CN105419835A - Processing method of coal low-temperature pyrolysis volatile component - Google Patents
Processing method of coal low-temperature pyrolysis volatile component Download PDFInfo
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- CN105419835A CN105419835A CN201510857696.4A CN201510857696A CN105419835A CN 105419835 A CN105419835 A CN 105419835A CN 201510857696 A CN201510857696 A CN 201510857696A CN 105419835 A CN105419835 A CN 105419835A
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- volatile matter
- dust removal
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/18—Modifying the properties of the distillation gases in the oven
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/14—Features of low-temperature carbonising processes
Abstract
The invention relates to a processing method of a coal low-temperature pyrolysis volatile component. The processing method of the coal low-temperature pyrolysis volatile component comprises the following steps: S1, carrying out dust removal treatment on the volatile component; S2, sequentially carrying out distillation, oil washing and fractionation on the volatile component, so as to obtain a light component and a heavy component; and S3, hydrogenating the heavy component, and then carrying out thermal high pressure separation, thermal low pressure separation, cold high pressure separation and cold low pressure separation on reaction products, so as to obtain olefin and a hydrogenated product. The processing method of the coal low-temperature pyrolysis volatile component has the advantages that clean and high-quality oil products with stable properties, such as synthesis gas, gasoline and diesel oil, can be produced, and the refinement degree is high; meanwhile, the heavy component is fully utilized, and a rectification process does not need to be carried out, so that the production energy consumption is low.
Description
Technical field
The present invention relates to coal chemical technology, be specifically related to a kind of working method of low-temperature pyrolysis of coal volatile matter.
Background technology
The low temperature pyrogenation of coal is also called the low-temperature pyrolysis of coal, refers to and is heated under the condition of isolated air by coal, generates the process of the products such as coal gas, tar and coke.China is the first big country of coke production in the world, and China's coking industry production in the end of the year 2014 40,000 ten thousand tons, coke, accounts for more than 60% of world's coke ultimate production.Tar production capacity has reached 2,000 ten thousand tons, to 2014 the end of the year China's coal tar processing ability reached about 1,700 ten thousand tons/year, coal tar deep processing variety and quality is constantly improved.
The volatile matter that low-temperature pyrolysis of coal produces, mainly comprises H
2, CO, CH
4with coal tar wet goods.Wherein, the black with pungent odour generated when coal tar is coal destructive distillation or chocolate viscous liquid, be called for short tar.Coal tar is a kind of complex mixture of hydrocarbon polymer, and major part is be worth higher rare kind.In today of petrochemical complex high speed development, coal tar chemical industry still occupies critical role, has the effect do not replaced providing in polycyclic aromatic hydrocarbons and high-carbon materials stock.
While tar production capacity increases fast, should acutely aware domestic tar main process flow process be atmospheric distillation process, for keeping the cutting yield of tarry cut under atmospheric pressure state, the possibility that temperature reduces be very little; Technological process conservation measures is unfavorable, and coal tar processing cost is higher, and coal tar processing development is faced with product and becomes more meticulous the letters such as degree is low, added value of product is low, state of the art is low problem to be solved.
Summary of the invention
For this reason, to be solved by this invention is that existing low-temperature pyrolysis of coal volatile matter working method becomes more meticulous that degree is low, the disadvantageous problem of conservation measures, thus a kind of energy-conserving and environment-protective are provided, working method that the degree that becomes more meticulous is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
The working method of a kind of low-temperature pyrolysis of coal volatile matter of the present invention, comprises the following steps:
S1, dust removal process is carried out to described volatile matter;
S2, described volatile matter is distilled successively, oil wash and fractionation, obtain light constituent and heavy constituent;
S3, described heavy constituent is carried out hydrotreatment, reaction product carries out thermal high separation again, thermal low is separated, cold anticyclone is separated, cold low is separated, obtain alkene and hydrogenated products.
In described step S2, described distilation steps comprises one-level underpressure distillation step and second depressurized distilation steps; Described oil wash step comprises one-level oil wash step and secondary oil wash step; Carry out described one-level oil wash step after described one-level underpressure distillation step, then carry out described second depressurized distilation steps and described secondary oil wash step successively; Described fractionating step is output alkene, gasoline and diesel oil successively; Described secondary oil wash step output synthetic gas.
The temperature of described one-level underpressure distillation step and described second depressurized distilation steps is 300 DEG C ~ 550 DEG C, and pressure is 0.010MPa ~ 0.099MPa.
The temperature of described one-level oil wash step and described secondary oil wash step is 200 DEG C ~ 550 DEG C, and pressure is 0.1MPa ~ 2.0MPa.
In described step S3, the reaction conditions of described hydrogenation step is: temperature of reaction 300 DEG C ~ 550 DEG C, pressure 12Mpa ~ 17Mpa, hydrogen to oil volume ratio 400:1-2000:1, volume space velocity 0.1/h
-1~ 2.0/h
-1.
In described step S3, described thermal high separating step service temperature is 300 DEG C ~ 550 DEG C, working pressure is 10Mpa ~ 30Mpa; Described thermal low separating step service temperature is 300 DEG C ~ 550 DEG C, working pressure is 1.0Mpa ~ 5.0Mpa; Described cold anticyclone separating step service temperature is 10 DEG C ~ 100 DEG C, working pressure is 10Mpa ~ 30Mpa; Described cold low separating step service temperature is 10 DEG C ~ 100 DEG C, working pressure is 1.0Mpa ~ 5.0Mpa.
In described step S1, described dust removal step is comprised at least one of being assembled in dedusting, electrostatic precipitation by the dedusting of particle fixed bed, cyclone dust removal, micro swirl and carries out dedusting; After described dust removal step, the particle diameter of the residual dust in described volatile matter is less than 5 μm.
In described step S1, described dust removal step comprise carry out successively cyclone dust removal step, particle fixed bed dust removal step, micro swirl assemble dust removal step, electrostatic precipitation step; Wherein, described micro swirl is assembled in dust removal step, and filler is porous spherical filler.
In described step S3, described heavy constituent also comprises the step removed the gred to described heavy constituent before carrying out hydrotreatment.
In described step S3, described hydrogenation step is undertaken by boiling bed hydrogenation reactor.
Technique scheme of the present invention has the following advantages compared to existing technology:
The working method of a kind of low-temperature pyrolysis of coal volatile matter described in the embodiment of the present invention, comprises the following steps: S1, carry out dust removal process to described volatile matter; S2, described volatile matter is distilled successively, oil wash and fractionation, obtain light constituent and heavy constituent; S3, described heavy constituent is carried out hydrotreatment, reaction product carries out thermal high separation again, thermal low is separated, cold anticyclone is separated, cold low is separated, obtain alkene and hydrogenated products.Not only can produce that the products such as synthetic gas, gasoline, diesel oil clean, the high-quality oil product of stable performance, the degree that becomes more meticulous is high; And make full use of heavy constituent, and without the need to rectification process, production energy consumption.
Accompanying drawing explanation
In order to make content of the present invention be more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the schema of the working method of a kind of low-temperature pyrolysis of coal volatile matter described in the embodiment of the present invention.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, embodiments of the present invention are described in further detail.
The present invention can implement in many different forms, and should not be understood to be limited to embodiment set forth herein.On the contrary, provide these embodiments, make the disclosure to be thorough and complete, and design of the present invention fully will be conveyed to those skilled in the art, the present invention will only be limited by claim.
Embodiment 1
The present embodiment provides a kind of working method of low-temperature pyrolysis of coal volatile matter, as shown in Figure 1, comprises the following steps:
S1, dust removal process is carried out to volatile matter.
The low temperature pyrogenation volatile matter of coal, without the need to carrying out cooling process, is generally 500 DEG C ~ 600 DEG C, directly carries out dust removal step.Dust removal step is comprised at least one of being assembled in dedusting, electrostatic precipitation by the dedusting of particle fixed bed, cyclone dust removal, micro swirl and carries out dedusting; After dust removal step, the particle diameter of the residual dust in volatile matter is less than 5 μm.
As one embodiment of the present of invention, in the present embodiment, dust removal step comprise carry out successively cyclone dust removal step, particle fixed bed dust removal step, micro swirl assemble dust removal step, electrostatic precipitation step; Wherein, micro swirl is assembled in dust removal step, and filler is porous spherical filler, is preferably seven apertures in the human head ball.
S2, volatile matter is distilled successively, oil wash and fractionation, obtain light constituent and heavy constituent.
As one embodiment of the present of invention, in the present embodiment, distilation steps comprises one-level underpressure distillation step and second depressurized distilation steps, is all implemented by vacuum flasher; Oil wash step comprises one-level oil wash step and secondary oil wash step, is all implemented by oil scrubber.Carry out one-level oil wash step after one-level underpressure distillation step, then carry out second depressurized distilation steps, fractionating step and secondary oil wash step successively.That is: the volatile matter after dedusting is introduced into one-level vacuum flasher, and the component that its flash overhead fractionates out directly imports one-level oil scrubber without cooling, and a branch returns in tower through condensation as washing oil, and component at the bottom of tower enters second depressurized flashing tower; The overhead components mixing of one-level oil wash column overhead light constituent remainder and second depressurized flashing tower, directly enters atmospheric fractional tower without heat exchange and carries out fractionating step.Side line output alkene, gasoline and the diesel oil successively of separation column.The overhead components of separation column enters secondary oil scrubber, and the tower top of secondary oil scrubber separates and comprises H
2, CO, CH
4, H
2the synthetic gas of the gases such as S, separates lightweight oil component at the bottom of tower.
As one embodiment of the present of invention, the temperature of one-level underpressure distillation step and second depressurized distilation steps is 450 DEG C, and pressure is 0.05MPa.
As one embodiment of the present of invention, the temperature of one-level oil wash step and secondary oil wash step is 300 DEG C, and pressure is 1.0MPa.
S3, heavy constituent is carried out hydrotreatment, then carry out thermal high separation, thermal low is separated, cold anticyclone is separated, cold low is separated, and obtains hydrogen, alkene and hydrogenated products.
As one embodiment of the present of invention, hydrogenation step is undertaken by boiling bed hydrogenation reactor, and the reaction conditions of hydrogenation step is: temperature of reaction 450 DEG C, pressure 15Mpa, hydrogen to oil volume ratio 1000:1, volume space velocity 1.2/h
-1.Adopt boiling bed hydrogenation reactor, effectively delayed the work-ing life of catalyzer, further saved production cost.
Reaction product after hydrogenation is directed into thermal high knockout tower and carries out thermal high gas-liquid separation, after Pyatyi heat exchange, overhead components enters cold anticyclone knockout tower and carries out cold anticyclone separation, and component at the bottom of tower enters thermal low knockout tower and carries out thermal low separation.The overhead components of thermal low knockout tower is the hydrogenated products of output, and component at the bottom of tower enters one-level vacuum flasher and is again separated.The tower top output hydrogen of cold anticyclone knockout tower, component at the bottom of tower enters cold low knockout tower and carries out cold low separation.Cold low knockout tower tower top separates alkene, and component at the bottom of tower imports secondary washing oil tower as washing oil.
As one embodiment of the present of invention, in the present embodiment, thermal high separating step service temperature is 450 DEG C, working pressure is 20Mpa; Thermal low separating step service temperature is 450 DEG C, working pressure is 2.0Mpa; Cold anticyclone separating step service temperature is 60 DEG C, working pressure is 20Mpa; Cold low separating step service temperature is 60 DEG C, working pressure is 3.0Mpa.
Preferably, heavy constituent also comprises the step removed the gred to heavy constituent before carrying out hydrotreatment.That is, at the bottom of the tower of one-level vacuum flasher and second depressurized flashing tower, component---heavy constituent all imports to dashpot, filters in dashpot, removing lime-ash, then enters boiling bed hydrogenation reactor.
Embodiment 2
The present embodiment provides a kind of working method of low-temperature pyrolysis of coal volatile matter, comprises the following steps:
S1, dust removal process is carried out to volatile matter.
The low temperature pyrogenation volatile matter of coal, without the need to carrying out cooling process, is generally 500 DEG C ~ 600 DEG C, directly carries out dust removal step.Dust removal step is comprised at least one of being assembled in dedusting, electrostatic precipitation by the dedusting of particle fixed bed, cyclone dust removal, micro swirl and carries out dedusting; After dust removal step, the particle diameter of the residual dust in volatile matter is less than 5 μm.
As one embodiment of the present of invention, in the present embodiment, dust removal step comprises the particle fixed bed dust removal step and electrostatic precipitation step of carrying out successively.
S2, volatile matter is distilled successively, oil wash and fractionation, obtain light constituent and heavy constituent.
As one embodiment of the present of invention, in the present embodiment, distilation steps comprises one-level underpressure distillation step and second depressurized distilation steps, is all implemented by vacuum flasher; Oil wash step comprises one-level oil wash step and secondary oil wash step, is all implemented by oil scrubber.Carry out one-level oil wash step after one-level underpressure distillation step, then carry out second depressurized distilation steps, fractionating step and secondary oil wash step successively.That is: the volatile matter after dedusting is introduced into one-level vacuum flasher, and the component that its flash overhead fractionates out directly imports one-level oil scrubber without cooling, and a branch returns in tower through condensation as washing oil, and component at the bottom of tower enters second depressurized flashing tower; The overhead components mixing of one-level oil wash column overhead light constituent remainder and second depressurized flashing tower, directly enters atmospheric fractional tower without heat exchange and carries out fractionating step.Side line output alkene, gasoline and the diesel oil successively of separation column.The overhead components of separation column enters secondary oil scrubber, and the tower top of secondary oil scrubber separates and comprises H
2, CO, CH
4, H
2the synthetic gas of the gases such as S, separates lightweight oil component at the bottom of tower.
As one embodiment of the present of invention, the temperature of one-level underpressure distillation step and second depressurized distilation steps is 300 DEG C, and pressure is 0.010MPa.
As one embodiment of the present of invention, the temperature of one-level oil wash step and secondary oil wash step is 200 DEG C, and pressure is 0.1MPa.
S3, heavy constituent is carried out hydrotreatment, then carry out thermal high separation, thermal low is separated, cold anticyclone is separated, cold low is separated, and obtains hydrogen, alkene and hydrogenated products.
As one embodiment of the present of invention, hydrogenation step is undertaken by boiling bed hydrogenation reactor, and the reaction conditions of hydrogenation step is: temperature of reaction 300 DEG C, pressure 12Mpa, hydrogen to oil volume ratio 400:1, volume space velocity 0.1/h
-1.
Reaction product after hydrogenation is directed into thermal high knockout tower and carries out thermal high gas-liquid separation, after Pyatyi heat exchange, overhead components enters cold anticyclone knockout tower and carries out cold anticyclone separation, and component at the bottom of tower enters thermal low knockout tower and carries out thermal low separation.The overhead components of thermal low knockout tower is the hydrogenated products of output, and component at the bottom of tower enters one-level vacuum flasher and is again separated.The tower top output hydrogen of cold anticyclone knockout tower, component at the bottom of tower enters cold low knockout tower and carries out cold low separation.Cold low knockout tower tower top separates alkene, and component at the bottom of tower imports secondary washing oil tower as washing oil.
As one embodiment of the present of invention, in the present embodiment, thermal high separating step service temperature is 300 DEG C, working pressure is 10Mpa; Thermal low separating step service temperature is 300 DEG C, working pressure is 1.0Mpa; Cold anticyclone separating step service temperature is 10 DEG C, working pressure is 10Mpa; Cold low separating step service temperature is 10 DEG C, working pressure is 1.0Mpa.
Embodiment 3
The present embodiment provides a kind of working method of low-temperature pyrolysis of coal volatile matter, comprises the following steps:
S1, dust removal process is carried out to volatile matter.
The low temperature pyrogenation volatile matter of coal, without the need to carrying out cooling process, is generally 500 DEG C ~ 600 DEG C, directly carries out dust removal step.Dust removal step is comprised at least one of being assembled in dedusting, electrostatic precipitation by the dedusting of particle fixed bed, cyclone dust removal, micro swirl and carries out dedusting; After dust removal step, the particle diameter of the residual dust in volatile matter is less than 5 μm.
As one embodiment of the present of invention, in the present embodiment, dust removal step comprise carry out successively cyclone dust removal step, particle fixed bed dust removal step, micro swirl assemble dust removal step, electrostatic precipitation step; Wherein, micro swirl is assembled in dust removal step, and filler is porous spherical filler, is preferably seven apertures in the human head ball.
S2, volatile matter is distilled successively, oil wash and fractionation, obtain light constituent and heavy constituent.
As one embodiment of the present of invention, in the present embodiment, distilation steps comprises one-level underpressure distillation step and second depressurized distilation steps, is all implemented by vacuum flasher; Oil wash step comprises one-level oil wash step and secondary oil wash step, is all implemented by oil scrubber.Carry out one-level oil wash step after one-level underpressure distillation step, then carry out second depressurized distilation steps, fractionating step and secondary oil wash step successively.That is: the volatile matter after dedusting is introduced into one-level vacuum flasher, and the component that its flash overhead fractionates out directly imports one-level oil scrubber without cooling, and a branch returns in tower through condensation as washing oil, and component at the bottom of tower enters second depressurized flashing tower; The overhead components mixing of one-level oil wash column overhead light constituent remainder and second depressurized flashing tower, directly enters atmospheric fractional tower without heat exchange and carries out fractionating step.Side line output alkene, gasoline and the diesel oil successively of separation column.The overhead components of separation column enters secondary oil scrubber, and the tower top of secondary oil scrubber separates and comprises H
2, CO, CH
4, H
2the synthetic gas of the gases such as S, separates lightweight oil component at the bottom of tower.
As one embodiment of the present of invention, the temperature of one-level underpressure distillation step and second depressurized distilation steps is 550 DEG C, and pressure is 0.099MPa.
As one embodiment of the present of invention, the temperature of one-level oil wash step and secondary oil wash step is 550 DEG C, and pressure is 2.0MPa.
S3, heavy constituent is carried out hydrotreatment, then carry out thermal high separation, thermal low is separated, cold anticyclone is separated, cold low is separated, and obtains hydrogen, alkene and hydrogenated products.
As one embodiment of the present of invention, hydrogenation step is undertaken by boiling bed hydrogenation reactor, and the reaction conditions of hydrogenation step is: temperature of reaction 550 DEG C, pressure 17Mpa, hydrogen to oil volume ratio 2000:1, volume space velocity 2.0/h
-1.
Reaction product after hydrogenation is directed into thermal high knockout tower and carries out thermal high gas-liquid separation, after Pyatyi heat exchange, overhead components enters cold anticyclone knockout tower and carries out cold anticyclone separation, and component at the bottom of tower enters thermal low knockout tower and carries out thermal low separation.The overhead components of thermal low knockout tower is the hydrogenated products of output, and component at the bottom of tower enters one-level vacuum flasher and is again separated.The tower top output hydrogen of cold anticyclone knockout tower, component at the bottom of tower enters cold low knockout tower and carries out cold low separation.Cold low knockout tower tower top separates alkene, and component at the bottom of tower imports secondary washing oil tower as washing oil.
As one embodiment of the present of invention, in the present embodiment, thermal high separating step service temperature is 550 DEG C, working pressure is 30Mpa; Thermal low separating step service temperature is 550 DEG C, working pressure is 5.0Mpa; Cold anticyclone separating step service temperature is 100 DEG C, working pressure is 30Mpa; Cold low separating step service temperature is 100 DEG C, working pressure is 5.0Mpa.
Preferably, heavy constituent also comprises the step removed the gred to heavy constituent before carrying out hydrotreatment.That is, component at the bottom of the tower of one-level vacuum flasher and second depressurized flashing tower, namely heavy constituent all imports to dashpot, filters in dashpot, removing lime-ash, then enters boiling bed hydrogenation reactor.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among protection scope of the present invention.
Claims (10)
1. a working method for low-temperature pyrolysis of coal volatile matter, is characterized in that, comprises the following steps:
S1, dust removal process is carried out to described volatile matter;
S2, described volatile matter is distilled successively, oil wash and fractionation, obtain light constituent and heavy constituent;
S3, described heavy constituent is carried out hydrotreatment, reaction product carries out thermal high separation again, thermal low is separated, cold anticyclone is separated, cold low is separated, obtain alkene and hydrogenated products.
2. the working method of low-temperature pyrolysis of coal volatile matter according to claim 1, is characterized in that, in described step S2, described distilation steps comprises one-level underpressure distillation step and second depressurized distilation steps; Described oil wash step comprises one-level oil wash step and secondary oil wash step; Carry out described one-level oil wash step after described one-level underpressure distillation step, then carry out described second depressurized distilation steps, fractionating step and described secondary oil wash step successively; Described fractionating step is output alkene, gasoline and diesel oil successively; Described secondary oil wash step output synthetic gas.
3. the working method of low-temperature pyrolysis of coal volatile matter according to claim 2, is characterized in that, the temperature of described one-level underpressure distillation step and described second depressurized distilation steps is 300 DEG C ~ 550 DEG C, and pressure is 0.010MPa ~ 0.099MPa.
4. the working method of low-temperature pyrolysis of coal volatile matter according to claim 2, is characterized in that, the temperature of described one-level oil wash step and described secondary oil wash step is 200 DEG C ~ 550 DEG C, and pressure is 0.1MPa ~ 2.0MPa.
5. the working method of the low-temperature pyrolysis of coal volatile matter according to any one of claim 1-4, it is characterized in that, in described step S3, the reaction conditions of described hydrogenation step is: temperature of reaction 300 DEG C ~ 550 DEG C, pressure 12Mpa ~ 17Mpa, hydrogen to oil volume ratio 400:1 ~ 2000:1, volume space velocity 0.1/h
-1~ 2.0/h
-1.
6. the working method of the low-temperature pyrolysis of coal volatile matter according to any one of claim 1-5, is characterized in that, in described step S3, described thermal high separating step service temperature is 300 DEG C ~ 550 DEG C, working pressure is 10Mpa ~ 30Mpa; Described thermal low separating step service temperature is 300 DEG C ~ 550 DEG C, working pressure is 1.0Mpa ~ 5.0Mpa; Described cold anticyclone separating step service temperature is 10 DEG C ~ 100 DEG C, working pressure is 10Mpa ~ 30Mpa; Described cold low separating step service temperature is 10 DEG C ~ 100 DEG C, working pressure is 1.0Mpa ~ 5.0Mpa.
7. the working method of the low-temperature pyrolysis of coal volatile matter according to any one of claim 1-6, it is characterized in that, in described step S1, described dust removal step is comprised at least one of being assembled in dedusting, electrostatic precipitation by the dedusting of particle fixed bed, cyclone dust removal, micro swirl and carries out dedusting; After described dust removal step, the particle diameter of the residual dust in described volatile matter is less than 5 μm.
8. the working method of low-temperature pyrolysis of coal volatile matter according to claim 7, it is characterized in that, in described step S1, described dust removal step comprise carry out successively cyclone dust removal step, particle fixed bed dust removal step, micro swirl assemble dust removal step, electrostatic precipitation step; Wherein, described micro swirl is assembled in dust removal step, and filler is porous spherical filler.
9. the working method of the low-temperature pyrolysis of coal volatile matter according to any one of claim 1-8, is characterized in that, in described step S3, described heavy constituent also comprises the step removed the gred to described heavy constituent before carrying out hydrotreatment.
10. the working method of the low-temperature pyrolysis of coal volatile matter according to any one of claim 1-9, is characterized in that, in described step S3, described hydrogenation step is undertaken by boiling bed hydrogenation reactor.
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