CN104477988B - The recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor in sulfate process titanium dioxide production - Google Patents
The recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor in sulfate process titanium dioxide production Download PDFInfo
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- CN104477988B CN104477988B CN201410836256.6A CN201410836256A CN104477988B CN 104477988 B CN104477988 B CN 104477988B CN 201410836256 A CN201410836256 A CN 201410836256A CN 104477988 B CN104477988 B CN 104477988B
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- mother liquor
- centrifuge mother
- acid solution
- sulfuric acid
- 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
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The present invention discloses the recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor during a kind of sulfate process titanium dioxide produces, including adding the sulfuric acid solution that mass percent is 20 25% in centrifuge mother liquor, the centrifuge mother liquor adding sulfuric acid solution is used for the step of acidolysis leaching, by adding sulfuric acid solution in centrifuge mother liquor, and control the concentration of sulfuric acid solution, the volume ratio of temperature and centrifuge mother liquor and sulfuric acid solution, solve the problem that centrifuge mother liquor uses process blocking feed-line, and the problem that Hydrolysis product quality in early days occurs in storing transport process, raising system titanium dioxide yield and quality thereof.
Description
Technical field
The present invention relates to sulfate process titanium dioxide resources of production field of comprehensive utilization, be specifically related to a kind of sulfate process titanium dioxide and produce
The recoverying and utilizing method of middle ferrous sulfate heptahydrate centrifuge mother liquor.
Background technology
Sulfate process titanium dioxide need to use vacuum crystallization to titanium liquid except ferrum processes for the satisfied prescription hydrolyzed in producing
Mode makes the ferrum in titanium liquid remove with the form fractionation of ferrous sulfate heptahydrate crystal, simultaneously for guarantee system titanium dioxide
Ferrous sulfate heptahydrate crystal need to be washed by titanium yield, separates further in ferrous iron through centrifuge again and press from both sides after washing
The titanium liquid of band, it is 110 that ferrous sulfate heptahydrate can obtain ferrous sulfate concentration after centrifuge separates
140g/L, the diluted Ti solution of titanium dioxide concentration 40 80g/L.
Prior art is that centrifuge mother liquor is collected mother solution collecting tank, then by being pumped into the material after vacuum crystallization
Stock tank carries out after mixing ferrous sulfate heptahydrate filtration again, or soaks for acidolysis by being pumped into hydrolysis procedure
Taking, owing to this centrifuge mother liquor titanium dioxide concentration is on the low side, the stability of mother solution is 150 200, sulphuric acid in diluted Ti solution
Ferrous iron has been in hypersaturated state, the ferrous sulfate with the presence of 30% with fine ferrous sulfate heptahydrate crystal form, because of
Shortcoming of both the existence of this prior art is following, one is that centrifuge mother liquor precipitation during storing, transporting is a large amount of
Ferrous sulfate crystal, block feed-line, have a strong impact on production stable；Two is centrifuge mother liquor poor stability, returns
Return titanium liquid in systematic procedure and hydrolysis in early days occurs, product quality is caused serious harm.
Summary of the invention
In view of this, the recovery profit of ferrous sulfate heptahydrate centrifuge mother liquor during the application provides a kind of sulfate process titanium dioxide to produce
By method, solve centrifuge mother liquor and use the problem of process blocking feed-line, and send out in storing transport process
The problem of raw Hydrolysis product quality in early days, improves system titanium dioxide yield and quality thereof.
For solving above technical problem, the technical scheme that the present invention provides is seven water sulfur during a kind of sulfate process titanium dioxide produces
The recoverying and utilizing method of the ferrous centrifuge mother liquor of acid, is 20 25% including adding mass percent in centrifuge mother liquor
Sulfuric acid solution, by add sulfuric acid solution centrifuge mother liquor be used for acidolysis leaching step.
Preferably, the temperature of described sulfuric acid solution is 38 42 DEG C.
Use hot acid liquid dissolved dilution centrifuge mother liquor so that in centrifuge mother liquor, ferrous sulfate heptahydrate all dissolves, solution
Return to undersaturated condition, prevent mother solution from producing ferrous sulfate heptahydrate crystal, in storage, course of conveying, prevent pipe
The blockage problem in road.
Preferably, described centrifuge mother liquor is 1:2.0 3.0 with the volume ratio of sulfuric acid solution, learns through experiment, from
Heart mother solution generation amount is 50m3, in mother solution, the content of ferrous sulfate is 110 140g/L, titanium dioxide concentration 40
80g/L, temperature is 20 22 DEG C, and the addition of sulfuric acid solution is 125 150m3, under this volume ratio,
Ferrous sulfate heptahydrate in mother solution all dissolves, and solution returns to undersaturated condition, and the stability of mother solution can improve to 350
Above.
Being more highly preferred to, described centrifuge mother liquor is 1:2.5 3.0 with the volume ratio of sulfuric acid solution.
Preferably, described sulfuric acid solution is the acid solution produced in washing step in sulfate process titanium dioxide production process, uses
The acid solution produced in washing step, on the one hand can recycle the acid solution of this operation, on the other hand, be answered
For diluting centrifuge mother liquor, make acidity in mother solution increase, improve the stability of mother solution.
Preferably, the centrifuge mother liquor temperature after described addition sulfuric acid solution controls at 30 35 DEG C, and strict control is centrifuged
Mother solution temperature, makes ferrous sulfate heptahydrate in mother solution all dissolve.
Compared with prior art, its detailed description is as follows for the application: add 38 42 DEG C in centrifuge mother liquor, quality hundred
Proportion by subtraction is the sulfuric acid solution of 20 25%, and the centrifuge mother liquor having added sulfuric acid solution is used further to acidolysis leaching, solves
Centrifuge mother liquor uses the problem of process blocking feed-line, has recycled centrifuge mother liquor simultaneously, has improve system dioxy
Change titanium yield, the acid solution of generation in washing step during sulfuric acid solution uses sulfate process titanium dioxide production process simultaneously, on the one hand
The acid solution of this operation can be recycled, on the other hand, be applied to dilute centrifuge mother liquor, make acidity in mother solution
Increase, improve the stability of mother solution, additionally, be used for diluting centrifuge mother liquor by sulfuric acid solution, the acid in mother solution can be improved
Degree, brings up to more than 350 by the stability of mother solution, solves mother solution and hydrolysis shadow in early days occurs in storing transport process
The problem ringing product quality, improves product quality.
Detailed description of the invention
In order to make those skilled in the art be more fully understood that technical scheme, below in conjunction with specific embodiment
The present invention is described in further detail.
Embodiment one
The recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor in the production of a kind of sulfate process titanium dioxide, including to centrifugal mother
Liquid adds the sulfuric acid solution that mass percent is 20 25%, the centrifuge mother liquor adding sulfuric acid solution is used for acidolysis
The step of leaching.
Centrifuge mother liquor is collected mother solution collecting tank, in mother solution collecting tank, adds the sulphuric acid that temperature is 38 42 DEG C molten
Liquid, centrifuge mother liquor is 1:2.5 with the volume ratio of sulfuric acid solution, and its sulfuric acid solution uses sulfate process titanium dioxide production process
The acid solution produced in middle washing step.In centrifuge mother liquor, the content of ferrous sulfate is 135g/L, titanium dioxide concentration
45g/L, temperature is 21 DEG C, and after adding sulfuric acid solution, mixeding liquid temperature is about 35 DEG C, and now seven water sulphuric acid are sub-
Ferrum crystal all dissolves, and solution returns to undersaturated condition, prevents the blocking of pipeline to ask in storage, course of conveying
Topic, acidity increases so that the stability of mother solution improves to more than 350, it is ensured that stablizing of quality.
In sulfate process titanium dioxide production process, centrifuge mother liquor generation every day amount is 50m3, molten with sulphuric acid with centrifuge mother liquor
The volume ratio of liquid is that 1:2.5 calculates, and the addition of sulfuric acid solution is 125m3, therefore technical scheme one
Aspect solves centrifuge mother liquor and uses the problem of process blocking feed-line, and due to mother in storing transport process
Liquid poor stability, the problem that Hydrolysis product quality in early days occurs, improve system titanium dioxide yield and quality thereof,
On the other hand resource-effective purpose in production process is achieved.
Parameters index in the present embodiment production process is listed in table 1.
Table 1 embodiment one parameters index
From data above it is known that the temperature of centrifuge mother liquor is 21 DEG C, ferrous sulfate content is 135g/L, mother solution
Being in saturation, the ferrous sulfate part in solution, presented in ferrous sulfate heptahydrate crystal, is easily formed pipe
Road blocks, and after adding the sulfuric acid solution of 41.1 DEG C, the temperature of mixed liquor rises to 35.0 DEG C, and solution returns to insatiable hunger
And state, solve line clogging problem；Further it can be seen that centrifuge mother liquor is before adding sulfuric acid solution, female
Liquid stability is 150, and its stability is the best, easily causes the titanium dioxide quality finally produced unstable, and adds
After entering sulfuric acid solution, along with the raising of acidity, stability of solution increases to 350, it is ensured that the stability of quality.
Below it is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred implementation is not construed as
Limitation of the present invention, protection scope of the present invention should be as the criterion with claim limited range.For this skill
For the those of ordinary skill in art field, without departing from the spirit and scope of the present invention, it is also possible to make some changing
Entering and retouch, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (3)
1. the recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor during a sulfate process titanium dioxide produces, it is characterised in that:
Including in centrifuge mother liquor add mass percent be 20～the sulfuric acid solution of 25%, will add sulfuric acid solution centrifugal mother
Liquid is for the step of acidolysis leaching；Described centrifuge mother liquor is that ferrous sulfate heptahydrate obtains after centrifuge separates
Ferrous sulfate concentration is 110～140g/L, the diluted Ti solution of titanium dioxide concentration 40～80g/L；Described sulfuric acid solution
Temperature is 38～42 DEG C；Described centrifuge mother liquor is 1:2.0～3.0 with the volume ratio of sulfuric acid solution；Described addition sulphuric acid
Centrifuge mother liquor temperature after solution controls at 30～35 DEG C.
A kind of recoverying and utilizing method the most according to claim 1, it is characterised in that: described centrifuge mother liquor and sulphuric acid
The volume ratio of solution is 1:2.5～3.0.
A kind of recoverying and utilizing method the most according to claim 1, it is characterised in that: described sulfuric acid solution is sulphuric acid
The acid solution produced in washing step during method Producing Titanium Dioxide.
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| CN201410836256.6A CN104477988B (en) | 2014-12-26 | 2014-12-26 | The recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor in sulfate process titanium dioxide production |
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| CN201410836256.6A CN104477988B (en) | 2014-12-26 | 2014-12-26 | The recoverying and utilizing method of ferrous sulfate heptahydrate centrifuge mother liquor in sulfate process titanium dioxide production |
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| CN105110366B (en) * | 2015-07-20 | 2016-08-17 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method and apparatus of Production By Sulfuric Acid Process titanium white |
| CN105237425B (en) * | 2015-11-12 | 2017-12-01 | 中南大学 | Mother liquor pretreatment and circulation utilization method in a kind of chain type complex of ferrous glycine synthesis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0659687A1 (en) * | 1993-12-24 | 1995-06-28 | Bayer Ag | Process for the preparation of titanium dioxide |
| CN102556981A (en) * | 2010-12-24 | 2012-07-11 | 漯河市兴茂钛业有限公司 | Comprehensive utilization method for solid wastes and waste acid in production process of titanium dioxide |
| CN103708566A (en) * | 2013-12-26 | 2014-04-09 | 攀枝花东方钛业有限公司 | Method for improving filtering performance of ferrous sulfate |
-
2014
- 2014-12-26 CN CN201410836256.6A patent/CN104477988B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0659687A1 (en) * | 1993-12-24 | 1995-06-28 | Bayer Ag | Process for the preparation of titanium dioxide |
| CN102556981A (en) * | 2010-12-24 | 2012-07-11 | 漯河市兴茂钛业有限公司 | Comprehensive utilization method for solid wastes and waste acid in production process of titanium dioxide |
| CN103708566A (en) * | 2013-12-26 | 2014-04-09 | 攀枝花东方钛业有限公司 | Method for improving filtering performance of ferrous sulfate |
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