide, generally add 2.5 tons of water to carry out leaching operation by ilmenite per ton
(to remove the wherein solid impurity such as calcium sulfate).(the too low then leaching efficiency of dip temperature is low, during leaching for 40～80 DEG C of leaching temperature
Between it is long, leaching temperature is too high, although leaching time is short, but easily cause titanium liquid early stage hydrolyze).Then by the leaching titanium for obtaining
Liquid carries out subsequent treatment.
In order to ensure the whiteness of titanium dioxide product, it is necessary to ensure that the solid content of smart titanium liquid, so as to prevent insoluble solid miscellaneous
Matter causes hydrolysis particle uneven in hydrolytic process, has a strong impact on water washing effect so that metatitanic acid iron content is higher, serious shadow
Ring product quality.Therefore the control filter operation of step E is necessary in above-mentioned technological process, is filter press generally using equipment
Or tubular filter, diatomite, wood powder or perlite carry out drainage, to guarantee that filtrate solid content is less than or equal to 30ppm.In reality
The normal foulings of filter plate Jing in production, cause runner to block；The normal foulings of filter cloth Jing are hardened, and have a strong impact on filter efficiency, are controlled filtered
Scale problems in journey have become a great problem in sulfuric acid method titanium pigment production, seriously hinder the development of this technology.Through
To filter plate, the chemical analysis of filter cloth foulant, its main component is crystal of calcium sulfate.
In order to solve to control in filter process, a difficult problem for filter plant fouling and clogging has part producer to start to control
Filter operation moves forward to the sedimentation clear liquid for before vacuum crystallization operation, i.e., directly obtaining to above-mentioned steps C and is controlled filter operation,
This operation is so-called heat filtering, although the program can be prevented effectively from filter plate fouling, but winter temperature declines, and settle clear liquid
Ferrous crystallization is easily separated out, Severe blockage filter plate even cannot be produced in northern area, therefore actual production the method is still deposited
In larger defect.
The content of the invention
To solve the problems, such as to control filter plant fouling and clogging, the invention provides preventing in a kind of production process of titanium pigment
The method of control filter plant fouling.
The technical solution adopted in the present invention is：The method for preventing from controlling filter plant fouling in production process of titanium pigment,
Comprise the following steps：
(1) filtrate is preheating to acidolysis ilmenite and obtains after the crystallization that will be obtained after removing ferrous sulfate heptahydrate crystal and processing
To solid formation to be leached leaching temperature more than, filtrate after being preheated；
(2) filtration treatment is controlled to filtrate after preheating.
Inventor find, the step of above-mentioned background section in B, due to calcium sulfate in dilution heat of sulfuric acid solubility
Less (＜ 2.0g/l), therefore in leaching process, most of calcium sulfate is drained with sedimentation slag, but still has small part calcium sulfate
Dissolving, the leaching titanium liquid for obtaining is actually the saturated solution of calcium sulfate under the leaching temperature.
After leaching titanium liquid is through settling removal of impurities, the temperature of leaching titanium liquid is reduced using the method for vacuum crystallization or freezing and crystallizing
To 17～25 DEG C, now seven water ferrous irons in system reach saturation, and crystallization is separated out, by conventional solid-liquid separating equipment (as turned
Platform is filtered, centrifugation, sedimentation separation) remove the water ferrous iron of solid seven and obtain the filtration titanium liquid with certain iron titanium ratio.Due to leaching
The solubility for taking calcium sulfate in titanium liquid is minimum, although by crystallization operation, and the temperature of material is reduced to 17～25 DEG C, but due to
Without enough nucleus of crystals, and total calcium sulphate content is less, and in a short time (the usual 40min of crystallizing cycle) hardly has sulphur
Sour calcium crystal is separated out.
But and due to temperature reduction caused by vacuum crystallization institute, therefore filtrate is actually sulphur after the crystallization for finally obtaining
The supersaturated solution of sour calcium.Inventor is experimentally observed, and when filtrate is controlled filter operation after to crystallization, filter plate is complete
Complete and long-time in calcium sulfate supersaturated solution, extremely trickle nucleus of crystal can the progressively larger crystallization of long great achievement, day
The product moon is tired to cause filter plate runner completely plugged, has a strong impact on production efficiency and filter effect.
Therefore the present invention is by more than the leaching temperature of the preheating temperature of filtrate after crystallization to solid formation to be leached, as above institute
State, because the decline of temperature result in the supersaturated solution that filtrate after crystallization is actually calcium sulfate during vacuum crystallization,
And leach the saturated solution that titanium liquid is actually the calcium sulfate.Therefore, after crystallization the temperature of filtrate rise to leaching temperature with
When upper, filtrate becomes the saturated solution or unsaturation solution of calcium sulfate after crystallization so that in filter process, calcium sulphate crystal
Will not separate out.
As a further improvement on the present invention, filtrate after crystallization is preheating into the leaching temperature 1 higher than solid formation to be leached
～5 DEG C.Inventor is found through experiments, in preheating temperature slightly above when the leaching temperature of solid formation is leached, you can almost complete
Avoid controlling the precipitation of filter process calcium sulphate crystal entirely.
As a further improvement on the present invention, the pre-heating mean is indirectly heat, and indirectly heat is compared to directly heating
Energy consumption is lower, and faster, heating effect is evenly for the rate of heat addition.More preferably, the pre-heating mean is to be added indirectly using steam pipe coil
Heat.
The invention has the beneficial effects as follows：1) the filter plate fouling and clogging in control filter process can thoroughly be solved the problems, such as；2)
Improve the production efficiency of whole titanium white production technique；3) process is simple, it is easy to promote.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment one：
Control filter plant plate and frame filter press one, 220 square metres of filter area (filter plate specification 1.5m × 1.5m) is added
Filtrate (20 DEG C) carries out beating cloth after diatomite 500kg and 10 sides crystallize except iron, and filtrate is using steaming after then crystallizing except iron
To 77 DEG C, filtrate (77 DEG C) is controlled filtration to vapour coil pipe indirect preheating after preheating is crystallized except iron, it is ensured that the titanium Jing after control is filtered
Fluid solid content is less than or equal to 30ppm, when Entirety type pressure filter pressure reaches 0.4MPa, that is, changes drainage layer, and so on uses, and filters
Cloth was changed once per 15 days, and a filter plate was taken every 10 days, and thorough cleaning foulant is simultaneously weighed, continuously 12 months (this realities of operation
Apply solid formation to be leached in example and add water leaching temperature for 75 DEG C).
Comparative example one：
Control filter plant plate and frame filter press one, 220 square metres of filter area (filter plate specification 1.5m × 1.5m) is added
Filtrate (20 DEG C) carries out beating cloth after diatomite 500kg and 10 sides crystallize except iron, then enters except filtrate (20 DEG C) after iron crystallization
It is controlled filtration, it is ensured that titanium fluid solid content is less than or equal to 30ppm Jing after control is filtered, when Entirety type pressure filter pressure reaches
0.4MPa, that is, change drainage layer, and so on uses, and filter cloth was changed once per 15 days, and a filter plate was taken every 10 days, thoroughly clear
Reason foulant is simultaneously weighed, continuous operation 12 months (solid formation to be leached adds water leaching temperature for 75 DEG C in this comparative example).
Comparative example two：
Control filter plant plate and frame filter press one, 220 square metres of filter area (filter plate specification 1.5m × 1.5m) is added
Filtrate (20 DEG C) carries out beating cloth after diatomite 500kg and 10 sides crystallize except iron, and filtrate is using steaming after then crystallizing except iron
To 70 DEG C, filtrate (70 DEG C) is controlled filtration to vapour coil pipe indirect preheating after preheating is crystallized except iron, it is ensured that the titanium Jing after control is filtered
Fluid solid content is less than or equal to 30ppm, when Entirety type pressure filter pressure reaches 0.4MPa, that is, changes drainage layer, and so on uses, and filters
Cloth was changed once per 15 days, and a filter plate was taken every 10 days, and thorough cleaning foulant is simultaneously weighed, and (this is right within 12 months for continuous operation
Solid formation to be leached adds water leaching temperature for 75 DEG C in ratio).
Testing result is shown in Table one to be detected to the filter plate fouling condition of embodiment one, comparative example one, comparative example two.
Table one：Individual filter plate foulant is weighed situation (unit：Gram)
Claims (4)
1. the method for preventing from controlling filter plant fouling in production process of titanium pigment, it is characterised in that comprise the following steps：
(1) filtrate is preheating to what acidolysis ilmenite was obtained after the crystallization that will be obtained after removing ferrous sulfate heptahydrate crystal and processing
It is more than the leaching temperature of solid formation to be leached, filtrate after being preheated；
(2) filtration treatment is controlled to filtrate after preheating.
2. it is according to claim 1 prevent control filter plant fouling method, it is characterised in that：Filtrate is pre- after crystallizing
Heat is to 1～5 DEG C of the leaching temperature higher than solid formation to be leached.
3. it is according to claim 1 and 2 prevent control filter plant fouling method, it is characterised in that：The preheating side
Method is indirectly heat.
4. it is according to claim 3 prevent control filter plant fouling method, it is characterised in that：The pre-heating mean is
Using steam pipe coil indirectly heat.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610854595.6A CN106629838A (en) | 2016-09-27 | 2016-09-27 | Method for preventing scaling of controlled filtration equipment in titanium dioxide production process |
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| CN201610854595.6A CN106629838A (en) | 2016-09-27 | 2016-09-27 | Method for preventing scaling of controlled filtration equipment in titanium dioxide production process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109225148A (en) * | 2018-10-08 | 2019-01-18 | 济南裕兴化工有限责任公司 | It is a kind of improve washing efficiency filter aid and its application |
| CN112390286A (en) * | 2020-11-20 | 2021-02-23 | 中国有色集团（广西）平桂飞碟股份有限公司 | Fine filtration pretreatment process for titanium liquid produced by sulfuric acid method titanium dioxide |
| CN112619286A (en) * | 2020-12-17 | 2021-04-09 | 襄阳龙蟒钛业有限公司 | Method for purifying and crystallizing titanium dioxide solution |
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| CN101157447A (en) * | 2007-09-12 | 2008-04-09 | 合肥泰诺化工科技有限公司 | Method for removing ferrous and other metal salt from titanium white waste acid |
| CN202724794U (en) * | 2012-07-27 | 2013-02-13 | 富民龙腾钛业有限责任公司 | Filtering device applied to titanium dioxide hydrolysis |
| CN105152271A (en) * | 2015-07-31 | 2015-12-16 | 上海安赐机械设备有限公司 | Titanium dioxide white water reuse process and system thereof |
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| CN101157447A (en) * | 2007-09-12 | 2008-04-09 | 合肥泰诺化工科技有限公司 | Method for removing ferrous and other metal salt from titanium white waste acid |
| CN202724794U (en) * | 2012-07-27 | 2013-02-13 | 富民龙腾钛业有限责任公司 | Filtering device applied to titanium dioxide hydrolysis |
| CN105152271A (en) * | 2015-07-31 | 2015-12-16 | 上海安赐机械设备有限公司 | Titanium dioxide white water reuse process and system thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109225148A (en) * | 2018-10-08 | 2019-01-18 | 济南裕兴化工有限责任公司 | It is a kind of improve washing efficiency filter aid and its application |
| CN112390286A (en) * | 2020-11-20 | 2021-02-23 | 中国有色集团（广西）平桂飞碟股份有限公司 | Fine filtration pretreatment process for titanium liquid produced by sulfuric acid method titanium dioxide |
| CN112390286B (en) * | 2020-11-20 | 2023-03-14 | 中国有色集团（广西）平桂飞碟股份有限公司 | Fine filtration pretreatment process for titanium liquid produced by sulfate process titanium dioxide |
| CN112619286A (en) * | 2020-12-17 | 2021-04-09 | 襄阳龙蟒钛业有限公司 | Method for purifying and crystallizing titanium dioxide solution |
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Application publication date: 20170510 |