CN1899668A - Phosphate rock slurry catalytically oxidaizing process for removing low concentration SO2 - Google Patents
Phosphate rock slurry catalytically oxidaizing process for removing low concentration SO2 Download PDFInfo
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- CN1899668A CN1899668A CNA2006100110030A CN200610011003A CN1899668A CN 1899668 A CN1899668 A CN 1899668A CN A2006100110030 A CNA2006100110030 A CN A2006100110030A CN 200610011003 A CN200610011003 A CN 200610011003A CN 1899668 A CN1899668 A CN 1899668A
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- phosphorus ore
- ore slurry
- phosphate rock
- phosphorus
- sulfur dioxide
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Abstract
The present invention relates to catalytic oxidation process for eliminating low concentration SO2 with phosphate rock slurry. The phosphate rock slurry with rich catalytic transition metal ions and iron ions and oxygen is utilized in catalytically oxidizing the sulfuric acid tail with SO2 content not higher than 3 % to lower the SO2 content to not higher 300 mg/cu m. The failed phosphate rock slurry is returned to the wet process phosphoric acid producing shop. The present invention can reduce pollution on atmosphere and recover sulfur resource in low cost.
Description
One, technical field: the present invention relates to a kind of purifying treatment method that utilizes phosphorus ore slurry catalytic oxidation to absorb low-concentration sulfur dioxide, belong to technical field of phosphorous chemical industry.
Two, background technology: sulfur dioxide is pollutant main in the atmosphere, to the toxic effect of human body, still produce the main cause of acid rain simultaneously, existing desulfur technology exists investment big, the operating cost height, pipeline is perishable, the technological process complexity, problems such as operation operation is numerous and diverse, it is unsatisfactory especially concentration to be lower than the clean-up effect and the cost of 3% sulfur dioxide.Sulfuric acid tail gas is typical low-concentration sulfur dioxide (SO
2Volume content≤3%) waste gas also is SO in the atmosphere
2One of main source.The annual sulfuric acid total output of China be used to make phosphate fertilizer more than 50%, in phosphatization factory, carrying out effective sulfuric acid tail gas desulfurized treatment will be to SO
2Highly effective effect is played in the control of total emission volumn.
Liquid phase catalytic oxidation flue gas desulfurization is a kind of emerging sulfur method, and it mainly is to utilize the catalysed oxidn of transition metal ions such as Fe, Mn in the absorption liquid with SO in the flue gas
2Catalytic Oxygen changes into the H in the liquid phase
2SO
4Thereby, reach the purpose of desulfurization.This method does not produce solid waste, non-secondary pollution, be a kind of more green flue gas desulfurization technique, and the dilute sulfuric acid that desulfurization produces can adopt different process to produce valuable byproducts such as fertilizer, ferrous sulfate or bodied ferric sulfate, higher economy, environmental benefit are arranged.Phosphatization factory sulfuric acid tail gas generally adopts ammonia process, sodium method to administer, or directly discharging, and the former increases cost by complex operation, and the latter increases the weight of the atmospheric environment burden.Utilize transition metal ions (divalence or ferric ion) abundant in the phosphorus ore, but the SO in the liquid phase catalytic oxidation phosphatization factory relieving haperacidity tail gas
2, make it to be converted into H
2SO
4, sulfuric acid further decomposing phosphate rock generates phosphoric acid and CaSO
4, two processes all can reach the purpose of desulfurization.
In publication number CN1391975A, disclose and utilized sodium chloride improvement to contain the flue gas of sulfur dioxide and the wet method fume gas desulfurizing method of production high concentration sulfur dioxide.This method: " at first be to absorb operation; the flue gas that will contain low-concentration sulfur dioxide gas is handled through purifying, lowering the temperature; enter the absorption tower that absorbs operation after removing dust, sulfur trioxide and acid mist wherein, and the sodium hydroxide solution with 10～35% makes SO in the flue gas after 30～85 ℃ absorb down
2Concentration≤20～300ppm, qualified discharge; Be decomposition process then, absorbent and SO
2The hydrogen chloride gas that reacts after the mixed liquor that generates sodium sulfite and sodium hydrogensulfite with 120～180 ℃ of temperature reacts.The unnecessary hydrogen chloride gas body and function bisulfite in reaction back is received solution and is washed, and finally makes the sulfur dioxide gas of concentration 〉=97%, can be directly as the raw material of producing sulfur dioxide liquid or production sulfuric acid; Hydrogen chloride and sodium sulphite and bisulfite are received and are reflected that the sodium chloride that generates is the electrolysis raw material.Can be recycled, consume hardly.A small amount of SO is arranged in the absorption process
4 2-Ion generates, and uses barium chloride to remove SO
4 2-Ion generates medicinal barium sulfate.”
In publication number CN1449861A, disclose zinc oxide and removed sulfur dioxide in flue gas method and device.This method is: " at first granularity is accounted for more than 90% less than 100 orders, contain zinc oxide and carry out slurrying greater than 40% zinc calcine or Zn dust in the circulation absorption cell; Absorb then and contain sulfur dioxide concentration 0.03%～3%, temperature is at 10～150 ℃ flue gas; Absorb slag and deliver to the filter press filtration by filter pump from absorbing circulating slot, the absorption slag of output contains ZnSO
4About 40%, moisture about 30%; Can select to adopt thermal decomposition, acid decomposition, air oxidation a kind of mode wherein to handle; Heat decomposition temperature is greater than 350 ℃, and adopt zinc electrolysis waste electrolyte sour the decomposition, and 70～90 ℃ of control decomposition temperatures blast air after decomposition finishes and take off suction in decomposing slurries; Air oxidation process will absorb slag to be made 20～25% slurries and carries out in air groove, and bottom land is furnished with the air oxidation blowpipe, and groove central authorities are provided with agitator, all around mounting guiding board and whirlpool bubbler.”
China's phosphate rock resource is abundant, and in the phosphatization factory, the phosphorus ore slurry is cheap and easy to get, and phosphoric acid and phosphorus compound fertilizer production technology maturation are in demand.Contain abundant transition metal ions (SO in divalence or the trivalent gas in the phosphorus ore
2Method can make the up to standard even zero-emission of tail gas, and effectively reclaimed SO a large amount of in the flue gas
2, the phosphorus ore slurry that lost efficacy in the reaction back can be used as byproduct and is used to make phosphoric acid and phosphorus composite fertilizer, and contamination-free produces, and this method is for low concentration SO
2Gas (SO
2Volume content≤3%) improvement reduces and discharge SO in atmosphere
2Have great significance.
Three, summary of the invention:
The method that the purpose of this invention is to provide a kind of phosphorus ore slurry catalytic oxidative desulfurization low-concentration sulfur dioxide, utilize the catalytic action that contains abundant transition metal ions-ferrous ion and ferric ion in the phosphorus ore slurry, with phosphorus ore slurry as self oxygen in desulfurization absorbent and the sulfuric acid tail gas, the sulfuric acid tail gas of sulfur dioxide volumn concentration≤3% in the catalytic oxidation phosphatization factory makes in the sulfuric acid tail gas sulfur dioxide concentration reduce to≤300mg/m
3, absorbed simultaneously that phosphoric acid concentration rises in the phosphorus ore slurry of sulfur dioxide 〉=3%, the phosphorus ore slurry after the inefficacy can return the Wet-process Phosphoric Acid Production workshop and use, and unharmful substance enters in the environment.
The present invention finishes according to the following steps:
(1) with ground phosphate rock (Ca
5F (PO)
3Ball milling accounts for 85%～100% to granularity≤154 μ m's, and the ground phosphate rock chemical composition comprises composition shown in the table 1;
The main chemical compositions of table 1 ground phosphate rock
| Composition | P 2O 5 | MgO | CaO | SiO 2 | F | Fe 2O 3 | Al 2O 3 |
| Mass fraction/% | 11.17～ 39.62 | 0～ 10.85 | 19.42～ 54 | 0.21～ 38.8 | 0.51～ 4.43 | 0.18～ 10.88 | 0.06～ 19.02 |
(2) be 0.5～2.5: 1 preparation with ground phosphate rock and water by the solid-liquid mass ratio, mix to such an extent that phosphorus ore is starched absorbent, and control phosphorus slurry pH be 3～7;
The phosphorus ore slurry is squeezed in the reactor with pump, the sulfuric acid tail gas of sulfur dioxide volumn concentration≤3% also feeds in the reactor continuously, 20～65 ℃ of control temperature of reactor, divalence and ferric ion exist under the situation in the phosphorus ore slurry, 1. sulfur dioxide in the sulfuric acid tail gas and oxygen generation catalytic oxidation generate sulfuric acid, and the content of sulfur dioxide in the sulfuric acid tail gas is constantly descended, after the reaction beginning, the exit concentration of measured reaction device sulfur dioxide is when the exit concentration of sulfur dioxide drops to≤300mg/m
3, pH value≤1.1 of phosphorus ore slurry o'clock, reaction is finished, the phosphorus ore during phosphorus ore is starched and the H of generation
2SO
4Reaction back generates phosphoric acid (reaction is 2.) and lost efficacy, and finishes a reaction time, in this moment phosphorus ore slurry phosphoric acid quality percentage concentration rise to 〉=3%.Phosphorus ore slurry after the inefficacy can return the Wet-process Phosphoric Acid Production workshop and use, and the reactor domestic demand is changed fresh phosphorus ore slurry and begun second reaction time again.
When 2. reaction takes place, be attended by side reaction generation 3., 4. and 5..The key reaction equation that takes place in the catalytic oxidation process is:
Major advantage of the present invention has:
(1) at not tractable low concentration SO
2Tail gas (SO
2Concentration≤3%), adopts catalytic oxidation-absorption to carry out synchronously, made full use of the oxygen of self in the sulfuric acid tail gas, need not rouse under the condition of oxygen, but qualified discharge alleviates the atmospheric environment burden, reclaim the sulphur resource;
(2) adopt the phosphorus ore of practical application in the phosphatization plant produced to starch as desulfurization absorbent, cheap and easy to get, recyclable utilization;
(3) the phosphorus ore slurry absorbent of reaction back inefficacy can be made the raw material of phosphoric acid production;
(4) circulation of whole technique route is closed circuit, and technological process is simple, non-secondary pollution.
Four, the specific embodiment:
Embodiment 1: phosphorus ore is milled down to granularity≤154 μ m with ball mill and accounts for 90%, with ground phosphate rock (main chemical compositions: P
2O
5=31.54, MgO=0.13, CaO=43.5, SiO
2=14.92, F=3.41, Fe
2O
3=1.22, Al
2O
3=2.05) being mixed and made into the solid-liquid mass ratio with water is 1.3: 1 phosphorus ore slurry, controlling its pH value is 4.5, and phosphorus ore slurry is squeezed in the reactor with centrifugal pump, sulfuric acid tail gas feeds reactor continuously, air velocity is controlled at 4.0L/min, the reactor interior reaction temperature is controlled at 30 ℃～45 ℃, carries out catalytic oxidation, works as SO
2Exit concentration is 280mg/m
3, phosphorus slurry pH≤1.1 o'clock, reaction is finished, the phosphorus ore slurry lost efficacy, and the phosphoric acid quality percentage concentration is 3.5% in the survey phosphorus ore slurry, at this moment must change fresh phosphorus ore slurry again, phosphorus ore slurry after the inefficacy is got through centrifugal pump by the reactor bottom discharging opening, and sends into the phosphoric acid by wet process workshop.
Embodiment 2: phosphorus ore is milled down to granularity≤154 μ m with ball mill and accounts for 90%, with ground phosphate rock (main chemical compositions: P
2O
5=27.87, MgO=1.31, CaO=39.8, SiO
2=16.66, F=2.65, Fe
2O
3=1.59, Al
2O
3=2.22) being mixed and made into the solid-liquid mass ratio with water is 1: 1 phosphorus ore slurry, and control pH value is 5.3, and with centrifugal pump phosphorus ore is starched and to be squeezed in the reactor, sulfuric acid tail gas feeds reactor continuously, and air velocity is controlled at 3.0L/min, and temperature is controlled at 18 ℃～30 ℃, carry out catalytic oxidation, work as SO
2Exit concentration is 200mg/m
3, phosphorus slurry pH≤1.1 o'clock, reaction is finished,, the phosphorus ore slurry lost efficacy, and the phosphoric acid quality percentage concentration is 4% in the survey phosphorus ore slurry, at this moment must change fresh phosphorus ore slurry again, the ore pulp after the inefficacy is extracted out through centrifugal pump by the reactor bottom discharging opening, and sends into the phosphoric acid by wet process workshop.
Embodiment 3: be milled down to granularity≤154 μ m with ball mill and account for 90%, with ground phosphate rock (main chemical compositions: P
2O
5=33.45, MgO=0.08, CaO=47.04, SiO
2=11.57, F=4.43, Fe
2O
3=0.61, Al
2O
3=1.01) being mixed and made into the solid-liquid mass ratio with water is 2.5: 1 ore pulp absorption liquid, keeping the pH value is 4.2, and ore pulp is squeezed in the reactor with centrifugal pump, sulfuric acid tail gas feeds reactor continuously, air velocity is controlled at 3.5L/min, reaction temperature is controlled at 40 ℃～60 ℃, carries out catalytic oxidation, works as SO
2Exit concentration is 250mg/m
3, phosphorus slurry pH≤1.1 o'clock, reaction is finished, phosphorus ore slurry lost efficacy, and surveyed that the phosphoric acid quality percentage concentration is 3.5% in its phosphorus ore slurry, must change fresh ore pulp again, phosphorus ore slurry after the inefficacy is extracted out through centrifugal pump by the reactor bottom discharging opening, and sends into the phosphoric acid by wet process workshop.
Claims (2)
1, the method for a kind of phosphorus ore slurry catalytic oxidative desulfurization low-concentration sulfur dioxide, it is characterized in that: this method is finished according to the following steps: the ground phosphate rock ball milling is accounted for 85%～100% to granularity≤154 μ m; Is 0.5～2.5: 1 preparation with ground phosphate rock and water by the solid-liquid mass ratio, mixes to such an extent that phosphorus ore is starched, and control phosphorus slurry pH is 3～7; The phosphorus ore slurry is squeezed in the reactor with centrifugal pump, sulfuric acid tail gas also feeds in the reactor continuously, 20～65 ℃ of control temperature of reactor, divalence and ferric ion exist under the situation in the phosphorus ore slurry, and sulfur dioxide in the sulfuric acid tail gas and oxygen generation catalytic oxidation generate H
2SO
4, when the exit concentration of reactor sulfur dioxide drops to≤300mg/m
3, pH value≤1.1 of phosphorus ore slurry o'clock, reaction is finished; The phosphorus ore in the phosphorus ore slurry and the H of generation
2SO
4Reaction back generates phosphoric acid and lost efficacy, in this moment phosphorus ore slurry phosphoric acid concentration rise to 〉=3%.
2, the method for phosphorus ore slurry catalytic oxidative desulfurization low-concentration sulfur dioxide according to claim 1, it is characterized in that: the mass percent of the main chemical compositions of described ground phosphate rock is phosphorus pentoxide 11.17-39.62%, magnesia 0～10.85%, calcium oxide 19.42～54%, silica 0.21～38.8%, fluorine 0.51～4.43%, di-iron trioxide 0.18～10.88%, alundum (Al 0.06～19.02%.
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|---|---|---|---|
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|---|---|---|---|
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| CN100415348C CN100415348C (en) | 2008-09-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427180C (en) * | 2007-01-26 | 2008-10-22 | 昆明理工大学 | Method for deacidizing low sulfur dioxide concentration by using gas produced by biomass pyrolysis |
| CN103143253A (en) * | 2013-03-19 | 2013-06-12 | 瓮福（集团）有限责任公司 | Device for removing low-concentration sulfur dioxide from phosphate concentrate and application method of device |
| CN103191637A (en) * | 2013-04-23 | 2013-07-10 | 瓮福（集团）有限责任公司 | Industrial exhaust gas desulfurizer |
| CN103432869A (en) * | 2013-08-26 | 2013-12-11 | 瓮福（集团）有限责任公司 | Low-concentration sulfur dioxide absorption tower |
| CN103949150A (en) * | 2014-03-14 | 2014-07-30 | 云南磷化集团有限公司 | Method using catalytic oxidation of sulfur dioxide tail gas for PH adjustment agent of phosphate rock ore dressing |
| CN104667728A (en) * | 2015-01-26 | 2015-06-03 | 昆明川金诺化工股份有限公司 | Method for removing sulfur dioxide in sulfuric acid tail gas |
| CN104667732A (en) * | 2015-02-27 | 2015-06-03 | 昆明川金诺化工股份有限公司 | Method for absorbing sulfur dioxide in sulfuric acid tail gas by phosphoric acid via wet process |
| CN105289264A (en) * | 2015-10-08 | 2016-02-03 | 昆明理工大学 | Method for absorbing low-concentration SO2 (sulfur dioxide) by slurrying of yellow phosphorus electroprecipitating dust |
| CN105854540A (en) * | 2016-05-23 | 2016-08-17 | 河南红东方化工股份有限公司 | Desulfurizing technology for sulphuric-acid-production tail gas |
| CN106178920A (en) * | 2016-08-31 | 2016-12-07 | 陕西煤化能源有限公司 | A kind of rock phosphate in powder phosphoric acid gypsum flue gas desulphurization system and technique thereof |
| CN106345288A (en) * | 2016-08-24 | 2017-01-25 | 湖北祥云(集团)化工股份有限公司 | Method and system for utilizing phosphoric ore pulp to treat sulfur-containing flue gas |
| WO2017173717A1 (en) * | 2016-04-08 | 2017-10-12 | 成都千砺金科技创新有限公司 | Method for directly using phosphogypsum decomposition gas in wet phosphoric acid production |
| WO2017173716A1 (en) * | 2016-04-08 | 2017-10-12 | 成都千砺金科技创新有限公司 | Method for joint production of phosphogypsum decomposition gas and wet-process phosphoric acid |
| CN107398171A (en) * | 2017-06-14 | 2017-11-28 | 昆明理工大学 | A kind of method that acid gas in flue gas is removed using metal tailings |
| CN107899596A (en) * | 2017-10-30 | 2018-04-13 | 昆明理工大学 | A kind of desulfurization denitrification agent and preparation method thereof |
| CN108434977A (en) * | 2017-11-24 | 2018-08-24 | 云南民族大学 | A kind of method of phosphate ore pulp liquid phase catalytic oxidation simultaneous SO_2 and NO removal |
| CN113828140A (en) * | 2021-11-10 | 2021-12-24 | 昆明理工大学 | Strengthening method for wet desulphurization of phosphate slurry |
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2006
- 2006-06-30 CN CNB2006100110030A patent/CN100415348C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427180C (en) * | 2007-01-26 | 2008-10-22 | 昆明理工大学 | Method for deacidizing low sulfur dioxide concentration by using gas produced by biomass pyrolysis |
| CN103143253A (en) * | 2013-03-19 | 2013-06-12 | 瓮福（集团）有限责任公司 | Device for removing low-concentration sulfur dioxide from phosphate concentrate and application method of device |
| CN103191637A (en) * | 2013-04-23 | 2013-07-10 | 瓮福（集团）有限责任公司 | Industrial exhaust gas desulfurizer |
| CN103432869A (en) * | 2013-08-26 | 2013-12-11 | 瓮福（集团）有限责任公司 | Low-concentration sulfur dioxide absorption tower |
| CN103949150A (en) * | 2014-03-14 | 2014-07-30 | 云南磷化集团有限公司 | Method using catalytic oxidation of sulfur dioxide tail gas for PH adjustment agent of phosphate rock ore dressing |
| CN103949150B (en) * | 2014-03-14 | 2016-06-15 | 云南磷化集团有限公司 | SO 2 tail gas catalytic oxidation is for the method for flotation of phosphate rock pH adjuster |
| CN104667728A (en) * | 2015-01-26 | 2015-06-03 | 昆明川金诺化工股份有限公司 | Method for removing sulfur dioxide in sulfuric acid tail gas |
| CN104667732A (en) * | 2015-02-27 | 2015-06-03 | 昆明川金诺化工股份有限公司 | Method for absorbing sulfur dioxide in sulfuric acid tail gas by phosphoric acid via wet process |
| CN104667732B (en) * | 2015-02-27 | 2016-03-02 | 昆明川金诺化工股份有限公司 | A kind of method utilizing phosphoric acid by wet process to absorb sulfur dioxide in sulfuric acid tail gas |
| CN105289264A (en) * | 2015-10-08 | 2016-02-03 | 昆明理工大学 | Method for absorbing low-concentration SO2 (sulfur dioxide) by slurrying of yellow phosphorus electroprecipitating dust |
| WO2017173717A1 (en) * | 2016-04-08 | 2017-10-12 | 成都千砺金科技创新有限公司 | Method for directly using phosphogypsum decomposition gas in wet phosphoric acid production |
| WO2017173716A1 (en) * | 2016-04-08 | 2017-10-12 | 成都千砺金科技创新有限公司 | Method for joint production of phosphogypsum decomposition gas and wet-process phosphoric acid |
| CN105854540A (en) * | 2016-05-23 | 2016-08-17 | 河南红东方化工股份有限公司 | Desulfurizing technology for sulphuric-acid-production tail gas |
| CN106345288A (en) * | 2016-08-24 | 2017-01-25 | 湖北祥云(集团)化工股份有限公司 | Method and system for utilizing phosphoric ore pulp to treat sulfur-containing flue gas |
| CN106345288B (en) * | 2016-08-24 | 2019-04-26 | 湖北祥云(集团)化工股份有限公司 | A kind of method and system using phosphate ore pulp processing sulfur-containing smoke gas |
| CN106178920A (en) * | 2016-08-31 | 2016-12-07 | 陕西煤化能源有限公司 | A kind of rock phosphate in powder phosphoric acid gypsum flue gas desulphurization system and technique thereof |
| CN107398171A (en) * | 2017-06-14 | 2017-11-28 | 昆明理工大学 | A kind of method that acid gas in flue gas is removed using metal tailings |
| CN107899596A (en) * | 2017-10-30 | 2018-04-13 | 昆明理工大学 | A kind of desulfurization denitrification agent and preparation method thereof |
| CN108434977A (en) * | 2017-11-24 | 2018-08-24 | 云南民族大学 | A kind of method of phosphate ore pulp liquid phase catalytic oxidation simultaneous SO_2 and NO removal |
| CN113828140A (en) * | 2021-11-10 | 2021-12-24 | 昆明理工大学 | Strengthening method for wet desulphurization of phosphate slurry |
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