CN108636980A - A kind of technique of zero discharge of processing titanium chloride slag - Google Patents
A kind of technique of zero discharge of processing titanium chloride slag Download PDFInfo
- Publication number
- CN108636980A CN108636980A CN201810364367.XA CN201810364367A CN108636980A CN 108636980 A CN108636980 A CN 108636980A CN 201810364367 A CN201810364367 A CN 201810364367A CN 108636980 A CN108636980 A CN 108636980A
- Authority
- CN
- China
- Prior art keywords
- membrane
- technique
- titanium chloride
- solid
- dope
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/206—Manganese or manganese compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Abstract
The invention belongs to titanium white flour flow design fields, specifically disclose a kind of technique of zero discharge of processing titanium chloride slag, which includes the following steps:(1) alkali soaks;(2) it is separated by solid-liquid separation;(3) secondary precipitation;(4) micro-filtration/ultrafiltration membrance filter;(5) film purifications;(6) film concentrates;(7) secondary film purification;In present invention process for the purpose of handling the heavy metal ion impurities in titanium chloride slag and recycling chlorion, it converts solid slag to harmless solid and is back to construction material brick and tile, cement etc., it is again that chlorine industry is used with light salt brine by barrier separation integral process thickening-purification technology, pass through the implementation of this technique, the valuable resource in titanium chloride slag is not only recycled, it has more importantly handled for a full due to the serious titanium chloride slag of environmental pollution, breach the intractable bottleneck of chloridising solid slag, so that chloridising production titanium dioxide technique has strided forward essential step towards more environmentally friendly direction, with apparent advance.
Description
Technical field
The invention belongs to Titanium Dioxide Produced by Chloride Procedure chemical fields, and in particular to a kind of technique of zero discharge of titanium chloride slag processing.
Background technology
Currently, the method for production titanium dioxide mainly has sulfuric acid process and chloridising.Due to the long flow path of sulfuric acid process, pollution is tight
Weight, poor product quality and be gradually chlorinated method substitution.
In current Titanium Dioxide Produced by Chloride Procedure production, main flow is:
A, (such as by titanium material:High titanium slag) and reducing agent is (such as:Petroleum coke) it is sent into chlorination furnace after evenly mixing, it is passed through chlorine
Gas carries out fluidizing chlorination at a temperature of 800 DEG C~1000 DEG C;
B, separating-purifying is carried out to the crude titanium tetrachloride obtained after chlorination and removes the impurity such as magnesium, iron, silicon and vanadium, obtain essence
Titanium tetrachloride processed;
C, refining titanic chloride liquid obtained carries out pre- thermal evaporation and is converted into gas phase, and is preheated to 300 DEG C~500 DEG C;
And a small amount of compound modifying agent simultaneously is added (such as in gas phase titanium tetrachloride:Alchlor) be mixed into oxidation furnace with it is pre-
Heat to 1300 DEG C or more of oxygen mixes rapidly in oxidation furnace, at a temperature of 1300 DEG C~1800 DEG C, less than 0.1 second in carry out oxygen
Change reaction and generates solid phase titanium dioxide;
D, and then titanium dioxide solids powder is removed into reaction zone rapidly and reaction heat is made to remove rapidly;
E, chlorine obtained by the reaction in oxidation furnace is separated into return chlorination furnace through filter, synchronization is collected through filter
Titanium dioxide granule powder and be beaten into liquid, send postprocessing working procedures that rutile type titanium white finished product is made.
In Titanium Dioxide Produced by Chloride Procedure production process, a large amount of dust-slag collection is generated in chlorination workshop section cyclone separator bottom.According to report
Road, 0.2 ton or so solid slag will be generated by often producing 1t titanium tetrachlorides, these solid slags are mainly the metal produced by chlorination reaction
Chloride, and the high titanium slag and petroleum coke that the reaction was complete form, and main component not only contains KCl, NaCl, MgCl2、
CaCl2Deng being also enriched the salt of various metals impurity (aluminium, iron, titanium, cobalt, chromium, manganese, arsenic, vanadium), these salts are most of to exist
Exist in a chloride-form under high temperature, aluminium and silicon are outer with oxide presence, and unreacted carbon exists with simple substance form.If waste residue
It is directly deposited in without processing outdoor, wherein a large amount of chloride will be caused to meet water dissolution, environment is caused seriously to pollute.
Processing for titanium chloride slag still has no better method in foreign data other than using deep-well landfill.It is domestic
After enterprise mostly uses greatly water flushing, in lime and formation lime slag solidification send cinder field to stack or fill, and there is presently no to this slag
Carry out the effective ways of harmless treatment or recycling.
CN106044799 discloses a kind of titanium chloride slag and its processing method of filtrate, is exactly to use alkali neutralization titanium chloride slag
And wash, after heavy metal ion neutralization precipitation, chlorion is recycled in a manner of sodium chloride in chlorine industry salt dissolving water
In.Titanium Dioxide Produced by Chloride Procedure technique and chloralkali process are combined by the technique, have not only recycled a large amount of chlorion, but also processing is sunk
It has formed sediment heavy metal ion, technics comparing is advanced.But there are two problems:First, producing a large amount of slag, pressure-filtering process after acid is molten
Middle filter effect due to adhesiveness is too strong, fine and close is bad, or even occurs pressing the problem of not being discharged;Second is that using alkali by first-time filtrate
PH directly neutralize filtered to 12 or more, under the conditions of such high alkalinity, the amphiprotic substances such as aluminium, silicon can be dissolved in lye, be waited for
With the retention of NF membrane, concentration can be higher and higher and hydrolytic precipitation occurs on film surface, influences being smoothed out for membrane process, and
And the high result of aluminium, silicon concentration will cause aluminium, silicone content in nanofiltration clear liquid high in nanofiltration charging, and chloralkali process is not achieved
The requirement of salt dissolving light salt brine.
Application number 201710555832.3 discloses washery slag acid waste water zero-emission in a kind of Titanium Dioxide Produced by Chloride Procedure production process
Put technique.After the patent is by adding alkali neutralization to filter titanium chloride slag acid waste water, by reverse osmosis concentration, then in nanofiltration point
It leaves away and removes polyvalent metal ion, obtain the brine that salt content is 12%, be used for electrolytic caustic soda.The process employs a upper patents
Thinking, but the technique for using first reverse osmosis concentration NF membrane desalination again, it appears that more advanced.But it goes over, there are still
Following problem:First, remaining substantial portion of foreign ion after neutralization precipitation, the pH=6.5 of the neutralization precipitation of the technique~
7, although precipitating the impurity such as most Al, Si, Fe, the precipitation of the polyvalent metal ions such as Zn, Mn, Cu, Ni, Ba, Sr is also not
Completely, still there is significant component of foreign ion to remain in mixed liquor, can cause reverse osmosis concentration degree limited in this way.Second is that
The concentration brine strength of reverse osmosis membrane is not achieved 12%, due to neutralization precipitation pH the problem of, cause reverse osmosis membrane intake in still
With the presence of quite a few foreign ion, although there is the retention of ultrafiltration membrane before reverse osmosis membrane, ultrafiltration membrane is to the ion in solution
Do not play crown_interception, thus polyvalent metal ion concentration does not reduce in reverse osmosis membrane water inlet, with the progress of concentration, impurity from
Sub- concentration constantly increases, and the carbonate and sulfate ion of concentration height form precipitation and film surface are precipitated together in meeting and solution,
Being normally carried out for membrane process is influenced, causes the salinity of concentration that 12% concentration is not achieved at all.Third, the problem of membrane process, one
The reverse osmosis operating pressure of person is 0.6~1MPa, and so low pressure can not offset the infiltration that 12% salinity generates at all
Pressure, let alone concentration water outlet, the two be it is reverse osmosis after nanofiltration, nanofiltration process how much to reduce nanofiltration water outlet salinity,
Even and if it is reverse osmosis after dope salinity reach 12%, be centainly less than 12% by salinity after nanofiltration.
Invention content
The problem of technical solution of present invention process is aiming at above-mentioned technique and the improvement project proposed, first
Polyvalent metal ion concentration in waste water is further decreased by secondary precipitation, secondly before concentration again with NF membrane to waste water
In polyvalent metal ion retained, with ensure concentration water inlet in polyvalent metal ion concentration it is very low, concentration can reach
Or the concentration more than 12% greatly reduces concentrated third, using pH=3~6.5 that hydrochloric acid adjusts water inlet before film concentration
The risk of precipitated crystal in journey.
Purpose to realize the present invention, the present invention adopt the following technical scheme that:
A kind of technique of zero discharge of processing titanium chloride slag, includes the following steps:
(1) alkali soaks:Titanium chloride slag sodium hydroxide lye is leached into wherein chlorion, and precipitate heavy metal therein from
Son, while pH is adjusted 5.5~6.5, form slurry;
(2) it is separated by solid-liquid separation:Slurry is separated by solid-liquid separation, filter residue and filtrate are obtained;Filter residue can be used as making construction material
Such as the raw material reuse of cement, brick and tile;
(3) secondary precipitation:PH is adjusted to exist jointly to being separated by solid-liquid separation the filtrate sodium carbonate come out and sodium hydroxide in step (2)
9~10, further precipitation removal heavy metal ion therein, forms secondary slurry;
(4) micro-filtration/ultrafiltration membrance filter:Micro-filtration/ultrafiltration membrance filter, underflow is used to return to the secondary slurry in step (3)
In step (1), clear liquid then uses hydrochloric acid tune pH to be used for next procedure after 3~6.5;
(5) film purifications:First time removal filtration is carried out to sour Filtrate in step (4) using a NF membrane
A NF membrane dope and clear liquid are obtained, nanofiltration dope returns to step (1);
(6) film concentrates:Nanofiltration clear liquid in step (5) is concentrated with reverse osmosis or electrodialysis, obtains dope and clear liquid,
Counter-infiltration clear liquid returns to step (1);
(7) secondary film purification:Cleaned again to counter-infiltration dope with NF membrane, obtain secondary NF membrane dope and
Clear liquid, nanofiltration clear liquid can be that salt dissolving water is used, and nanofiltration dope then returns to step (1).
In above-mentioned technique, in step 2 solid-liquid separation process using filtering, centrifugation, gravity or one kind in inclined plate sedimentation or
Several solid-liquid separation means combinations.
Film used is micro-filtration/ultrafiltration membrane in step 4, material can be the inorganics such as ceramics, metal or PES,
PVDF, PS, PP, PTFE organic material, aperture are 2nm~1.5um.
In step 5 and 7, NF membrane used is 96% or more to MgSO4 rejections at 0.75MPa and room temperature.
In step 6, concentration film used is reverse osmosis membrane or electrodialytic membranes, and reverse osmosis membrane is right at 1.5MPa and room temperature
NaCl rejections are 98% or more.
Advantageous effect
In this patent technique for the purpose of handling the heavy metal ion impurities in titanium chloride slag and recycling chlorion, by solid
Waste residue is converted into harmless solid and is back to construction material brick and tile, cement etc., then is by barrier separation integral process thickening-purification technology
Chlorine industry is used with light salt brine, by the implementation of this technique, has not only recycled the valuable resource in titanium chloride slag, heavier
What is wanted has been handled for a full due to the serious titanium chloride slag of environmental pollution, and the intractable bottle of chloridising solid slag is breached
Neck so that chloridising production titanium dioxide technique has strided forward essential step towards more environmentally friendly direction, has apparent advance, with
The above two patents technique, which is compared, has following superiority:
(1) process modification of secondary precipitation, significantly in titanium chloride slag waste water polyvalent metal ion concentration, barium ions
0.545mg/L is dropped to from 2.862mg/L, manganese ion drops to 0.068mg/L from 36.38mg/L, and calcium ion is dropped to from 114mg/L
28.56mg/L, magnesium ion drop to 31.15mg/L from 53.81mg/L, and strontium ion drops to 0.373mg/L from 0.773mg/L;
(2) it is reduced by the pH of the water inlet before the purification and concentration of a NF membrane, substantially increasing concentration film can concentrate
Concentration, highest can concentrate 10 times or more, and the concentration of brine can reach 122g/L, and the brine rate of recovery is 90% or more, film concentration
Process is stablized, and fouling deposited phenomenon does not occur.
(3) due to the improvement of concentration technology (including electrodialytic use when necessary), the raising of brine strength in concentrate,
So that after final secondary NF membrane purification, the salinity of nanofiltration water outlet has still reached between 90~115g/L.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is described in further detail.It should be appreciated that described herein, specific examples are only used to explain the present invention, does not limit
In the present invention.
Following embodiment is operated according to process flow chart as shown in the figure:
Embodiment 1
Alkali soaks:60kg titanium chloride slags are leached with sodium hydroxide lye, while adjusting pH=6, control solid-to-liquid ratio is 1:15
(weight ratio) is stirred to react 10h, is formed and neutralize slurry;Solid-liquid point is carried out using plate and frame filter press or centrifuge to neutralizing slurry
From, solid filter residue is obtained, filtrate enters secondary precipitation technique, and the content for neutralizing sodium chloride in filtrate at this time is 5361mg/L,
Volume is 850L, and impurity A l, Si content is respectively 0.146mg/L, 0.404mg/L;
Secondary precipitation:PH is adjusted jointly with sodium carbonate and sodium hydroxide to neutralizing the clear liquid that slurry ceramic membrane is separated by solid-liquid separation out
=10, secondary slurry is formed after being stirred to react 1h, with the secondary slurry of ceramic membrane filter, it is 3% to control the solid content in dope, dense
Liquid returns to alkali soaking technology and enters UF membrane process after ceramic membrane clear liquid adjusts pH=4 with hydrochloric acid;
Membrane separation process:Filtrate first uses a nanofiltration to filter after exchanging acid, and it is 2.5 to control a NF membrane operating pressure
~3.5MPa obtains a NF membrane dope 165L and clear liquid 585L;NF membrane clear liquid directly uses reverse osmosis concentration, waits for anti-
When salt content in infiltration dope reaches 12.2%, dope 30L is obtained;Counter-infiltration clear liquid is used as in alkali leaching process, counter-infiltration dope
Enter in secondary nanofiltration technique, control secondary nanofiltration operating pressure be 2.5~3MPa, obtain secondary NF membrane dope 7.5L and
Clear liquid 22.5L, salt content is 10.37% at this time, and impurity content Al, Si content is respectively 0.1mg/L and 0.138mg/L, whole
Do not occur that concentrate is muddy in a membrane process and crystalline deposit phenomenon.
Embodiment 2
Alkali soaks:60kg titanium chloride slags are leached with sodium hydroxide lye, while adjusting pH=6.5, control solid-to-liquid ratio is 1:
10 (weight ratios) are stirred to react 10h, are formed and neutralize slurry;It is combined using plate and frame filter press and ceramic membrane to neutralizing slurry
It is separated by solid-liquid separation, obtains solid filter residue, filtrate enters secondary precipitation technique, and the content for neutralizing sodium chloride in filtrate at this time is
8041mg/L, volume 500L, impurity A l, Si content are respectively 0.163mg/L, 0.507mg/L;
Secondary precipitation:PH is adjusted jointly with sodium carbonate and sodium hydroxide to neutralizing the clear liquid that slurry ceramic membrane is separated by solid-liquid separation out
=9.5, secondary slurry is formed after being stirred to react 2h, with the secondary slurry of ceramic membrane filter, it is 2% to control the solid content in dope,
Dope returns to alkali soaking technology and enters UF membrane process after ceramic membrane clear liquid adjusts pH=4.5 with hydrochloric acid;
Membrane separation process:Filtrate first uses a nanofiltration to filter after exchanging acid, and it is 2.5 to control a NF membrane operating pressure
~3.5MPa obtains a NF membrane dope 110L and clear liquid 440L;NF membrane clear liquid directly uses reverse osmosis concentration, waits for anti-
When salt content in infiltration dope reaches 11.5%, dope 30L is obtained;Counter-infiltration clear liquid is used as in alkali leaching process, counter-infiltration dope
It enters in secondary nanofiltration technique, it is 2.5~3MPa to control secondary nanofiltration operating pressure, obtains secondary NF membrane dope 6L and clear
Liquid 24L, salt content is 9.8% at this time, and impurity content Al, Si content is respectively 0.105mg/L and 0.23mg/L, entire film mistake
Do not occur that concentrate is muddy in journey and crystalline deposit phenomenon.
Embodiment 3
Alkali soaks:60kg titanium chloride slags are leached with sodium hydroxide lye, while adjusting pH=5.5, control solid-to-liquid ratio is 1:
12 (weight ratios) are stirred to react 10h, are formed and neutralize slurry;It is separated by solid-liquid separation using centrifuge to neutralizing slurry, obtains solid
Filter residue, filtrate enter secondary precipitation technique, at this time neutralize filtrate in sodium chloride content be 6701mg/L, volume 700L,
Impurity A l, Si content is respectively 0.12mg/L, 0.38mg/L;
Secondary precipitation:PH is adjusted jointly with sodium carbonate and sodium hydroxide to neutralizing the clear liquid that slurry ceramic membrane is separated by solid-liquid separation out
=9.5, secondary slurry is formed after being stirred to react 1h, with the secondary slurry of ceramic membrane filter, the solid content controlled in dope is
2.5%, dope returns to alkali soaking technology and enters UF membrane process after ceramic membrane clear liquid adjusts pH=5 with hydrochloric acid;
Membrane separation process:Filtrate first uses a nanofiltration to filter after exchanging acid, and it is 2.5 to control a NF membrane operating pressure
~3.5MPa obtains a NF membrane dope 140L and clear liquid 560L;NF membrane clear liquid is first contained with the reverse osmosis concentrated salt that is reduced to
After amount is 5%, then concentrates counter-infiltration dope with electrodialysis and obtain dope when the salt content in electrodialysis dope reaches 15%
25L;Reverse osmosis and electrodialysis clear liquid is used as in alkali leaching process, and electrodialysis dope enters in secondary nanofiltration technique, and control is secondary
Nanofiltration operating pressure is 2.5~3MPa, obtains secondary NF membrane dope 5L and clear liquid 20L, and salt content is 12% at this time, and impurity contains
Amount is that Al, Si content are respectively 0.093mg/L and 0.12mg/L, does not occur concentrate muddiness in entire membrane process and crystallizes and sink
Shallow lake phenomenon.
Claims (6)
1. a kind of technique of zero discharge of processing titanium chloride slag, it is characterised in that:Include the following steps:
(1) alkali soaks:Titanium chloride slag sodium hydroxide lye is leached into wherein chlorion, and precipitates heavy metal ion therein, together
When adjust pH 5.5~6.5, form slurry;
(2) it is separated by solid-liquid separation:Slurry is separated by solid-liquid separation, filter residue and filtrate are obtained;
(3) secondary precipitation:To be separated by solid-liquid separation filtrate sodium carbonate out in step (2) and sodium hydroxide adjust jointly pH 9~
10, further precipitation removal heavy metal ion therein, forms secondary slurry;
(4) micro-filtration/ultrafiltration membrance filter:Micro-filtration/ultrafiltration membrance filter, underflow is used to return to step the secondary slurry in step (3)
(1) in, clear liquid then uses hydrochloric acid tune pH to be used for next procedure after 3~6.5;
(5) film purifications:First time removal filtration is carried out using a NF membrane to sour Filtrate in step (4) to obtain
NF membrane dope and clear liquid, nanofiltration dope return to step (1);
(6) film concentrates:Nanofiltration clear liquid in step (5) is concentrated with reverse osmosis or electrodialysis, obtains dope and clear liquid, reverse osmosis
Saturating clear liquid returns to step (1);
(7) secondary film purification:It is cleaned again to counter-infiltration dope with NF membrane, obtains secondary NF membrane dope and clear
Liquid, nanofiltration clear liquid can be that salt dissolving water is used, and nanofiltration dope then returns to step (1).
2. a kind of technique of zero discharge of processing titanium chloride slag according to claim 1, it is characterised in that:Filter in step (2)
Slag can be used as making the raw material reuse of construction material such as cement, brick and tile.
3. a kind of technique of zero discharge of processing titanium chloride slag according to claim 1, it is characterised in that:It is solid in step (2)
Liquid separating technology is using the solid-liquid separation means combination of one or more of filtering, centrifugation, gravity or inclined plate sedimentation.
4. a kind of technique of zero discharge of processing titanium chloride slag according to claim 1, it is characterised in that:Institute in step (4)
It is micro-filtration/ultrafiltration membrane with film, material is ceramics, metal inorganic material or PES, PVDF, PS, PP, PTFE organic material,
Aperture is 2nm~1.5um.
5. a kind of technique of zero discharge of processing titanium chloride slag according to claim 1, it is characterised in that:Step (5) and (7)
In, NF membrane used is 96% or more to MgSO4 rejections at 0.75MPa and room temperature.
6. a kind of technique of zero discharge of processing titanium chloride slag according to claim 1, it is characterised in that:In step (6), institute
Concentration film is reverse osmosis membrane or electrodialytic membranes, reverse osmosis membrane at 1.5MPa and room temperature, to NaCl rejections be 98% with
On.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810364367.XA CN108636980B (en) | 2018-04-20 | 2018-04-20 | Zero-emission process for treating titanium chloride slag |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810364367.XA CN108636980B (en) | 2018-04-20 | 2018-04-20 | Zero-emission process for treating titanium chloride slag |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108636980A true CN108636980A (en) | 2018-10-12 |
CN108636980B CN108636980B (en) | 2020-07-28 |
Family
ID=63746896
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810364367.XA Active CN108636980B (en) | 2018-04-20 | 2018-04-20 | Zero-emission process for treating titanium chloride slag |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108636980B (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112250265A (en) * | 2020-10-16 | 2021-01-22 | 何淑会 | Sludge curing agent, preparation method thereof and sludge curing and stabilizing treatment method |
CN112591789A (en) * | 2020-12-24 | 2021-04-02 | 中国石油化工股份有限公司 | Method for obtaining byproduct ammonium fertilizer in process of purifying titanium liquid from olefin polymerization industrial waste acid residues |
CN112678866A (en) * | 2020-12-24 | 2021-04-20 | 中国石油化工股份有限公司 | Method for recycling waste acid sludge in olefin polymerization industry |
CN113548911A (en) * | 2021-08-31 | 2021-10-26 | 西南科技大学 | Method for preparing potassium chloride fertilizer by using chlorine-containing titanium extraction slag |
CN113718292A (en) * | 2021-08-27 | 2021-11-30 | 河南佰利联新材料有限公司 | Method for recycling waste residues in titanium dioxide production by chlorination process |
CN115415291A (en) * | 2022-07-06 | 2022-12-02 | 宜宾天原海丰和泰有限公司 | Method for treating chlorination slag of titanium dioxide by chlorination process |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107055914A (en) * | 2017-06-05 | 2017-08-18 | 南京工大环境科技有限公司 | A kind of reverse osmosis concentrated water concentration technology again |
CN107253776A (en) * | 2017-07-10 | 2017-10-17 | 四川绿沃创新环保工程有限公司 | Washery slag acid waste water technique of zero discharge in a kind of Titanium Dioxide Produced by Chloride Procedure production process |
-
2018
- 2018-04-20 CN CN201810364367.XA patent/CN108636980B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107055914A (en) * | 2017-06-05 | 2017-08-18 | 南京工大环境科技有限公司 | A kind of reverse osmosis concentrated water concentration technology again |
CN107253776A (en) * | 2017-07-10 | 2017-10-17 | 四川绿沃创新环保工程有限公司 | Washery slag acid waste water technique of zero discharge in a kind of Titanium Dioxide Produced by Chloride Procedure production process |
Non-Patent Citations (1)
Title |
---|
段克胜: "反渗透膜的结垢及预防", 《中国石油和化工勘察设计协会热工专委会、热工中心站2013年年会论文集》 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112250265A (en) * | 2020-10-16 | 2021-01-22 | 何淑会 | Sludge curing agent, preparation method thereof and sludge curing and stabilizing treatment method |
CN112591789A (en) * | 2020-12-24 | 2021-04-02 | 中国石油化工股份有限公司 | Method for obtaining byproduct ammonium fertilizer in process of purifying titanium liquid from olefin polymerization industrial waste acid residues |
CN112678866A (en) * | 2020-12-24 | 2021-04-20 | 中国石油化工股份有限公司 | Method for recycling waste acid sludge in olefin polymerization industry |
CN112591789B (en) * | 2020-12-24 | 2023-06-23 | 中国石油化工股份有限公司 | Method for obtaining by-product ammonium fertilizer in process of purifying titanium liquid from olefin polymerization industrial waste acid sludge |
CN112678866B (en) * | 2020-12-24 | 2023-07-04 | 中国石油化工股份有限公司 | Recycling treatment method of olefin polymerization industrial waste acid residues |
CN113718292A (en) * | 2021-08-27 | 2021-11-30 | 河南佰利联新材料有限公司 | Method for recycling waste residues in titanium dioxide production by chlorination process |
CN113548911A (en) * | 2021-08-31 | 2021-10-26 | 西南科技大学 | Method for preparing potassium chloride fertilizer by using chlorine-containing titanium extraction slag |
CN115415291A (en) * | 2022-07-06 | 2022-12-02 | 宜宾天原海丰和泰有限公司 | Method for treating chlorination slag of titanium dioxide by chlorination process |
CN115415291B (en) * | 2022-07-06 | 2024-04-19 | 宜宾天原海丰和泰有限公司 | Treatment method of titanium dioxide chloride slag by chlorination process |
Also Published As
Publication number | Publication date |
---|---|
CN108636980B (en) | 2020-07-28 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108636980A (en) | A kind of technique of zero discharge of processing titanium chloride slag | |
CN108372185B (en) | Titanium chloride slag resource utilization method and device | |
CN106044799B (en) | Titanium chloride slag and its method for comprehensive utilization of filtrate in chloride process titanium dioxide powder craft | |
CN103011203B (en) | Method for treatment of chlorinated waste molten salt generated in TiCl4 production process | |
CN105948174B (en) | Chloride process titanium dioxide flour flow design wastewater utilization method | |
CN109626420A (en) | A method of titanium dioxide and iron oxide are prepared using fluoride purification ferrotianium material | |
JP5444024B2 (en) | Recycling of zinc plating waste liquid | |
US20140356262A1 (en) | Method for treating tailings pond liquor | |
AU2014203695B2 (en) | Process for Manufacture of Sodium Hydroxide and Sodium Chloride Products from Waste Brine | |
CN108328808A (en) | A kind of titanium chloride slag filtrate film integrated processing method and device | |
US10294117B2 (en) | Extraction of products from titanium-bearing minerals | |
CN109607572A (en) | A method of comprehensive utilization subsurface brine production refined brine and calcium and magnesium compound | |
CN106277005B (en) | A kind of method that ice crystal, calcium carbonate and sodium sulphate are reclaimed in the resource from calcium fluoride sludge | |
US20080075645A1 (en) | Process for Complete Utilisation of Olivine Constituents | |
CN111115673A (en) | Method for utilizing all components of caustic sludge | |
CN103382033A (en) | Step-by-step extraction process for solids generated in brine purification | |
CA3201882A1 (en) | Acid wash of red mud (bauxite residue) | |
CN113582224A (en) | Resource utilization method for titanium white waste acid leaching fused salt chlorination slag | |
CN106315640A (en) | Method for treating high-evaporation mother liquid in alumina production | |
RU2373140C1 (en) | Method of complex purification of aqueous solutions of metal chlorides from iron and sulphate ion impurities | |
CN102765749B (en) | Method for comprehensively recycling titanium and niobium from crude titanium tetrachloride precipitate mud | |
CN208662090U (en) | A kind of titanium chloride slag resource utilization device | |
TWI524925B (en) | Fluorine recovery device and fluorine recovery method | |
CN206069459U (en) | A kind of recycle device of industrial acidic wastewater | |
JP2022510772A (en) | Method of extracting products from titanium-supported materials |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |