CN102041128A - Chemical deashing method for coal - Google Patents
Chemical deashing method for coal Download PDFInfo
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- CN102041128A CN102041128A CN2010105717417A CN201010571741A CN102041128A CN 102041128 A CN102041128 A CN 102041128A CN 2010105717417 A CN2010105717417 A CN 2010105717417A CN 201010571741 A CN201010571741 A CN 201010571741A CN 102041128 A CN102041128 A CN 102041128A
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- 239000003245 coal Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000126 substance Substances 0.000 title claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 53
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 26
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 26
- 239000004571 lime Substances 0.000 claims abstract description 26
- 238000002386 leaching Methods 0.000 claims abstract description 25
- 239000002699 waste material Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 13
- 238000006396 nitration reaction Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 150000007513 acids Chemical class 0.000 claims description 8
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 8
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 8
- 238000005352 clarification Methods 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 239000011707 mineral Substances 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002912 waste gas Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 150000007522 mineralic acids Chemical class 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000006115 defluorination reaction Methods 0.000 abstract 1
- 238000009991 scouring Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 238000001354 calcination Methods 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000012546 transfer Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Solid Fuels And Fuel-Associated Substances (AREA)
Abstract
The invention discloses a chemical deashing method for coal, belonging to the technical field of clean coal. A novel deashing acid solution is adopted for deashing coal and is a mixed acid of hydrofluoric acid and at least one other inorganic acid, wherein the mass percentage content of the hydrofluoric acid is 5-30%, the mass percentage content of other inorganic acids is 10-40%, and total acid concentration is 10-40%; during acid leaching, the mass ratio of the deashing acid solution to the raw material coal is (1-6):1, reaction temperature is 10-80DEG C, and the process of acid leaching lasts for 4-24 hours; and meanwhile, after exhaust gas and scouring water, generated in a defluorination processing, are graded and reused and a waste mixed acid solution is repeatedly reused, a lime solution is adopted for absorption. The method provided by the invention is suitable for deashing larger coal particles of which the diameter is 1-5mm, and can achieve a better deashing effect. A moderate reaction condition is adopted to ensure that the deashing mixed acid containing hydrofluoric acid is difficult to volatilize, so that energy consumption and cost are lowered and environmental pollution is lightened at the same time.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity coal, be specifically related to a kind of chemical deliming method of coal.
Background technology
The rich coal resources of China, great variety of goods, but inorganic mineral (ash content) content is higher, thereby on certain degree, limited in industrial widespread use.Particularly coal is used for the application in fields such as oil engine at carbon electrode manufacturing, graphite product, gac, high temperature lubricating, oil replacement, and pit ash content has been proposed high requirement.Also there are the big problem of cost consumption in the storage of ash coal, transportation.Therefore, the exploitation of the deliming technology of coal becomes the clean coal technology that obtains broad research for a long time.
At present, the ash removal from raw coal method for preparing high-purity coal, ultrapure coal mainly is divided into physics method, chemical deliming method, physical chemistry deliming method three major types.
Wherein, chemical method has the characteristics of thorough, the suitable face width of deliming, thereby occupies critical role in producing the technology of ultrapure coal.The chemical deliming method has hydrofluoric acid method, acid-base method, melting alkali leaching process, chemical coal technology etc., ash content can be reduced to about 0.5% when effect is better, but because complex process, the cost height is restricted its development.
When adopting the chemical method deliming, the granularity of general requirement feed coal is thinner, and raw coal size is thin more, and the deliming rate is high more, and cleans ash almost reduces with being lowered into of raw material granularity is linear.
Present pickling chemical deliming technology, the general nitration mixture that adopts HF or hydrofluoric acid containing, to the proposition of raw material granularity and ash content high requirement, producing of ultrapure coal, the general nitration mixture of hydrofluoric acid containing that adopts is not higher than 10% to ash oontent, be preferably in below 3.0%, the feed coal of particle diameter below 1mm carries out deliming.
The advantage that it has been generally acknowledged that chemical method is the grinding rate that feed coal needn't reach monomer dissociation, and the effect of deliming is not limited by the raw material pit ash.But in fact present pickling chemical deliming method is for guaranteeing the deliming effect, and still the particle fineness to feed coal has proposed high requirement, helps acid solution like this can fully contact with the coal surface, and the micropore that diffuses into coal rapidly carries out deliming.But coal is milled down to a certain degree can increase energy consumption, and will bring difficulty to subsequent disposal such as filtration, washings, and significant loss is big, has reduced production efficiency.Because the de-ash coal granularity is meticulous, caused the limitation of its range of application simultaneously.
Summary of the invention
The chemical deliming method that the purpose of this invention is to provide the low coal of the high production cost of a kind of production efficiency that addresses the above problem.
The technical scheme that the present invention solves the problems of the technologies described above is: a kind of chemical deliming method of coal, adopt following steps: feed coal is mixed with the deliming acid solution carry out acid-leaching reaction, after the reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, the deliming product is washed, then the deliming product is dried, deliming product after the oven dry carries out defluorinate to be handled, the reuse repeatedly of waste mixed acid liquid, described deliming acid solution is the nitration mixture of hydrofluoric acid and at least a other mineral acids, and wherein, the quality percentage composition of hydrofluoric acid is 5%-30%, the quality percentage composition of other mineral acids is 10-40%, and total acid concentration is 10-40%.
As preferably: the quality percentage composition of hydrofluoric acid is 8%-15%, and the quality percentage composition of other mineral acids is 10-20%.
As preferably: described other mineral acids are at least a in hydrochloric acid, nitric acid, the sulfuric acid.
As preferably: during acid-leaching reaction, the physique of deliming acid solution and feed coal is than being (1-6): 1, and temperature of reaction is 10-80 ℃, leaching time 4-24 hour, so-called physique ratio, i.e. ratio between the quality of the volume of deliming acid solution and feed coal.
Further: during acid-leaching reaction, the deliming acid solution is (2-4) with the physique ratio of feed coal: 1, and temperature of reaction is 20-60 ℃, leaching time is 6-12 hour.
As preferably: the waste gas that produces when defluorinate is handled, adopt lime solution to absorb processing.
As preferably: after the washing, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.
As preferably: waste mixed acid liquid after the reuse, adds lime and handles repeatedly, extracts the discharging of Calcium Fluoride (Fluorspan) after-filtration.
Beneficial effect of the present invention is: the one, through a large amount of experiments, adopted the nitration mixture prescription of new hydrofluoric acid containing, make it go for the deliming that particle diameter is the big coal particle of 1-5mm, simultaneously can reach deliming effect preferably, ash oontent can be no more than 5.0% coal deliming after ash oontent drop to below 0.9%.From the angle of heat transfer, mass transfer, momentum transfer, the granularity of coal is thin more, and surface-area is big more, is beneficial to sour deliming reaction more.Present technique is in conjunction with coal characteristics, by a large amount of experimental exploring deliming mechanism, obtained being applicable to the reaction conditions of big particle diameter coal (1-5mm) deliming, and by changing reaction conditions, can obtain low ash (Ad＜2.0%) even ultralow culm (Ad＜1.0%), and in deliming, sulphur content is reduced to below 2.0%, make deliming efficient improve, ature of coal obtains deep purifying;
The 2nd, adopted gentle reaction conditions, make the deliming nitration mixture of hydrofluoric acid containing not volatile, make full use of, cut down the consumption of energy, alleviated environmental pollution when having saved cost;
The 3rd, recycle, waste gas is absorbed for the classification of the waste water that produces in the present technique production process, waste mixed acid liquid, adopt lime to handle at last, further alleviated environmental pollution, environmental friendliness.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1
A kind of chemical deliming method of coal, the step that adopts is: with particle diameter is 1-5mm, ash oontent is that 4.9% contain culm and deliming solution carry out the acid-leaching reaction deliming under 10 ℃ of temperature, reaction times is 4 hours, deliming solution is the nitration mixture of hydrofluoric acid and hydrochloric acid, wherein fluohydric acid content is 5%, content of hydrochloric acid is 10%, behind the acid-leaching reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, behind the oven dry deliming product, in calcining furnace, the deliming product is carried out defluorinate and handle, adopt lime solution to absorb calciner emission simultaneously, the deliming waste mixed acid after the reuse, adds lime and handles repeatedly, extracts the Calcium Fluoride (Fluorspan) filtering emission, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.The ash oontent of the de-ash coal that obtains at last is 0.9%.
Embodiment 2
A kind of chemical deliming method of coal, the step that adopts is: with particle diameter is 1-5mm, ash oontent is that 4.9% contain culm and deliming solution carry out the acid-leaching reaction deliming under 80 ℃ of temperature, reaction times is 24 hours, deliming solution is the nitration mixture of hydrofluoric acid and hydrochloric acid, wherein fluohydric acid content is 30%, content of hydrochloric acid is 40%, behind the acid-leaching reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, behind the oven dry deliming product, in calcining furnace, the deliming product is carried out defluorinate and handle, adopt lime solution to absorb calciner emission simultaneously, the deliming waste mixed acid after the reuse, adds lime and handles repeatedly, extracts the Calcium Fluoride (Fluorspan) filtering emission, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.The ash oontent of the de-ash coal that obtains at last is 0.5%.
Embodiment 3
A kind of chemical deliming method of coal, the step that adopts is: with particle diameter is 1-5mm, ash oontent is that 4.9% contain culm and deliming solution carry out the acid-leaching reaction deliming under 60 ℃ of temperature, reaction times is 12 hours, deliming solution is the nitration mixture of hydrofluoric acid and hydrochloric acid, wherein fluohydric acid content is 15%, content of hydrochloric acid is 20%, behind the acid-leaching reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, behind the oven dry deliming product, in calcining furnace, the deliming product is carried out defluorinate and handle, adopt lime solution to absorb calciner emission simultaneously, the deliming waste mixed acid after the reuse, adds lime and handles repeatedly, extracts the Calcium Fluoride (Fluorspan) filtering emission, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.The ash oontent of the de-ash coal that obtains at last is 0.6%.
Embodiment 4
A kind of chemical deliming method of coal, the step that adopts is: with particle diameter is 1-5mm, ash oontent is that 4.9% contain culm and deliming solution carry out the acid-leaching reaction deliming under 60 ℃ of temperature, reaction times is 12 hours, deliming solution is hydrofluoric acid, the nitration mixture of hydrochloric acid and nitric acid, wherein fluohydric acid content is 15%, content of hydrochloric acid is 10%, nitric acid content is 10%, behind the acid-leaching reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, behind the oven dry deliming product, the deliming product carried out defluorinate in calcining furnace and handle, adopt lime solution to absorb calciner emission simultaneously, the deliming waste mixed acid is repeatedly after the reuse, adding lime handles, extract the Calcium Fluoride (Fluorspan) filtering emission, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.The ash oontent of the de-ash coal that obtains at last is 0.52%.
Embodiment 5
A kind of chemical deliming method of coal, the step that adopts is: with particle diameter is 1-5mm, ash oontent is that 4.9% contain culm and deliming solution carry out the acid-leaching reaction deliming under 60 ℃ of temperature, reaction times is 12 hours, deliming solution is hydrofluoric acid, hydrochloric acid, nitration mixture, wherein fluohydric acid content is 20%, content of hydrochloric acid is 8%, nitric acid content is 2%, sulfuric acid content is 5%, behind the acid-leaching reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, behind the oven dry deliming product, the deliming product carried out defluorinate in calcining furnace and handle, adopt lime solution to absorb calciner emission simultaneously, the deliming waste mixed acid is repeatedly after the reuse, adding lime handles, extract the Calcium Fluoride (Fluorspan) filtering emission, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.The ash oontent of the de-ash coal that obtains at last is 0.61%.
Embodiment 6
A kind of chemical deliming method of coal, the step that adopts is: with particle diameter is 1-5mm, ash oontent is that 4.9% contain culm and deliming solution carry out the acid-leaching reaction deliming under 60 ℃ of temperature, reaction times is 12 hours, deliming solution is hydrofluoric acid, nitration mixture, wherein fluohydric acid content is 15%, nitric acid content is 7%, sulfuric acid content is 10%, behind the acid-leaching reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, behind the oven dry deliming product, the deliming product carried out defluorinate in calcining furnace and handle, adopt lime solution to absorb calciner emission simultaneously, the deliming waste mixed acid is repeatedly after the reuse, adding lime handles, extract the Calcium Fluoride (Fluorspan) filtering emission, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.The ash oontent of the de-ash coal that obtains at last is 0.53%.
Claims (8)
1. the chemical deliming method of a coal, adopt following steps: feed coal is mixed with the deliming acid solution carry out acid-leaching reaction, after the reaction with deliming product and solution separating, obtain deliming product and waste mixed acid liquid, the deliming product is washed, then the deliming product is dried, deliming product after the oven dry carries out defluorinate to be handled, the reuse repeatedly of waste mixed acid liquid is characterized in that, described deliming acid solution is the nitration mixture of hydrofluoric acid and at least a other mineral acids, wherein, the quality percentage composition of hydrofluoric acid is 5%-30%, and the quality percentage composition of other mineral acids is 10-40%, and total acid concentration is 10-40%.
2. the chemical deliming method of a kind of coal according to claim 1, it is characterized in that: the quality percentage composition of hydrofluoric acid is 8%-15%, the quality percentage composition of other mineral acids is 10-20%.
3. the chemical deliming method of a kind of coal according to claim 1 is characterized in that: described other mineral acids are at least a in hydrochloric acid, nitric acid, the sulfuric acid.
4. the chemical deliming method of a kind of coal according to claim 1 is characterized in that: during acid-leaching reaction, the physique of deliming acid solution and feed coal is than being (1-6): 1, and temperature of reaction is 10-80 ℃, leaching time 4-24 hour.
5. the chemical deliming method of a kind of coal according to claim 4 is characterized in that: during acid-leaching reaction, the physique of deliming acid solution and feed coal is than being (2-4): 1, and temperature of reaction is 20-60 ℃, leaching time is 6-12 hour.
6. the chemical deliming method of a kind of coal according to claim 1 is characterized in that: the waste gas that produces when defluorinate is handled, adopt lime solution to absorb processing.
7. the chemical deliming method of a kind of coal according to claim 1 is characterized in that: after the washing, behind the washing water grading recycle, add lime and handle, behind the clarification filtration, discharge.
8. the chemical deliming method of a kind of coal according to claim 1 is characterized in that: waste mixed acid liquid after the reuse, adds lime and handles repeatedly, extracts the discharging of Calcium Fluoride (Fluorspan) after-filtration.
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| CN 201010571741 CN102041128B (en) | 2010-12-03 | 2010-12-03 | Chemical deashing method for coal |
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| CN 201010571741 CN102041128B (en) | 2010-12-03 | 2010-12-03 | Chemical deashing method for coal |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421560A (en) * | 2013-01-10 | 2013-12-04 | 泸州兰良水泥有限公司 | Coal-based heavy fuel oil and production method thereof |
| CN103421559A (en) * | 2013-01-10 | 2013-12-04 | 泸州兰良水泥有限公司 | Pure coal water slurry and production method thereof |
| CN103421567A (en) * | 2013-01-10 | 2013-12-04 | 泸州兰良水泥有限公司 | Pure coal and production method thereof |
| CN104291333A (en) * | 2014-09-10 | 2015-01-21 | 重庆大学 | Method for preparing stone coal based mesoporous activated carbon with high specific surface area |
| CN104774635A (en) * | 2015-03-27 | 2015-07-15 | 陕西省石油化工研究设计院 | Treatment method for acid washing and deashing of coal liquefaction residue |
| CN105154165A (en) * | 2015-07-10 | 2015-12-16 | 江苏徐矿能源股份有限公司 | Method for reducing ash in inferior slime |
| CN105670731A (en) * | 2016-02-19 | 2016-06-15 | 山东省计量科学研究院 | Method for carrying out supercritical deashing through five-membered ring structure amidine group polyamidine |
| CN106867619A (en) * | 2017-03-30 | 2017-06-20 | 韩越秦 | A kind of sour coupled desulfurization method of coal |
| CN107478667A (en) * | 2016-11-15 | 2017-12-15 | 西安科技大学 | A kind of deliming processing method applied to XRD test analysis coal samples |
| CN107573978A (en) * | 2017-10-19 | 2018-01-12 | 兖矿集团有限公司 | Chemical method prepares the removing system and method for acid-soluble mineral in ultra-clean coal |
| CN110272772A (en) * | 2019-08-05 | 2019-09-24 | 中南大学 | A kind of ultrapure anthracitic preparation method |
| PL425261A1 (en) * | 2018-04-17 | 2019-10-21 | Syntoil Spółka Akcyjna | Method for purification of carbonizate |
| CN111250021A (en) * | 2020-01-22 | 2020-06-09 | 中国矿业大学 | Environment-friendly fine coal chemical deashing equipment and method |
| US12006215B2 (en) | 2018-04-17 | 2024-06-11 | Syntoil Spolka Akcyjna | Method of carbonizate purification |
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| CN103421560B (en) * | 2013-01-10 | 2015-07-08 | 泸州兰良水泥有限公司 | Coal-based heavy fuel oil and production method thereof |
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| CN112368340B (en) * | 2018-04-17 | 2022-03-04 | 合成石油股份公司 | Method for purifying carbonate |
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| CN110272772A (en) * | 2019-08-05 | 2019-09-24 | 中南大学 | A kind of ultrapure anthracitic preparation method |
| CN111250021A (en) * | 2020-01-22 | 2020-06-09 | 中国矿业大学 | Environment-friendly fine coal chemical deashing equipment and method |
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Application publication date: 20110504 Assignee: YUNNAN TIANLI COAL CHEMICAL CO.,LTD. Assignor: YIBIN TIANYUAN GROUP Co.,Ltd. Contract record no.: X2023980044415 Denomination of invention: A Chemical Deashing Method for Coal Granted publication date: 20130424 License type: Common License Record date: 20231031 |