CN113025364A - System and method for treating direct coal liquefaction residues - Google Patents
System and method for treating direct coal liquefaction residues Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 61
- 239000000203 mixture Substances 0.000 claims abstract description 101
- 239000007788 liquid Substances 0.000 claims abstract description 92
- 238000000197 pyrolysis Methods 0.000 claims abstract description 76
- 238000000605 extraction Methods 0.000 claims abstract description 55
- 238000002309 gasification Methods 0.000 claims abstract description 52
- 238000000926 separation method Methods 0.000 claims abstract description 39
- 239000012265 solid product Substances 0.000 claims abstract description 37
- 238000000227 grinding Methods 0.000 claims abstract description 36
- 238000012545 processing Methods 0.000 claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims description 51
- 239000002245 particle Substances 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 23
- 239000011269 tar Substances 0.000 claims description 21
- 238000003801 milling Methods 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
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- 238000003786 synthesis reaction Methods 0.000 abstract description 21
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- 239000003034 coal gas Substances 0.000 description 15
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- 238000000746 purification Methods 0.000 description 10
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- 238000006243 chemical reaction Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
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- 238000011143 downstream manufacturing Methods 0.000 description 4
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
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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
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/46—Gasification of granular or pulverulent flues in suspension
- C10J3/48—Apparatus; Plants
- C10J3/485—Entrained flow gasifiers
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- Chemical & Material Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a coal direct liquefaction residue treatment process, in particular to a system and a method for treating coal direct liquefaction residue. The system comprises: the co-pyrolysis unit is used for directly liquefying the mixture of the residue and the raw coal by pyrolyzing the coal to obtain a co-pyrolysis solid product; the extraction unit is used for extracting the co-pyrolysis solid product to obtain an extraction liquid and a solid-liquid mixture; the solid-liquid separation unit is used for carrying out solid-liquid separation on the solid-liquid mixture to obtain raffinate; the grinding unit is used for drying and grinding the raffinate and the raw coal to obtain a first powdery mixture; and the gasification unit is used for gasifying the first powdery mixture. The system and the method not only realize the deep processing treatment of the direct coal liquefaction residues, but also can obtain more oil products and synthesis gas products with high added values through the processes of co-pyrolysis, extraction, grinding and gasification, so that the direct coal liquefaction residues are fully recycled and utilized.
Description
Technical Field
The invention relates to a coal direct liquefaction residue treatment process, in particular to a system and a method for treating coal direct liquefaction residue.
Background
Coal is directly liquefied, one of the coal liquefaction methods is a process of converting coal into liquid fuel through hydrocracking under the action of hydrogen and a catalyst. Besides obtaining the required liquefied product in the direct coal liquefaction process, some hydrocarbon molecules and CO can be generatedxGas, process water and liquefaction residues (also called coal direct liquefaction residues) generated in the solid-liquid separation process.
The direct coal liquefaction residue is solid hazardous waste and mainly contains inorganic substances and organic substances, wherein the organic substances comprise liquefied heavy oil, asphalt substances and unconverted coal, and the inorganic substances comprise mineral substances in the coal and an additional catalyst.
How to reasonably and efficiently utilize the direct coal liquefaction residues is a difficult problem which needs to be solved urgently by a coal liquefaction process. There are many methods for treating coal direct liquefaction residues as reported in the following prior art.
CN103923703B discloses a method for producing crude synthesis gas by using coal direct liquefaction residue as raw material. The method comprises the following steps: s1, preparing coal water slurry from the direct coal liquefaction residues; and S2, mixing the coal water slurry with oxygen to carry out gasification reaction to obtain crude synthesis gas. The method realizes the full and efficient utilization of the direct coal liquefaction residues, converts the sulfur with higher content in the direct coal liquefaction residues into H2S in the gasification process and carries out recovery treatment in the subsequent crude synthesis gas purification process, so that the efficient utilization process has no pollution to the environment, the added value of products is high, the treatment process is simple, and no adverse effect is caused to the equipment operation; meanwhile, because the heat value of the direct coal liquefaction residue is high, and the Fe-based catalyst which is required by coal liquefaction and is enriched in the direct coal liquefaction residue has a catalytic effect on the coal gasification process, the content of effective gas components in the finally obtained crude synthesis gas is high. However, in the method, coal liquefaction residues, the quenching and tempering oil and raw coal are respectively adopted to prepare coal water slurry for gasification to prepare synthesis gas, and the liquefied residue oil product is not effectively recovered.
CN103695057B discloses a method for preparing coal water slurry by using coal direct liquefaction residues, the coal water slurry and a gasification method thereof. The method for preparing the coal water slurry by using the direct coal liquefaction residues comprises the following steps: s1, extracting the direct coal liquefaction residues, carrying out solid-liquid separation, and drying to obtain an extract residue; and S2, crushing and grinding the raffinate, adding water and an optional surfactant into the raffinate, and stirring to obtain the coal water slurry. After the coal direct liquefaction residue is extracted, heavy oil and asphalt substances in the coal direct liquefaction residue can be separated from unconverted coal and ash, and the unconverted coal and the ash are collectively called raffinate. The coal water slurry can be formed after crushing and grinding the raffinate and adding water and optional surfactant. The coal water slurry can be used as common fuel and can be used in gasification production. Therefore, the raffinate of the direct coal liquefaction residue is effectively utilized, and the utilization rate and the added value of the direct coal liquefaction residue are improved. However, the method adopts extracting agents such as tetrahydrofuran, direct coal liquefaction oil and the like at the temperature of between 0.1 and 1.0MPa and between 80 and 280 ℃ and H2Or N2Heavy oil and asphaltene substances in the extracted coal direct liquefaction residue are possibly incompletely extracted under the environment, so that the subsequent raffinate has high cohesiveness; in addition, the content of sulfur and nitrogen in the liquefaction residue is also high.
However, the above methods have a problem that the direct coal liquefaction residue is not sufficiently utilized, and therefore, a method for efficiently treating the direct coal liquefaction residue is demanded.
Disclosure of Invention
One of the purposes of the invention is to overcome the problem of insufficient utilization of the direct coal liquefaction residue in the prior art;
one of the purposes of the invention is to provide a method for treating coal direct liquefaction residues to obtain oil products and synthesis gas products with more high added values.
In order to achieve the above object, a first aspect of the present invention provides a processing system for processing a coal direct liquefaction residue, comprising:
the co-pyrolysis unit is used for directly liquefying the mixture of the residue and the raw coal by pyrolyzing the coal to obtain a co-pyrolysis solid product;
the extraction unit is used for extracting the co-pyrolysis solid product to obtain an extraction liquid and a solid-liquid mixture;
the solid-liquid separation unit is used for carrying out solid-liquid separation on the solid-liquid mixture to obtain raffinate;
the grinding unit is used for drying and grinding the raffinate and the raw coal to obtain a first powdery mixture;
and the gasification unit is used for gasifying the first powdery mixture.
In a second aspect, the present invention provides a method for treating a coal direct liquefaction residue, the method comprising:
(1) co-pyrolyzing the mixture of the direct coal liquefaction residues and the raw coal to obtain a co-pyrolysis solid product;
(2) extracting the co-pyrolysis solid product by using an extracting agent to obtain an extract and a solid-liquid mixture;
(3) carrying out solid-liquid separation on the solid-liquid mixture to obtain an extract;
(4) mixing the extraction residues and the raw coal in proportion, drying and grinding to obtain a first powdery mixture;
(5) gasifying the first powdery mixture.
In a third aspect, the present invention provides a method for treating a coal direct liquefaction residue using the system of the first aspect of the present invention, comprising:
(I) co-pyrolyzing the mixture of the direct coal liquefaction residues and the raw coal in a co-pyrolysis unit to obtain a co-pyrolysis solid product;
(II) extracting the co-pyrolysis solid product in an extraction unit by using an extracting agent to obtain an extraction liquid and a solid-liquid mixture;
(III) carrying out solid-liquid separation on the solid-liquid mixture in a solid-liquid separation unit to obtain raffinate;
(IV) drying and grinding the raffinate and the raw coal in a grinding unit according to a certain proportion to obtain a first powdery mixture;
(V) gasifying the first powdered mixture in a gasification unit;
preferably, the first pulverized mixture is gasified in a dry pulverized coal entrained flow gasifier.
The system and the method not only realize the deep processing treatment of the direct coal liquefaction residues, but also can obtain more oil products and synthesis gas products with high added values through the processes of pyrolysis, extraction, grinding and gasification, so that the direct coal liquefaction residues are fully recycled and utilized. In addition, the method of firstly pyrolyzing and then extracting is adopted to improve the yield of pyrolysis oil gas, thereby improving the economy of the whole process.
Drawings
FIG. 1 is a schematic diagram of one embodiment of a system for treating direct coal liquefaction residues according to the present invention.
Description of the reference numerals
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| 7 | Raw coal crushing and |
8 | Oil |
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12 | Ash treatment unit |
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a system for treating coal direct liquefaction residues, which comprises:
the co-pyrolysis unit is used for directly liquefying the mixture of the residue and the raw coal by pyrolyzing the coal to obtain a co-pyrolysis solid product;
the extraction unit is used for extracting the co-pyrolysis solid product to obtain an extraction liquid and a solid-liquid mixture;
the solid-liquid separation unit is used for carrying out solid-liquid separation on the solid-liquid mixture to obtain raffinate;
the grinding unit is used for drying and grinding the raffinate and the raw coal to obtain a first powdery mixture;
and the gasification unit is used for gasifying the first powdery mixture.
According to the invention, in the co-pyrolysis unit, the mixture of the coal direct liquefaction residue and the raw coal is co-pyrolyzed to produce co-pyrolysis solid products, tar and coal gas.
Preferably, a co-pyrolysis solid product outlet of the co-pyrolysis unit is communicated with an inlet of an extraction unit, an outlet of the extraction unit is communicated with an inlet of the solid-liquid separation unit, and a raffinate outlet of the solid-liquid separation unit is communicated with an inlet of the grinding unit.
According to the invention, the co-pyrolysis solid product obtained by the co-pyrolysis unit is extracted in the extraction unit to obtain the upper clear extraction liquid and the lower solid-liquid mixture. The solid-liquid mixture is a mixture of solid residues and a small amount of liquid.
According to the invention, the solid-liquid mixture is subjected to solid-liquid separation in a solid-liquid separation unit to obtain raffinate and a small amount of filtrate.
According to the invention, the raffinate and the raw coal are dried and milled in a milling unit to obtain a first powdery mixture. Preferably, in the milling unit, an air blowing device is provided for blowing air to the milling system during milling.
Preferably, the system further comprises a raw coal crushing and drying unit for crushing and drying the raw coal. More preferably, the outlet of the raw coal crushing and drying unit is respectively communicated with the inlet of the co-pyrolysis unit and the inlet of the pulverizing unit.
Preferably, the system further comprises a conveying unit for conveying the first powdered mixture into the gasification unit, more preferably, the conveying unit is in communication with the outlet of the milling unit and the inlet of the gasification unit.
According to the invention, in the gasification unit, the first pulverulent mixture is subjected to a gasification reaction to produce synthesis gas and, at the same time, ash.
Preferably, the gasification unit is a dry coal powder entrained flow gasifier. Preferably, the first powdery mixture contains particles having a particle diameter of 90 μm or more in a volume content of not more than 10%. In this context, the particle volume content is determined by a laser particle size analyzer sampling test.
Preferably, the gasifier lining of the gasification unit is a waterwall, refractory brick or a mixture of both, preferably a waterwall.
Preferably, the system further comprises a synthesis gas purification unit for receiving the coal gas produced by the co-pyrolysis unit and/or the synthesis gas produced by the gasification unit for further purification treatment.
Preferably, the system further comprises an oil deep processing unit for receiving the tar produced by the co-pyrolysis unit, the extract liquor produced by the extraction unit and the filtrate produced by the solid-liquid separation unit for deep processing treatment.
Preferably, the system further comprises an ash handling unit for handling ash produced by the gasification unit.
Preferably, the system further comprises a tar recovery unit to collect tar produced by the co-pyrolysis unit and a gas recovery unit to collect gas produced by the co-pyrolysis unit.
In a second aspect, the present invention provides a method for treating a coal direct liquefaction residue, the method comprising:
(1) co-pyrolyzing the mixture of the direct coal liquefaction residues and the raw coal to obtain a co-pyrolysis solid product;
(2) extracting the co-pyrolysis solid product by using an extracting agent to obtain an extraction liquid and a solid-liquid mixture;
(3) carrying out solid-liquid separation on the solid-liquid mixture to obtain an extract;
(4) mixing the extraction residues and the raw coal in proportion and grinding the mixture into powder to obtain a first powdery mixture;
(5) gasifying the first powdery mixture.
According to the method of the invention, preferably, in the step (1), the mass ratio of the coal direct liquefaction residue to the raw coal is 1 (1-100), preferably 1: (3-20).
Preferably, the conditions of the co-pyrolysis include: the temperature is 200 ℃ to 600 ℃, preferably 450 ℃ to 550 ℃.
The mixture of the direct coal liquefaction residues and the raw coal is subjected to co-pyrolysis to generate co-pyrolysis solid products, tar and coal gas. Preferably, the tar is subjected to an oil-further-processing treatment, such as introducing the tar into an oil-further-processing unit for further processing into a finished oil; the coal gas is introduced into a syngas purification unit to enhance syngas quality and yield.
According to the method of the present invention, in step (2), the co-pyrolysis solid product is extracted using an extractant; preferably, the extractant is selected from at least one of coal tar, coal direct liquefaction oil and tetrahydrofuran. Preferably, the mass ratio of the extractant to the solid product after pyrolysis is (3-15):1, preferably (5-10): 1.
Preferably, the conditions of the extraction include: the temperature is 150 ℃ to 300 ℃, preferably 200 ℃ to 280 ℃. The pressure of the extraction can be selected according to the actual circumstances, for example, atmospheric pressure.
Extracting to obtain an upper clear extraction liquid and a lower solid-liquid mixture.
In the step (3), the solid-liquid mixture is subjected to solid-liquid separation to obtain raffinate and filtrate.
And (3) drying and grinding the obtained raffinate and the raw coal according to a certain ratio, preferably, in the step (4), when grinding is carried out, the mass ratio of the raffinate to the raw coal is 1 (0.1-100), preferably 1: (1-20).
In one embodiment, the milling is performed in a mill, more preferably the mill is a roller disc mill.
In order to obtain a powder having a small particle size suitable for gasification of dry pulverized coal, it is preferable to blow hot air during the pulverization. More preferably, the hot air is nitrogen, flue gas, or a mixed gas of air and nitrogen, wherein the oxygen content is less than 8 vol%.
In order to further obtain powder with smaller particle size, preferably, the inlet temperature of the hot air is 140-300 ℃, and the outlet temperature of the hot air is 35-100 ℃; more preferably, the hot air inlet temperature is 150-200 ℃ and the hot air outlet temperature is 35-60 ℃.
Preferably, the amount of inlet hot air required per 1kg of throughput is 0.5-5Nm3Preferably 1-3Nm3. Here, the throughput is the weight of the mixture of the raffinate and the raw coal.
Preferably, the pressure difference between the hot air inlet and the hot air outlet is not more than 2000 Pa.
Preferably, the total water content of the first powdery mixture obtained by milling is 2 to 4%, and preferably, the volume content of particles having a particle size of 90 μm or more in the first powdery mixture is not more than 10%.
Preferably, in step (5), the gasification is carried out in a dry coal powder entrained flow gasifier.
Preferably, the conditions of the gasification include: the pressure is 0.1-10MPa, and the temperature is 1000-1600 ℃.
Preferably, the synthesis gas generated by gasification enters a downstream process after being purified, and the ash generated by gasification can be used for building material processing after being treated by ash.
According to the invention, preferably, the method further comprises drying and crushing the raw coal; preferably, the drying conditions include: the temperature is 100-150 ℃, preferably 100-120 ℃. Preferably, the raw coal is crushed to a particle size of 20mm or less, preferably 10mm or less.
Preferably, after crushing and drying, a part of raw coal and the direct coal liquefaction residue are mixed in proportion for co-pyrolysis, and the other part of raw coal and the raffinate are mixed in proportion for grinding.
According to the present invention, preferably, the method further comprises subjecting the tar produced in the co-pyrolysis process, the extract liquor produced in the extraction process, and the filtrate produced in the solid-liquid separation process to oil deep processing treatment, for example, oil deep processing treatment in an oil deep processing unit, to obtain a product oil. Wherein, the extracting agent removed from the extracting solution and the filtrate can be recycled for the extracting process.
In a third aspect, the present invention provides a method for treating coal direct liquefaction residues by using the system of the first aspect of the present invention, comprising:
(I) co-pyrolyzing the mixture of the direct coal liquefaction residues and the raw coal in a co-pyrolysis unit to obtain a co-pyrolysis solid product;
(II) extracting the co-pyrolysis solid product in an extraction unit by using an extracting agent to obtain an extraction liquid and a solid-liquid mixture;
(III) carrying out solid-liquid separation on the solid-liquid mixture in a solid-liquid separation unit to obtain raffinate;
(IV) drying and grinding the raffinate and the raw coal in a grinding unit according to a certain proportion to obtain a first powdery mixture;
(V) gasifying the first powdered mixture in a gasification unit;
preferably, the first pulverized mixture is gasified in a dry pulverized coal entrained flow gasifier.
Preferably, in the step (IV), the mass ratio of the raffinate to the raw coal is 1 (0.1-100), preferably 1: (1-20).
Preferably, hot air is blown in during the milling process. More preferably, the hot air is nitrogen, flue gas, or a mixed gas of air and nitrogen, wherein the oxygen content is less than 8 vol%.
Preferably, the inlet temperature of the hot air is 140-300 ℃, and the outlet temperature of the hot air is 35-100 ℃; more preferably, the hot air inlet temperature is 150-200 ℃ and the hot air outlet temperature is 35-60 ℃.
Preferably, the amount of inlet hot air required per 1kg of throughput is 0.5-5Nm3Preferably 1-3Nm3. Here, the throughput is the weight of the mixture of the raffinate and the raw coal.
Preferably, the pressure difference between the hot air inlet and the hot air outlet is not more than 2000 Pa.
The first pulverulent mixture obtained after milling preferably has a total water content of from 2 to 4%.
Preferably, the first powdery mixture contains particles having a particle diameter of 90 μm or more in a volume content of not more than 10%.
Preferably, in step (V), the gasification unit is a dry coal powder entrained flow gasifier.
Preferably, the conditions of the gasification include: the pressure is 0.1-10MPa, and the temperature is 1000-1600 ℃.
Preferably, the synthesis gas generated by gasification is introduced into a synthesis gas purification unit for synthesis gas purification treatment and then enters a downstream process, and the ash generated by gasification is introduced into an ash treatment unit for ash treatment and then is used for building material processing.
According to the invention, preferably, the method further comprises introducing the tar produced by the co-pyrolysis unit, the extract liquor produced by the extraction unit and the filtrate produced by the solid-liquid separation unit into an oil deep processing unit for oil deep processing treatment to obtain the finished oil. Wherein the extracting agent removed from the extract and the filtrate can be recycled to the extraction unit for the extraction process.
The specific definitions of the steps of the process according to the second aspect of the invention apply equally to the process according to the third aspect of the invention, and are not to be considered superfluous here.
Fig. 1 shows a schematic diagram of an embodiment of the system according to the present invention, which comprises:
the system comprises a co-pyrolysis unit 1, an extraction unit 2, a solid-liquid separation unit 3, a grinding unit 4, a gasification unit 5, a conveying unit 6, a raw coal crushing and drying unit 7, an oil deep processing unit 8, a synthetic gas purification unit 9, a tar recovery unit 10, a coal gas recovery unit 11 and an ash treatment unit 12. The method for treating the direct coal liquefaction residue by using the system comprises the following steps:
(a) introducing a mixture of the direct pyrolysis coal liquefaction residue and raw coal into a co-pyrolysis unit 1 for co-pyrolysis to generate co-pyrolysis solid products, tar and coal gas, wherein the generated tar is collected by a tar recovery unit 10 and further introduced into an oil deep-processing unit 8 to produce finished oil, and the generated coal gas is collected by a coal gas recovery unit 11 and further introduced into a synthesis gas purification unit 9 for further treatment for a downstream process;
(b) introducing the co-pyrolysis solid product into an extraction unit 2, and extracting by using an extracting agent, wherein the extracting agent is selected from at least one of coal tar, coal direct liquefaction oil and tetrahydrofuran; the mass ratio of the extracting agent to the pyrolyzed solid product is (3-15) to 1, and the extraction conditions comprise: the temperature is 150-;
(c) introducing the solid-liquid mixture into a solid-liquid separation unit 3 for solid-liquid separation to obtain raffinate and a small amount of filtrate, introducing the small amount of filtrate and extract into an oil deep processing unit 8 for further treatment to obtain finished oil, wherein an extracting agent removed in the oil deep processing unit 8 can be circularly used in an extraction unit 2;
(d) introducing the raffinate and the raw coal (the mass ratio of the raffinate to the raw coal is 1 (0.1-100)) into a grinding unit 4 for drying and grinding, wherein the conditions for drying and grinding comprise: blowing hot air in the milling process, wherein the hot air is preferably nitrogen, flue gas or mixed gas of air and nitrogen, and the content of oxygen is less than 8% by volume; preferably, the inlet temperature of the hot air is 140-300 ℃, and the outlet temperature of the hot air is 35-100 ℃; preferably, the amount of inlet hot air required per 1kg of throughput is 0.5-5Nm3(ii) a Preferably, the pressure difference between the hot air inlet and the hot air outlet is not more than 2000Pa, so as to obtain a first powdery mixture, wherein the total water content of the first powdery mixture is 2-4%, and the volume content of particles with the particle size of more than 90 mu m is not more than 10%.
(e) Introducing the first powdery mixture into a gasification unit 5 for gasification under the following conditions: the pressure is 0.1-10MPa, the temperature is 1000-1600 ℃, the generated synthesis gas is introduced into a synthesis gas purification unit 9 for treatment for downstream processes, and the generated ash is introduced into an ash treatment unit 12 for treatment and then used for building material processing.
Compared with the prior art, the method provided by the invention has the following beneficial technical effects:
(i) the molecular fracture of the raw coal and the direct coal liquefaction residues is more sufficient after high-temperature pyrolysis, so that the oil gas yield can be improved by the extraction process after pyrolysis, and the economy of the whole process is improved;
(ii) the raw coal and the direct coal liquefaction residues are subjected to co-pyrolysis, extraction and gasification, so that large-scale treatment of the direct coal liquefaction residues can be realized;
(iii) in the method, the adjustable proportion of the raw coal and the direct coal liquefaction residue is large, and the process flexibility is good;
(iii) after the co-pyrolysis and the extraction, solid particles become small, and the energy consumption of a milling system can be reduced.
The present invention will be described in detail below by way of examples.
Example 1
Mixing the coal direct liquefaction residue (50kg/h) and crushed and dried raw coal (50kg/h, particle size of 10mm) into a co-pyrolysis unit 1, co-pyrolyzing at 550 deg.C under normal pressure to produce tar (18kg/h), co-pyrolysis solid product, and coal gas (800 Nm/h)3H, wherein CO and H2Content 52% of the total volume of the gas).
In the extraction unit 2, the co-pyrolysis solid product and an extracting agent (tetrahydrofuran) are mixed according to the solid-liquid mass ratio of 1:5, and extraction is carried out under the conditions of normal pressure and 200 ℃ to obtain an extraction liquid and a solid-liquid mixture.
In the solid-liquid separation unit 3, the solid-liquid mixture was subjected to solid-liquid separation to obtain a raffinate (61.5kg/h) and a small amount of filtrate. The tar, the extract and the filtrate are introduced into an oil product deep processing unit 8 for processing to obtain finished oil (27.6 kg/h).
Mixing the raffinate and crushed and dried raw coal according to the mass ratio of 1:12, and feeding the mixture into a grinding unit 4, wherein the inlet temperature of hot air (mixed gas of air and nitrogen, wherein the volume content of oxygen is 5%) in the grinding unit is 180 ℃, and the outlet temperature is 50 ℃; the amount of inlet hot air required per 1kg of throughput was 2Nm3(ii) a The pressure difference between the hot air inlet and the hot air outlet is 1200Pa, and a first powdery mixture is obtained.
The first powdery mixture (with total water content of 1.7% and volume content of particles with particle size of more than 90 μm of 6%) is conveyed to a gasification unit 5 through a conveying unit 6 for dry pulverized coal gasification, and the gasification conditions comprise: the pressure was 4MPa and the temperature was 1400 ℃ yielding synthesis gas.
The content of effective gas in the obtained synthetic gas is 82 percent, the carbon conversion rate is 99 percent, the cold coal gas efficiency is 81 percent, and the specific oxygen consumption is 344kg/kNm3(CO+H2) Specific coal consumption of 576kg/kNm3(CO+H2)。
Example 2
Mixing the directly liquefied coal residue (50kg/h) with crushed and dried raw coal (200kg/h, particle size of 10mm)Feeding into a co-pyrolysis unit 1, co-pyrolyzing at 500 deg.C and normal pressure to produce tar (34.5kg/h), co-pyrolysis solid product and coal gas (3000 Nm)3H, wherein CO and H are contained in the gas2Content 54 vol% of the total gas).
In the extraction unit 2, the co-pyrolysis solid product and an extracting agent (tetrahydrofuran) are mixed according to the solid-liquid mass ratio of 1:6, and extraction is carried out under the conditions of normal pressure and 300 ℃ to obtain an extraction liquid and a solid-liquid mixture.
In the solid-liquid separation unit 3, the solid-liquid mixture was subjected to solid-liquid separation to obtain a raffinate (173.6kg/h) and a small amount of filtrate. The tar, the extract and the filtrate are introduced into an oil product deep processing unit 8 for processing to obtain the finished oil (48.2 kg/h).
Mixing the raffinate and crushed and dried raw coal according to the proportion of 1:4, and feeding the mixture into a grinding unit 4, wherein the inlet temperature of hot air (mixed gas of air and nitrogen, wherein the content of oxygen is 5 vol%) of the grinding unit is 190 ℃, and the outlet temperature is 60 ℃; the required inlet hot air volume per 1kg of throughput was 3Nm3(ii) a The pressure difference of the hot air inlet and the hot air outlet is 1400Pa, and a first powdery mixture is obtained.
The first powdery mixture (with total water content of 1.6% and volume content of particles with particle size of more than 90 μm of 6.6%) is conveyed to a gasification unit 5 through a conveying unit 6 for dry coal powder gasification, and the gasification conditions comprise: the pressure was 4MPa and the temperature was 1400 ℃ yielding synthesis gas.
The content of the effective gas of the obtained synthetic gas is 84 percent, the carbon conversion rate is 99 percent, the cold coal gas efficiency is 81.4 percent, and the specific oxygen consumption is 352kg/kNm3(CO+H2) Specific coal consumption is 554kg/kNm3(CO+H2)。
Example 3
Mixing the coal direct liquefaction residue (50kg/h) and crushed and dried raw coal (450kg/h, particle size of 10mm) into a co-pyrolysis unit 1, and co-pyrolyzing at 600 deg.C and normal pressure to produce tar (60kg/h), co-pyrolysis solid product, and coal gas (7600 Nm)3H, wherein CO and H2Content 56% of the total gas volume);
in the extraction unit 2, the co-pyrolysis solid product and an extracting agent (tetrahydrofuran) are mixed according to the solid-liquid mass ratio of 1:8, and extraction is carried out under the conditions of normal pressure and 250 ℃ to obtain an extraction liquid and a solid-liquid mixture.
In the solid-liquid separation unit 3, the solid-liquid mixture was subjected to solid-liquid separation to obtain a raffinate (296kg/h) and a small amount of filtrate. The tar, the extract and the filtrate are introduced into an oil product deep processing unit 8 for processing to obtain finished oil (164 kg/h).
Mixing the raffinate and crushed and dried raw coal according to the mass ratio of 1:2, and feeding the mixture into a grinding unit 4, wherein the inlet temperature of hot air (mixed gas of air and nitrogen, wherein the volume content of oxygen is 5%) in the grinding unit is 150 ℃, and the outlet temperature is 40 ℃; the required inlet hot air volume per 1kg of throughput was 3Nm3(ii) a The pressure difference between the hot air inlet and the hot air outlet is 1600Pa, and a first powdery mixture is obtained.
The first powdery mixture (with total water content of 1.8% and volume content of particles with particle size of more than 90 μm of 7.2%) is conveyed to a gasification unit 5 through a conveying unit 6 for dry coal powder gasification, and the gasification conditions comprise: the pressure was 4MPa and the temperature was 1400 ℃ yielding synthesis gas.
The content of effective gas in the obtained synthetic gas is 84 percent, the carbon conversion rate is 99 percent, the cold coal gas efficiency is 84 percent, and the specific oxygen consumption is 332kg/kNm3(CO+H2) Specific coal consumption is 588kg/kNm3(CO+H2)。
Example 4
Treating the coal direct liquefaction residue as described in example 1, except that the inlet temperature of hot air of the pulverizing unit was set to 110 ℃ and the outlet temperature was set to 40 ℃; the rest is the same as in example 1. The first powdery mixture finally obtained contained 28% by volume of particles having a particle diameter of 90 μm or more.
The content of the effective gas of the finally obtained synthetic gas is 76 percent, the carbon conversion rate is 97 percent, the cold coal gas efficiency is 76 percent, and the specific oxygen consumption is 364kg/kNm3(CO+H2) Specific coal consumption of 592kg/kNm3(CO+H2)。
Example 5
The direct coal liquefaction residue was treated in the same manner as in example 1, except that hot air was not blown during the pulverization in the pulverizing unit. The first powdery mixture finally obtained contained 100% by volume of particles having a particle diameter of 90 μm or more. Is not suitable for dry coal powder gasification.
Comparative example 1
Referring to the method described in example 1, except that the co-pyrolysis was not performed, the direct coal liquefaction residue was mixed with an extractant (tetrahydrofuran) at a solid-liquid mass ratio of 1:5 directly in the extraction unit 2, and extraction was performed under normal pressure at 280 ℃ to obtain an extract and a solid-liquid mixture. The rest is the same as in example 1.
18.5kg/h of finally obtained finished oil, 76kg/h of raffinate, 76 percent of effective gas content of gasified synthetic gas, 96 percent of carbon conversion rate, 78 percent of cold gas efficiency and 368kg/kNm of specific oxygen consumption3(CO+H2) Specific coal consumption of 596kg/kNm3(CO+H2)。
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (12)
1. A system for processing coal direct liquefaction residues, comprising:
the co-pyrolysis unit is used for directly liquefying the mixture of the residue and the raw coal by pyrolyzing the coal to obtain a co-pyrolysis solid product;
the extraction unit is used for extracting the co-pyrolysis solid product to obtain an extraction liquid and a solid-liquid mixture;
the solid-liquid separation unit is used for carrying out solid-liquid separation on the solid-liquid mixture to obtain raffinate;
the grinding unit is used for drying and grinding the raffinate and the raw coal to obtain a first powdery mixture;
and the gasification unit is used for gasifying the first powdery mixture.
2. The system of claim 1, wherein the co-pyrolysis solid product outlet of the co-pyrolysis unit is in communication with an inlet of an extraction unit, an outlet of the extraction unit is in communication with an inlet of the solid-liquid separation unit, and a raffinate outlet of the solid-liquid separation unit is in communication with an inlet of the milling unit.
3. The system according to claim 1 or 2, further comprising a raw coal crushing and drying unit for crushing and drying raw coal, more preferably, an outlet of the raw coal crushing and drying unit is respectively communicated with an inlet of the co-pyrolysis unit and an inlet of the pulverizing unit;
preferably, the system further comprises a conveying unit for conveying the first powdered mixture into the gasification unit, more preferably, the conveying unit is in communication with the outlet of the milling unit and the inlet of the gasification unit.
4. The system of claim 1 or 2, wherein the gasification unit is a dry coal powder entrained flow gasifier;
preferably, the first powdery mixture contains particles having a particle diameter of 90 μm or more in a volume content of not more than 10%.
5. System according to claim 1 or 2, wherein in the milling unit, an air blowing device is provided for blowing air to the milling system during milling.
6. A method of treating coal direct liquefaction residue, comprising:
(1) co-pyrolyzing the mixture of the direct coal liquefaction residues and the raw coal to obtain a co-pyrolysis solid product;
(2) extracting the co-pyrolysis solid product by using an extracting agent to obtain an extraction liquid and a solid-liquid mixture;
(3) carrying out solid-liquid separation on the solid-liquid mixture to obtain an extract;
(4) mixing the extraction residues and the raw coal in proportion and grinding the mixture into powder to obtain a first powdery mixture;
(5) gasifying the first powdery mixture.
7. The method according to claim 6, wherein in the step (1), the mass ratio of the coal direct liquefaction residue to the raw coal is 1 (1-100), preferably 1: (3-20);
preferably, the conditions of the co-pyrolysis include: the temperature is 200-600 ℃;
preferably, the tar produced by the co-pyrolysis is subjected to oil further processing.
8. The process of claim 6, wherein, in step (2), the extractant is selected from at least one of coal tar, coal direct liquefaction oil, and tetrahydrofuran;
preferably, the mass ratio of the extracting agent to the solid product after pyrolysis is (3-15):1, preferably (5-10): 1;
preferably, the conditions of the extraction include: the temperature is 150 ℃ and 300 ℃.
9. The method according to claim 6, wherein in the step (4), the mass ratio of the raffinate to the raw coal is 1 (0.1-100), preferably 1: (1-20);
preferably, hot air is blown in during the milling process;
preferably, the hot air is nitrogen, flue gas or mixed gas of air and nitrogen, wherein the oxygen content is less than 8% by volume;
preferably, the inlet temperature of the hot air is 140-300 ℃, and the outlet temperature of the hot air is 35-100 ℃;
preferably, the amount of inlet hot air required per 1kg of throughput is 0.5-5Nm3Preferably 1-3Nm3；
Preferably, the pressure difference between an inlet and an outlet of the hot air is not more than 2000 Pa;
preferably, the first powdery mixture contains particles having a particle diameter of 90 μm or more in a volume content of not more than 10%.
10. The method of claim 6, wherein in step (5), the gasification is carried out in a dry coal powder entrained flow gasifier;
preferably, the conditions of the gasification include: the pressure is 0.1-10MPa, and the temperature is 1000-1600 ℃;
preferably, the method also comprises the steps of drying and crushing the raw coal,
more preferably, the drying conditions include: the temperature is 100-150 ℃;
more preferably, the raw coal is crushed to a particle size of 20mm or less, preferably 10mm or less.
11. A method of processing coal direct liquefaction residue using the system of any of claims 1-5, comprising:
(I) co-pyrolyzing the mixture of the direct coal liquefaction residues and the raw coal in a co-pyrolysis unit to obtain a co-pyrolysis solid product;
(II) extracting the co-pyrolysis solid product in an extraction unit by using an extracting agent to obtain an extraction liquid and a solid-liquid mixture;
(III) carrying out solid-liquid separation on the solid-liquid mixture in a solid-liquid separation unit to obtain raffinate;
(IV) drying and grinding the raffinate and the raw coal in a grinding unit according to a certain proportion to obtain a first powdery mixture;
(V) gasifying the first powdered mixture in a gasification unit;
preferably, the first pulverized mixture is gasified in a dry pulverized coal entrained flow gasifier.
12. The process according to claim 11, wherein in step (IV), the mass ratio of the raffinate to the raw coal is 1 (0.1-100), preferably 1: (1-20);
preferably, hot air is blown in during the milling process;
preferably, the hot air is nitrogen, flue gas or mixed gas of air and nitrogen, wherein the oxygen content is less than 8% by volume;
preferably, the inlet temperature of the hot air is 140-300 ℃, and the outlet temperature of the hot air is 35-100 ℃;
preferably, the pressure difference of the hot air inlet and the hot air outlet is not more than 2000 Pa;
preferably, the first powdery mixture contains particles having a particle diameter of 90 μm or more in a volume content of not more than 10%.
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