CN104772317A - Comprehensive treatment method for waste fused salts and dust collection slag produced through titanium tetrachloride fused salt chlorination - Google Patents
Comprehensive treatment method for waste fused salts and dust collection slag produced through titanium tetrachloride fused salt chlorination Download PDFInfo
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- CN104772317A CN104772317A CN201410014683.6A CN201410014683A CN104772317A CN 104772317 A CN104772317 A CN 104772317A CN 201410014683 A CN201410014683 A CN 201410014683A CN 104772317 A CN104772317 A CN 104772317A
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- fused salt
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Abstract
The present invention discloses a comprehensive treatment method for waste fused salts and dust collection slag produced through titanium tetrachloride fused salt chlorination. The method comprises that: waste fused salts discharged from a fused salt chlorination furnace are crushed, and the crushed slag is subjected to powder grinding; dust collection slag is subjected to beating diffusion to achieve a solid-liquid mixing state; the waste fused salt powder and the solid-liquid mixing state dust collection slag are uniformly mixed into a mixed material; the mixed material is subjected to oxidation calcination under the atmosphere condition of introduction of air and water vapor, the generated hydrogen chloride and the generated chlorine gas pass through a leaching system to generate hydrochloric acid, and the generated waste gas achieves the standard emission; and the calcined caking slag is subjected to crushing screening, an alkali liquid neutralization treatment is performed, and part of the chloride which is not completely removed reacts with an alkali liquid so as to generate the corresponding hydroxide and the corresponding salt water. According to the present invention, the environmental hazards caused by the waste fused salts and the dust collection slag are reduced, the chlorine ions and partial valuable elements in the waste fused salts and the dust collection slag are recovered, and the treated slag with the wide use is obtained.
Description
Technical field
The present invention relates to a kind of integrated conduct method that titanium tetrachloride fused salt chlorimation produces waste fused salt and dust-slag collection.
Background technology
Fused salt chlorimation is that titanium slag and petroleum coke are immersed in fused-salt medium (primarily of KCl, NaCl, MgCl
2, and CaCl
2composition) in, generate TiCl with the chlorine generation chemical reaction passed into
4.Its major advantage to process the high raw material of calcium and magnesium oxides content; Shortcoming produces a large amount of waste fused salts and dust-slag collection, and these solid waste are mostly outdoor at present banks up, and is difficult to process.
In fused salt chlorimation process, the granularity of chlorination temperature, chlorine speed, material and porosity, the composition of joining charcoal amount, chlorine gas concentration, material chlorine when fused-salt medium system all have a significant impact chlorination process.Along with the carrying out of chlorination reaction, not easily can accumulate gradually with the oxide impurity of chlorine generation chemical reaction in material, cause degenerating of molten salt nature, so will according to condition of production periodic exhaustion fused salt.Simultaneously from the mist of chlorination furnace roof effusion, main component is TiCl
4, SiCl
4, AlCl
3, FeCl
3, CO, CO
2and a small amount of FeCl
2, MgCl
2, CaCl
2, MnCl
2the solid particle being less easily entrained by out in addition, enters cooling dust-precipitator, by cooling of slowing down, makes FeCl wherein
2, MgCl
2, CaCl
2, MnCl
2, AlCl
3, FeCl
3contour boiling chlorinated thing and being got off by the solid particle major part that air-flow is taken out of the deposition that is condensed, just defines dust-slag collection.The waste fused salt that fused salt chlorimation process produces mostly is easy molten chloride, complicated component, and direct stacking can cause environmental pollution, stacks, but easily cause the problem such as underground water pollution, salinization soil although domestic after generally adopting limestone vegetation process.The easy deliquescence of dust-slag collection generated discharges pungent gas, and due to containing a large amount of chlorions, meets rainwater drip washing and can cause underground water pollution, even if adopt the mode of deep well injection also to there is problem of environmental pollution.
So adopt rationally effective processing method, the fused salt chlorimation of integrated treatment titanium tetrachloride produces waste fused salt and dust-slag collection, alleviates environmental pollution, seems very important.Namely the present invention is the waste fused salt and the dust-slag collection that propose a kind of reasonable effective method integrated treatment titanium tetrachloride fused salt chlorimation generation, alleviates environmental pollution damage, simultaneously to reach the object of secondary resource comprehensive reutilization.
Summary of the invention
The technical problem to be solved in the present invention is: propose a kind of for the waste fused salt of titanium tetrachloride fused salt chlorimation generation and the integrated conduct method of dust-slag collection, reach the object of resource recycling, and solve during titanium tetrachloride is produced the problem of environmental pollution producing waste fused salt and dust-slag collection and bring.
Technical scheme of the present invention is: first the waste fused salt that Molten salt chlorination furnace is discharged is carried out break process, and by broken sizing powder; Fused salt chlorimation produces dust-slag collection and disperses through making beating, is prepared into solid-liquid mixing shape; Mixing of waste fused salt powder and solid-liquid mixing shape dust-slag collection being prepared burden by a certain percentage is prepared into compound; Compound oxidizing roasting under the atmospheric condition passing into air, steam, most chloride can with oxygen, steam generation chemical reaction, chemical equation (for iron, aluminium chloride) is as follows, various chloride can change corresponding oxide into, and produces a large amount of hydrogen chloride gas, chlorine and oxygen; The hydrogen chloride produced and chlorine are through elution circuit process, and generate hydrochloric acid, the waste gas of generation is up to standard directly emptying; Caking slag after roasting, through crushing and screening, carries out alkali lye neutralisation treatment, and the partial oxidation thing do not removed completely and alkali lye generation chemical reaction, generate corresponding hydroxide and salt solution; The process slag obtained after washing and filtering can be used as construction material, and the industrial brine obtained can be used for chlorine industry after treatment.The program makes the secondary resource discarded be recycled on the one hand, obtains the process slag with extensive use; Also mitigate on the other hand the environmental pollution damage that waste fused salt and dust-slag collection bring.
4FeCl
3+3O
2=2 Fe
2O
3+6Cl
2(1)
2Cl
2+2H
2O=4HCl+O
2(2)
2FeCl
3+3H
2O=2Fe
2O
3+6HCl (3)
4AlCl
3+3O
2=2 Al
2O
3+6Cl
2(4)
2Cl
2+2H
2O=4HCl+O
2(5)
2AlCl
3+3H
2O=2Al
2O
3+6HCl (6)
The fused salt chlorimation waste fused salt slag of described employing, through jaw crushing crusher machine, rear employing flour mill abrasive dust is to 80-160 order.
Described fused salt chlorimation dust-slag collection is pulled an oar at normal temperatures and is dispersed, and is prepared as liquid-solid admixture.
The batching mass ratio 2:1 ~ 1:1 of described waste fused salt slag and dust-slag collection.
Described oxidizing roasting temperature range is 400 ~ 700 DEG C.
Described oxidizing roasting time range is 6 ~ 12h.
Described oxidizing roasting air intake scope is 160 ~ 200L/h.
Described oxidizing roasting equipment is tunnel cave or down-draft kiln.
Described steam intake scope is 50 ~ 100L/h.
Described elution circuit drip washing temperature range is 30 ~ 60 DEG C.
The NaOH concentration range of described alkaline leaching is 0.5-2.5mol/L.
The solid-to-liquid ratio scope of described alkaline leaching is 0.3:1 ~ 1:1.
The temperature range of described alkaline leaching is 45 ~ 80 DEG C.
Beneficial effect of the present invention is embodied in:
1, titanium tetrachloride fused salt chlorimation produces waste fused salt and dust-slag collection discarded object, and this waste fused salt and dust-slag collection output are comparatively large, complicated component, and mostly be easy molten chloride, if stack process, the pollution of environment can be caused, alleviate through process the harm that waste fused salt slag and dust-slag collection cause environment.
2, utilize the method for high temperature oxidation roasting that the most chloride in slag can be made to generate corresponding oxide, chlorine and hydrogen chloride gas to oxygen generation chemical reaction, these gases can obtain hydrochloric acid through elution circuit, to reach the object recycling this part chlorion, solve the recycling problem of secondary resource.
3, by alkaline leaching, chloride residual in fired slags and alkali lye are reacted, changes the deposit of hydroxide into, wash the process slag obtained and extensive use can make construction material.
4, a large amount of industrial brine that process produces may be used for chlorine industry through process, realizes the comprehensive reutilization object of resource.
Process titanium tetrachloride fused salt chlorimation in this approach and produce waste fused salt slag and dust-slag collection, the immense pressure that waste fused salt slag and dust-slag collection bring to environment can be alleviated on the one hand, effectively can reclaim the most of chlorion in waste fused salt and dust-slag collection and part valuable element on the other hand, there is good prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is flow chart of the present invention.
Detailed description of the invention
Embodiment 1
As shown in Figure 1, a kind of integrated conduct method producing waste fused salt and dust-slag collection for titanium tetrachloride fused salt chlorimation: the broken slag after process through jaw crusher break process, and is adopted flour mill abrasive dust to 80 order by the waste fused salt of first Molten salt chlorination furnace being discharged; Fused salt chlorimation production process generation dust-slag collection is pulled an oar and is dispersed at normal temperature 20 DEG C, is prepared into solid-liquid mixing shape; Mixing of waste fused salt abrasive dust and solid-liquid mixing shape dust-slag collection being prepared burden is prepared into compound, and the batching mass ratio of waste fused salt slag and dust-slag collection is 1.5:1; Compound oxidizing roasting under the atmospheric condition passing into air, steam, oxidizing roasting equipment is tunnel cave, and oxidizing roasting temperature is 600 DEG C, and the oxidizing roasting time is 8h, and air intake is 180L/h, and steam intake is 80L/h.Most chloride can with oxygen, steam generation chemical reaction, various chloride can change corresponding oxide into, and generates a large amount of hydrogen chloride gas, chlorine and oxygen; The hydrogen chloride produced and chlorine are through elution circuit, and generate hydrochloric acid, elution circuit drip washing temperature range is 55 DEG C, the waste gas qualified discharge of generation; Caking slag after roasting, through crushing and screening, carries out alkali lye neutralisation treatment, and alkali lye is NaOH solution, and the NaOH concentration of alkaline leaching is 1.5mol/L, and the solid-to-liquid ratio of alkaline leaching is 0.5:1, and the temperature of alkaline leaching is 60 DEG C.Residual partial oxidation thing and alkali lye react, and generate corresponding hydroxide and salt solution; The process slag obtained after washing and filtering can be used as construction material, and the industrial brine obtained can be used for chlorine industry after treatment.The program alleviates on the one hand the environmental hazard that waste fused salt and dust-slag collection bring, and has reclaimed the chlorion in waste fused salt and dust-slag collection and part valuable element on the other hand.
Embodiment 2
As shown in Figure 1, the integrated conduct method of waste fused salt and dust-slag collection is produced: the broken slag after process through a jaw crusher break process, and is adopted flour mill abrasive dust to 100 order by the waste fused salt of first Molten salt chlorination furnace being discharged for titanium tetrachloride fused salt chlorimation; Fused salt chlorimation production process generation dust-slag collection is pulled an oar and is dispersed at normal temperature 20 DEG C, is prepared into solid-liquid mixing shape; Mixing of waste fused salt abrasive dust and solid-liquid mixing shape dust-slag collection being prepared burden is prepared into compound, and the batching mass ratio of waste fused salt slag and dust-slag collection is 1:1; Compound oxidizing roasting under the atmospheric condition passing into air, steam, oxidizing roasting equipment down-draft kiln, oxidizing roasting temperature is 700 DEG C, and the oxidizing roasting time is 6h, and air intake is 200L/h, and steam intake is 100L/h.Most chloride can with oxygen, steam generation chemical reaction, various chloride can change corresponding oxide into, and generates a large amount of hydrogen chloride gas, chlorine and oxygen; The hydrogen chloride produced and chlorine are through elution circuit, and generate hydrochloric acid, elution circuit drip washing temperature is 60 DEG C, the waste gas qualified discharge of generation; Caking slag after roasting, through crushing and screening, carries out alkali lye neutralisation treatment, and alkali lye is NaOH solution, and the NaOH concentration of alkaline leaching is 2mol/L, and the solid-to-liquid ratio of alkaline leaching is 0.8:1, and the temperature of alkaline leaching is 80 DEG C.Residual partial oxidation thing and alkali lye react, and generate corresponding hydroxide and salt solution; The process slag obtained after washing and filtering can be used as construction material, and the industrial brine obtained can be used for chlorine industry after treatment.
Embodiment 3
As shown in Figure 1, the integrated conduct method of waste fused salt and dust-slag collection is produced: the broken slag after process through a jaw crusher break process, and is adopted flour mill abrasive dust to 160 order by the waste fused salt of first Molten salt chlorination furnace being discharged for titanium tetrachloride fused salt chlorimation; Fused salt chlorimation production process generation dust-slag collection is pulled an oar and is dispersed at normal temperature 20 DEG C, is prepared into solid-liquid mixing shape; Mixing of waste fused salt abrasive dust and solid-liquid mixing shape dust-slag collection being prepared burden is prepared into compound, and the batching mass ratio of waste fused salt slag and dust-slag collection is 1:1; Compound oxidizing roasting under the atmospheric condition passing into air, steam, oxidizing roasting equipment down-draft kiln, oxidizing roasting temperature is 400 DEG C, and the oxidizing roasting time is 6h, and air intake is 160L/h, and steam intake is 50L/h.Most chloride can with oxygen, steam generation chemical reaction, various chloride can change corresponding oxide into, and generates a large amount of hydrogen chloride gas, chlorine and oxygen; The hydrogen chloride produced and chlorine are through elution circuit, and generate hydrochloric acid, elution circuit drip washing temperature is 35 DEG C, the waste gas qualified discharge of generation; Caking slag after roasting, through crushing and screening, carries out alkali lye neutralisation treatment, and alkali lye is NaOH solution, and the NaOH concentration of alkaline leaching is 0.5mol/L, and the solid-to-liquid ratio of alkaline leaching is 0.3:1, and the temperature of alkaline leaching is 80 DEG C.Residual partial oxidation thing and alkali lye react, and generate corresponding hydroxide and salt solution; The process slag obtained after washing and filtering can be used as construction material, and the industrial brine obtained can be used for chlorine industry after treatment.
Claims (3)
1. titanium tetrachloride fused salt chlorimation produces waste fused salt and a dust-slag collection integrated conduct method, it is characterized in that, comprises the following steps:
The waste fused salt that Molten salt chlorination furnace is discharged is carried out break process, and by broken sizing powder to 80 ~ 160 order;
At normal temperatures dust-slag collection making beating is dispersed, be prepared into solid-liquid mixing shape;
Mixing of waste fused salt powder and solid-liquid mixing shape dust-slag collection being prepared burden is prepared into compound, the batching mass ratio 2:1 ~ 1:1 of waste fused salt slag and dust-slag collection;
Compound oxidizing roasting under the atmospheric condition passing into air, steam, wherein oxidizing roasting temperature range is 400 ~ 700 DEG C, oxidizing roasting time range is 6 ~ 12h, and air intake scope is 160 ~ 200L/h, and steam intake scope is 50 ~ 100L/h;
The hydrogen chloride of generation and chlorine are passed into elution circuit drip washing, and drip washing temperature range is 30 ~ 60 DEG C;
Caking slag after roasting, through crushing and screening, carries out alkali lye neutralisation treatment, then carries out washing and filtering, and the NaOH concentration range of alkaline leaching is 0.5 ~ 2.5mol/L, and solid-to-liquid ratio scope is 0.3:1 ~ 1:1, and temperature range is 45 ~ 80 DEG C.
2. a kind of titanium tetrachloride fused salt chlorimation according to claim 1 produces waste fused salt and dust-slag collection integrated conduct method, it is characterized in that: waste fused salt slag adopts jaw crusher to carry out fragmentation, and broken slag adopts flour mill abrasive dust.
3. a kind of titanium tetrachloride fused salt chlorimation according to claim 1 produces waste fused salt and dust-slag collection integrated conduct method, it is characterized in that: oxidizing roasting equipment is tunnel cave or down-draft kiln.
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Cited By (11)
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| CN106586962A (en) * | 2016-11-23 | 2017-04-26 | 昆明理工大学 | Method for recycling hydrochloric acid through vapor neutral hydrolysis of titanium tetrachloride dust collection residues |
| CN106629832A (en) * | 2016-10-25 | 2017-05-10 | 锦州钛业有限公司 | Method for removing low-melting-point complex in elution tower for producing titanium tetrachloride through fused salt chlorination |
| WO2017174012A1 (en) * | 2016-04-07 | 2017-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Molten-salt chlorinated-slag resource processing method |
| CN107413815A (en) * | 2017-05-11 | 2017-12-01 | 深圳泛科环保产业发展有限公司 | A kind of dechlorination method of chloride material |
| CN108372185A (en) * | 2018-04-20 | 2018-08-07 | 江苏久吾高科技股份有限公司 | A kind of titanium chloride slag resource utilization method and its device |
| CN111348668A (en) * | 2020-03-16 | 2020-06-30 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN111545551A (en) * | 2020-05-14 | 2020-08-18 | 攀钢集团钛业有限责任公司 | Device and method for treating chlorinated dust collection slag |
| CN112299448A (en) * | 2020-11-20 | 2021-02-02 | 河南佰利联新材料有限公司 | Method for recovering sodium chloride from titanium white molten salt slag by chlorination process |
| CN113735162A (en) * | 2021-08-23 | 2021-12-03 | 云南国钛金属股份有限公司 | Anti-overflow device and method for molten salt slag box |
| CN115353146A (en) * | 2022-07-06 | 2022-11-18 | 宜宾天原海丰和泰有限公司 | Treatment method of titanium tetrachloride dust collection slag |
| CN108372185B (en) * | 2018-04-20 | 2024-05-03 | 江苏久吾高科技股份有限公司 | Titanium chloride slag resource utilization method and device |
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| WO2017174012A1 (en) * | 2016-04-07 | 2017-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Molten-salt chlorinated-slag resource processing method |
| CN106629832A (en) * | 2016-10-25 | 2017-05-10 | 锦州钛业有限公司 | Method for removing low-melting-point complex in elution tower for producing titanium tetrachloride through fused salt chlorination |
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| CN107413815A (en) * | 2017-05-11 | 2017-12-01 | 深圳泛科环保产业发展有限公司 | A kind of dechlorination method of chloride material |
| 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 |
| CN108372185A (en) * | 2018-04-20 | 2018-08-07 | 江苏久吾高科技股份有限公司 | A kind of titanium chloride slag resource utilization method and its device |
| CN111348668A (en) * | 2020-03-16 | 2020-06-30 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN111348668B (en) * | 2020-03-16 | 2022-03-15 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN111545551A (en) * | 2020-05-14 | 2020-08-18 | 攀钢集团钛业有限责任公司 | Device and method for treating chlorinated dust collection slag |
| CN112299448A (en) * | 2020-11-20 | 2021-02-02 | 河南佰利联新材料有限公司 | Method for recovering sodium chloride from titanium white molten salt slag by chlorination process |
| CN113735162A (en) * | 2021-08-23 | 2021-12-03 | 云南国钛金属股份有限公司 | Anti-overflow device and method for molten salt slag box |
| CN113735162B (en) * | 2021-08-23 | 2023-08-29 | 云南国钛金属股份有限公司 | Anti-overflow device and method for molten salt slag box |
| CN115353146A (en) * | 2022-07-06 | 2022-11-18 | 宜宾天原海丰和泰有限公司 | Treatment method of titanium tetrachloride dust collection slag |
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