CN104726713A - Process for comprehensive recovery of metal-containing oxides in disabled SCR (selective catalytic reduction) denitration catalyst - Google Patents
Process for comprehensive recovery of metal-containing oxides in disabled SCR (selective catalytic reduction) denitration catalyst Download PDFInfo
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Abstract
The invention relates to a method for disposal and recovery of wastes and particularly relates to a process for comprehensive recovery of metal-containing oxides in a disabled SCR (selective catalytic reduction) denitration catalyst. The process for comprehensive recovery of the metal-containing oxides in the disabled SCR denitration catalyst comprises the following steps: (1) performing pretreatment on raw materials: performing sweeping, ultrasonic treatment, bubbling and water washing on the disabled SCR denitration catalyst and performing high-temperature roasting at the temperature of 500-700 DEG C; (2) crushing: crushing the SCR denitration catalyst after high-temperature roasting, and crushing till the particle size is not more than 200 mu m to obtain uniform powder; (3) dissolving in a sodium solution; (4) separating and extracting titanium; (5) separating and extracting vanadium; and (6) reutilizing tungsten. By using the process provided by the invention, the yield of the metal oxides in the disabled SCR denitration catalyst is higher, wherein the recovery rate of TiO2 can be 95% or more, the recovery rate of V2O5 can be 95% or more, and the yield of a sodium tungstate product can be 98% or more.
Description
Technical field
The present invention relates to a kind of waste treatment recovery method, particularly one inefficacy SCR denitration containing metal oxide comprehensive recycling process.
Background technology
The principle of selective catalytic reduction (Selective Catalytic Reduction, SCR) is under catalyst action, reductive agent NH
3by NO and NO at 290-400 DEG C
2be reduced into N
2, and there is NH hardly
3oxidizing reaction, thus improve N
2selectivity, decrease NH
3consumption.SCR system is made up of ammonia supply system, ammonia/air-injection system, catalytic reaction system and Controlling System etc., and for avoiding flue gas to reheat consumed energy, after generally SCR reactor being placed in economizer, before air preheater, namely high dirt section is arranged.The horizontal pipe of ammonia before air preheater adds, and mixes with flue gas.Due to maturation and the high denitration rate of technology, SCR method now worldwide becomes the prevailing technology of large scale industry denitration of boiler smoke.By the end of the year 2010, the denitrating flue gas unit capacity that China has put into operation will be more than 200,000,000 kW, and account for 28% of coal group of motors capacity, wherein SCR unit accounts for 95%.
Along with the widespread use of SCR technique, the quantity of waste catalyst will get more and more.Present extensive application be take titanium oxide as the catalyzer of matrix, dispose if do not add these waste catalyst and arbitrarily bank up, a large amount of land resources can be taken on the one hand, increase the cost of enterprise; Some poisonous and harmful substances that catalyzer is in use adsorbed on the other hand enter into physical environment, and particularly water body, brings serious harm to environment; Waste catalyst wherein contained various valuable metal resource could not be recycled utilization, also causes the huge waste of efficient resource.So carrying out spent catalyst recovery and utilizing both can turn waste into wealth, changed evil for benefit, and a corresponding yarn can also be solved and arrange potential problem of environmental pollution, thus bring considerable economic benefit and social benefit.
Summary of the invention
The invention provides a kind of inefficacy SCR denitration containing metal oxide comprehensive recycling process, Footwall drift oxide compound and sodium wolframate from discarded denitrating catalyst, thus turn waste into wealth, change evil for beneficial.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of inefficacy SCR denitration containing metal oxide comprehensive recycling process, this technique comprises the steps:
1. raw materials pretreatment: get inefficacy SCR denitration through purging, ultrasonic, bubbling carries out high-temperature roasting after washing under 500-700 DEG C of condition;
2. pulverize: the SCR denitration after high-temperature roasting is pulverized, is crushed to granularity≤200 μm, obtain uniform powder;
3. sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:3 ~ 8ml, NaOH solution concentration is 300 ~ 800g/L, and then adds solubility promoter Na
2cO
3, thermostatically heating at temperature is 70 ~ 100 DEG C also stirs, and obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation;
4. be separated and carry titanium: in precipitation X, add Na
2sO
4powder and suitable quantity of water mixing, Na
2sO
4add-on be 1 ~ 5 times of precipitation X quality; In the mixture obtained, add the vitriol oil, temperature of reaction is 130 ~ 170 DEG C, reaction times 2 ~ 6h, and the add-on of the vitriol oil is 1.5 ~ 2.5 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2, after drying, under 400-600 DEG C of condition, carry out high-temperature calcination, obtain TiO
2finished product;
5. vanadium extraction is separated: add sulphuric acid soln adjust ph to 8.0 ~ 9.0 in solution X after, then add appropriate NH
4nO
3, carry out solid-liquid separation after stirring reaction, after filtration, obtain NH
4vO
3with secondary filtrate;
6. recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 4.0 ~ 5.0, then add appropriate NaCl, be obtained by reacting Na
2wO
42H
2o, obtains sodium wolframate product through evaporative crystallization after separating impurity composition.
As preferably, a kind of inefficacy SCR denitration containing metal oxide comprehensive recycling process, this technique comprises the steps:
1. raw materials pretreatment: get inefficacy SCR denitration through purging, after ultrasonic, bubbling is washed, wash away the ash content of remained on surface and solvable inorganics even load thing, drop in electric furnace, under 500-700 DEG C of condition, carry out high-temperature roasting can adsorbable carbon deposit, arsenic and organic impurity to remove surface, constant temperature 4 hours;
2. pulverize: the SCR denitration after high-temperature roasting is pulverized, is crushed to granularity≤200 μm, obtain uniform powder;
3. sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:3 ~ 8ml, NaOH solution concentration is 300 ~ 800g/L, and then adds the solubility promoter Na of 0.8 ~ 3 times of powder quality
2cO
3, thermostatically heating at temperature is 70 ~ 100 DEG C also stirs 30 ~ 120 minutes, obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation;
4. be separated and carry titanium: in precipitation X, add Na
2sO
4powder and suitable quantity of water mixing, the object adding water is for dissolving Na
2sO
4powder, add-on according to circumstances can regulate, and meets and makes Na
2sO
4powder dissolution, Na
2sO
4add-on be 1 ~ 5 times of precipitation X quality; In the mixture obtained, add the vitriol oil, temperature of reaction is 130 ~ 170 DEG C, reaction times 2 ~ 6h, and the add-on of the vitriol oil is 1.5 ~ 2.5 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2, after drying, under 400-600 DEG C of condition, carry out high-temperature calcination, obtain TiO
2finished product;
5. vanadium extraction is separated: in solution X, add the sulphuric acid soln that volumetric concentration is 8 ~ 15%, behind adjust ph to 8.0 ~ 9.0, then add NH
4nO
3, 1L solution NH
4nO
3add-on is 12 ~ 18g, carries out solid-liquid separation, obtain NH after filtration after stirring reaction
4vO
3with secondary filtrate;
6. recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 4.0 ~ 5.0, then add NaCl, 1L solution NaCl add-on is 12 ~ 18g, is obtained by reacting Na
2wO
42H
2o, through refining, filtration, ion exchange process, obtains sodium wolframate product through evaporative crystallization after separating impurity composition.
With regard to current SCR denitration composition, no matter catalyzer is honeycomb fashion, board-like or other forms, its composition is all similar, by TiO
2, V
2o
5, WO
3form Deng material.Wherein WO
3account for 5% ~ 10%, V
2o
5account for 1% ~ 5%, TiO
2account for the overwhelming majority 85% ~ 90%.
As preferably, step 4. in the usage quantity of dilution titanium liquid water be 2 ~ 5 times of volumes of previous solu volume.
Utilize technique of the present invention, in inefficacy SCR denitration, the productive rate of metal oxide is higher, wherein: TiO
2the rate of recovery can reach more than 95%, V
2o
5the rate of recovery can reach more than 95%, the productive rate of sodium wolframate product can reach more than 98%; The quality of Footwall drift oxide compound is higher, can use as the raw material producing new catalyst for denitrating flue gas completely; Sodium wolframate product of many uses, wherein for the manufacture of petroleum industry and Aeronautics and Astronautics material, renewable income is considerable.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention and/or change all will fall into scope.
In the present invention, if not refer in particular to, all parts, per-cent are weight unit, and the equipment adopted and raw material etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the ordinary method of this area.
The source of inefficacy SCR denitration: in the SCR reactor on certain coal-burning power plant's unit.
Embodiment 1
A kind of inefficacy SCR denitration containing metal oxide comprehensive recycling process, Fig. 1 is shown in this technical process, and detailed process is as follows:
1, raw materials pretreatment: get the denitrating catalyst of inefficacy through purging, after ultrasonic, bubbling is washed, wash away the ash content of remained on surface and solvable inorganics even load thing, drop in electric furnace, under 650 DEG C of conditions, carry out high-temperature roasting can adsorbable carbon deposit, arsenic and organic impurity to remove surface, constant temperature 4 hours.
2, pulverize: the denitrating catalyst after high-temperature roasting is added in crusher, is crushed to granularity≤200 μm, obtain uniform powder.
3, sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:5ml, NaOH solution concentration is 600g/L.Solubility promoter Na is added in mixture
2cO
3, the add-on of solubility promoter is 0.8 times of powder quality, and thermostatically heating at temperature is 90 DEG C also stirs 60 minutes, obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation.
4, titanium is carried in separation: in precipitation X, add sodium sulfate powder and suitable quantity of water mixing, the add-on of water is dissolved to make sodium sulfate powder, Na
2sO
4add-on be 5 times of precipitation X quality.Add the vitriol oil to mixture, temperature of reaction is 160 DEG C, reaction times 3h, and the add-on of the vitriol oil is 1.8 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2.After drying, under 400 DEG C of conditions, carry out high-temperature calcination, obtain TiO
2finished product.
5, vanadium extraction is separated: in solution X, add the sulphuric acid soln that volumetric concentration is 10%, after adjust ph to 8.0, then add NH
4nO
3, 1L solution NH
4nO
3add-on is 18g, carries out solid-liquid separation, obtain NH after filtration after stirring reaction
4vO
3with secondary filtrate;
6, recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 4.0, then add NaCl, 1L solution NaCl add-on is 18g, is obtained by reacting Na
2wO
42H
2o, through the technique such as refining, filtration, ion-exchange, separating impurity composition, then obtain sodium wolframate product through evaporative crystallization, thus complete the production technique of Footwall drift oxide compound and recycling in SCR waste flue gas denitration catalyst.
Reclaim in product, the productive rate of metal oxide is higher, wherein: TiO
2the rate of recovery can reach 97%, V
2o
5the rate of recovery can reach 95%, the productive rate of sodium wolframate product can reach 96%.
Embodiment 2
1, raw materials pretreatment: get the denitrating catalyst of inefficacy through purging, after ultrasonic, bubbling is washed, wash away the ash content of remained on surface and solvable inorganics even load thing, drop in electric furnace, under 650 DEG C of conditions, carry out high-temperature roasting can adsorbable carbon deposit, arsenic and organic impurity to remove surface, constant temperature 4 hours.
2, pulverize: the denitrating catalyst after high-temperature roasting is added in crusher, is crushed to granularity≤200 μm, obtain uniform powder.
3, sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:6ml, NaOH solution concentration is 500g/L.Solubility promoter Na is added in mixture
2cO
3, the add-on of solubility promoter is 2 times of powder quality, and thermostatically heating at temperature is 100 DEG C also stirs 90 minutes, obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation.
4, titanium is carried in separation: in precipitation X, add sodium sulfate powder and water, mixing, Na
2sO
4add-on be precipitation X quality doubly.Add the vitriol oil to mixture, temperature of reaction is 150 DEG C, reaction times 4h, and the add-on of the vitriol oil is 2 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2.After drying, under 600 DEG C of conditions, carry out high-temperature calcination, obtain TiO
2finished product;
5, vanadium extraction is separated: in solution X, add the sulphuric acid soln that volumetric concentration is 8%, after adjust ph to 8.5, then add NH
4nO
3, 1L solution NH
4nO
3add-on is 15g, carries out solid-liquid separation, obtain NH after filtration after stirring reaction
4vO
3with secondary filtrate;
6, recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 4.5, then add NaCl, 1L solution NaCl add-on is 15g, is obtained by reacting Na
2wO
42H
2o, through the technique such as refining, filtration, ion-exchange, separating impurity composition, then obtain sodium wolframate product through evaporative crystallization, thus complete the production technique of Footwall drift oxide compound and recycling in SCR waste flue gas denitration catalyst.
Reclaim in product, the productive rate of metal oxide is higher, wherein: TiO
2the rate of recovery can reach 95%, V
2o
5the rate of recovery can reach 96%, the productive rate of sodium wolframate product can reach 96%.
Embodiment 3
1, raw materials pretreatment: get the denitrating catalyst of inefficacy through purging, after ultrasonic, bubbling is washed, wash away the ash content of remained on surface and solvable inorganics even load thing, drop in electric furnace, under 650 DEG C of conditions, carry out high-temperature roasting can adsorbable carbon deposit, arsenic and organic impurity to remove surface, constant temperature 4 hours.
2, pulverize: the denitrating catalyst after high-temperature roasting is added in crusher, is crushed to granularity≤200 μm, obtain uniform powder.
3, sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:4ml, NaOH solution concentration is 400g/L.Solubility promoter Na is added in mixture
2cO
3, the add-on of solubility promoter is 3 times of powder quality, and thermostatically heating at temperature is 80 DEG C also stirs 60 minutes, obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation.
4, titanium is carried in separation: in precipitation X, add sodium sulfate powder and water, mixing, Na
2sO
4add-on be 3 times of precipitation X quality.Add the vitriol oil to mixture, temperature of reaction is 170 DEG C, reaction times 6h, and the add-on of the vitriol oil is 2.5 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2.After drying, under 500 DEG C of conditions, carry out high-temperature calcination, obtain TiO
2finished product.
5, vanadium extraction is separated: in solution X, add the sulphuric acid soln that volumetric concentration is 15%, after adjust ph to 9.0, then add NH
4nO
3, 1L solution NH
4nO
3add-on is 12g, carries out solid-liquid separation, obtain NH after filtration after stirring reaction
4vO
3with secondary filtrate;
6, recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 5.0, then add NaCl, 1L solution NaCl add-on is 12g, is obtained by reacting Na
2wO
42H
2o, through the technique such as refining, filtration, ion-exchange, separating impurity composition, then obtain sodium wolframate product through evaporative crystallization, thus complete the production technique of Footwall drift oxide compound and recycling in SCR waste flue gas denitration catalyst.
Reclaim in product, the productive rate of metal oxide is higher, wherein: TiO
2the rate of recovery can reach 90%, V
2o
5the rate of recovery can reach 91%, the productive rate of sodium wolframate product can reach 94%.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (3)
1. an inefficacy SCR denitration containing metal oxide comprehensive recycling process, is characterized in that this technique comprises the steps:
1. raw materials pretreatment: get inefficacy SCR denitration through purging, ultrasonic, bubbling carries out high-temperature roasting after washing under 500-700 DEG C of condition;
2. pulverize: the SCR denitration after high-temperature roasting is pulverized, is crushed to granularity≤200 μm, obtain uniform powder;
3. sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:3 ~ 8ml, NaOH solution concentration is 300 ~ 800g/L, and then adds solubility promoter Na
2cO
3, thermostatically heating at temperature is 70 ~ 100 DEG C also stirs, and obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation;
4. be separated and carry titanium: in precipitation X, add Na
2sO
4powder and suitable quantity of water mixing, Na
2sO
4add-on be 1 ~ 5 times of precipitation X quality; In the mixture obtained, add the vitriol oil, temperature of reaction is 130 ~ 170 DEG C, reaction times 2 ~ 6h, and the add-on of the vitriol oil is 1.5 ~ 2.5 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2, after drying, under 400-600 DEG C of condition, carry out high-temperature calcination, obtain TiO
2finished product;
5. vanadium extraction is separated: add sulphuric acid soln adjustment pH value to 8. 0 ~ 9.0 in solution X after, then add appropriate NH
4nO
3, carry out solid-liquid separation after stirring reaction, after filtration, obtain NH
4vO
3with secondary filtrate;
6. recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 4.0 ~ 5.0, then add appropriate NaCl, be obtained by reacting Na
2wO
42H
2o, obtains sodium wolframate product through evaporative crystallization after separating impurity composition.
2. inefficacy SCR denitration containing metal oxide comprehensive recycling process according to claim 1, is characterized in that: step 4. middle usage quantity of diluting titanium liquid water is 2 ~ 5 times of volumes of previous solu volume.
3. inefficacy SCR denitration containing metal oxide comprehensive recycling process according to claim 1, is characterized in that this technique comprises the steps:
1. raw materials pretreatment: get inefficacy SCR denitration through purging, after ultrasonic, bubbling is washed, wash away the ash content of remained on surface and solvable inorganics even load thing, drop in electric furnace, under 500-700 DEG C of condition, carry out high-temperature roasting can adsorbable carbon deposit, arsenic and organic impurity to remove surface, constant temperature 4 hours;
2. pulverize: the SCR denitration after high-temperature roasting is pulverized, is crushed to granularity≤200 μm, obtain uniform powder;
3. sodium liquid dissolves: by powder obtained in the previous step and NaOH solution with the ratio hybrid reaction of 1g:3 ~ 8ml, NaOH solution concentration is 300 ~ 800g/L, and then adds the solubility promoter Na of 0.8 ~ 3 times of powder quality
2cO
3, thermostatically heating at temperature is 70 ~ 100 DEG C also stirs 30 ~ 120 minutes, obtains solidliquid mixture, will be precipitated X and solution X after its solid-liquid separation;
4. be separated and carry titanium: in precipitation X, add Na
2sO
4powder and suitable quantity of water mixing, Na
2sO
4add-on be 1 ~ 5 times of precipitation X quality; In the mixture obtained, add the vitriol oil, temperature of reaction is 130 ~ 170 DEG C, reaction times 2 ~ 6h, and the add-on of the vitriol oil is 1.5 ~ 2.5 times of precipitation X quality; Thin up titanium liquid all generates white precipitate TiO (OH) through hydrolysis to solution
2, after drying, under 400-600 DEG C of condition, carry out high-temperature calcination, obtain TiO
2finished product;
5. be separated vanadium extraction: in solution X, add the sulphuric acid soln that volumetric concentration is 8 ~ 15%, after regulating pH value to 8. 0 ~ 9.0, then add NH
4nO
3, 1L solution NH
4nO
3add-on is 12 ~ 18g, carries out solid-liquid separation, obtain NH after filtration after stirring reaction
4vO
3with secondary filtrate;
6. recycle tungsten: secondary filtrate salt adding acid for adjusting pH value to 4.0 ~ 5.0, then add NaCl, 1L solution NaCl add-on is 12 ~ 18g, is obtained by reacting Na
2wO
42H
2o, obtains sodium wolframate product through evaporative crystallization after separating impurity composition.
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| CN105293573A (en) * | 2015-11-19 | 2016-02-03 | 无锡中新绿能科技有限公司 | Recycling method of waste SCR denitration catalyst |
| CN105668634A (en) * | 2016-01-13 | 2016-06-15 | 江苏龙净科杰催化剂再生有限公司 | Method for recycling waste SCR denitration catalyst |
| CN106216364A (en) * | 2016-08-31 | 2016-12-14 | 北京北科欧远科技有限公司 | A kind of SCR waste catalyst recovery method and system |
| CN108913901A (en) * | 2018-07-05 | 2018-11-30 | 安徽思凯瑞环保科技有限公司 | The method of thick titanium valve is extracted from SCR catalyst using wet processing |
| CN110385044A (en) * | 2019-07-24 | 2019-10-29 | 中国科学院过程工程研究所 | A kind of method of useless SCR catalyst dearsenification desiliconization |
| CN111302397A (en) * | 2020-03-13 | 2020-06-19 | 中国科学院城市环境研究所 | Method and device for recovering waste denitration catalyst |
| CN113265542A (en) * | 2020-12-16 | 2021-08-17 | 韶关市诚一金属材料科技有限公司 | Method for extracting metal elements from flue gas denitration catalyst |
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