CN103613127A - Recycling method of low-boiling point matters in titanium tetrachloride production - Google Patents
Recycling method of low-boiling point matters in titanium tetrachloride production Download PDFInfo
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- CN103613127A CN103613127A CN201310616239.7A CN201310616239A CN103613127A CN 103613127 A CN103613127 A CN 103613127A CN 201310616239 A CN201310616239 A CN 201310616239A CN 103613127 A CN103613127 A CN 103613127A
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Abstract
The invention relates to a recycling method of low-boiling point matters in titanium tetrachloride production, belonging to the field of titanium tetrachloride production. A technical problem to be solved in the invention is to provide a method of recycling the low-boiling point matters in titanium tetrachloride production, which is low in cost and less in energy consumption. The recycling method comprises the following steps: a, reacting, wherein a mixture formed by mixing the low-boiling point matters with mud slurry or low-boiling point matters are used as materials to react with TiO2, reaction equation is as follows: TiO2+SiCl4=TiCl4+SiO2, and in the reaction process, temperature is not lower than 650 DEG C and pressure is not higher than 500 Pa; b, recycling, wherein TiCl4 generated in the last step is recycled, and generated SiO2 is exhausted. The method disclosed by the invention not only avoids carrying out neutralizing treatment on the low-boiling point matters and mud slurry, and is small in pollution, but also has less devices, a high SiCl4 utilization rate, high TiCl4 yield, and obvious economic benefits and social benefits.
Description
Technical field
The recoverying and utilizing method that the present invention relates to low boilers in titanium tetrachloride production, belongs to titanium tetrachloride production field.
Background technology
In titanium tetrachloride production technique, mainly comprise two production processes: chloride process and refining step.First in chloride process, rich titanium slag and the refinery coke of high hopper join transfer roller by certain ratio of components, add in chlorination furnace continuously, and pass into chlorine through transfer roller, and at high temperature reaction generates TiCl
4, under the effect of system negative pressure, taken out of chlorination furnace simultaneously.The gas of taking out of from chlorination furnace is except TiCl
4also mainly contain SiCl outward,
4, AlCl
3, FeCl
3, MgCl
2, CaCl
2, HCl, CO, CO
2and part MnCl
2, FeCl
2with part solid particulate.When they enter dust-precipitator, due to reduction of speed cooling effect, wherein AlCl
3, FeCl
3, FeCl
2deng the major part of high boiling point muriate and the solid particulate taken out of by air-flow, be condensed and deposit, form dirt slag.By dust-precipitator mixed gas out, enter titanium tetrachloride elution circuit, the titanium tetrachloride that cooling drip washing obtains contains a lot of impurity, after sedimentation, filtering, obtains the thick TiCl of faint yellow or reddish-brown
4, produce a large amount of mud simultaneously.From elution circuit gas out, finally enter exhaust treatment system, through washing and two-stage milk of lime or NaOH solution neutralizing treatment, then enter atmosphere by chimney.For the refining step stage, the crude titanic chloride that chloride process is produced adopts fore-distillation method to remove FeCl
3, AlCl
3, VOCl
2deng high-boiling-point impurity, adopt Low-valent Titanium substitution method to remove and TiCl
4the VOCl that boiling point is close
3, with one-level rectificating method, remove SiCl subsequently
4etc. low boilers impurity, wherein two-stage rectification is further except high boiling product impurity, to produce smart TiCl
4.After one-level rectifying, in the low boilers that one-level rectifying produces, contain SiCl
4and TiCl
4, but TiCl
4content is in the majority, SiCl
4content is only 20% left and right; Through additional rectifying, reclaim TiCl in low boilers
4, SiCl in low boilers now
4content high to 60%, the low boilers finally producing is outer row after utilizing lime slurry neutralization to process.
In titanium tetrachloride production technique, the TiCl that contains 40% left and right in the mud that chloride process produces
4, it is met water hydrolysis and is acid, and directly outer row can cause environmental pollution.At present to the processing mode of mud, be: mud is returned into chlorination furnace and reclaimed, or outer row after utilizing lime slurry neutralization to process.There is following problem in these two kinds of processing modes: mud is returned in chlorination furnace and reclaimed, wherein, when the solid matter content of mud is higher, need utilize the TiCl of output
4after diluting, just can return in chlorination furnace, can cause part TiCl like this
4drip washing repeatedly, energy consumption is large; And adopt lime slurry neutralization to process, in mud, contain the TiCl that weight ratio is 40% left and right
4, directly processing not only causes TiCl
4waste, affect titanium yield, and in treating processes, need with large quantities of lime breast, cost is high.Yet, in the low boilers that in refining step, two stage rectification produces, mainly contain SiCl
4and TiCl
4, SiCl
4with TiCl
4the same, meet after water is hydrolyzed and be acid.At present, to the processing mode of low boilers, be also to adopt lime slurry neutralization to process rear outer row, so also can cause TiCl in low boilers
4waste, titanium yield is low; In addition, a large amount of milk of lime is used, and expense is high; Meanwhile, in treating processes, the acid mist of formation, can corrode field apparatus and the health that affects staff.
Defect based on above-mentioned processing mud and low boilers method, the present invention will provide a kind of by the scheme of low boilers comprehensive reutilization, to improve the output of titanium tetrachloride and to reduce production costs.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of cost is low, the method for less energy consumption is recycled lower boiling in titanium tetrachloride production technique, and it comprises the following steps:
A, reaction: take that low boilers and mud are mixed to form mixture or low boilers is raw material and TiO
2reaction, reaction equation is: TiO
2+ SiCl
4=TiCl
4+ SiO
2, in reaction process, temperature is not less than 650 ℃, and pressure is not higher than 500Pa;
B, recovery: reclaim the TiCl generating in above-mentioned steps
4, discharge the SiO generating
2;
Wherein, in a step, mud is the material that during titanium tetrachloride is produced, chloride process sedimentation produces, and low boilers is the material producing in refining step during titanium tetrachloride is produced.
During key of the present invention is titanium tetrachloride to produce, low boilers is recycled, or mud is recycled together with low boilers, to improve titanium yield, increases the output of titanium tetrachloride.
Further, in mud, contain the TiCl that weight ratio is 40% left and right
4, in low boilers, mainly contain SiCl
4and TiCl
4.
Further, SiCl in the low boilers of recycling and mud
4and TiCl
4for liquid.
Wherein, when in mud, solid matter content is greater than 500g/L, after mixing of low-boiling thing and mud make the solid matter content of mixture be 300g/L～500g/L, then with TiO
2reaction; When solid matter content is less than 500g/L in mud, adopt low boilers and TiO
2reaction.
Further, when in mud, solids content is less than 500g/L, mud directly returns to chlorination furnace, by chloride process and refining step, is filtered, is purified to reclaim TiCl
4.
Wherein, mixture and TiO
2during reaction, mixture adds and TiO with flow 0.5～1.8t/h
2reaction.
Further, mixture and TiO
2during reaction, the preferred streams weight range that adds mixture is 0.5～1.0t/h.
Wherein, low boilers and TiO
2during reaction, low boilers adds and TiO with flow 0.5～1.8t/h
2reaction.
Further, low boilers and TiO
2during reaction, the preferred streams weight range that adds low boilers is 0.5～1.0t/h.
Wherein, a step, adopts spray gun and atomizer to combine and uses after atomized feed (mixture or low boilers), then with TiO
2reaction.
Wherein, the temperature of reaction preferable range of a step is 650～725 ℃.
Wherein, the reaction pressure preferable range of a step is-50～300Pa.
Wherein, mixture or low boilers and TiO in above-mentioned a step
2at chlorination furnace roof, react.
Further, TiO
2for former reactant, i.e. titanium slag in chlorination furnace.
Beneficial effect of the present invention is: 1, method provided by the invention is by SiCl in mixture or low boilers
4with TiO
2reaction, improves SiCl
4utilization ratio and TiCl
4output; 2, avoid milk of lime and low boilers, mud neutralizing treatment, reduce TiCl
4production cost; 3, reclaim TiCl in mud and low boilers
4, improve titanium yield; 4, avoid TiCl in mud
4and SiCl in low boilers
4and TiCl
4hydrolysis forms the corrosion of acid mist to equipment, and reduces the impact healthy on staff; 5, technical solution of the present invention, equipment is few, and less investment is simple to operate, has obvious economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the schema of low boilers recoverying and utilizing method of the present invention.
Embodiment
The technical scheme that the invention is further illustrated by the following examples.
The recoverying and utilizing method of low boilers in titanium tetrachloride production, comprises the following steps:
A, reaction: take and after low boilers and mud mix, form mixture or low boilers is raw material and TiO
2reaction, reaction equation is: TiO
2+ SiCl
4=TiCl
4+ SiO
2, in reaction process, temperature is not less than 650 ℃, and pressure is not higher than 500Pa;
B, recovery: reclaim the TiCl generating in above-mentioned steps
4, discharge the SiO generating
2;
Wherein, in a step, mud is the material that during titanium tetrachloride is produced, chloride process sedimentation produces, and low boilers is the material that during titanium tetrachloride is produced, refining step produces.
Wherein, TiCl in above-mentioned b step
4with the TiCl generating in former chlorination furnace
4, by follow-up elution circuit and refining step to purify, to reclaim.
Wherein, when in mud, solid matter content is greater than 500g/L, after mixing of low-boiling thing and mud make the solid matter content of mixture be 300g/L～500g/L, then with TiO
2reaction; When solid matter content is less than 500g/L in mud, adopt low boilers and TiO
2reaction.In mixture, solid matter is mainly the high boiling product that in former chlorination furnace, chlorination reaction produces, as FeCl
3, FeCl
2, MnCl
2and unreacted titanium slag and refinery coke.
Wherein, mixing mud and low boilers, adopt conventional mechanical to stir mud and low boilers evenly mixed.
Wherein, mixture and TiO
2during reaction, mixture adds and TiO with flow 0.5～1.8t/h
2reaction.
Preferably, in order to make SiCl
4and TiO
2sufficient reacting, and make full use of remaining temperature in former chlorination furnace, mixture adds and TiO with flow 0.5～1.0t/h
2reaction.
Wherein, when the solid matter content of mud is greater than 500g/L, mud is returned to chlorination furnace larger to the loss of pump, therefore mixing mud and low boilers are to reduce solid matter content wherein; If the solid matter content of mixture is still too high, when surpassed 500g/L, larger to the loss of pump or other equipment; In mixture solid matter content hour, SiCl in mixture
4content is higher, SiCl
4can all not participate in reaction, cause SiCl
4enrichment, the burden of increase refining step; Therefore controlling the solid matter content scope of mixture is 300g/L～500g/L.
Further, when the flow of mixture is excessive, reaction not exclusively, causes SiCl
4enrichment, mixture may enter chlorination reaction in the former stove of chlorination furnace bottom influences; And mixture flow rate is too small, cannot make full use of the waste heat of former chlorination furnace; Therefore be 0.5～1.8t/h by controlling the flow of mixture.
Wherein, low boilers and TiO
2during reaction, low boilers adds and TiO with flow 0.5～1.8t/h
2reaction.
Preferably, for making sufficient reacting in a step, low boilers adds and TiO with flow 0.5～1.0t/h
2reaction.
Further, when the flow of low boilers is excessive, SiCl
4cannot total overall reaction, cause SiCl
4enrichment low boilers enters chlorination reaction in the former stove of chlorination furnace bottom influences; Low boilers flow is too small, can not make full use of the waste heat of chlorination furnace; Therefore be 0.5～1.8t/h by controlling the flow of low boilers.
Further, mixture or low boilers are by above-mentioned flow range and TiO
2reaction, SiCl
4content is comparatively sufficient, and basic fully reaction, can not cause SiCl
4enrichment again.Because impurity in mixture or low boilers is mainly FeCl
3, FeCl
2, titanium slag, refinery coke etc., its content is less and composition is simple, substantially not with TiO
2reaction, so in a step, there is not side reaction.Wherein, a step, in order to make full use of the waste heat of chlorination furnace, reacts fully, adopt spray gun and atomizer to combine and use after aerosolized mixture or low boilers, then with TiO
2reaction.
Wherein, due to the impact of chlorination reaction in former chlorination furnace, chlorination furnace head temperature is 650～850 ℃, and pressure is-500～500Pa.By controlling the flow of mixture or low boilers and adjusting factory's actual operational parameters, to make a step reaction temperature be 650～725 ℃, and reaction pressure is-50～300Pa, makes a step reaction abundant, SiCl
4utilization ratio is high.
Wherein, mixture or low boilers and TiO in a step
2at chlorination furnace top, carry out, therefore do not affect chlorination reaction in former stove.
The equipment the present invention relates to is that contriver sets out according to actually operating, but the present invention program is not limited to limited condition, everyly belongs to change and the conversion that above-mentioned scope is done, and all should belong to the present invention.Below by specific embodiment, further illustrate the present invention program.
Embodiment:
Below, contriver has done respectively mixture and low boilers recycles to produce TiCl
4embodiment, the conditional parameter wherein relating to and recovery utilization rate are as shown in embodiment in table 1 and table 2; And contriver is to adopt lime slurry neutralization to process mud and low boilers method production TiCl
4comparative example make comparisons.Table 1 is identical with the material content of producing titanium tetrachloride in each experimental group in table 2, and in chlorination furnace, the content of rich titanium slag, refinery coke and chlorine is identical.When actually operating, pressure is wayward is concrete value, is generally less scope.
In following table 1 and 2, SiCl
4utilization ratio refers to and TiO
2the SiCl of reaction
4with SiCl in the mixture that participates in recycling or low boilers
4ratio; TiCl in embodiment
4the TiCl that output is produced for recycling mixture or low boilers method
4with in former chlorination furnace, produce TiCl
4total amount, and TiCl in comparative example
4output is produced TiCl before being and adopting
4the output of method gained, wherein to produce how many tons of statement TiCl every day
4output; In embodiment, processing cost refers to and recycles mixture or the related equipment of low boilers, the expense of energy consumption, and in comparative example processing cost for adopting lime slurry neutralization to process TiCl
4the mud producing in production and the expense of low boilers, wherein to process the expense of material per ton, expense is average cost simultaneously.
Table 1 mixture different treatment condition is produced TiCl
4comparison
Table 2 low boilers different treatment condition is produced TiCl
4comparison
By table 1 data in 2, can be found out: in the situation that raw material is identical, the inventive method is recycled low boilers to produce TiCl
4compared with former production titanium tetrachloride method, have the following advantages: 1, titanium tetrachloride output increases; 2, avoid adopting the neutralizing treatment of milk of lime to mud and low boilers, pollute little; 3, SiCl
4utilization ratio is high, realizes material comprehensive utilization; 4, the present invention program does not need newly added equipment and station, and mainly utilizes the negative pressure of the interior waste heat of former chlorination furnace and system, and energy consumption is low, has obvious economic benefit and social benefit.
Claims (10)
- Titanium tetrachloride produce in the recoverying and utilizing method of low boilers, comprise the following steps:A, reaction: take that low boilers and mud are mixed to form mixture or low boilers is raw material and TiO 2reaction, reaction equation is: TiO 2+ SiCl 4=TiCl 4+ SiO 2, in reaction process, temperature is not less than 650 ℃, and pressure is not higher than 500Pa;B, recovery: reclaim the TiCl that above-mentioned steps generates 4, discharge the SiO generating 2;Wherein, in a step, mud is the material that during titanium tetrachloride is produced, chloride process sedimentation produces, and low boilers is the material that during titanium tetrachloride is produced, refining step produces.
- Titanium tetrachloride according to claim 1 produce in the recoverying and utilizing method of low boilers, it is characterized in that: described a step, when in mud, solid matter content is greater than 500g/L, after mixing of low-boiling thing and mud make the solid matter content of mixture be 300g/L～500g/L, then with TiO 2reaction; When solid matter content is less than 500g/L in mud, adopt low boilers and TiO 2reaction.
- 3. the recoverying and utilizing method of low boilers in titanium tetrachloride production according to claim 1, is characterized in that: described a step, mixture and TiO 2during reaction, mixture adds and TiO with flow 0.5～1.8t/h 2reaction.
- 4. the recoverying and utilizing method of low boilers in titanium tetrachloride production according to claim 1, is characterized in that: described a step, mixture and TiO 2during reaction, mixture adds and TiO with flow 0.5～1.0t/h 2reaction.
- 5. the recoverying and utilizing method of low boilers in titanium tetrachloride production according to claim 1, is characterized in that: described a step, low boilers and TiO 2during reaction, low boilers adds and TiO with flow 0.5～1.8t/h 2reaction.
- 6. the recoverying and utilizing method of low boilers in titanium tetrachloride production according to claim 1, is characterized in that: described a step, low boilers and TiO 2during reaction, low boilers adds and TiO with flow 0.5～1.0t/h 2reaction.
- 7. the recoverying and utilizing method of low boilers in producing according to titanium tetrachloride described in claim 1～6 any one, is characterized in that: described a step, raw material adopts spray gun and atomizer to combine and uses after atomization, then with TiO 2reaction.
- 8. the recoverying and utilizing method of low boilers in titanium tetrachloride production according to claim 1, is characterized in that: the temperature of reaction of described a step is 650～725 ℃.
- 9. the recoverying and utilizing method of low boilers in titanium tetrachloride production according to claim 1, is characterized in that: the reaction pressure of described a step is-50～300Pa.
- 10. in producing according to the titanium tetrachloride described in claim 1～9 any one, the recoverying and utilizing method of low boilers, is characterized in that: mixture or low boilers and TiO in described a step 2reaction is reacted in chlorination furnace roof.
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Cited By (4)
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| CN104118905A (en) * | 2014-08-06 | 2014-10-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Refining process of crude titanium tetrachloride |
| CN104192894A (en) * | 2014-08-14 | 2014-12-10 | 仙桃市中星电子材料有限公司 | Refining method of titanium tetrachloride |
| CN111517365A (en) * | 2020-06-10 | 2020-08-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium tetrachloride production method and system |
| CN113912108A (en) * | 2021-11-30 | 2022-01-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for deeply removing impurities in refining of titanium tetrachloride with high vanadium content |
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| CN113912108A (en) * | 2021-11-30 | 2022-01-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for deeply removing impurities in refining of titanium tetrachloride with high vanadium content |
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