CN104056841A - Processing method of titanium extraction tailings - Google Patents
Processing method of titanium extraction tailings Download PDFInfo
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- CN104056841A CN104056841A CN201310288715.7A CN201310288715A CN104056841A CN 104056841 A CN104056841 A CN 104056841A CN 201310288715 A CN201310288715 A CN 201310288715A CN 104056841 A CN104056841 A CN 104056841A
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Abstract
The invention provides a processing method of titanium extraction tailings. The titanium extraction tailings contain a water soluble chloride; the method includes washing the titanium extraction tailings with water, so that the content of chlorine elements in the processed titanium extraction tailings is below 0.06 wt%. Through the processing method of the titanium extraction tailings, the titanium extraction tailings with the chlorine element content below 0.06% can be obtained.
Description
Technical field
The present invention relates to vanadium and titanium resources comprehensive utilization field, concrete relate to a kind of processing method of carrying titanium tailings.
Background technology
Titanium tetrachloride is the important intermediate raw material of producing titanium sponge and titanium dioxide, both at home and abroad the general high titanium slag (TiO that adopts
2content is in 90% left and right) allocate carbon dust into, under high temperature (950 DEG C of left and right) condition, carry out chlorination reaction producing titanium tetrachloride t 5 bx with chlorine.
Climbing steel (group) company adopts the vanadium titano-magnetite slag that carries out producing after blast furnace process (to be commonly called as " blast furnace slag ", wherein TiO
2content is in 20% left and right), blast furnace slag at high temperature adds carbon melting and obtains carbide slag.Generally, just can there is chlorination (being commonly called as " low temperature chlorination ") reaction in carbide slag key reaction composition TiC, thereby the titanium in " blast furnace slag " is carried out to extraction and application in the time of apparent 400 DEG C.
The content of participating in the main component TiC of low temperature chlorination reaction in carbide slag is only 12-15 % by weight, even if TiC is chlorinated the consumption that reacts completely, still the residue (carrying titanium tailings) after can chlorination reactions more than residual 85 % by weight, in other words, in carbide slag, compositions more than 85 % by weight has been transformed into and has carried titanium tailings.
Because TiC chlorination reaction is a violent exothermic reaction, carbide slag easily produces localized hyperthermia in chlorination furnace, thereby make chlorination reaction except the main reaction of TiC, also be accompanied by the side reaction of the elements such as vanadium in carbide slag, iron, calcium, magnesium, manganese, band is served water soluble chloride and is stayed and carry in titanium tailings, contain chlorine element owing to carrying in titanium tailings, limited effective utilization of carrying titanium tailings.How disposal and utilization is carried titanium tailings is an important step extracting titanium in steel climbing high slag.
At present, also do not carry correlative study and the reported in literature of processing, recovery and the utilization of titanium tailings both at home and abroad.
Summary of the invention
The object of this invention is to provide a kind of processing method of carrying titanium tailings, the method can effectively reduce the content of Cl element of carrying in titanium tailings, thereby makes the titanium tailings of carrying after treatment can realize refuse reclamation.
The present invention studies discovery, carrying in titanium tailings of being changed by carbide slag contains water soluble chloride, in common buildings material, the content requirement of chlorine element is less than 6/10000ths, could meet conventional building material or the needs as cement additire, and changed by carbide slag carry titanium tailings, its content of Cl element, generally in 2-5 % by weight, causes the application of carrying titanium tailings to be restricted.Therefore, the present inventor reduces the content of carrying chlorine element in titanium tailings by washing, realized the refuse reclamation of carrying titanium tailings, the filtrate obtaining is carried out to calcium chloride recycling after washing filtering simultaneously, realizes the comprehensive utilization of carrying titanium tailings.
The invention provides a kind of processing method of carrying titanium tailings, described in carry titanium tailings and contain water soluble chloride, wherein, the method comprises washes the described titanium tailings of carrying, making the treated content of carrying chlorine element in titanium tailings is below 0.06 % by weight.
Pass through technique scheme, wash carrying titanium tailings, the content that makes to carry the chlorine element in titanium tailings is reduced to below 0.06 % by weight, greatly reduce the chlorine element existing with ionic forms to proposing the impact of titanium tailings application, realize the recycling of the refuse of carrying titanium tailings, and having solved the processing difficult problem of the discarded object of long-term puzzlement enterprise, energy-saving and emission-reduction, have alleviated environmental pressure.
Other features and advantages of the present invention are described in detail the detailed description of the invention part subsequently.
Brief description of the drawings
Accompanying drawing is to be used to provide a further understanding of the present invention, and forms a part for description, is used from explanation the present invention, but is not construed as limiting the invention with detailed description of the invention one below.In the accompanying drawings:
Fig. 1 is the process chart of a kind of embodiment of a kind of processing method of carrying titanium tailings provided by the invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.Should be understood that, detailed description of the invention described herein only, for description and interpretation the present invention, is not limited to the present invention.
The invention provides a kind of processing method of carrying titanium tailings, described in carry titanium tailings and contain water soluble chloride, wherein, the method comprises washes the described titanium tailings of carrying, making the treated content of carrying chlorine element in titanium tailings is below 0.06 % by weight.
The processing method of carrying titanium tailings described in provided by the invention is mainly, with fresh water or the chloride aqueous solution, the described titanium tailings of carrying is stirred to washing, the described water soluble chloride of carrying in titanium tailings is dissolved out, until the described content of Cl element of carrying in titanium tailings is reduced to below 0.06 % by weight.The described titanium tailings of carrying can be the various titanium tailings of carrying of this area routine, for example, can for content of Cl element be 2-5 % by weight carry titanium tailings.
In the present invention, described in to carry the water soluble chloride that contains in titanium tailings can be the water soluble chloride conventionally containing in titanium tailings of carrying well known by persons skilled in the art, can be for example the chloride of one or more elements in iron, calcium, magnesium and manganese.
Proposing method the present invention that titanium tailings washes and there is no special requirement described, can be any one washing methods well known by persons skilled in the art.Washing number of times also do not limit, can once wash also and can repeatedly wash, as long as can make through washing the content of carrying chlorine element in titanium tailings after treatment be 0.06 % by weight below.In order to save the consumption of water, the present invention preferably adopts relatively small amount water to carry out repeatedly agitator treating to carrying titanium tailings.Certainly, the number of times of washing is more many is more conducive to obtain that content of Cl element reduces carries titanium tailings, but number of times is more, is unfavorable for improving treatment effeciency, is also unfavorable for cost-saving.Under preferable case of the present invention, the process of described washing is carried out at least 3 times.The chloride aqueous solution obtaining after washing can be proposed for next group the washing of titanium tailings.Can using water wisely.More preferably in situation, the process of described washing is carried out 3-5 time, and the content that is conducive to obtain chlorine element is to carry titanium tailings below 0.06 % by weight, simultaneously to the chlorion in washings, is also a kind of effectively enrichment.
In the present invention, under preferable case, in each water-washing process, the weight ratio of the consumption of carrying titanium tailings and cleaning solution to be washed is 1:0.5-3, more preferably 1:1.
The present invention does not have special requirement to the cleaning solution adopting in water-washing process, described cleaning solution can be fresh water (for example running water, or not with to carry titanium tailings contacted and have the water of washing chlorion ability) or the chloride aqueous solution, the described chloride aqueous solution is to separate with the treated titanium tailings of carrying the liquid obtaining after washing.
In the present invention, to a collection of, when carrying titanium tailings and repeatedly washing, the filtrate obtaining can be washed the titanium tailings of carrying of other batches.Under preferable case, described in carry titanium tailings to wash for the last time the cleaning solution of employing be fresh water.
In the present invention, the processing method of carrying titanium tailings described in can also comprise: carry titanium tailings for many batches and synchronously wash, and the chlorinated water solution obtaining after titanium tailings is washed and separated of carrying of last batch is washed for the titanium tailings of carrying to latter a batch.In this case, preferably, the last washing of the chlorinated water solution that obtains after washing and separating be the fresh titanium tailings of carrying.In the present invention, the described fresh titanium tailings of carrying refers to and not to carry titanium tailings through washing.Adopt method of the present invention, carry titanium tailings to wash for the last time the cleaning solution of employing be fresh water when described, and the last washing of the described chlorinated water solution obtaining after washing and separating is fresh while carrying titanium tailings, can the content that obtains chlorine element be below 0.06 % by weight carry titanium tailings in, using water wisely most effectively.
In the present invention, filtrate is processed and mainly referred to filtrate is carried out to calcium chloride recycling.Filtrate is carried out to calcium chloride recycling can adopt any one method well known by persons skilled in the art to carry out.Under preferable case of the present invention, adopt following methods to process: first adopting alkaline matter (being preferably calcium oxide or milk of lime) to regulate the pH of filtrate is that 10(is under this pH value environment, iron, magnesium and manganese ion in filtrate form Precipitation, but most of calcium ion still exists with ionic condition) make one or more ions in iron, magnesium and the manganese in this filtrate form Precipitation, stir after 5-10min, if the pH of filtrate still remains on 10 filtrations, then the filtrate of filtering gained is carried out to decompression distillation, reclaim calcium chloride crystal.
Need to carry out calcium chloride recycling to filtrate time, the filtrate at every turn producing directly can be carried out to calcium chloride recycling, also the filtrate that has more generation can be collected and once carries out calcium chloride recycling.Can need to specifically select according to practical operation, the present invention does not have special requirement.
Provided by the inventionly put forward a kind of preferred embodiment that titanium tailings washes and can flow process as shown in Figure 1 carry out described.As shown in Figure 1, to carry titanium tailings and carry out 3-5 washing, in the process of each washing, the weight ratio of the consumption of carrying titanium tailings and cleaning solution to be washed is 1:0.5-3, and after washing with the treated washing process of carrying titanium tailings and separate the liquid obtaining and can carry out next group and carry titanium tailings, particularly, put forward the process that titanium tailings washes and can comprise the following steps described:
(1) get three batches and carry titanium tailings and be expressed as X, Y, Z, with fresh water S-1 successively to carrying titanium tailings X, Y, Z carry out agitator treating and filter, and obtain filter residue X-1, Y-1, Z-1.The filtrate obtaining is reclaimed pending;
(2) successively filter residue X-1, Y-1, Z-1 carried out respectively agitator treating and filtered with fresh water S-2, obtaining filter residue X-2, Y-2, Z-2.By the filtrate obtaining with carry titanium tailings Y
1(carrying titanium tailings for the 4th batch) carried out agitator treating and filtered, and obtains filter residue Y
1-1, the filtrate obtaining is reclaimed pending;
(3) with fresh water S-3 successively to filter residue X-2, Y-2, Z-2, Y
1-1 carries out agitator treating and filtration, obtains filter residue X-3, Y-3, Z-3, Y
1-2, wherein, the content of the chlorine element of filter residue X-3 is below 0.06 % by weight.By the filtrate obtaining with carry titanium tailings Z
1(carrying titanium tailings for the 5th batch) carried out agitator treating and filtered, and obtains filter residue Z
1-1, the filtrate obtaining is reclaimed pending;
(4) with fresh water S-4 successively to filter residue Y-3, Z-3, Y
1-2, Z
1-1 washes and filters, and obtains filter residue Y-4, Z-4, Y
1-3, Z
1-2, wherein, the content of the chlorine element of filter residue Y-4 is below 0.06 % by weight.The filtrate obtaining and next group are not carried out to agitator treating and filtered through the titanium tailings of carrying of washing, obtain filter residue, the filtrate obtaining is reclaimed pending;
In the time that titanium tailings is carried in processing continuously, can realize continuous processing according to step (4) continuation operation afterwards in step (4) and carry titanium tailings.
Due to the amount difference (2-5 % by weight) to some extent of carrying titanium tailings and containing chlorine element, be to carry titanium tailings below 0.06 % by weight in order to obtain the content of chlorine element, preferably select the weight ratio of the consumption of carrying titanium tailings and cleaning solution to be washed in the number of times of washing and each washing according to the amount of carrying the chlorine element containing in titanium tailings.
Pending filtrate is carried out to calcium chloride recycling, this processing procedure can comprise: under agitation adding continuously, lentamente milk of lime to regulate the pH of filtrate is 10, stir after 5min, if the pH of filtrate still remains on 10 filtrations, then the filtrate of filtering gained is carried out to decompression distillation, reclaim calcium chloride crystal.
In the present invention, the condition of washing does not have special requirement, and those skilled in the art can select time and the temperature of washing according to actual conditions.Under preferable case, the time of washing is 10-15min, and the present invention does not have special requirement to the temperature of washing yet, can carry out at ambient temperature, can under higher temperature, carry out for the solubility that improves water soluble chloride yet.Under preferable case, the temperature of washing is 15-90 DEG C.In order to reduce washing energy consumption, preferably the temperature of washing is 15-35 DEG C.
In the present invention, the described mode of filtering after titanium tailings is washed of carrying is not had to special requirement, can adopt any one mode well known by persons skilled in the art to carry out, for example simple filtration or suction filtration.The preferred described filter type of the present invention is suction filtration, can further shorten filtration time, enhances productivity.More preferably, will under the described condition that is 0.09Mpa in vacuum after carrying titanium tailings and washing, carry out suction filtration.
In the present invention, under preferable case, also need to be dried to filtering the filter residue that obtains, carry titanium tailings product with what obtain recovery.Dry mode and condition do not have special requirement, can be mode well known by persons skilled in the art and condition.
By the processing method of carrying titanium tailings provided by the invention, can obtain content of Cl element and be and carry titanium tailings below 0.06 % by weight, can be as conventional building material or as cement additire.
Below will describe the present invention by embodiment.In following examples, the content of Cl element of carrying in titanium tailings is analyzed by chemical titration, content of Cl element in filter residue passes through colorimetrically analysing, that measures each batch of using in following examples carries titanium tailings all from Pangang (Group)Panzhihua Iron and Steel Research Institute(PISI) Co., Ltd., this is carried and in titanium tailings, contains iron chloride, calcium chloride, magnesium chloride and manganese chloride, and this content of carrying chlorine element in titanium tailings is 2.5 % by weight.
Embodiment 1
At 30 DEG C, carry out this experiment:
(1) get three batches be respectively 500g carry titanium tailings X, Y, Z put into beaker, filter carrying under the condition that titanium tailings X, Y, Z carry out agitator treating 10min and be 0.09Mpa in vacuum successively with 500mL running water S-1, obtain filter residue X-1, Y-1, Z-1.The filtrate obtaining is reclaimed pending;
(2) successively filter residue X-1, Y-1, Z-1 are carried out respectively to agitator treating 10min with 500mL running water S-2 and the condition that is 0.09Mpa in vacuum under filter, obtain filter residue X-2, Y-2, Z-2.The filtrate obtaining and 500g are carried to titanium tailings Y
1(carrying titanium tailings for the 4th batch) carried out agitator treating and filtered, and obtains filter residue Y
1-1, the filtrate obtaining is reclaimed pending;
(3) use 500mL running water S-3 successively to filter residue X-2, Y-2, Z-2 and Y
1-1 carry out respectively agitator treating 10min and the condition that is 0.09Mpa in vacuum under filter, obtain filter residue X-3, Y-3, Z-3 and Y
1-2, wherein, the content that obtains chlorine element after filter residue X-3 is dry be 0.03 % by weight carry titanium tailings product.By the filtrate obtaining with carry titanium tailings Z
1(carrying titanium tailings for the 5th batch) carry out agitator treating 10min and the condition that is 0.09Mpa in vacuum under filter, obtain filter residue Z
1-1, the filtrate obtaining is reclaimed pending;
(4) use 500mL running water S-4 successively to filter residue Y-3, Z-3, Y
1-2 and Z
1-1 carry out respectively agitator treating 10min and the condition that is 0.09Mpa in vacuum under filter, obtain filter residue Y-4, Z-4, Y
1-3, Z
1-2, wherein, the content that obtains chlorine element after filter residue Y-4 is dry be 0.03 % by weight carry titanium tailings product.The filtrate obtaining and next group are carried to titanium tailings and carry out agitator treating and filter, obtain filter residue, the filtrate obtaining is reclaimed pending.
Under agitation add continuously, lentamente milk of lime to regulate the pH of filtrate pending filtrate and be 10, still remain on 10 filtrations at the pH that stirs filtrate after 5min clock, filtrate is carried out to decompression distillation, reclaim calcium chloride dihydrate.
Embodiment 2
(1) get 1500g and carry titanium tailings X and put into beaker, carry out agitator treating 10min and filter with 1500mL running water, obtain filter residue X-1.The filtrate obtaining is reclaimed pending;
(2) with 1500mL running water, above-mentioned filter residue X-1 carried out agitator treating 10min and filtered, obtaining filter residue X-2.The filtrate obtaining is reclaimed pending;
(3) with 1500mL running water, above-mentioned filter residue X-2 carried out agitator treating 10min and filtered, obtaining filter residue X-3.Wherein, the content that obtains chlorine element after filter residue X-3 is dry be 0.05 % by weight carry titanium tailings product.
(4) above-mentioned filtrate is merged, place, until natural evaporation volume during about 1000 milliliters, under agitation adding continuously, lentamente milk of lime to regulate the pH of filtrate pending filtrate is 10, after the pH of filtrate being remained on to 10 after stirring 5min clock, filter, then filtrate is carried out to decompression distillation, dry, reclaim calcium chloride dihydrate.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned detailed description of the invention, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible combinations.
In addition, between various embodiment of the present invention, also can be combined, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. put forward a processing method for titanium tailings, described in carry titanium tailings and contain water soluble chloride, it is characterized in that, the method comprises washes the described titanium tailings of carrying, making the treated content of carrying chlorine element in titanium tailings is below 0.06 % by weight.
2. method according to claim 1, wherein, described in carry chlorine element in titanium tailings content be 2-5 % by weight.
3. method according to claim 1, wherein, the process of described washing is carried out 3-5 time.
4. method according to claim 3, wherein, in the process of each washing, the weight ratio of the consumption of carrying titanium tailings and cleaning solution to be washed is 1:0.5-3.
5. method according to claim 4, wherein, described cleaning solution is fresh water or the chloride aqueous solution, the described chloride aqueous solution is to separate with the treated titanium tailings of carrying the liquid obtaining after washing.
6. according to the method described in any one in claim 3-5, wherein, described in carry titanium tailings to wash for the last time the cleaning solution of employing be fresh water.
7. according to the method described in any one in claim 3-5, wherein, described method also comprises: carry titanium tailings for many batches and synchronously wash, and the chlorinated water solution obtaining after titanium tailings is washed and separated of carrying of last batch is washed for the titanium tailings of carrying to latter a batch, wherein, the last washing of the chlorinated water solution that obtains after washing and separating be the fresh titanium tailings of carrying.
8. method according to claim 1, wherein, the condition of washing comprises: the time is 10-15min, temperature is 15-90 DEG C.
9. method according to claim 1, wherein, described water soluble chloride is the chloride of one or more elements in iron, calcium, magnesium and manganese.
10. method according to claim 1, wherein, the method also comprises carries out calcium chloride recycling to filtrate.
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Cited By (11)
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| CN105271857A (en) * | 2015-11-17 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Online dechlorination technology of chlorination process tailing slag extracted titanium |
| CN105385855A (en) * | 2015-11-17 | 2016-03-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Dechlorination method for chlorination process titanium extracting tailing slag |
| CN110605293A (en) * | 2019-09-11 | 2019-12-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Initial dechlorination process for titanium extraction tailings |
| CN111573718A (en) * | 2020-05-25 | 2020-08-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium extraction tailings |
| CN111646499A (en) * | 2020-06-29 | 2020-09-11 | 攀钢集团钒钛资源股份有限公司 | Titanium extraction tailing washing treatment method |
| CN111961774A (en) * | 2020-08-06 | 2020-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Resource utilization method of titanium extraction tailing dechlorination wastewater |
| CN112588799A (en) * | 2020-11-16 | 2021-04-02 | 浙江浙能技术研究院有限公司 | Method for dechlorinating dried ash |
| CN113372029A (en) * | 2021-07-21 | 2021-09-10 | 攀钢冶金材料有限责任公司 | Low-carbon type super-sulfate cement, preparation method thereof and cement mortar |
| 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 |
| CN113563891A (en) * | 2021-08-31 | 2021-10-29 | 西南科技大学 | Arsenic-containing soil improvement liquid, preparation method thereof and method for treating arsenic-containing soil |
| CN113620628A (en) * | 2021-08-31 | 2021-11-09 | 西南科技大学 | Recycling method of chlorine element in titanium extraction slag |
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| CN105385855A (en) * | 2015-11-17 | 2016-03-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Dechlorination method for chlorination process titanium extracting tailing slag |
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| CN111573718B (en) * | 2020-05-25 | 2022-07-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium extraction tailings |
| CN111646499A (en) * | 2020-06-29 | 2020-09-11 | 攀钢集团钒钛资源股份有限公司 | Titanium extraction tailing washing treatment method |
| CN111961774A (en) * | 2020-08-06 | 2020-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Resource utilization method of titanium extraction tailing dechlorination wastewater |
| CN112588799A (en) * | 2020-11-16 | 2021-04-02 | 浙江浙能技术研究院有限公司 | Method for dechlorinating dried ash |
| CN113372029A (en) * | 2021-07-21 | 2021-09-10 | 攀钢冶金材料有限责任公司 | Low-carbon type super-sulfate cement, preparation method thereof and cement mortar |
| 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 |
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