CN106044799A - Method for comprehensively utilizing titanium chloride residues and filter liquid thereof in chlorination-process technologies for titanium dioxide powder - Google Patents
Method for comprehensively utilizing titanium chloride residues and filter liquid thereof in chlorination-process technologies for titanium dioxide powder Download PDFInfo
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- CN106044799A CN106044799A CN201610357911.9A CN201610357911A CN106044799A CN 106044799 A CN106044799 A CN 106044799A CN 201610357911 A CN201610357911 A CN 201610357911A CN 106044799 A CN106044799 A CN 106044799A
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- China
- Prior art keywords
- filtrate
- titanium
- chloride
- filter liquid
- titanium dioxide
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/24—Cements from oil shales, residues or waste other than slag
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Abstract
The invention relates to a method for treating byproducts in chlorination-process technologies for titanium dioxide powder, and particularly discloses a method for comprehensively utilizing titanium chloride residues and filter liquid thereof in chlorination-process technologies for titanium dioxide powder. The method includes dissolving the titanium chloride residues in diluted hydrochloric acid to obtain acidic solution and neutralizing the acidic solution by the aid of sodium hydroxide solution; carrying out pH (potential of hydrogen) regulation, deionized water treatment and multi-step filter processes to obtain the filter liquid with sodium chloride which is a main component; feeding the obtained filter liquid to brine working procedures of chlorine-alkali systems and carrying out re-saturation treatment on the filter liquid to obtain raw materials for chlorine-alkali production. The method has the advantages that metal reducing agents do not need to be added into the acidic solution with the titanium chloride residues; steps for carrying out evaporative crystallization on the filter liquid can be omitted; the ultimately obtained filter liquid can be used as the production raw materials for chlorine-alkali technologies, and accordingly the chlorination-process technologies for the titanium dioxide powder can be organically combined with the chlorine-alkali production technologies.
Description
Technical field
The present invention relates to the production technology of titanium tetrachloride in a kind of chloride process titanium dioxide powder craft, especially a kind of titanium tetrachloride
Production process in the processing method of by-product that produces.
Background technology
At present, the method producing titanium dioxide mainly has sulfuric acid process and chloridising.Due to the long flow path of sulfuric acid process, pollute tight
Weight, poor product quality and be progressively chlorinated method replace.
In current Titanium Dioxide Produced by Chloride Procedure produces, its main flow process is:
A, titanium material (such as: high titanium slag) is uniformly mixed with reducing agent (such as: petroleum coke) after send in chlorination furnace, be passed through chlorine and exist
Fluidizing chlorination is carried out at a temperature of 800 DEG C～1000 DEG C；
B, the rough titanium tetrachloride obtained is carried out separating-purifying remove the impurity such as magnesium, ferrum, silicon and vanadium after chlorination, obtain refined four
Titanium chloride；
C, prepared refining titanic chloride liquid carry out pre-thermal evaporation and are converted into gas phase, and are preheated to 300 DEG C～500 DEG C；And in
This adds a small amount of compound modifying agent (such as: aluminum chloride) at gas phase titanium tetrachloride simultaneously and is mixed into oxidation furnace and is preheating to
The oxygen of more than 1300 DEG C mixes rapidly at oxidation furnace, at a temperature of 1300 DEG C～1800 DEG C, less than 0.1 second in carry out oxidation anti-
Solid phase titanium dioxide should be generated；
D, then rapidly by titanium dioxide solids powder removal reaction zone and make reaction heat remove rapidly；
E, chlorine oxidation reaction in furnace obtained separate return chlorination furnace through filter, and synchronization is through the two of filter collection
Titan oxide particles powder is also beaten into liquid, send postprocessing working procedures to make Rutile type titanium dioxide finished product.
Titanic chloride production process in Titanium Dioxide Produced by Chloride Procedure production link, will produce substantial amounts of waste residue.The source of waste residue
It is mainly during electro-smelting produces high titanium slag the flue dust flying upward and volatilizing and collect；Broken preparing finished articles high titanium slag and chlorination
Dispensing produces hammers the meticulous titanium slag produced in broken winnowing process into shape；Fluidizing chlorination produces thick TiCl4 During discharge slag, receipts
Dirt slag etc..Waste residue not only includes KCl, NaCl, MgCl2And CaCl2, also it is enriched by rich-titanium material and petroleum coke are brought into many
Planting metal impurities (aluminum, ferrum, calcium, magnesium, potassium, cobalt, chromium, manganese etc.), these type of metal impurities are most of with chloride after high-temp chlorination
Form exists, and aluminum and silicon exist the most in the form of an oxide, and unreacted carbon exists with simple substance form.Waste residue is without process
Directly stack and substantial amounts of chloride in waste residue will be caused to meet water dissolution, to environment.
Though prior art having much about processing chloride slag and the technique of filtrate thereof, but these techniques being to titanium chloride slag
Processing cost is too high, and the most well recycles titanium chloride slag filtrate.CN103447283A discloses a kind of chlorine
Change the method for disposal of titanium slag, have an advantage in that the concentration that in being produced by Titanium Dioxide Produced by Chloride Procedure, washing tail gas produces is 20%～30%
The by-product hydrochloric acid of (mass concentration) is used for processing titanium chloride slag, it is achieved that the integrated treatment of two kinds of by-products.Its shortcoming is: 1)
The scheme of this patent is addition iron reduction heavy metal ion in the acid solution of titanium chloride slag, although this method also can rise
To preferable effect, but the iron filings added bring new deposit, make the waste residue total amount after process increase, and create new
Pollution, and processing cost is higher；2) filtrate of last gained is evaporated concentrating by the method, and this needs to consume substantial amounts of energy
Source, the filtering residue that first-time filtrate produces after processing does not has Appropriate application, can only stack, pollutes environment；3) Titanium Dioxide Produced by Chloride Procedure produces
The by-product hydrochloric acid that middle washing tail gas produces is not converted to valuable resource, causes the waste of resource.
Summary of the invention
The present invention solves that problems of the prior art provide titanium chloride slag in a kind of chloride process titanium dioxide powder craft
And the method for comprehensive utilization of filtrate.
The technical solution adopted for the present invention to solve the technical problems is: in chloride process titanium dioxide powder craft titanium chloride slag and
The method of comprehensive utilization of filtrate, comprises the following steps:
A, the metal chloride in titanium chloride slag is dissolved in dilute hydrochloric acid, obtains a filtering residue through a filter pressing and once filter
Liquid；
B, adding sodium hydroxide solution in first-time filtrate, the pH of regulation filtrate, to neutral, stand after it reacts, continuously adds
Sodium hydroxide solution is to the pH ＞ 12 of first-time filtrate, and the form making heavy metal ion precipitate with hydroxide separates out, and obtains alkalescence
Solution；
C, above-mentioned alkaline solution is carried out secondary filter pressing, obtain secondary filtering residue and secondary filtrate, gained secondary filtering residue and deionization
After water stirring, three filter pressings, obtain three filtering residues and three filtrates so that three filtering residue institute chloride ion-containing≤1%；Three filtering residues
Can be as the raw material of manufacture of cement；
After D, gained secondary filtrate and three filtrate mixing, carry out ultrafiltration membrance filter, obtain four filtrates and backwash slurry；
E, four filtrates obtain the dense water containing high price (>=+divalent) metal ion and five filtrates by NF membrane after filtering again,
Five filtrate send the brine section of chlor-alkali system to carry out after the saturated process of weight the raw material as chlor-alkali production.
The present invention is actually and adds the salt in sodium hydroxide solution, with first-time filtrate in the acid solution of first-time filtrate
Acid reacts, and generates sodium chloride solution.Sodium chloride solution is the raw material of chlor-alkali production technique, but produced by above-mentioned steps
Containing substantial amounts of heavy metal ion in sodium chloride solution, it is impossible to be directly used in chloralkali process, it is necessary to first by wherein heavy metal ion
Remove.To this end, the present invention devises a kind of method processing and utilize above-mentioned first-time filtrate, at regulation pH, deionized water
The methods such as reason and more steps of filtration obtain the filtrate that main component is sodium chloride, are then delivered to the brine section of chlor-alkali production system
Directly the saturated raw material that can serve as chlor-alkali production of weight uses, and three times filtering residue can use as the raw material producing cement.
Thus can save the evaporative crystallization to titanium chloride slag filtrate and bring the step of new precipitation with metallic reducing agent, and generation is available for
The resource utilized.
As a further improvement on the present invention, the sodium hydroxide solution described in step B is the production of chlor-alkali production system
During produce spent caustic solution or product aqueous slkali.The by-product in chloride process titanium dioxide powder craft and chloralkali process is realized with this
The spent caustic solution of middle generation or the mutual utilization of product aqueous slkali, at utmost avoid the waste of resource, it is achieved chloride process titanium dioxide
Powder craft and the combination of chlor-alkali production technique.
As a further improvement on the present invention, the dense water containing high price (>=+divalent) metal ion described in E step is mixed
Enter in the first-time filtrate of described step A and be circulated process.Due in the dense water that produces through nanofiltration containing heavy metal ion, though
The amount of right dense water is less, if but each batch processed complete after all by will be to environment in concentrated water discharge to environment, can
Subsequent treatment is carried out with the first-time filtrate of next batch so that it is middle heavy metal ion is converted into hydroxide and sinks after it being mixed
Form sediment, so circulate, the discharge of heavy metal ion can be avoided.
As a further improvement on the present invention, the backwash slurry described in D step is mixed in secondary filtering residue follows
Ring processes.With realize resource make full use of and avoid serosity is carried out individual processing.
As a further improvement on the present invention, the dilute hydrochloric acid in described step A be produced by Titanium Dioxide Produced by Chloride Procedure in tail gas
Washing produce concentration be 20% 30%(mass concentration) by-product hydrochloric acid and pressure filter flushing water allotment obtain.To make full use of
By-product resource, saves titanium chloride slag and the processing cost of filtrate thereof.
The invention has the beneficial effects as follows: 1) need not with metallic reducing agent in the acid solution of titanium chloride slag, after filtration
Filtering residue total amount will not increase, reduce pollution to environment；2) step that filtrate is evaporated crystallization can be saved, save the energy
And Simplified flowsheet；3) last gained filtrate can be as the raw materials for production of chloralkali process, and used by the present invention, sodium hydroxide solution can
To use the spent caustic solution or product aqueous slkali produced in chloralkali process, it is achieved chloride process titanium dioxide powder craft and chlor-alkali production technique
Combination；4) in filtrate processing procedure, all resources are obtained for Appropriate application, produce without new useless solid, waste liquid.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
Embodiment:
Below by the experimental data using the method for the present invention to be drawn in laboratory treatment titanium chloride slag and filtrate water thereof.
1, the titanium chloride slag of 50g, waste residue is dissolved in 250g by chlorine contained exhaust gas processing system water-wash stream at normal temperatures and pressures
In 20% waste hydrochloric acid of journey generation and the acid solution of pressure filter flushing water composition, mechanical agitator during dissolving, is utilized to stir
20min, pH≤1 of solution after dissolving, obtain suspension, filter suspension and obtain a filtering residue and first-time filtrate, record one
Secondary filtering residue chloride ion content is 3.23%, and filtrate sodium chloride concentration is 53.23 g/L；
2, in first-time filtrate, the spent caustic solution that concentration is 20% produced in the production process of chlor-alkali production system is added, to adjusting
The pH of joint filtrate, to neutral, stands after it reacts, continuously add above-mentioned sodium hydroxide solution to a filtering solution pH >=
13, the form making heavy metal ion precipitate with hydroxide separates out；
3, alkaline solution is carried out secondary filter, obtain secondary filtering residue and secondary filtrate, add in gained secondary filtering residue
After deionized water 250g stirring, filter pressing again, obtain three filtering residues and three filtrates, recording three filtering residue institute chloride ion-containings is
0.43%, filtrate sodium chloride content is 8.5g/L；
4, after gained secondary filtrate and three filtrates mix, ultrafiltration membrance filter is carried out, to remove fine impurities remaining in solution
Granule, and obtain four filtrates and backwash slurry, ultrafilter membrane backwash slurry and secondary filtering residue and deionized water are mixed jointly
Sending to after conjunction and carry out three filter pressings, recording filtrate ss is 23ppm；Backwash slurry processes the secondary filtering residue in batch with next and mixes
Circular treatment is carried out after conjunction.
5, four filtrates carry out removal of heavy metal ions process by NF membrane again, and obtain containing heavy metal ion after filtration is dense
Water and five filtrates that sodium chloride concentration is 32.32g/L, five times filtrate send the brine section of chlor-alkali system to carry out the saturated process of weight
Afterwards as the raw material of chlor-alkali production.Dense water containing heavy metal ion processes after the first-time filtrate in batch mixes with next and follows
Ring processes.
Experiment records every 100g titanium chloride slag can obtain, after the method for the present invention processes, the chlorination that concentration is 32.32g/L
Sodium solution about 350ml, for chlor-alkali production technique raw materials for production sodium chloride 11.312g.
Claims (5)
1. titanium chloride slag and the method for comprehensive utilization of filtrate thereof in chloride process titanium dioxide powder craft, comprises the following steps:
A, the metal chloride in titanium chloride slag is dissolved in dilute hydrochloric acid, obtains a filtering residue through a filter pressing and once filter
Liquid；It is characterized in that, further comprising the steps of:
B, adding sodium hydroxide solution in first-time filtrate, the pH of regulation filtrate, to neutral, stand after it reacts, continuously adds
Sodium hydroxide solution is to the pH ＞ 12 of first-time filtrate, and the form making heavy metal ion precipitate with hydroxide separates out, and obtains alkalescence
Solution；
C, above-mentioned alkaline solution is carried out secondary filter pressing, obtain secondary filtering residue and secondary filtrate, gained secondary filtering residue and deionization
After water stirring, three filter pressings, obtain three filtering residues and three filtrates so that three filtering residue institute chloride ion-containing≤1%；
After D, gained secondary filtrate and three filtrate mixing, carry out ultrafiltration membrance filter, obtain four filtrates and backwash slurry；
E, four filtrates obtain the dense water containing high price (>=+divalent) metal ion and five filtrates by NF membrane after filtering again,
Five filtrate send the brine section of chlor-alkali system to carry out after the saturated process of weight the raw material as chlor-alkali production.
Titanium chloride slag the most according to claim 1 and the method for comprehensive utilization of filtrate thereof, it is characterised in that: institute in step B
The sodium hydroxide solution stated is the spent caustic solution or product aqueous slkali produced in the production process of chlor-alkali production system.
Titanium chloride slag the most according to claim 1 and the method for comprehensive utilization of filtrate thereof, it is characterised in that: by E step
The described dense water containing high price (>=+divalent) metal ion is mixed in the first-time filtrate of described step A and is circulated process.
Titanium chloride slag the most according to claim 1 and the method for comprehensive utilization of filtrate thereof, it is characterised in that: by D step
Described backwash slurry is mixed in secondary filtering residue and is circulated process.
5. according to the titanium chloride slag described in Claims 1 to 4 any claim and the method for comprehensive utilization of filtrate thereof, its feature
Be: the dilute hydrochloric acid in described step A be produced by Titanium Dioxide Produced by Chloride Procedure in washing tail gas produce concentration be 20% 30%(matter
Amount concentration) by-product hydrochloric acid and pressure filter flushing water allotment and obtain.
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| CN201610357911.9A CN106044799B (en) | 2016-05-26 | 2016-05-26 | Titanium chloride slag and its method for comprehensive utilization of filtrate in chloride process titanium dioxide powder craft |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108002586A (en) * | 2017-12-01 | 2018-05-08 | 攀枝花钢企欣宇化工有限公司 | A kind of purifying treatment method of chlorinated exhaust wastewater eluting |
| CN108328808A (en) * | 2018-04-20 | 2018-07-27 | 宜宾天原海丰和泰有限公司 | A kind of titanium chloride slag filtrate film integrated processing method and device |
| CN108328781A (en) * | 2017-07-12 | 2018-07-27 | 江苏久吾高科技股份有限公司 | The wastewater treatment method and device generated in a kind of Titanium Dioxide Produced by Chloride Procedure production process |
| CN108372185A (en) * | 2018-04-20 | 2018-08-07 | 江苏久吾高科技股份有限公司 | A kind of titanium chloride slag resource utilization method and its device |
| CN108675499A (en) * | 2018-05-30 | 2018-10-19 | 龙蟒佰利联集团股份有限公司 | A kind of method of chloride slag mashing waste water integrated treatment |
| CN111498910A (en) * | 2020-05-26 | 2020-08-07 | 宜宾天原海丰和泰有限公司 | Resource utilization method of chlorination waste residue |
| CN112520777A (en) * | 2020-12-03 | 2021-03-19 | 山东鲁北企业集团总公司 | Process for preparing calcium chloride by using byproduct hydrochloric acid slag water of titanium white |
| CN113428878A (en) * | 2021-07-21 | 2021-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing chlorine alkali chemical industry primary salt water and refined salt water from fused salt chlorination 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 |
| CN114835085A (en) * | 2022-04-25 | 2022-08-02 | 宜宾天原科创设计有限公司 | Combined treatment method for titanium dioxide byproduct hydrochloric acid and chloride dust-collecting slag by chlorination process |
| CN108372185B (en) * | 2018-04-20 | 2024-05-03 | 江苏久吾高科技股份有限公司 | Titanium chloride slag resource utilization method and device |
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| CN103447283A (en) * | 2013-08-30 | 2013-12-18 | 漯河兴茂钛业股份有限公司 | Safe disposal method for waste residue produced by production of titanium tetrachloride by using titanium dioxide by chlorination process |
| CN104498723A (en) * | 2014-12-16 | 2015-04-08 | 湖南稀土金属材料研究院 | Method for extracting scandium oxide from titanium slag chlorinated waste salt |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108328781A (en) * | 2017-07-12 | 2018-07-27 | 江苏久吾高科技股份有限公司 | The wastewater treatment method and device generated in a kind of Titanium Dioxide Produced by Chloride Procedure production process |
| CN108002586A (en) * | 2017-12-01 | 2018-05-08 | 攀枝花钢企欣宇化工有限公司 | A kind of purifying treatment method of chlorinated exhaust wastewater eluting |
| CN108328808A (en) * | 2018-04-20 | 2018-07-27 | 宜宾天原海丰和泰有限公司 | A kind of titanium chloride slag filtrate film integrated processing method and device |
| CN108372185A (en) * | 2018-04-20 | 2018-08-07 | 江苏久吾高科技股份有限公司 | A kind of titanium chloride slag resource utilization method and its device |
| CN108372185B (en) * | 2018-04-20 | 2024-05-03 | 江苏久吾高科技股份有限公司 | Titanium chloride slag resource utilization method and device |
| CN108675499A (en) * | 2018-05-30 | 2018-10-19 | 龙蟒佰利联集团股份有限公司 | A kind of method of chloride slag mashing waste water integrated treatment |
| CN111498910A (en) * | 2020-05-26 | 2020-08-07 | 宜宾天原海丰和泰有限公司 | Resource utilization method of chlorination waste residue |
| CN112520777A (en) * | 2020-12-03 | 2021-03-19 | 山东鲁北企业集团总公司 | Process for preparing calcium chloride by using byproduct hydrochloric acid slag water of titanium white |
| CN113428878A (en) * | 2021-07-21 | 2021-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing chlorine alkali chemical industry primary salt water and refined salt water from fused salt chlorination 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 |
| CN114835085A (en) * | 2022-04-25 | 2022-08-02 | 宜宾天原科创设计有限公司 | Combined treatment method for titanium dioxide byproduct hydrochloric acid and chloride dust-collecting slag by chlorination process |
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Effective date of registration: 20191018 Address after: 644004 No.61, West Gangyuan Road, Lingang Economic Development Zone, Yibin City, Sichuan Province Co-patentee after: Yibin Tianyuan Haifeng Hetai Co., Ltd. Patentee after: YiBin TianYuan Group Co., Ltd. Address before: 644000 No. 1, middle Yuan Road, lower Jiangbei, Sichuan, Yibin Patentee before: YiBin TianYuan Group Co., Ltd. |
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Inventor after: Deng Min Inventor after: Yan Hua Inventor after: Wang Honglei Inventor after: Mao Yanming Inventor after: Wan Li Inventor before: Deng Min Inventor before: Yan Hua Inventor before: Mao Yanming Inventor before: Wan Li |