CN106399604B - A kind of method of titanium extraction tailings dechlorination decarburization - Google Patents
A kind of method of titanium extraction tailings dechlorination decarburization Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B3/00—General features in the manufacture of pig-iron
- C21B3/04—Recovery of by-products, e.g. 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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
The present invention relates to the recycling fields of titanium extraction tailings, disclose a kind of method of titanium extraction tailings dechlorination decarburization, this method comprises: (1) mixes titanium extraction tailings with antichlor source；(2) mixture obtained by step (1) is calcined.The method and process of titanium extraction tailings dechlorination decarburization provided by the invention is simple, process is short and dechlorination decarburization effect is good, is very suitable for industrial application.
Description
Technical field
The present invention relates to the utilization technology fields of titanium extraction tailings, and in particular, to a kind of titanium extraction tailings dechlorination decarburization
Method.
Background technique
Contain a large amount of titanium dioxide in steel climbing high slag, fails extensive efficiently utilization at present, climb steel and just develop high temperature cabonization-
Low temperature chlorination technique extracts the titanium in its blast furnace slag, and gained waste residue is titanium extraction tailings after mentioning titanium.Titanium extraction tailings chemical component with
Slag cements is close, and has hydration activity, and titanium extraction tailings can be used as the use of the construction materials such as slag micropowder, but mention titanium tail
Chlorinity is up to 2-5% in slag, far beyond standard value 0.06%；In addition, its free carbon content is up to 5-10%, make its burning
Damage is higher than the 3% of standard requirements.The reason of these two aspects, hampers it in the application of building trade.Therefore, seek economically feasible
Removing titanium extraction tailings in the method for chlorine and carbon titanium extraction tailings can be made to utilize on a large scale as slag micropowder, mention titanium for blast furnace slag and attack
It closes and solves trouble and worry.
CN104056841A discloses a kind of processing method of titanium extraction tailings, and the titanium extraction tailings contain water-soluble chlorination
Object, wherein this method include the titanium extraction tailings are washed so that in treated titanium extraction tailings chlorine element content
For 0.06 weight % or less.This method needs a large amount of water, and cannot be removed effectively the free carbon in titanium extraction tailings.
CN103936050A discloses the non-pollution processing method and system of a kind of chloridising titanium extraction tailings, this method packet
It includes: being cooled down using cold wind to the high temperature titanium extraction tailings being discharged in chlorination furnace, obtain the hot tailings that temperature is 120-150 DEG C；
Vacuum cleaning more than twice is carried out to hot tailings sequence to filter.This method is equally to be handled using washing titanium extraction tailings,
And the free carbon in titanium extraction tailings can not be effectively removed.
CN104016598A discloses a kind of dechlorination method of titanium extraction tailings, and this method includes mixing titanium extraction tailings with water
Washing, obtains level-one residue and level-one filtrate, then calcines level-one residue, and calcined level-one residue is continued successively
It is washed and is calcined.Its disclosed method is complex, when treating capacity is larger, brings certain difficulty to operation.
CN105271857A discloses a kind of pre-column technique of chloridising titanium extraction tailings, which is characterized in that including with
Lower step: 1) chloridising titanium extraction tailings enter mashing tank by chlorination furnace slag-drip opening, and the temperature of chloridising titanium extraction tailings is 400-
550℃；2) the water stirring to pulp in chloridising titanium extraction tailings and mashing tank forms slurry, and the grain slag mass ratio for controlling slurry is
3.2-4:1；3) slurry makes to be piped to cinder field by slush pump；To realize except chloro- tailings transports integration；4) it beats
Titanium extraction tailings after the slurry water content of natural subsidence to tailings in cinder field is 12-20%, and chloride ion content is below 0.3%；
5) tailings after natural subsidence is directly entered rotary kiln by belt, in 600-700 DEG C of calcining 20-40min.
CN105385855A discloses a kind of dechlorination method of chloridising titanium extraction tailings, which is characterized in that proposes chloridising
Titanium tailings and water are stirred to form slurry, and pulp water mass ratio is 1:2-4, are then obtained by way of filtering-washing-filtering
The titanium extraction tailings of qualified titanium extraction tailings, the qualification meet: chloride ion content is lower than 0.2%, water content 12%-
20wt%.
The dechlorination method and process of titanium extraction tailings disclosed in the prior art is complicated, long flow path, and cannot effectively remove and mention
Carbon in titanium tailings needs to develop a kind of simple process, process therefore, it is desirable to further efficiently use titanium extraction tailings
The processing method of titanium extraction tailings short, dechlorination decarburization effect is good.
Summary of the invention
The purpose of the invention is to overcome titanium extraction tailings dechlorination method process flow in the prior art is long, treating capacity by
Limit, and cannot effectively decarburization defect, provide a kind of method of titanium extraction tailings dechlorination decarburization, this method simple process, process are short
And dechlorination decarburization effect is good.
The present inventor has found that the titanium extraction tailings dechlorination method that the prior art provides can not incite somebody to action in the course of the research
Carbon removes together, if necessary to efficiently use titanium extraction tailings, it is also necessary to which additional step removes carbon, entire technique
Long flow path, treating capacity are limited, strongly limit the utilization of titanium extraction tailings, the present inventor further study show that, will mention
Titanium tailings is mixed with antichlor source, then calcines mixture, in calcination process, chloride in titanium extraction tailings and de-
Chlorine agent reaction generates metal chloride, chlorine and hydrogen chloride etc., escapes in gaseous form, thus realize dechlorination, and calcination process
In, the free carbon in the burning of free carbon effectively removing titanium extraction tailings is effectively saved in addition, free carbon can be used as heat source
Heat loss.
Based on this, the present invention provides a kind of methods of titanium extraction tailings dechlorination decarburization, this method comprises:
(1) titanium extraction tailings are mixed with antichlor source；
(2) mixture obtained by step (1) is calcined.
The method of titanium extraction tailings dechlorination decarburization provided by the invention can remove together chlorine and carbon, and simple process,
Process is short, dechlorination decarburization effect is good, and under preferable case, when antichlor is ferrous sulfate and/or boric acid, the temperature of calcining is 600-
At 800 DEG C, titanium extraction tailings chlorinity can be made to be reduced to 0.06% hereinafter, free carbon content is reduced to 1% hereinafter, meeting mine simultaneously
The purpose that titanium extraction tailings are used as slag micropowder is realized in requirement of the slag micro mist to chloride ion content and scaling loss.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of method of titanium extraction tailings dechlorination decarburization, this method comprises:
(1) titanium extraction tailings are mixed with antichlor source；
(2) mixture obtained by step (1) is calcined.
In the present invention, it is preferred to after the titanium extraction tailings extract the titanium in blast furnace slag for high temperature cabonization-low temperature chlorination technique
Gained waste residue.
A preferred embodiment of the invention, it is described to mention titanium tail on the basis of the total weight of the titanium extraction tailings
Slag contains: the Al of MgO, 8-20 weight % of CaO, 8-20 weight % of 15-30 weight %2O3, 20-30 weight % SiO2、3-
The TiO of 10 weight %2, 2-13 weight % CaCl2And the free carbon of 5-12 weight %.
It should be noted that may also contain micro magnesium chloride and chlorination in the titanium extraction tailings in addition to above-mentioned substance
Ferrous iron since its amount is less, therefore does not provide.
Method according to the present invention, it is preferable that the titanium extraction tailings and the weight ratio of antichlor are 100:0.1-8,
Further preferably 100:1-4.The dechlorination effect of titanium extraction tailings, and energy can either be effectively realized using this kind of preferred embodiment
Enough maximized reduction antichlor usage amounts.
In the present invention, as long as titanium extraction tailings are mixed with antichlor source, to the specific phase in the antichlor source
It is not particularly limited.Those skilled in the art can accordingly be selected according to the specific type of antichlor.
In the present invention, the antichlor source can be solid powder, or the form of solution.
When antichlor source is solid powder, there is no particular limitation to its granularity by the present invention, preferably less than 0.1mm.
In the present invention, the granularity refers to the maximum linear distance between any two difference on particle.For example,
When the particle is spherical, the granularity refers to its diameter.
The present invention is wider to the range of choice of the antichlor, as long as chlorine can be generated with chloride reaction in titanium extraction tailings
Change hydrogen and/or chlorine, hydrogen chloride and/or chlorine overflow in gaseous form, and then realizes the purpose of dechlorination.
In the present invention, the antichlor can be selected from least one of sulfide, sulphur, acid, salt and oxide.
A preferred embodiment of the invention, the sulfide are iron sulfide, aluminium sulfide, zinc sulphide and vulcanized lead
At least one of.
A preferred embodiment of the invention, it is described acid be sulfuric acid, phosphoric acid, nitric acid, boric acid and oxalic acid in extremely
Few one kind.
A preferred embodiment of the invention, the salt are sulfate and/or sulphite.
A preferred embodiment of the invention, the oxide can be metal oxide, or non-gold
Belong to oxide, it is further preferred that the oxide be silica, iron oxide, aluminium oxide, zinc oxide and lead oxide in extremely
Few one kind.
In the present invention, the most preferably described antichlor is at least one of iron sulfide, ferrous sulfate and boric acid.Inventor
It finds in the course of the research, using this kind of preferred antichlor, the chlorine in calcium chloride can be made to be more likely to form hydrogen chloride, chlorine
Gas, to be removed with gas phase.
There is no particular limitation for temperature and time of the present invention to the calcining, and the temperature of the preferably described calcining is 500-
1200 DEG C, the time of calcining is 10-200min；It is further preferred that the temperature of the calcining be 600-800 DEG C, calcining when
Between be 10-120min.
A preferred embodiment of the invention, the calcining carry out under conditions of being passed through oxygen-containing gas.
Method provided by the invention calcines titanium extraction tailings and antichlor source at a certain temperature, in titanium extraction tailings
Chloride and antichlor and the corresponding metal chloride of oxygen reaction generation, chlorine and hydrogen chloride etc., chlorine and hydrogen chloride etc. with
The form of gas is escaped with air-flow, thus realize the removing of chlorine, meanwhile, free carbon is reacted with oxygen realizes decarburization, in addition carbon
Calcining a part of heat source can also be provided.
The method of titanium extraction tailings dechlorination decarburization provided by the invention does not need water-washing process disclosed in the prior art, the present invention
Inventor be found that while in titanium extraction tailings that chlorine mainly exists in the form of calcium chloride, but there are partial adsorbates chlorine and some
The complicated Cl-containing mineral of indissoluble can make most of chlorine enter liquid phase in the form of an ion and separate by adding water washing, but repeatedly wash
Wash the chlorine for still having 0.2% or more in rear titanium extraction tailings.Therefore, the present inventor passes through addition antichlor source and the side of calcining
Formula realizes the removing together of chlorine and carbon.
In order to it is significantly more efficient removing titanium extraction tailings in chlorine and carbon, the preferably described oxygen-containing gas also contain vapor and/
Or sulfur dioxide, the most preferably described oxygen-containing gas are steam-laden air.Vapor can promote the removing of chlorine, using this kind
Preferred embodiment is more advantageous to the dechlorinating ability for improving the titanium extraction tailings dechlorination decarbonization method.
There is no particular limitation for amount of the present invention to the steam-laden water vapor in air, it is preferable that vapor
Volume content is 5-20%.
Method according to the present invention, titanium extraction tailings dechlorination decarburization generate tail gas in contain hydrogen chloride and/or chlorine,
It is preferred that hydrogen chloride and/or chlorine purification are recycled.Those skilled in the art can select according to site specific, example
Such as, can be absorbed by water mist to be used to produce hydrochloric acid after hydrogen chloride and/or chlorine recycling.
Invention is further explained by the following examples, but the present invention is not limited to this.
Titanium extraction tailings main chemical compositions used in following embodiment and comparative example are as shown in table 1.
Table 1
| Ingredient | CaO | SiO2 | TiO2 | Al2O3 | MgO | Cl | C |
| Content, weight % | 28 | 25 | 8 | 13 | 8 | 2.5 | 10 |
Wherein, Cl is mainly with CaCl2Form exist, have on a small quantity with MgCl2Or FeCl2Form exists, due to MgCl2With
FeCl2Content it is less, therefore do not provide.
In the present invention, the hydration activity is indicated by hydration activity index, and hydration activity index is big, hydration activity
It is good.The hydration activity index of titanium extraction tailings and treated tailings passes through the measurement of GBT18046-20087 appendix A the method, institute
It states hydration activity index and refers to 28 days indexes；Content of Cl element in titanium extraction tailings passes through ammonium thiocyanate described in GBT176-2008
Volumetric method analysis measures；C element content in titanium extraction tailings is measured by gas volumetric method analysis.
Embodiment 1
Titanium extraction tailings are uniformly mixed the (mass ratio of titanium extraction tailings and iron sulfide with vulcanization iron powder (granularity < 0.1mm)
It for 100:4), is subsequently placed in high temperature resistant reactor, is put into Muffle furnace, be passed through steam-laden air (vapor volume
Content be 10%) under the conditions of, calcine 90min at 700 DEG C, take out it is cooling after, chlorine and carbon contains in measurement treated tailings
Amount and hydration activity index, the results are shown in Table 2.
Embodiment 2
Titanium extraction tailings are mixed with ferrous sulfate aqueous solution (mass ratio of titanium extraction tailings and ferrous sulfate be 100:3.5, mention
The mass ratio of titanium tailings and water is 100:20), it is subsequently placed in high temperature resistant reactor, is put into Muffle furnace, be passed through air item
Under part, calcine 120min at 600 DEG C, take out it is cooling after, the content and hydration activity of chlorine and carbon in measurement treated tailings
Index, the results are shown in Table 2.
Embodiment 3
Titanium extraction tailings are mixed with boric acid aqueous solution (mass ratio of titanium extraction tailings and boric acid be 100:1, titanium extraction tailings and water
Mass ratio be 100:30), be subsequently placed in high temperature resistant reactor, be put into Muffle furnace, in the case where being passed through air conditions, 800
Calcine 20min at DEG C, take out it is cooling after, the content and hydration activity index of chlorine and carbon in measurement treated tailings, as a result such as
Shown in table 2.
Embodiment 4
According to the method for the titanium extraction tailings dechlorination decarburization of embodiment 1, the difference is that, the temperature of calcining is 1000 DEG C.Measurement
The content and hydration activity index of chlorine and carbon in treated tailings, the results are shown in Table 2.
Embodiment 5
According to the method for the titanium extraction tailings dechlorination decarburization of embodiment 1, the difference is that, the gas being passed through in calcination process is sky
Gas, without being passed through steam-laden air.The content and hydration activity index of chlorine and carbon in measurement treated tailings, as a result such as
Shown in table 2.
Embodiment 6
According to the method for the titanium extraction tailings dechlorination decarburization of embodiment 1, the difference is that, vulcanization iron powder is replaced with into identical grain
The zinc oxide of degree.The content and hydration activity index of chlorine and carbon in measurement treated tailings, the results are shown in Table 2.
Comparative example 1
Titanium extraction tailings are handled using multi-stage water wash, washing titanium extraction tailings 20min are added water and stirred by liquid-solid ratio 2:1, after filtering
Washing titanium extraction tailings 20min is added water and stirred by liquid-solid ratio 2:1 again, altogether after 4 times are washed, the tailings that is obtained by filtration that treated.
The content and hydration activity index of chlorine and carbon in measurement treated tailings, the results are shown in Table 2.
Comparative example 2
According to the method for the titanium extraction tailings dechlorination decarburization of embodiment 5, the difference is that, it is added without vulcanization iron powder, titanium will be mentioned
Tailings is under conditions of being passed through air, dinectly bruning.The content and hydration activity index of chlorine and carbon in measurement treated tailings,
The results are shown in Table 2.
Table 2
| Chlorine, weight % | Carbon, weight % | Hydration activity index, % | |
| Untreated titanium extraction tailings | 2.5 | 10 | 115 |
| Embodiment 1 | 0.055 | 2.6 | 105 |
| Embodiment 2 | 0.058 | 0.9 | 105 |
| Embodiment 3 | 0.056 | 1.0 | 103 |
| Embodiment 4 | 0.05 | 0.3 | 43 |
| Embodiment 5 | 0.09 | 2.5 | 107 |
| Embodiment 6 | 0.1 | 2.1 | 105 |
| Comparative example 1 | 0.26 | 9.5 | 103 |
| Comparative example 2 | 0.7 | 3.2 | 106 |
As can be seen from the above Examples and Comparative Examples, the method and process letter of titanium extraction tailings dechlorination decarburization provided by the invention
List, process is short and dechlorination decarburization effect is good.It can be seen that from the data of embodiment 1 and comparative example 1 using existing method for washing not
Chlorine and carbon can effectively be removed, can be seen that from the data of embodiment 5 and comparative example 2 do not add antichlor can not be by chlorine
It is effectively removed with carbon, can be seen that from the data of embodiment 1 and embodiment 5 and be passed through the sky containing vapor in calcination process
Gas is more conducive to the removing of chlorine.Chlorinity in the preferred case, can be reduced to 0.06% hereinafter, same by method provided by the invention
When free carbon content be reduced to 1% hereinafter, realizing the purpose that uses as slag micropowder of titanium extraction tailings.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (9)
1. a kind of method of titanium extraction tailings dechlorination decarburization, which is characterized in that this method comprises:
(1) titanium extraction tailings are mixed with antichlor source；
(2) mixture obtained by step (1) is calcined；
Wherein, antichlor is selected from least one of sulfide, sulphur, acid, salt and oxide, the calcining be passed through it is oxygenous
It is carried out under conditions of body, which includes steam-laden air；
The sulfide is at least one of iron sulfide, aluminium sulfide, zinc sulphide and vulcanized lead；
The acid is at least one of sulfuric acid, phosphoric acid, nitric acid, boric acid and oxalic acid；
The salt is sulfate and/or sulphite；
The oxide is at least one of silica, iron oxide, aluminium oxide, zinc oxide and lead oxide.
2. according to the method described in claim 1, wherein, the weight ratio of the titanium extraction tailings and antichlor is 100:0.1-8.
3. according to the method described in claim 1, wherein, the weight ratio of the titanium extraction tailings and antichlor is 100:1-4.
4. according to the method described in claim 1, wherein, the antichlor source is solid powder and/or solution form.
5. according to the method described in claim 1, wherein, the antichlor be in iron sulfide, ferrous sulfate and boric acid at least
It is a kind of.
6. according to the method described in claim 1, wherein, the temperature of the calcining is 500-1200 DEG C；The time of the calcining
For 10-200min.
7. according to the method described in claim 1, wherein, the temperature of the calcining is 600-800 DEG C；The time of the calcining is
10-120min。
8. method described in any one of -4 according to claim 1, wherein on the basis of the total weight of the titanium extraction tailings,
The titanium extraction tailings contain: the Al of MgO, 8-20 weight % of CaO, 8-20 weight % of 15-30 weight %2O3, 20-30 weight
Measure the SiO of %2, 3-10 weight % TiO2, 2-13 weight % CaCl2And the free carbon of 5-12 weight %.
9. method described in any one of -4 according to claim 1, wherein contain in the tail gas that titanium extraction tailings dechlorination decarburization generates
There are hydrogen chloride and/or chlorine, this method further includes recycling hydrogen chloride and/or chlorine purification.
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| CN107572526B (en) * | 2017-09-12 | 2021-02-02 | 攀钢集团研究院有限公司 | Method for decarbonizing carbide slag powder |
| CN108191280B (en) * | 2018-02-28 | 2020-12-29 | 攀钢冶金材料有限责任公司 | Method for dechlorinating and decarbonizing chlorination tailings and concrete admixture |
| CN108315512B (en) * | 2018-02-28 | 2019-12-31 | 攀钢冶金材料有限责任公司 | Method for dechlorinating and decarbonizing titanium extraction tailings |
| CN108516716A (en) * | 2018-04-25 | 2018-09-11 | 攀钢集团攀枝花钢铁研究院有限公司 | The dechlorination process of titanium extraction tailings and the preparation process of slag micropowder |
| CN109252053B (en) * | 2018-11-14 | 2020-06-23 | 西南科技大学 | Method for extracting titanium, carbon and chlorine components from titanium-containing slag by virtue of sectional roasting separation |
| CN110002779A (en) * | 2019-05-17 | 2019-07-12 | 攀钢集团攀枝花钢铁研究院有限公司 | With the method for titanium extraction tailings production slag micropowder |
| CN110127740A (en) * | 2019-05-28 | 2019-08-16 | 重庆大学 | A kind of titanium extraction tailings dechlorination decarbonization method of heterogeneous reaction collaboration |
| CN111847943A (en) * | 2020-07-17 | 2020-10-30 | 攀钢集团研究院有限公司 | Slag micro powder and preparation method thereof |
| CN112588799B (en) * | 2020-11-16 | 2021-11-02 | 浙江浙能技术研究院有限公司 | Method for dechlorinating dried ash |
| CN113699404B (en) * | 2021-08-25 | 2022-06-24 | 苏州大学 | Composite salt for purifying aluminum waste and preparation and use methods thereof |
| CN114740143B (en) * | 2022-04-12 | 2023-10-27 | 四川大学 | Deep dechlorination method and device based on occurrence form of chloride ions in chlorination tailings |
| CN115351053B (en) * | 2022-09-23 | 2023-06-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of chlorination tailings |
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