CN102295969A - Method having high removal rate and costing little time for simultaneous removal of sulfur and arsenic in sulfur coal - Google Patents
Method having high removal rate and costing little time for simultaneous removal of sulfur and arsenic in sulfur coal Download PDFInfo
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- CN102295969A CN102295969A CN2011102114215A CN201110211421A CN102295969A CN 102295969 A CN102295969 A CN 102295969A CN 2011102114215 A CN2011102114215 A CN 2011102114215A CN 201110211421 A CN201110211421 A CN 201110211421A CN 102295969 A CN102295969 A CN 102295969A
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Abstract
The invention provides a method having a high removal rate and costing little time for simultaneous removal of sulfur and arsenic in sulfur coal. The method comprises the following steps: grinding dry sulfur coal blocks into powder with a particle size of 0.03 to 5 millimeter, putting obtained powder in a reacting furnace, heating the powder to a temperature of 250 to 400 DEG C in the presence of protective atmosphere, stopping supplying protective atmosphere, supplying chlorine at a flow rate of 0.1 to 200 L/min, and carrying out treatment for one hour to two hours, wherein, volume content of oxygen in chlorine is less than 20%; cooling the powder to a temperature of 4 to 100 DEG C, transferring the powder to a leaching groove, adding dilute hydrochloric acid with a concentration of 0.1 to 3 M, and leaching the powder for five minutes at a temperature of 20 to 100 DEG C, wherein, addition amount of dilute hydrochloric acid is 3 to 30 times of the amount of coal dust; filtering leaching liquid after cooling, rinsing coal solid a plurality of times with water at a temperature of 4 to 100 DEG C, and carrying out drying to obtain purified coal. The method provided in the invention enables the removal rate of sulfur in sulfur coal to be about 80% and the removal rate of arsenic in sulfur coal to be about 95%. The method not only enables S and As in sulfur coal to be removed, but also enables the most of other harmful impurities like Hg, Se, Cd, Pb, Cu, Zn, Fe, K, Na, F and Cl in sulfur coal to be removed simultaneously.
Description
Technical field
Gao Xiao ﹑ removes the wherein method of sulphur and arsenic fast simultaneously before the present invention relates to a kind of high sulphur coal and using.
Background technology
China is maximum in the world coal consumption state.Wherein coal for power generation, Industrial Boiler account for more than 90% of national coal consumption with coal, building materials with coal and coal consumption of living, and these coals all are to be used for incendiary.Although the industrial measure of having taked desulfurization and burning back desulfurization in the burning because desulfurization degree is not high, still has the SO of a great deal of
2Be discharged in the air.Chinese SO in 2010 because of the coal burning generation
2The airborne release amount is above 36,000,000 tons.SO
2Discharge not only serious threat and the healthy of local resident, and the soil of havoc locality, water source, metal and cement works, the financial loss that caused thus in 2000 reaches 1,764 hundred million yuans.In addition, metallurgical coal and coal for locomotive have particular requirement to sulphur content in the coal, and sulphur content is low in the general requirement coal reaches about 1% (w/w).Therefore, the sulphur that removes wherein before the coal combustion has become the task of top priority.In fact except sulphur, also contain in the coal very big detrimental impurity Shen ﹑ mercury of people's toxicity etc., these objectionable impuritiess overwhelming majority enters air in coal combustion process, severe contamination air.China's eighties, annual fire coal was 5.45 hundred million tons, and the arsenic quantity discharged is more than 5000 tons.The sky, big city such as China Lanzhou, Kweiyang, Chengdu, Chongqing, arsenic contamination also is more serious in the atmosphere, and the southwest is because the use of arsenic coal has caused 3000 many cases arseniasis incidents, and the population that Guizhou Province is threatened by arseniasis has 100,000 people.Present Chinese sulphur content is at 2%(w/w) more than coal account for 25% of total reserves, along with the exploitation gradually of low sulphur coal finishes, the ratio of Chinese high sulphur coal will progressively improve.In addition, the southern china coal overwhelming majority is a high sulphur coal, so coal desulfurization seems particularly important at southern china.
The coal desulfurization mode is divided into desulfurization and burning back desulfurization three classes in the preceding Tuo Liu ﹑ burning of burning at present.When coal in the stove internal combustion time in stove the appropriate location spray into sweetening agent, be called desulfurization in the burning.Sweetening agent commonly used has Wingdale, rhombspar, also useful white lime and unslaked lime.Burning back desulfurization mainly is the SO that utilizes in absorption agent or the sorbent material removal flue gas
2, and make it be converted into stable sulfide or sulphur.The defective of desulfurization and burning back desulfurization is the high temperature SO that burning generates in the burning
2Can produce heavy corrosion to equipment, and need the extra sweetener that increases, cause higher desulphurization cost thereby consume chemical reagent.Because these two kinds of methods implement than being easier to, thus study at present and use at most.Desulfurization can reduce SO from root before the burning
2The source, reduce equipment corrosion, thereby comprehensive benefit may be better than the above two.Desulfurization mainly contains these four kinds of screenings, physics coal separation, chemical coal separation, desulfotomaculum bacteria before the burning.At present extensively the physics coal preparation method that adopts has 3 kinds of jigging, dense medium and flotation.The physics coal separation can be removed ash more than 60% and 50% pyritic sulphur, and desulfurization degree is lower, but simple, economical, can be widely used.Chemical method and microbial desulfurization can remove most mineral sulphur in the coal, but the organic sulfur removal rate are not high, and the microbial desulfurization overlong time, are difficult in the actual production utilize.The higher application that has also hindered them of conventional chemical method desulphurization cost.
Summary of the invention
In order to address the above problem, the purpose of this invention is to provide a kind of at high sulphur coal before use, can letter single, high imitate ﹑ remove simultaneously fast wherein sulphur and arsenic the rate of removing height, remove the method for sulphur and arsenic in the high sulphur coal when time spent is few.
Technical scheme of the present invention is: a kind ofly remove the rate height, remove the method for sulphur and arsenic in the high sulphur coal when time spent is few, it may further comprise the steps:
1) a certain amount of drying high-sulfur coal cinder is finely ground to the powder that particle diameter is the 0.03-5 millimeter, places container;
2) described container is placed Reaktionsofen, under protective atmosphere, be heated to 250-400 ℃, stop to feed protective atmosphere then, feed chlorine, handled 1-2 hour; Wherein, in the chlorine oxygen volume content less than 20%; The flow of chlorine is 0.1-200 L/min; Wherein, described protective atmosphere is argon gas, helium or nitrogen;
3) be cooled to 4-100 ℃ after, coal dust in the reaction vessel is transferred in the leaching groove, adding concentration is the dilute hydrochloric acid of 0.1-3M, and this coal dust intermixture was leached 5 minutes under 20-100 ℃ of condition; Wherein, the dilute hydrochloric acid add-on be coal dust 3-30 doubly;
4) cooled and filtered leaching liquid, the water washing coal solid several times with 4-100 ℃ obtains clean coal after the drying.
Further, also can add metal chloride in the described step 1, the 1-15 wt.% that described metal chloride add-on is described quality of pc; Metal chloride is NaCl, KCl, MgCl
2, CaCl
2, AlCl
3, FeCl
3In one or more mixing.
Further, also can add simple substance carbon in the described step 1; The add-on of described simple substance carbon is the 1-40 wt.% of quality of pc, and described simple substance carbon is refinery coke or activated carbon.
Principle of the present invention is: the present invention removes sulphur and arsenic in the high sulphur coal with chlorine simultaneously at low temperature (250-400 ℃).After the chlorination in the high sulphur coal sulphur and arsenic mainly with volatile S
2Cl
2(136 ℃ of boiling points), S (sublimation temperature 112-119 ℃), AsCl
3The volatilization of (130 ℃ of boiling points) form removes from coal.Carbon in the coal chlorine of getting along well with this understanding reacts.What the present invention removed sulphur and arsenic in the high sulphur coal mainly is based on following principle:
(1)
Desulfurization
FeS
2+Cl
2=FeCl
2+2S↑
The 2R-S(organosulfur)+Cl
2=2R-Cl+2S ↑
2S+Cl
2=S
2Cl
2↑
2FeCl
2+Cl
2=2FeCl
3↑
Fe
2O
3+3C+3Cl
2=2FeCl
3↑+3CO↑
(2)
Dearsenification
As
2S
3+3Cl
2=3S+2AsCl
3↑
As
2S
5+3Cl
2=5S+2AsCl
5↑
AsCl
5=2AsCl
3↑+Cl
2
Used industrial chlorine mainly is the by product of caustic soda industry, and its source is wide, cheap.Chlorination process carries out in the industrial chlorination furnace of complete closed, and as the fluidized bed type chlorination furnace, operating process does not have toxic substance leakages such as chlorine, and the residual chlorine in the tail gas is removed by chlorine gas absorption tower again and recycled.The industry chlorination furnace is applied to industrial production by U.S. DuPont company with it as far back as about nineteen fifty-five.
Particularly add metal chloride for example NaCl, KCl, MgCl
2, CaCl
2, AlCl
3, FeCl
3Deng purpose be that the iron arsenic mercury selenium that will contain in the coal etc. is converted into water-soluble various complex chlorides such as NaFeCl
4Or single muriate such as FeCl
3This type of complex chlorides is usually than the easily molten and difficult decomposition of single muriate; The purpose that adds simple substance carbon is to promote the metal oxide that contains in the coal such as the chlorination of ferric oxide, thereby promotes removing of sulphur and arsenic indirectly, such as the ferriferous oxide in the waste mantle that destroys parcel sulfide; Adding the chlorine effect is the chloridized raw material; With the dilute hydrochloric acid leaching, its effect is that metal composite muriate and the single muriate that will generate in the coal after the chlorine treatment extract in the solution, removes from the solid coal.During leaching, can this solidliquid mixture is several to tens minutes in room temperature to 100 ℃ heating, to quicken leaching.Filter then.Filter the washing of back water such as tap water and in elutant, do not have chlorion.
In the method for the invention, with the clean coal Zhong Tan ﹑ Liu ﹑ arsenic content after a series of national standard methods analysis raw coal and the processing.Input raw coal quality is when supposing experiment
, certain constituent content is in the raw coal
, the clean ature of coal amount that obtains after the chloridized is
, wherein certain constituent content is
, so before and after the chlorination this element remove percentage
Be expressed as:
Removal methods compared with prior art had the following advantages and beneficial effect when high sulphur coal of the present invention used preceding sulphur and arsenic:
1) this method can not only the effective elimination high sulphur coal in sulphur, and can efficiently remove arsenic in the high sulphur coal simultaneously.
2) this method can make that sulfur removal rate is about 80% in the high sulphur coal, and the arsenic decreasing ratio is about 95%;
3) the used industrial chlorine of this method mainly is the by product of caustic soda industry, and its source is wide, cheap.
4) this method maximum temperature can be 400 ℃, thereby energy consumption is lower, and because temperature is low,
Equipment is simple, and service life of equipment is long, and facility investment and working cost are few;
5) this method step is simple, and the time spent generally is less than 2 hours;
6) be reflected in the closed system and carry out, no chlorine leakage, muriate in the reaction end gas and chlorine hold
Easily remove by absorption, therefore whole process does not pollute environment, thereby this method
It is environmental protection;
7) this method carbon content in coal is not participated in reaction, thereby not loss, on the contrary, because coal Zhong Liu ﹑ iron
Deng removing of impurity, carbon content in coal content can improve after the chloridized.
8) this method can not only remove S and As in the high sulphur coal, and the overwhelming majority of other detrimental impurity such as Hg ﹑ Se ﹑ Cd ﹑ Pb ﹑ Cu ﹑ Zn ﹑ Fe ﹑ K ﹑ Na ﹑ F ﹑ Cl also is removed in this process simultaneously in the coal.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described further.
Embodiment 1
Particle diameter 0.05-0.07 millimeter 10.0000g high sulphur coal dried powder and particle diameter 0.05-0.07 millimeter 0.500g refinery coke dried powder and particle diameter 0.1-0.05 millimeter 1.000g NaCl dried powder are mixed, pack in the container, again this container is put into Reaktionsofen, under logical argon gas condition, be warming up to 300 ℃, stop logical argon gas then, feed chlorine, the flow of chlorine is 0.5L/min, reacted 2 hours, furnace temperature is cooled to 90 ℃ rapidly, coal dust is transferred in the leaching groove in the reaction vessel, adding concentration is the dilute hydrochloric acid 30ml of 0.1M, this coal dust intermixture is leached 5 minutes the cooled and filtered leaching liquid under 100 ℃ of conditions, water washing coal solid several times with 100 ℃ obtains clean coal after the drying.
The experimental result that removes of sulphur and arsenic is listed in the table 1 in the high sulphur coal:
| ? | S | As | C | W |
 |
%(w/w) | ppm | %(w/w) | g |
| Raw coal | 5.95 | 11.67 | 72.48 | 10.0012 |
| Clean coal | 1.12 | 0.48 | 74.81 | 9.6931 |
| Decreasing ratio | 81% | 96% | ? | ? |
Embodiment 2
Particle diameter 0.05-0.07 millimeter 10.0000g high sulphur coal dried powder and particle diameter 0.05-0.07 millimeter 0.500g refinery coke dried powder are mixed, pack in the container, again this container is put into Reaktionsofen, under logical argon gas condition, be warming up to 250 ℃, stop logical argon gas then, feed chlorine, the flow of chlorine is 150L/min, reacts 1 hour, and furnace temperature is cooled to 60 ℃ rapidly, coal dust is transferred in the leaching groove in the reaction vessel, adding concentration is the dilute hydrochloric acid 100ml of 1.1M, this coal dust intermixture is leached 5 minutes the cooled and filtered leaching liquid under 80 ℃ of conditions, water washing coal solid several times with 80 ℃ obtains clean coal after the drying.The experimental result that removes of sulphur and arsenic is listed in table 2 in the high sulphur coal:
| ? | S | As | C | W |
| %(w/w) | ppm | %(w/w) | g | |
| Raw coal | 5.95 | 11.67 | 72.48 | 10.0012 |
| Clean coal | 1.54 | 0.86 | 74.68 | 9.7315 |
| Decreasing ratio | 75% | 93% | ? | ? |
Embodiment 3
With particle diameter 0.05-0.07 millimeter 10.0000g high sulphur coal dried powder and particle diameter 0.1-0.05 millimeter 1.500g MgCl
2Dried powder mixes, pack in the container, again this container is put into Reaktionsofen, under logical argon gas condition, be warming up to 350 ℃, stop helium injection gas then, feed chlorine, the flow of chlorine is 60L/min, reacts 1.2 hours, and furnace temperature is cooled to 50 ℃ rapidly, coal dust is transferred in the leaching groove in the reaction vessel, adding concentration is the dilute hydrochloric acid 200ml of 1.8M, this coal dust intermixture is leached 5 minutes the cooled and filtered leaching liquid under 50 ℃ of conditions, water washing coal solid several times with 4 ℃ obtains clean coal after the drying.The experimental result that removes of sulphur and arsenic is listed in table 3 in the high sulphur coal:
| ? | S | As | C | W |
 |
%(w/w) | ppm | %(w/w) | g |
| Raw coal | 5.95 | 11.67 | 72.48 | 10.0012 |
| Clean coal | 1.39 | 0.74 | 73.82 | 9.7957 |
| Decreasing ratio | 77% | 94% | ? | ? |
Embodiment 4
CaCl with particle diameter 0.05-0.07 millimeter 10.0000g high sulphur coal dried powder and particle diameter 0.1-0.05 millimeter 1.000g KCl dried powder and particle diameter 0.1-0.05 millimeter 0.2g
2Dried powder mixes, in the container of packing into.Again this container is put into.Then Reaktionsofen is warming up to 370 ℃ under logical argon gas condition, stops logical nitrogen then, feed chlorine, the flow of chlorine is 200L/min, reacts 1.1 hours, after the chlorination, open on the Reaktionsofen again, furnace temperature is cooled to 4 ℃ rapidly, coal dust in the reaction vessel is transferred in the leaching groove, adding concentration is the dilute hydrochloric acid 200ml of 1.8M, this coal dust intermixture was leached 5 minutes under 50 ℃ of conditions, the cooled and filtered leaching liquid, the water washing coal solid several times with 30 ℃ obtains clean coal after the drying.The experimental result that removes of sulphur and arsenic is listed in table 4 in the high sulphur coal:
| ? | S | As | C | W |
 |
%(w/w) | ppm | %(w/w) | g |
| Raw coal | 5.95 | 11.67 | 72.48 | 10.0012 |
| Clean coal | 1.23 | 0.65 | 74.42 | 9.8957 |
| Decreasing ratio | 80% | 95% | ? | ? |
Embodiment 5
NaCl, particle diameter 0.1-0.05 millimeter 0.500g CaCl with particle diameter 0.05-0.07 millimeter 10.0000g high sulphur coal dried powder and particle diameter 0.05-0.07 millimeter 0.500g refinery coke dried powder and particle diameter 0.1-0.05 millimeter 0.500g
2The FeCl of dried powder and particle diameter 0.1-0.05 millimeter 0.500g
3The dried powder grain mixes, in the container of packing into.Again this container is put into and be arranged in Reaktionsofen.Then Reaktionsofen is warming up to 400 ℃ under logical argon gas condition, stops logical argon gas then, change logical chlorine, the chlorine flowrate of feeding is 100L/min, reaction 1.8 hours, with impurity such as sulphur in the chlorination high sulphur coal and arsenic.After the chlorination, furnace temperature is cooled to 4 ℃ rapidly, coal dust in the reaction vessel is transferred in the leaching groove, adding concentration is 3M dilute hydrochloric acid solution 300ml, this coal dust intermixture is leached 5 minutes cold filtration under 20 ℃ of conditions, use 4 ℃ of hot wash coal solid several times again, obtain clean coal after the drying.The experimental result that removes of sulphur and arsenic is listed in table 5 in the high sulphur coal:
| ? | S | As | C | W |
 |
%(w/w) | ppm | %(w/w) | g |
| Raw coal | 5.95 | 11.67 | 72.48 | 10.0012 |
| Clean coal | 1.49 | 0.69 | 74.47 | 9.8641 |
| Decreasing ratio | 76% | 94% | ? | ? |
Claims (3)
1. the method for removing the rate height, removing sulphur and arsenic in the high sulphur coal when time spent is few is characterized in that, may further comprise the steps:
1) a certain amount of exsiccant high-sulfur coal cinder is finely ground to the powder that particle diameter is the 0.03-5 millimeter, places container;
2) described container is placed Reaktionsofen, under protective atmosphere, be heated to 250-400 ℃, stop logical protective atmosphere then, feed chlorine, handled 1-2 hour; Wherein, in the chlorine oxygen volume content less than 20%; The flow of chlorine is 0.1-200 L/min; Wherein, described protective atmosphere is argon gas, helium or nitrogen;
3) be cooled to 4-100 ℃ after, coal dust in the reaction vessel is transferred in the leaching groove, adding concentration is the dilute hydrochloric acid of 0.1-3M, and this coal dust intermixture was leached 5 minutes under 20-100 ℃ of condition; Wherein, the dilute hydrochloric acid add-on be coal dust 3-30 doubly;
4) cooled and filtered leaching liquid, the water washing coal solid several times with 4-100 ℃ obtains clean coal after the drying.
2. method according to claim 1 also can add metal chloride in the described step 1, the 1-15 wt.% that described metal chloride add-on is described quality of pc; Metal chloride is NaCl, KCl, MgCl
2, CaCl
2, AlCl
3, FeCl
3In one or more mixing.
3. method according to claim 1 and 2 also can add simple substance carbon in the described step 1; The 1-40 wt.% that described simple substance carbon add-on is a quality of pc, described simple substance carbon are refinery coke or activated carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110211421 CN102295969B (en) | 2011-07-27 | 2011-07-27 | Method for simultaneous removal of sulfur and arsenic in sulfur coal with high removal rate and little time |
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|---|---|---|---|
| CN 201110211421 CN102295969B (en) | 2011-07-27 | 2011-07-27 | Method for simultaneous removal of sulfur and arsenic in sulfur coal with high removal rate and little time |
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| Publication Number | Publication Date |
|---|---|
| CN102295969A true CN102295969A (en) | 2011-12-28 |
| CN102295969B CN102295969B (en) | 2013-09-18 |
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|---|---|---|---|
| CN 201110211421 Expired - Fee Related CN102295969B (en) | 2011-07-27 | 2011-07-27 | Method for simultaneous removal of sulfur and arsenic in sulfur coal with high removal rate and little time |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468344A (en) * | 2013-08-27 | 2013-12-25 | 广州高成环保科技有限公司 | Oxygen producer for increasing coal burn-off rate |
| CN106675683A (en) * | 2017-01-12 | 2017-05-17 | 安徽理工大学 | Method for carrying out microwave-assisted low-quality coal desulfurization |
| CN110172583A (en) * | 2019-07-03 | 2019-08-27 | 中南大学 | A kind of method of the minimizing efficient process containing arsenic smoke dust |
| CN110527578A (en) * | 2019-09-30 | 2019-12-03 | 山西焦煤集团有限责任公司 | A kind of method that microwave-assisted halogen simple substance carries out big partial size coal desulfurization |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4081250A (en) * | 1976-08-27 | 1978-03-28 | California Institute Of Technology | Coal desulfurization process |
| US4118200A (en) * | 1977-07-08 | 1978-10-03 | Cato Research Corporation | Process for desulfurizing coal |
| EP0060354A1 (en) * | 1981-03-12 | 1982-09-22 | Carson, Dennis M. | Method of treating coal to remove sulphur and ash |
| GB2097423A (en) * | 1981-03-31 | 1982-11-03 | Foster Wheeler Energy Corp | Desulphurising coal with c12 |
-
2011
- 2011-07-27 CN CN 201110211421 patent/CN102295969B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4081250A (en) * | 1976-08-27 | 1978-03-28 | California Institute Of Technology | Coal desulfurization process |
| US4118200A (en) * | 1977-07-08 | 1978-10-03 | Cato Research Corporation | Process for desulfurizing coal |
| EP0060354A1 (en) * | 1981-03-12 | 1982-09-22 | Carson, Dennis M. | Method of treating coal to remove sulphur and ash |
| GB2097423A (en) * | 1981-03-31 | 1982-11-03 | Foster Wheeler Energy Corp | Desulphurising coal with c12 |
Non-Patent Citations (1)
| Title |
|---|
| EUNG HA CHO: "Coal desulfurization with aqueous chloride", 《METALLURGICAL TRANSACTIONS B》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468344A (en) * | 2013-08-27 | 2013-12-25 | 广州高成环保科技有限公司 | Oxygen producer for increasing coal burn-off rate |
| CN103468344B (en) * | 2013-08-27 | 2015-01-28 | 广州高成环保科技有限公司 | Oxygen producer for increasing coal burn-off rate |
| CN106675683A (en) * | 2017-01-12 | 2017-05-17 | 安徽理工大学 | Method for carrying out microwave-assisted low-quality coal desulfurization |
| CN106675683B (en) * | 2017-01-12 | 2020-06-30 | 安徽理工大学 | Microwave-assisted low-quality coal desulfurization method |
| CN110172583A (en) * | 2019-07-03 | 2019-08-27 | 中南大学 | A kind of method of the minimizing efficient process containing arsenic smoke dust |
| CN110527578A (en) * | 2019-09-30 | 2019-12-03 | 山西焦煤集团有限责任公司 | A kind of method that microwave-assisted halogen simple substance carries out big partial size coal desulfurization |
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|---|---|
| CN102295969B (en) | 2013-09-18 |
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