CN106044799B - Titanium chloride slag and its method for comprehensive utilization of filtrate in chloride process titanium dioxide powder craft - Google Patents
Titanium chloride slag and its method for comprehensive utilization of filtrate in chloride process titanium dioxide powder craft Download PDFInfo
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- CN106044799B CN106044799B CN201610357911.9A CN201610357911A CN106044799B CN 106044799 B CN106044799 B CN 106044799B CN 201610357911 A CN201610357911 A CN 201610357911A CN 106044799 B CN106044799 B CN 106044799B
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- filtrate
- chloride
- titanium
- slag
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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
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a kind of processing method of the accessory substance in chloride process titanium dioxide powder craft, specifically disclose titanium chloride slag and its method for comprehensive utilization of filtrate in a kind of chloride process titanium dioxide powder craft, this method utilizes the acid solution for being dissolved in watery hydrochloric acid formation in sodium hydroxide solution with titanium chloride slag, by adjusting pH, deionized water processing obtains the filtered fluid that main component is sodium chloride with the method for more steps of filtration, then send the brine section of chlor-alkali system to carry out after weight saturated process as the raw material of chlor-alkali production obtained filtered fluid.It is an advantage of the invention that：1）Metallic reducing agent need not be added into the acid solution of titanium chloride slag；2）Save the step of crystallization is evaporated to filtrate；3）The filtrate finally obtained can realize the combination of chloride process titanium dioxide powder craft and chlor-alkali production technique as the raw materials for production of chloralkali process.
Description
Technical field
The present invention relates to a kind of production technology of titanium tetrachloride in chloride process titanium dioxide powder craft, especially a kind of titanium tetrachloride
Production process in caused accessory substance processing method.
Background technology
At present, the method for producing titanium dioxide mainly has sulfuric acid process and chloridising.Because the long flow path of sulfuric acid process, pollution are tight
Weight, poor product quality and be progressively chlorinated method substitution.
In current Titanium Dioxide Produced by Chloride Procedure production, its main flow is：
A, by titanium material（Such as：High titanium slag）With reducing agent（Such as：Petroleum coke）Uniformly it is sent into after mixing in chlorination furnace, 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 rough titanium tetrachloride obtained after chlorination and removes the impurity such as magnesium, iron, silicon and vanadium, obtain essence
Titanium tetrachloride processed；
C, obtained refining titanic chloride liquid 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 is simultaneously added in gas phase titanium tetrachloride（Such as：Alchlor）Be mixed into oxidation furnace with it is pre-
Heat mixes rapidly to more than 1300 DEG C of oxygen in oxidation furnace, at a temperature of 1300 DEG C~1800 DEG C, less than 0.1 second in carry out oxygen
Change reaction generation solid phase titanium dioxide；
D, and then titanium dioxide solids powder is removed into reaction zone rapidly and reaction heat is removed rapidly；
E, the chlorine that oxidation reaction in furnace obtains is separated into return chlorination furnace by filter, it is synchronous to be collected by filter
Titanium dioxide granule powder and be beaten into liquid, send postprocessing working procedures that rutile type titanium white finished product is made.
Titanic chloride production process in Titanium Dioxide Produced by Chloride Procedure production link, to produce substantial amounts of waste residue.The source of waste residue
The flue dust for mainly flying upward during electro-smelting production high titanium slag and volatilizing and collecting；Broken preparing finished articles high titanium slag and chlorination
Caused meticulous titanium slag in broken winnowing process is hammered in dispensing production into shape；Fluidizing chlorination produces thick TiCl4 During discharge clinker, receive
Dirt slag etc..Not only include KCl, NaCl, MgCl in waste residue2And CaCl2, also it is enriched more by what is brought into rich-titanium material and petroleum coke
Kind metal impurities（Aluminium, iron, calcium, magnesium, potassium, cobalt, chromium, manganese etc.）, such metal impurities are after high-temp chlorination largely with chloride
Form is present, and aluminium and silicon mainly exist in the form of an oxide, and unreacted carbon exists with simple substance form.Waste residue is without processing
Directly stacking will cause substantial amounts of chloride in waste residue to meet water dissolving, and environment is polluted.
Though there is the technique much on processing chloride slag and its filtrate in the prior art, these techniques are to titanium chloride slag
Processing cost is too high, and titanium chloride slag filtrate is not recycled well.CN103447283A discloses a kind of chlorine
Change the method for disposal of titanium slag, the advantage is that concentration caused by washing tail gas is 20%~30% during Titanium Dioxide Produced by Chloride Procedure is produced
(mass concentration）By-product hydrochloric acid be used for handle titanium chloride slag, realize the integrated treatment of two kinds of accessory substances.Its shortcoming is：1）
The scheme of the patent is toward addition iron reduction heavy metal ion in the acid solution of titanium chloride slag, although this method can also rise
To preferable effect, but the iron filings added bring new deposit, increase the waste residue total amount after processing, generate new
Pollution, and processing cost is higher；2）The filtrate of last gained is evaporated concentration by this method, and this needs to consume substantial amounts of energy
Source, caused filter residue does not utilize rationally after first-time filtrate processing, can only stack, and pollutes environment；3）Titanium Dioxide Produced by Chloride Procedure produces
By-product hydrochloric acid caused by middle washing tail gas is not converted to valuable resource, causes the waste of resource.
The content of the invention
The present invention provides titanium chloride slag in a kind of chloride process titanium dioxide powder craft to solve problems of the prior art
And its 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 its
The method of comprehensive utilization of filtrate, comprises the following steps：
A, the metal chloride in titanium chloride slag is dissolved in watery hydrochloric acid, a filter residue and once is obtained through a press filtration
Filtrate；
B, sodium hydroxide solution is added into first-time filtrate, the pH of filtrate is adjusted to neutrality, stands after its reaction, continue
Sodium hydroxide solution is added to the pH ＞ 12 of first-time filtrate, heavy metal ion is separated out in the form of hydroxide precipitates, obtains
Alkaline solution；
C, above-mentioned alkaline solution is subjected to secondary press filtration, obtains secondary filter residue and secondary filtrate, the secondary filter residue of gained and gone
After ionized water stirring, press filtration three times, filter residue three times and three times filtrate are obtained so that filter residue institute chloride ion-containing≤1% three times；Three times
Filter residue can be as the raw material of manufacture of cement；
D, the secondary filtrate of gained and three times after filtrate mixing, carries out ultrafiltration membrance filter, obtains four filtrates and recoil washery slag
Slurry；
E, four filtrates are obtained after being filtered again with NF membrane containing high price（>=+divalent）The concentrated water of metal ion and five times
Filtrate, five filtrates send the brine section of chlor-alkali system to carry out raw material as chlor-alkali production after weight saturated process.
The present invention is actually to add sodium hydroxide solution in the acid solution of first-time filtrate, with the salt in first-time filtrate
Acid reacts, and generates sodium chloride solution.Sodium chloride solution is the raw material of chlor-alkali production technique, but as caused by above-mentioned steps
Contain 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 will wherein heavy metal ion
Remove.Therefore, the present invention devise it is a kind of handle and using the method for above-mentioned first-time filtrate, by adjusting pH, at deionized water
The methods of reason and more steps of filtration, obtains the filtered fluid that main component is sodium chloride, is then delivered to the brine section of chlor-alkali production system
The raw material that directly heavy saturation can serve as chlor-alkali production is used, and filter residue can use as the raw material of production cement three times.
It is possible thereby to the step of saving to the evaporative crystallization of titanium chloride slag filtrate with adding metallic reducing agent to bring new precipitation, and produce and be 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 caused spent caustic solution or product aqueous slkali.The accessory substance and chloralkali process in chloride process titanium dioxide powder craft are realized with this
In caused spent caustic solution or product aqueous slkali mutual utilization, at utmost avoid the waste of resource, realize chloride process titanium dioxide
Powder craft and the combination of chlor-alkali production technique.
As a further improvement on the present invention, high price will be contained described in E steps（>=+divalent）The concentrated water of metal ion is mixed
Enter and circular treatment is carried out in the first-time filtrate of the step A.Contain heavy metal ion due to passing through in concentrated water caused by nanofiltration, though
The amount of right concentrated water is less, if but each batch processed it is complete after all concentrated water discharge will be polluted into environment to environment, can
Subsequent treatment is carried out after it is mixed with the first-time filtrate of next batch, wherein heavy metal ion is converted into hydroxide and is sunk
Form sediment, so circulation, the discharge of heavy metal ion can be avoided.
As a further improvement on the present invention, the backwash slurry described in D steps is mixed into secondary filter residue and followed
Ring processing.To realize that resource makes full use of and avoided individually to handle slurries.
As a further improvement on the present invention, the watery hydrochloric acid in the step A is tail gas in being produced by Titanium Dioxide Produced by Chloride Procedure
Concentration caused by washing is 20% 30%（Mass concentration）By-product hydrochloric acid and filter press flushing water allotment and obtain.To make full use of
By-product resource, save titanium chloride slag and its processing cost of filtrate.
The beneficial effects of the invention are as follows：1）Metallic reducing agent need not be added into the acid solution of titanium chloride slag, after filtering
Filter residue total amount will not increase, reduce the pollution to environment；2）The step of crystallization is evaporated to filtrate can be saved, saves the energy
And simplify technique；3）Last gained filtrate can be as the raw materials for production of chloralkali process, and sodium hydroxide solution can used in the present invention
Using caused spent caustic solution or product aqueous slkali in chloralkali process, to realize chloride process titanium dioxide powder craft and chlor-alkali production technique
Combination；4）In filtrate processing procedure, all resources are obtained for reasonable utilization, are produced without new useless solid, waste liquid.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment：
Experimental data to be drawn using the method for the present invention in laboratory treatment titanium chloride slag and its filtrate water below.
1st, 50g titanium chloride slag, at normal temperatures and pressures waste residue be dissolved in 250g by chlorine contained exhaust gas processing system water-wash stream
In the acid solution of 20% waste hydrochloric acid caused by journey and filter press flushing water composition, stirred using mechanical agitator during dissolving
20min, pH≤1 of solution after dissolving obtain suspension, and filtering suspension obtains a filter residue and first-time filtrate, measures one
Secondary filter residue chloride ion content is 3.23%, and filtrate sodium chloride concentration is 53.23 g/L；
2nd, the spent caustic solution that caused concentration is 20% in the production process of chlor-alkali production system is added into first-time filtrate,
To regulation filtrate pH to neutrality, stand after its reaction, continuously add above-mentioned sodium hydroxide solution to filtering solution
PH >=13, heavy metal ion is set to be separated out in the form of hydroxide precipitates；
3rd, the solution of strong basicity is subjected to secondary filter, secondary filter residue and secondary filtrate is obtained, into the secondary filter residue of gained
Add deionized water 250g and stir after, press filtration again, obtain filter residue three times and three times filtrate, measure three times filter residue it is chloride from
Son is 0.43%, and filtrate sodium chloride content is 8.5g/L；
4th, the secondary filtrate of gained and three times after filtrate mixing, carries out ultrafiltration membrance filter, remaining tiny in solution to remove
Impurity particle, and four filtrates and backwash slurry are obtained, milipore filter backwash slurry and secondary filter residue and deionized water are total to
Press filtration three times is carried out with being sent to after mixing, it is 23ppm to measure filtrate ss；Backwash slurry and the secondary filter in next processing batch
Circular treatment is carried out after slag mixing.
5th, four filtrates carry out removal of heavy metal ions processing with NF membrane again, are obtained after filtering containing the dense of heavy metal ion
Water and five filtrates that sodium chloride concentration is 32.32g/L, five filtrates send the brine section of chlor-alkali system to carry out weight saturated process
Raw material as chlor-alkali production afterwards.Concentrated water containing heavy metal ion is followed after being mixed with the first-time filtrate in next processing batch
Ring processing.
Experiment can obtain the chlorination that concentration is 32.32g/L after measuring method processing of every 100g titanium chloride slags by the present invention
Sodium solution about 350ml, for chlor-alkali production technique productions raw material sodium chloride 11.312g.
Claims (5)
1. titanium chloride slag and its method for comprehensive utilization of filtrate, comprise the following steps in chloride process titanium dioxide powder craft：
A, the metal chloride in titanium chloride slag is dissolved in watery hydrochloric acid, obtains a filter residue through a press filtration and once filter
Liquid；
It is characterized in that：It is further comprising the steps of：
B, sodium hydroxide solution is added into first-time filtrate, the pH of filtrate is adjusted to neutrality, stands after its reaction, continuously add
Sodium hydroxide solution makes heavy metal ion be separated out in the form of hydroxide precipitates, obtains alkalescence to the pH ＞ 12 of first-time filtrate
Solution；
C, above-mentioned alkaline solution is subjected to secondary press filtration, obtains secondary filter residue and secondary filtrate, the secondary filter residue of gained and deionization
After water stirring, press filtration three times, filter residue three times and three times filtrate are obtained so that filter residue institute chloride ion-containing≤1% three times；
D, the secondary filtrate of gained and three times after filtrate mixing, carries out ultrafiltration membrance filter, obtains four filtrates and backwash slurry；
E, four filtrates are contained >=concentrated water of the high volence metal ion of+divalent and five filtrates after being filtered again with NF membrane,
Five filtrates send the brine section of chlor-alkali system to carry out raw material as chlor-alkali production after weight saturated process.
2. titanium chloride slag according to claim 1 and its method for comprehensive utilization of filtrate, it is characterised in that：Institute in step B
The sodium hydroxide solution stated is caused spent caustic solution or product aqueous slkali in the production process of chlor-alkali production system.
3. titanium chloride slag according to claim 1 and its method for comprehensive utilization of filtrate, it is characterised in that：By in E steps
The concentrated water of the described high volence metal ion containing >=+divalent, which is mixed into the first-time filtrate of the step A, carries out circular treatment.
4. titanium chloride slag according to claim 1 and its method for comprehensive utilization of filtrate, it is characterised in that：By in D steps
Described backwash slurry, which is mixed into secondary filter residue, carries out circular treatment.
5. the method for comprehensive utilization of the titanium chloride slag and its filtrate according to Claims 1 to 4 any claim, its feature
It is：Watery hydrochloric acid in the step A is that mass concentration caused by washing tail gas is 20% in being produced as Titanium Dioxide Produced by Chloride Procedure
30% by-product hydrochloric acid and filter press flushing water is allocated and obtained.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| 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 |
| CN111498910B (en) * | 2020-05-26 | 2022-09-16 | 宜宾海丰和锐有限公司 | 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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| CN103447283B (en) * | 2013-08-30 | 2017-06-09 | 漯河兴茂钛业股份有限公司 | The Safe disposal method of waste residue produced by Titanium Dioxide Produced by Chloride Procedure production titanium tetrachloride |
| CN104498723B (en) * | 2014-12-16 | 2016-07-06 | 湖南稀土金属材料研究院 | The method extracting Scia from titanium slag chlorized abraum salt |
| CN105502791B (en) * | 2016-01-21 | 2018-08-07 | 厦门嘉戎技术股份有限公司 | A kind of coal chemical industrial waste water salinity extracting method and equipment |
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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 |