CN104774635A - Treatment method for acid washing and deashing of coal liquefaction residue - Google Patents
Treatment method for acid washing and deashing of coal liquefaction residue Download PDFInfo
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- CN104774635A CN104774635A CN201510137360.0A CN201510137360A CN104774635A CN 104774635 A CN104774635 A CN 104774635A CN 201510137360 A CN201510137360 A CN 201510137360A CN 104774635 A CN104774635 A CN 104774635A
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- coal
- coal liquefaction
- solid
- liquefaction residue
- hydrochloric acid
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/023—Working-up pitch, asphalt, bitumen by chemical means reaction with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a treatment method for acid washing and deashing of coal liquefaction residue. The treatment method comprises: crushing a coal liquefaction residue raw material into fine particles, carrying out reaction washing on the fine particles with a hydrochloric acid solution under a microwave condition to obtain primary solid, further carrying out reaction washing with a mixed acid solution containing hydrofluoric acid, carrying out solid-liquid separation, and carrying out water washing on the solid to remove the attached soluble substance so as to obtain the coal tar pitch with the ash content of less than 2%, wherein the coal tar pitch can be used as the raw material for manufacturing active carbon, petroleum coke, and high-quality coal water slurry, can further be used as the asphalt modification agent in the fields of combustion, coking, hydrogen production through gasification, novel chemical industry materials and the like, can achieve the most effective utilization, and has advantages of economy and environmental protection of the coal liquefaction project.
Description
Technical field
The invention belongs to coal liquifaction chemical processing field, be specifically related to a kind for the treatment of process of pickling deliming of coal liquefaction residue.
Background technology
The feature of the disposable energy of China is " many coal, few oil, lack Sweet natural gas ", in order to the uncertain problem of the anxiety and supply that solve crude oil, diversification reduces the risk of oil supply, exploitation coal liquifaction technology is one of Strategic Measure of China's energy construction, the DCL/Direct coal liquefaction liquefaction technology of current Some Domestic enterprise, that dry coal dust and sulphur iron catalyst and solvent oil are mixed and made into coal oil mixture, coal and the common hydrocracking of heavy solvent in pyroreaction device, reactants separate obtains combustible gas, liquid fuel (gasoline, diesel etc.) and solid residue, and the kerosene of other enterprises altogether the technology of refining be with petroleum refinery's residual oil substitute DCL/Direct coal liquefaction use solvent oil, common hydrocracking is mixed with coal, the cleaning liquid fluid fuel of production high value.
No matter be that DCL/Direct coal liquefaction liquefaction technology and kerosene refine technology altogether, underpressure distillation or solvent extraction and separation is adopted to go out liquid fuel in process of production, capital output accounts for the coal liquefaction residue of coal dust about 30%, coal liquefaction residue is primarily of inorganics and organism two portions composition, and wherein organic matter comprises heavy coal liquids, bitumen and unconverted coal; Inorganics comprises minerals in coal and gelatin liquefaction sulphur iron catalyst, coal liquefaction residue is a kind of high ash, high-sulfur, compounding substances that thermal value is high, people study and find that coal liquefaction residue is a kind of raw material with applications well prospect, coal liquefaction residue is used to gasification hydrogen-producing, to meet the demand to hydrogen in DCL/Direct coal liquefaction hydrogenation process; Coal liquefaction residue has very golf calorific value, can be used as boiler oil; Coal liquefaction residue is for the preparation of modifying asphalt aspect, and it can produce mesophase pitch through process, and then produces high-performance carbon fibre material, realizes the high value added utilization of coal liquefaction residue.
Patent ZL 200910086158.4 discloses a kind of method that coal liquefaction residue prepares mesophase pitch, patent ZL200910087907.5 discloses a kind of method that coal directly-liquefied residue prepares asphalt base carbon fiber, patent ZL201010225042.7 discloses a kind of method and its application of extracting heavy coal liquids and mesophase pitch class material from coal directly-liquefied residue, patent ZL 201010299540.6 discloses a kind of coal directly-liquefied residue extracting process and application, patent ZL201310211244.x discloses one isolated bitumen and methods and applications thereof from the direct liquid of coal, patent ZL201410021264.5 discloses a kind of modifying asphalt, the serialization of coal directly-liquefied residue normal pressure is utilized to prepare method and the application thereof of modifying asphalt, above patent can be found out, adopt solvent extraction or solvent extraction method to the separation of coal liquefaction residue, first inorganics in coal liquefaction residue is separated, and then high added value research is carried out to organic matter, extraction agent used is toluene, naphtalene oil, coal tar, middle distillate from coal liquefaction, tetrahydrofuran (THF), N, N-dimethylformamide, N methyl 2 pyrrolidone etc., extracting and separating goes out asphaltic substances, prepare mesophase pitch, modifying asphalt, impregnating pitch etc., solvent extraction technology separation condition is relatively harsh, filter plant requires high, extraction agent has partial loss and cost is higher, and it is not high to extract organic yield from residue yet, the bitumen obtained is not suitable as raw material and the high-quality fuel of gac.Previous cycle expanding economy and increasingly serious environmental stress, make coal chemical industry effectively utilize the demand of technology more urgent to coal liquefaction residue.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of this invention is to provide a kind for the treatment of process of pickling deliming of coal liquefaction residue, primary ore material in coal liquefaction residue and sulphur iron catalyst are sloughed, thus obtain the coal-tar pitch that ash content is less than 2%, can be used as the raw material manufacturing gac, refinery coke, high-quality coal water slurry, also as asphalt modifier, in burning, coking, gasification hydrogen-producing, new type chemical material etc., there is low ash content low sulphur coal pitch and reach the feature the most effectively utilized.
To achieve these goals, the technical solution used in the present invention is: a kind for the treatment of process of pickling deliming of coal liquefaction residue, comprises the following steps:
1) first coal liquefaction residue thing is pulverized the solid particulate for being less than 0.2mm, this solid particulate and concentration are that 20 ~ 90 g/L hydrochloric acid solns mix pulping in slurrying pond, and the mass ratio of hydrochloric acid soln and solid particulate is (3 ~ 7): 1;
A) above-mentioned slurry is in pickling tub, and first frequency of utilization is 2450MHz microwave complex reaction;
B) hydrochloric acid reaction cleaning coal liquefaction residue thing, reaction cleaning temperature is 20-85 degree, and scavenging period is 0.5-8 hour, and then carries out solid-liquid separation, obtains primary stage solids;
2) primary stage solids is collected, the mixed acid-respons cleaning of hydrochloric acid and hydrofluoric acid is used in reactive tank, wherein concentration of hydrochloric acid is 20 ~ 70 g/L, hydrofluoric acid concentration is 10 ~ 50g/L, mixed acid is (2 ~ 7) with the mass ratio of solid particulate: 1, and the temperature of reaction solution remains 30-85 degree, cleaning 0.5-6 hour, and then carry out solid-liquid separation, obtain secondary solid;
3) secondary solid is entered water wash column washing, use temperature is that the water of 10-95 degree rinses, and except the reactant of attachment removal, during to PH6.5-7.5, then dehydration, drying, obtain low-ash coal-tar pitch.
Described hydrochloric acid soln and mixed acid solution reusable, enter spent acid treatment system afterwards.
Described hydrochloric acid soln reaction cleaning solid particulate, microwave complex reaction 2-12 minute.
Described solid-liquid separation method be filter, centrifugal or settlement separate in one or more.
Compared with prior art, the invention has the beneficial effects as follows:
1) particle diameter of solid particulate is less than 0.2mm, effectively can improve the contact area of solid reactant, is conducive to hydrochloric acid and fully reacts with becoming grey mineral substance.
2) microwave can improve reaction conditions, and accelerate speed of reaction, micro-wave energy effectively improves leaching kinetics, and hydrochloric acid medium can carry out selectivity process to the sulphur iron catalyst etc. in liquefied residue, reaches the object of high-efficiency desulfurization deliming.
3) adopt acidic solution to sulphur iron catalyst and become grey mineral substance selective reaction, by control inorganic acid concentration, temperature of reaction, pickling time, in coal-tar pitch, ash content significantly reduces, coal-tar pitch yield about 80%.
4) have deliming effective, technical process is simple, and operational condition is gentle, does not use expensive organic solvent, the advantages such as processing costs is low.
Embodiment
Below in conjunction with embodiment, the technical scheme of invention is described further.
Embodiment 1
Ash content (the A of coal liquefaction residue
d) 15.8%, sulphur content (S
t) 2.3%.
A treatment process for the pickling deliming of coal liquefaction residue, comprises the following steps:
Get 0.20kg coal liquefaction residue to pulverize, Solids Particle Diameter≤0.2mm, add 0.8kg water, high speed dispersion, make slurry, add 0.13kg hydrochloric acid soln (content of hydrochloric acid 30%), then put into the microwave equipment of 2.45GHz, microwave treatment 6 minutes, then above-mentioned reactant is sent in acid-resistant container, keep reacting liquid temperature 70 DEG C, 3 hours reaction times, then reacting liquid filtering, obtain 0.18 kg solid, solid is put into reactor, and add the mixing of 0.9kg mixed acid solution, in mixed acid solution, concentration of hydrochloric acid is 40 g/L, hydrofluoric acid concentration is 35g/L, reacting liquid temperature 60 degree, 3 hours reaction times, then filter, reclaim solid, again with temperature 60 DEG C of water cleaning solids, wash with water to PH6.5-7.5, dehydration, 0.167kg coal-tar pitch is obtained after dry, ash content (A in coal-tar pitch
d) 1.8%.
Embodiment 2
Ash content (the A of coal liquefaction residue
d) 17.4%, sulphur content (S
t) 2.5%.
A treatment process for the pickling deliming of coal liquefaction residue, comprises the following steps:
Get 0.30kg coal liquefaction residue to pulverize, Solids Particle Diameter≤0.2mm, with 1.1kg hydrochloric acid soln mixed pulp, concentration of hydrochloric acid solution is 50 g/L, then send into the microwave equipment of 2.45GHz, microwave treatment 5 minutes, then above-mentioned reactant is poured in acid-resistant container, keep reacting liquid temperature 70 DEG C, after 5 hours time, by reacting liquid filtering, obtain 0.26kg solid, in the reactor, 0.27kg solid adds the mixing of 1kg mixed acid solution, in mixed acid solution, concentration of hydrochloric acid is 45 g/L, hydrofluoric acid concentration is 40g/L, solution is heated to 65 degree, 4 hours reaction times, then filter, reclaim solid, again with temperature 70 DEG C of water cleaning solids, wash with water to PH6.5-7.5, dehydration, 0.242 kg coal-tar pitch is obtained after dry, ash content (A in coal-tar pitch
d) 1.7%.
Embodiment 3
Ash content (the A of coal liquefaction residue
d) 17.4%, sulphur content (S
t) 2.5%.
A treatment process for the pickling deliming of coal liquefaction residue, comprises the following steps:
Get 0.30kg coal liquefaction residue to pulverize, Solids Particle Diameter≤0.2mm, with 1.3kg hydrochloric acid soln mixed pulp, concentration of hydrochloric acid solution is 40 g/L, then put into the microwave equipment of 2.45GHz, microwave treatment 6 minutes, then above-mentioned reactant is sent in acid-resistant container, keep reacting liquid temperature 65 DEG C, 3 hours reaction times, by reacting liquid filtering, obtain 0.26kg solid, reusable 1kg mixed acid solution and 0.27kg solids mixing in reactor, in reusable mixed acid solution, concentration of hydrochloric acid is 30 g/L, hydrofluoric acid concentration is 25g/L, solution is heated to 70 degree, 2 hours reaction times, then filter, reclaim solid, again with temperature 90 DEG C of water cleaning solids, wash with water to PH6.5-7.5, dehydration, 0.25kg coal-tar pitch is obtained after dry, ash content (A in coal-tar pitch
d) 1.9%.
Embodiment 4
Ash content (the A of coal liquefaction residue
d) 15.1%, sulphur content (S
t) 2.2%.
A treatment process for the pickling deliming of coal liquefaction residue, comprises the following steps:
Get 0.2kg coal liquefaction residue to pulverize, Solids Particle Diameter≤0.2mm, add 1 kg hydrochloric acid soln, concentration of hydrochloric acid solution is 40 g/L, high speed dispersion, make slurry, then the microwave equipment of 2.45GHz is put into, microwave treatment 6 minutes, again above-mentioned reaction solution is sent in container, keep temperature 75 DEG C, 4 hours reaction times, then filter, obtain 0.18 kg solid, solid is put into reactor, and add the mixing of 0.9kg mixed acid solution, in mixed acid solution, concentration of hydrochloric acid is 40 g/L, hydrofluoric acid concentration is 35g/L, be heated to 70 degree, react 3 hours, then filter, reclaim solid, again with temperature 70 DEG C of water cleaning solids, wash with water to PH6.5-7.5, dehydration, 0.165 kg coal-tar pitch is obtained after dry, A
d(ash content) 1.6%.
Embodiment 5
Ash content (the A of coal liquefaction residue
d) 15.1%, sulphur content (S
t) 2.2%.
A treatment process for the pickling deliming of coal liquefaction residue, comprises the following steps:
Get 0.3kg coal liquefaction residue to pulverize, Solids Particle Diameter≤0.2mm, add 1.2 kg hydrochloric acid solns, concentration of hydrochloric acid solution is 50 g/L, high speed dispersion, make slurry, then the microwave equipment of 2.45GHz is put into, microwave treatment 5 minutes, above-mentioned reactant is sent in container, reaction solution keeps temperature 70 DEG C, 4 hours reaction times, then filter, obtain 0.26 kg solid, solid is put into reactor, and add the mixing of 1.2kg mixed acid solution, in mixed acid solution, concentration of hydrochloric acid is 40 g/L, hydrofluoric acid concentration is 30g/L, reaction solution is heated to 70 degree, react 4 hours, then filter, reclaim filter cake, again with temperature 60 DEG C of water cleaning solids, wash with water to PH6.5-7.5, dehydration, 0.247 kg coal-tar pitch is obtained after dry, ash content (A
d) 1.5%.
According to embodiment 1-5, adopt acidic solution to sulphur iron catalyst and become grey mineral substance selective reaction, by control inorganic acid concentration, temperature of reaction, pickling time, in coal-tar pitch, ash content significantly reduces, coal-tar pitch yield about 80%.
Claims (4)
1. a treatment process for the pickling deliming of coal liquefaction residue, is characterized in that, comprise the following steps:
1) first coal liquefaction residue thing is pulverized the solid particulate for being less than 0.2mm, this solid particulate and concentration are that 20 ~ 90 g/L hydrochloric acid solns mix pulping in slurrying pond, and the mass ratio of hydrochloric acid soln and solid particulate is (3 ~ 7): 1;
A) above-mentioned slurry is in pickling tub, and first frequency of utilization is 2450MHz microwave complex reaction;
B) hydrochloric acid reaction cleaning coal liquefaction residue thing, reaction cleaning temperature is 20-85 degree, and scavenging period is 0.5-8 hour, and then carries out solid-liquid separation, obtains primary stage solids;
2) primary stage solids is collected, the mixed acid-respons cleaning of hydrochloric acid and hydrofluoric acid is used in reactive tank, wherein concentration of hydrochloric acid is 20 ~ 70 g/L, hydrofluoric acid concentration is 10 ~ 50g/L, mixed acid is (2 ~ 7) with the mass ratio of solid particulate: 1, and the temperature of reaction solution remains 30-85 degree, cleaning 0.5-6 hour, and then carry out solid-liquid separation, obtain secondary solid;
3) secondary solid is entered water wash column washing, use temperature is that the water of 10-95 degree rinses, and except the reactant of attachment removal, during to PH6.5-7.5, then dehydration, drying, obtain low-ash coal-tar pitch.
2. the treatment process of the pickling deliming of a kind of coal liquefaction residue according to claim 1, is characterized in that, described hydrochloric acid soln and mixed acid solution reusable, enter spent acid treatment system afterwards.
3. the treatment process of the pickling deliming of a kind of coal liquefaction residue according to claim 1, is characterized in that, described hydrochloric acid soln reaction cleaning solid particulate, microwave complex reaction 2-12 minute.
4. the treatment process of the pickling deliming of a kind of coal liquefaction residue according to claim 1, is characterized in that, described solid-liquid separation method be filter, centrifugal or settlement separate in one or more.
Priority Applications (1)
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| CN201510137360.0A CN104774635A (en) | 2015-03-27 | 2015-03-27 | Treatment method for acid washing and deashing of coal liquefaction residue |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109133055A (en) * | 2018-08-03 | 2019-01-04 | 山西煤炭进出口集团科学技术研究院有限公司 | A kind of preparation method and application of high-purity medium temperature coal pitch super active carbon |
| CN110317625A (en) * | 2019-06-28 | 2019-10-11 | 郑州大学 | A kind of processing method of coal directly-liquefied residue desulfurization and deashing |
| CN110540851A (en) * | 2019-08-20 | 2019-12-06 | 佛山市富龙环保科技有限公司 | Processing technology of waste mineral oil dregs |
| CN113088309A (en) * | 2021-03-04 | 2021-07-09 | 唐钢美锦（唐山）煤化工有限公司 | Method and device for reducing ash content in coke powder |
| CN113376278A (en) * | 2021-06-09 | 2021-09-10 | 宁夏大学 | Method for extracting polycyclic aromatic hydrocarbon from coal gasification fine slag |
| CN115249589A (en) * | 2022-07-11 | 2022-10-28 | 哈尔滨工业大学 | Method for preparing activated carbon for supercapacitor by using coal gasification fine ash |
| CN115385617A (en) * | 2022-08-12 | 2022-11-25 | 金陵科技学院 | High-performance concrete and preparation method thereof |
| CN117430375A (en) * | 2023-12-18 | 2024-01-23 | 内蒙古工业大学 | Coal liquefaction residue carbon material and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105670731B (en) * | 2016-02-19 | 2018-07-20 | 山东省计量科学研究院 | A method of carrying out overcritical deliming using five-membered ring structure amidino groups reunion amidine |
| CN109133055A (en) * | 2018-08-03 | 2019-01-04 | 山西煤炭进出口集团科学技术研究院有限公司 | A kind of preparation method and application of high-purity medium temperature coal pitch super active carbon |
| CN110317625A (en) * | 2019-06-28 | 2019-10-11 | 郑州大学 | A kind of processing method of coal directly-liquefied residue desulfurization and deashing |
| CN110540851A (en) * | 2019-08-20 | 2019-12-06 | 佛山市富龙环保科技有限公司 | Processing technology of waste mineral oil dregs |
| CN110540851B (en) * | 2019-08-20 | 2021-06-08 | 佛山市富龙环保科技有限公司 | Processing technology of waste mineral oil dregs |
| CN113088309A (en) * | 2021-03-04 | 2021-07-09 | 唐钢美锦（唐山）煤化工有限公司 | Method and device for reducing ash content in coke powder |
| CN113376278A (en) * | 2021-06-09 | 2021-09-10 | 宁夏大学 | Method for extracting polycyclic aromatic hydrocarbon from coal gasification fine slag |
| CN115249589A (en) * | 2022-07-11 | 2022-10-28 | 哈尔滨工业大学 | Method for preparing activated carbon for supercapacitor by using coal gasification fine ash |
| CN115385617A (en) * | 2022-08-12 | 2022-11-25 | 金陵科技学院 | High-performance concrete and preparation method thereof |
| CN117430375A (en) * | 2023-12-18 | 2024-01-23 | 内蒙古工业大学 | Coal liquefaction residue carbon material and preparation method and application thereof |
| CN117430375B (en) * | 2023-12-18 | 2024-02-20 | 内蒙古工业大学 | Coal liquefaction residue carbon material and preparation method and application thereof |
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Application publication date: 20150715 |