CN116531797A - Equipment and process for enriching aromatic hydrocarbon in intermediate phase of medium-low temperature coal tar - Google Patents
Equipment and process for enriching aromatic hydrocarbon in intermediate phase of medium-low temperature coal tar Download PDFInfo
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- CN116531797A CN116531797A CN202310272158.3A CN202310272158A CN116531797A CN 116531797 A CN116531797 A CN 116531797A CN 202310272158 A CN202310272158 A CN 202310272158A CN 116531797 A CN116531797 A CN 116531797A
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- 150000004945 aromatic hydrocarbons Chemical class 0.000 title claims abstract description 53
- 239000011280 coal tar Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 27
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 59
- 239000002904 solvent Substances 0.000 claims abstract description 58
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims description 195
- 239000002994 raw material Substances 0.000 claims description 75
- 238000003860 storage Methods 0.000 claims description 66
- 238000005191 phase separation Methods 0.000 claims description 25
- 230000006835 compression Effects 0.000 claims description 22
- 238000007906 compression Methods 0.000 claims description 22
- 230000005855 radiation Effects 0.000 claims description 22
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 11
- 239000003208 petroleum Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000004891 communication Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000110 cooling liquid Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000012847 fine chemical Substances 0.000 abstract description 13
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 abstract description 12
- GYFAGKUZYNFMBN-UHFFFAOYSA-N Benzo[ghi]perylene Chemical group C1=CC(C2=C34)=CC=C3C=CC=C4C3=CC=CC4=CC=C1C2=C43 GYFAGKUZYNFMBN-UHFFFAOYSA-N 0.000 abstract description 8
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 abstract description 8
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004821 distillation Methods 0.000 abstract description 7
- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 abstract description 4
- -1 alkyl naphthalene Chemical compound 0.000 abstract description 4
- 238000004440 column chromatography Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010575 fractional recrystallization Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 66
- 239000000543 intermediate Substances 0.000 description 22
- 238000011084 recovery Methods 0.000 description 7
- 125000000962 organic group Chemical group 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-M phenolate Chemical compound [O-]C1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-M 0.000 description 1
- 229940031826 phenolate Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000009044 synergistic interaction Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0419—Solvent extraction of solutions which are liquid in combination with an electric or magnetic field or with vibrations
- B01D11/0423—Applying ultrasound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C15/00—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
-
- 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
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/02—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents with two or more solvents, which are introduced or withdrawn separately
-
- 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
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/30—Controlling or regulating
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/30—Aromatics
Abstract
The invention provides a device and a process for enriching aromatic hydrocarbon in a mesophase of medium-low temperature coal tar, wherein the process comprises the steps of a and b, the step a is used for separating and obtaining light distillate oil-II mainly containing alkane, and the light distillate oil-I obtained by distillation and the component can be mixed and modulated to be sold as light oil; the light phenol oil and the enriched refined aromatic hydrocarbon separated in the step b are fine chemicals with high added value, and from the viewpoint of fractional utilization, different high-value fine chemicals such as alkoxyphenol, naphthalene, alkyl naphthalene, anthracene, pyrene, benzo [ ghi ] perylene and the like can be obtained by pressure gradient column chromatography and fractional recrystallization. The method is operated under mild conditions, the used solvent is recycled, the method has the characteristics of environment friendliness, high efficiency, low energy consumption, low investment cost and the like, the defects of long route, easiness in secondary pollution, high production cost and the like in the traditional process for producing the condensed aromatic hydrocarbon are overcome, and the source of fine chemicals of the condensed aromatic hydrocarbon is effectively enriched.
Description
Technical Field
The invention relates to the technical field of coal chemical industry, in particular to equipment and a process for enriching aromatic hydrocarbon in a mesophase of medium-low temperature coal tar.
Background
The medium-low temperature coal tar is a byproduct produced in the process of producing semicoke (semi coke) by medium-low temperature carbonization or in the process of modifying, the organic component of the medium-low temperature coal tar is rich in aromatic hydrocarbon, alkane, alkene and organic matters containing hetero atoms, and the annual output of the medium-low temperature coal tar tends to increase year by year along with the layout and upgrading development of regional coal chemical industry. In short, the organic component of the medium-low temperature coal tar is an important source of various fine chemical intermediates and high-value end products in chemical production. However, the existing subsequent deep processing of medium and low temperature coal tar mainly comprises distillation, catalytic hydrogenation, carbonization and the like, and the obtained products mainly comprise light fraction (gasoline and diesel oil), heavy fraction (fuel, paving asphalt and the like) and carbon material (needle coke, graphite electrode and the like), and the overall added value is not high. In order to further accelerate the high-quality development of regional energy industry and promote the construction of demonstration areas of energy industry revolution, the directional refined value-increasing utilization of the medium-low temperature coal tar is urgently needed according to the molecular composition and component property difference of the medium-low temperature coal tar.
The medium-low temperature coal tar has the advantages that due to the inherent coke quenching production process, carbon and inorganic matters with different particle sizes are endowed in the system, the product quality of fine chemicals such as subsequent aromatic hydrocarbon is seriously affected, the tiny particles are difficult to remove in the existing separation process, and the process flow is complicated.
Disclosure of Invention
In order to solve the defects, the invention provides equipment and a process for enriching aromatic hydrocarbon in the intermediate phase of medium-low temperature coal tar, which are operated under mild conditions, and the used solvent is recycled, so that the method has the characteristics of environment friendliness, high efficiency, low energy consumption, low investment cost and the like, overcomes the defects of long route, easiness in secondary pollution, high production cost and the like in the traditional process for producing the condensed aromatic hydrocarbon, and effectively enriches the sources of fine chemicals of the condensed aromatic hydrocarbon.
In a first aspect, the invention provides a middle-low temperature coal tar mesophase aromatic hydrocarbon enrichment device, which comprises a raw material tank I (12), a primary extraction kettle (5), an alkane storage tank (10), a condenser I (15), an alkane buffer tank (17), a secondary extraction kettle (6), a raw material tank II (13), a raw material tank III (14), a condenser II (16), a grading solvent storage tank (11) and a phase separation tank (18); the outlet of the raw material tank I (12) is connected with the inlet of the primary extraction kettle (5) through a pipeline, the first outlet of the primary extraction kettle (5) is connected with the inlet of the secondary extraction kettle (6) through a pipeline, the outlet of the primary extraction kettle (5) is connected with the inlet of the condenser I (15) through a pipeline, the outlet of the condenser I (15) is connected with the inlet of the alkane buffer tank (17) through a pipeline, the outlet of the alkane buffer tank (17) is connected with the inlet of the alkane storage tank (10) through a pipeline, and the outlet of the alkane storage tank (10) is connected with the inlet of the primary extraction kettle (5) through a pipeline; the outlet of the raw material tank II (13) and the outlet of the raw material tank III (14) are connected with the inlet of the secondary extraction kettle (6) through pipelines, the outlet of the secondary extraction kettle (6) is connected with the inlet of the condenser II (16) through pipelines, the outlet of the condenser II (16) is connected with the inlet of the phase separation tank (18) through pipelines, the outlet of the phase separation tank (18) is connected with the inlet of the grading solvent storage tank (11) through pipelines, and the outlet of the grading solvent storage tank (11) is connected with the inlet of the secondary extraction kettle (6) through pipelines.
In one embodiment of the invention, a discharge valve I (26) is arranged at the bottom of a primary extraction kettle (5), an electric auxiliary heating device and an ultrasonic radiating device are arranged on the outer wall of the primary extraction kettle (5), the electric auxiliary heating device and the ultrasonic radiating device are respectively connected with a magnetic heating controller I (3), a motor I (42), a pressure gauge I (22) and an emptying valve III (34) are arranged at the top of the primary extraction kettle (5), a stirrer I (23) is arranged in the middle of the primary extraction kettle (5), and the stirrer I (23) is connected with the motor I (42).
In one embodiment of the invention, the primary extraction kettle (5) is connected with the feeding device through a pipeline, and a feed liquid valve I (36) is arranged on the pipeline between the primary extraction kettle (5) and the feeding device;
in one embodiment of the invention, the primary extraction kettle (5) is connected with the gas compression pump (1) through a pipeline, and a gas interception valve I (39) and a compressed gas three-way valve (37) are arranged on the pipeline between the primary extraction kettle (5) and the gas compression pump (1);
in one embodiment of the invention, a feeding pump I (1), a raw material valve I (28) and a three-way valve III (38) are arranged on a pipeline between a raw material tank I (12) and a primary extraction kettle (5);
in one embodiment of the invention, a gas valve I (32) is arranged on a pipeline between the primary extraction kettle (5) and the condenser I (15);
in one embodiment of the invention, a control valve I (21) is arranged on a pipeline between the condenser I (15) and the alkane buffer tank (17);
in one embodiment of the invention, a circulating pump (8) is arranged on a pipeline between the alkane buffer tank (17) and the alkane storage tank (10);
in one embodiment of the invention, the bottom of the alkane storage tank (10) is connected with a three-way valve III (38), the top of the alkane storage tank (10) is provided with a vent valve I (19), and the side wall of the alkane storage tank (10) is provided with a light distillate oil-II extraction outlet.
In one embodiment of the invention, a discharge valve II (27) is arranged at the bottom of the secondary extraction kettle (6), an electric auxiliary heating device and an ultrasonic radiation device are arranged on the outer wall of the secondary extraction kettle (6), the electric auxiliary heating device and the ultrasonic radiation device are respectively connected with a magnetic heating controller II (4), a motor II (43), a pressure gauge II (25) and an emptying valve IV (35) are arranged at the top of the secondary extraction kettle (6), a stirrer II (24) is arranged at the middle part of the secondary extraction kettle (6), and the stirrer II (24) is connected with the motor II (43).
In one embodiment of the invention, a discharge valve I (26) is arranged on the pipelines of the secondary extraction kettle (6) and the primary extraction kettle (5);
in one embodiment of the invention, the secondary extraction kettle (6) is connected with the compressed gas three-way valve (37) through a pipeline, and a gas cut-off valve II (45) is arranged on the pipeline of the secondary extraction kettle (6) and the compressed gas three-way valve (37);
in one embodiment of the invention, a gas valve II (33) is arranged on a pipeline between the secondary extraction kettle (6) and the condenser II (16);
in one embodiment of the invention, a control valve III (44) is arranged on a pipeline between the condenser II (16) and the phase separation tank (18);
in one embodiment of the invention, a control valve II (29) and a circulating pump II (9) are arranged on a pipeline between the phase separation tank (18) and the graded solvent storage tank (11);
in one embodiment of the invention, a three-way valve II (31) is arranged on a pipeline between the grading solvent storage tank (11) and the secondary extraction kettle (6);
in one embodiment of the invention, the top of the grading solvent storage tank (11) is provided with a vent valve II (20), the inlet of the grading solvent storage tank (11) is connected with the circulating pump II (9), and the outlet of the grading solvent storage tank (11) is connected with the three-way valve II (31);
in one embodiment of the invention, a raw material tank II (13) is connected with a three-way valve II (31) through a pipeline, a feeding pump II (7) is arranged on the pipeline between the raw material tank II (13) and the three-way valve II (31), and a raw material valve II (40) is arranged on the pipeline between the raw material tank II (13) and the feeding pump II (7);
in one embodiment of the invention, a raw material tank III (14) is connected with a feed pump II (7) through a pipeline, and a raw material valve III (41) is arranged on the pipeline between the raw material tank III (14) and the feed pump II (7);
in one embodiment of the invention, the raw material tank II (13) and the raw material tank III (14) are connected with a three-way valve I (30) through pipelines, the three-way valve I (30) is also connected with a feeding device through a pipeline, and a control valve IV (46) is arranged on the pipeline of the three-way valve I (30) and the feeding device.
In a second aspect, the invention provides a process for enriching aromatic hydrocarbon in a mesophase of low-temperature coal tar, which comprises the following steps:
a: the middle-low temperature coal tar intermediate phase is placed in a first-stage extraction kettle (5) through a conveying system, and a first-stage matched extracting agent is adopted to extract the light distillate oil-II in the organic components of the middle-low temperature coal tar intermediate phase to obtain enriched crude aromatic hydrocarbon;
b: and (3) conveying the second-level extraction agent to a second-level extraction kettle (6) and extracting the mixture to obtain enriched refined aromatic hydrocarbon.
In one embodiment of the present invention, step a comprises the following process:
a1 Replacement of residual air in the system by N by a gas compression pump (1) 2 The method comprises the steps of opening a feed liquid valve I (36), metering a medium-low temperature coal tar mesophase and then pumping the medium-low temperature coal tar mesophase into a primary extraction kettle (5), opening a stirring device, adjusting a vent valve III (34) according to a pressure gauge I (22), opening a raw material valve I (28), a feed pump I (2) and a three-way valve III (38), adding a first-stage matched extractant in a raw material tank I (12) into the primary extraction kettle (5), closing the feed pump I (2), opening a gas compression pump (1), a compressed gas three-way valve (37) and a gas interception valve I (39), and ensuring a gas path together with and filling N 2 Then closing a valve corresponding to the stamping system, opening a magnetocaloric controller I (3), heating the primary extraction kettle (5) to 30-45 ℃, and opening an ultrasonic radiation device to extract for 0.3-0.5h;
a2 The motor I (42) and the ultrasonic radiation device are closed, the gas valve I (32) is opened, the thermal control system is opened to heat the primary extraction kettle (5) to 90-105 ℃ for a certain time, the condenser I (15) is opened, the cooling liquid is conveyed to the alkane buffer tank (22) through the control valve I (21), the liquid in the alkane buffer tank (22) is conveyed to the alkane storage tank (10) for storage by the circulating pump II (8), and the solvent in the alkane storage tank (10) and the first-stage extraction agent in the raw material tank I (12) enter the primary extraction kettle (5) again for secondary extraction;
a3 Repeating the extraction steps for a plurality of times, opening a discharge valve I (26), closing a gas cut-off valve I (39) and a gas valve I (32), and transferring the enriched crude aromatic hydrocarbon into a secondary extraction kettle (6).
In one embodiment of the present invention, step b comprises the following process:
b1 Opening a raw material valve II (40), a raw material valve III (41), a feeding pump II (7) and a three-way valve II (30) to ensure that a conveying pipeline is smooth, enabling second-stage extraction agents of a raw material tank II (13) and a raw material tank III (14) to enter a second-stage extraction kettle (6) according to a proportion, sequentially opening a compressed gas three-way valve (37), a gas compression pump (1) and a gas cut-off valve II (45) to ensure gas path communication, and adjusting N in the second-stage extraction kettle (6) according to a pressure gauge II (25) 2 The pressure is 0.1-0.3MPa, then the gas compression pump (1) is closed, the magnetocaloric controller II (4) is started to heat the secondary extraction kettle (6) to 40-55 ℃, and the ultrasonic radiation is started to extract for 0.4-0.6h;
b2 Closing the ultrasonic radiation devices of the motor II (43) and the magnetocaloric controller II (4), opening the gas valve II (33), and heating the secondary extraction kettle (6) to 80-100 ℃;
b3 Opening a gas valve II (33) and a condenser II (16), allowing condensate to enter a phase separation tank (18) after passing through a control valve III (44), separating a second graded extractant and intermediate phase phenol oil after passing through a phase separation, sequentially opening a control valve II (29) and a feed pump II (9), conveying the second graded extractant to a graded solvent storage tank (11), wherein the graded solvent storage tank (11) is provided with an emptying valve II (20), and allowing the second graded extractant in the tank to circulate to a second extraction kettle (6) after passing through a three-way valve I (31);
b4 Repeating the extraction steps for a plurality of times, opening a discharge valve II (27), closing a gas cut-off valve II (45) and a gas valve II (33), and collecting the product enriched refined aromatic hydrocarbon.
In one embodiment of the invention, the intermediate phase aromatic hydrocarbon enrichment process of the medium-low temperature coal tar further comprises the following steps: c, recovering and re-grading the extraction solvent; step c comprises the following steps:
c1 After step a1 is finished, opening the vent valve III (34) to discharge N 2 The volatile gas is collected and recycled after reaching normal pressure, the circulating solvent enters the circulation through an alkane storage tank (10) and a three-way valve III (38), and the quality of the extraction solution is 95% of that of the previous extraction solvent;
c2 After the step b2 is finished, the phase separation tank (18) is cooled to minus 10 ℃, the second-stage extractant and the light phenol oil are separated, a control valve IV (46) and a three-way valve I (30) are opened, fresh extract is calculated and distributed to enter a raw material tank II (13) and a raw material tank III (14) through the control valve three-way valve I (30), and the extraction ratio of the second-stage extractant to the enriched crude aromatic hydrocarbon is ensured.
In one embodiment of the invention, in step a and step b, the number of extraction cycles is greater than or equal to 3;
in one embodiment of the invention, in step a, the first stage extractant consists of petroleum ether having a boiling range of 30 to 60℃and petroleum ether having a boiling range of 60 to 90℃in a mass ratio (0.8 to 1.2): 1, the composition is as follows;
in one embodiment of the invention, in step b, the second graded extractant consists of methanol and ethanol in a mass ratio (1.8-2.2): 1.
In summary, the invention provides equipment and a process for enriching aromatic hydrocarbon in the mesophase of medium-low temperature coal tar, which have the beneficial effects that:
the invention adopts graded extractant with boiling point lower than 90 ℃ and operates under mild condition, and the extraction solvent has high recycling efficiency and low energy consumption. The invention adopts inert gas N 2 As the system protection gas, the occurrence of explosion and other scenes caused by the enrichment of volatile gas is avoided. The invention designs a brand new low-boiling point grading solvent for separating and enriching aromatic hydrocarbon, adopts alkane to selectively destroy intermolecular winding in middle-low temperature coal tar intermediate phase, adopts alkanol grading solvent to destroy strong hydrogen bond action and strong hydrogen bond/pi-pi composite action in enriching crude aromatic hydrocarbon, has weak toxicity, low price and easy recovery compared with traditional extracting agents with high boiling points of N-methylpyrrolidone and N, N-dimethylformamide, and effectively reduces energy consumption, thus being a green process technology.
Further, the invention starts from the intermediate phase organic group component of the medium-low temperature coal tar, the step a is separated to obtain light distillate oil-II mainly containing alkane, and the light distillate oil-I obtained by distillation and the component can be used as light oil for sale; the light phenol oil and the enriched refined aromatic hydrocarbon separated in the step b are fine chemicals with high added value, and from the viewpoint of fractional utilization, different high-value fine chemicals such as alkoxyphenol, naphthalene, alkyl naphthalene, anthracene, pyrene, benzo [ ghi ] perylene and the like can be obtained by pressure gradient column chromatography and fractional recrystallization.
Furthermore, the method has the characteristics of reasonable process route, simple flow, mild operation condition, short production period and flexible operation, and can obtain a high-value fine chemical matrix by mildly and directionally separating different organic components according to the difference between the molecular properties of the organic group components, thereby being a green and efficient method for separating and producing fine chemicals.
Drawings
Fig. 1 is a schematic structural diagram of a device for enriching aromatic hydrocarbons in a mesophase of medium-low temperature coal tar according to an embodiment of the present invention.
Fig. 2 is a flow chart of a process for enriching aromatic hydrocarbon in a mesophase of medium-low temperature coal tar according to an embodiment of the present invention.
Main element symbol description:
1, a gas compression pump; 2. a feed pump I; 3. a magnetocaloric controller I; 4. a magnetocaloric controller II; 5. a first-stage extraction kettle; 6. a second-stage extraction kettle; 7. a feed pump II; 8. a circulating pump II; 9. circulation pumps II, 10 and alkane storage tanks; 11. grading solvent storage tank; 12. a raw material tank I; 13. a raw material tank II; 14. a raw material tank III; 15. a condenser I; 16. a condenser II; 17. an alkane buffer tank; 18. a phase separation tank; 19. a blow-off valve I; 20. a blow-off valve II; 21. a control valve I; 22. a pressure gauge I; 23. a stirrer I; 24. a stirrer II; 25. a pressure gauge II; 26. a discharge valve I; 27. a discharge valve II; 28. a raw material valve I; 29. a control valve II; 30. a three-way valve I; 31. a three-way valve II; 32. a gas valve I;33 gas valve II; 34. a blow-off valve III; 35. a vent valve IV; 36. a feed liquid valve I; 37. a compressed gas three-way valve; 38. a three-way valve III; 39. a gas shut-off valve I; 40. a raw material valve II; 41. a raw material valve III; 42. a motor I; 43. a motor II; 44. a control valve III; 45. a gas shut-off valve II; 46. and a control valve IV.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, an embodiment discloses a middle-low temperature coal tar mesophase aromatic hydrocarbon enrichment device, which mainly comprises a primary extraction kettle 5, a secondary extraction kettle 6, a condenser I15, a condenser II 16, a raw material tank I12, a raw material tank II 13, a raw material tank III 14, an alkane storage tank 10, a graded solvent storage tank 11, an alkane buffer tank 17, a phase separation tank 18, and a pressure pipeline system, a magnetocaloric control system, an extract liquid conveying and recycling system, a valve control system and a pipeline system which are matched with the middle-low temperature coal tar mesophase aromatic hydrocarbon enrichment device.
The outlet of the raw material tank I12 is connected with the inlet of the primary extraction kettle 5 through a pipeline, the first outlet of the primary extraction kettle 5 is connected with the inlet of the secondary extraction kettle 6 through a pipeline, the outlet of the primary extraction kettle 5 is connected with the inlet of the condenser I15 through a pipeline, the condenser I15 cools the first-stage extracting agent and the light distillate oil-II gas, the outlet of the condenser I15 is connected with the inlet of the alkane buffer tank 17 through a pipeline, the alkane buffer tank 17 is used for collecting condensate, the outlet of the alkane buffer tank 17 is connected with the inlet of the alkane storage tank 10 through a pipeline, and the outlet of the alkane storage tank 10 is connected with the inlet of the primary extraction kettle 5 through a pipeline.
The outlets of the raw material tank II 13 and the raw material tank III 14 are connected with the inlet of the secondary extraction kettle 6 through pipelines, the outlet of the secondary extraction kettle 6 is connected with the inlet of the condenser II 16 through pipelines, the outlet of the condenser II 16 is connected with the inlet of the phase separation tank 18 through pipelines, the outlet of the phase separation tank 18 is connected with the inlet of the grading solvent storage tank 11 through pipelines, and the outlet of the grading solvent storage tank 11 is connected with the inlet of the secondary extraction kettle 6 through pipelines.
The bottom of the primary extraction kettle 5 is provided with a discharge valve I26, the outer wall of the primary extraction kettle 5 is provided with an electric auxiliary heating device and an ultrasonic radiation device, the electric auxiliary heating device and the ultrasonic radiation device are respectively connected with a magnetocaloric controller I3, the top of the primary extraction kettle 5 is provided with a motor I42, the middle part of the primary extraction kettle 5 is provided with a stirrer I23, and the stirrer I23 is connected with the motor I42. The top of the primary extraction kettle 5 is provided with a pressure gauge I22 and a blow-off valve III 34, and the pressure gauge I22 detects the pressure in the kettle and the blow-off valve III 34 regulates and controls the pressure in the kettle.
The first-stage extraction kettle 5 is connected with a feeding device through a pipeline, and a feed liquid valve I36 is arranged on the pipeline between the first-stage extraction kettle 5 and the feeding device; the primary extraction kettle 5 is used for passing N 2 The air inlet pipeline is connected with the gas compression pump 1, and N is arranged between the primary extraction kettle 5 and the gas compression pump 1 2 The air inlet pipeline is provided with a gas cut-off valve I39 and a compressed gas three-way valve 37; a pipeline between the raw material tank I12 and the primary extraction kettle 5 is provided with a feed pump I1, a raw material valve I28 and a three-way valve III 38; a gas valve I32 is arranged on a pipeline between the primary extraction kettle 5 and the condenser I15; a control valve I21 is arranged on a pipeline between the condenser I15 and the alkane buffer tank 17; a circulating pump 8 is arranged on a pipeline between the alkane buffer tank 17 and the alkane storage tank 10.
The bottom of the alkane storage tank 10 is connected with a three-way valve III 38, the top of the alkane storage tank 10 is provided with a vent valve I19, and the side wall of the alkane storage tank 10 is provided with a light distillate oil-II extraction outlet.
The bottom of the secondary extraction kettle 6 is provided with a discharge valve II 27, the outer wall of the secondary extraction kettle 6 is provided with an electric auxiliary heating device and an ultrasonic radiation device, the electric auxiliary heating device and the ultrasonic radiation device are respectively connected with a magnetocaloric controller II 4, the top of the secondary extraction kettle 6 is provided with a motor II 43, the middle part of the secondary extraction kettle 6 is provided with a stirrer II 24, and the stirrer II 24 is connected with the motor II 43. The top of the secondary extraction kettle 6 is provided with a pressure gauge II 25 and an emptying valve IV 35, and the pressure gauge is used for detecting the pressure in the kettle and regulating the pressure in the kettle through the emptying valve IV 35
The pipelines of the secondary extraction kettle 6 and the primary extraction kettle 5 are provided with a discharge valve I26; the secondary extraction kettle 6 is connected with a compressed gas three-way valve 37 through a pipeline, and a gas cut-off valve II 45 is arranged on the pipeline of the secondary extraction kettle 6 and the compressed gas three-way valve 37; a gas valve II 33 is arranged on a pipeline between the secondary extraction kettle 6 and a condenser II 16, the condenser II 16 cools the secondary extraction agent and the intermediate phase phenol oil gas, and a control valve III 44 is arranged on a pipeline between the condenser II 16 and the phase separation tank 18; a control valve II 29 and a circulating pump II9 are arranged on a pipeline between the phase separation tank 18 and the grading solvent storage tank 11; a three-way valve II 31 is arranged on a pipeline between the grading solvent storage tank 11 and the secondary extraction kettle 6; the top of the grading solvent storage tank 11 is provided with a vent valve II 20, the inlet of the grading solvent storage tank 11 is connected with a circulating pump II9, and the outlet of the grading solvent storage tank 11 is connected with a three-way valve II 31.
The material tank II 13 is connected with the three-way valve II 31 through a pipeline, a feeding pump II 7 is arranged on the pipeline between the material tank II 13 and the three-way valve II 31, and a material valve II 40 is arranged on the pipeline between the material tank II 13 and the feeding pump II 7; the raw material tank III 14 is connected with the feed pump II 7 through a pipeline, and a raw material valve III 41 is arranged on the pipeline between the raw material tank III 14 and the feed pump II 7; the material tank II 13 and the material tank III 14 are connected with a three-way valve I30 through pipelines, the three-way valve I30 is also connected with a feeding device through a pipeline, and a control valve IV 46 is arranged on the pipeline of the three-way valve I30 and the feeding device.
Example 2
A process for enriching aromatic hydrocarbon in a mesophase of medium-low temperature coal tar comprises the following steps:
step a: the intermediate phase of the medium-low temperature coal tar is placed in a first-stage extraction kettle 5 through a conveying system, the first-stage extraction agent prepared from low-boiling-point paraffin is adopted to extract the intermediate phase of the medium-low temperature coal tar to remove light distillate oil-II in organic components of the intermediate phase, so as to obtain enriched crude aromatic hydrocarbon, and the light distillate oil-II and the light distillate oil-I obtained by distillation are mixed and prepared to be used as light oil for sale. The first-stage extraction agent in the embodiment consists of petroleum ether with the boiling range of 30-60 ℃ and petroleum ether with the boiling range of 60-90 ℃, wherein the mass ratio of the petroleum ether with the boiling range of 30-60 ℃ to the petroleum ether with the boiling range of 60-90 ℃ is 1:3,1:2,1:1,2:1,3:1.
step b: and (3) conveying the second-level extraction agent to a second-level extraction kettle 6 through a system, and extracting the mixture to obtain enriched refined aromatic hydrocarbon. In the embodiment, the second grading extractant consists of methanol and ethanol, and the mass ratio of the methanol to the ethanol is 1:3,1:2,1:1,2:1,3:1.
step c: the solvent recovery system realizes recovery and re-grading of the extraction solvent, and ensures the extraction efficiency of the steps a and b.
Step a comprises the following steps:
a1, firstly, the gas compression pump 1 is started, and N is used for 2 Displacing the residual air in the apparatus to ensure that the apparatus is maintained in an inert environment; then a feed liquid valve I36 is opened, the intermediate phase of the medium-low temperature coal tar preheated to a certain temperature is metered and then is pumped into a first-stage extraction kettle 5, a motor 1 42 is opened in the conveying process to drive a stirrer I23 so as to ensure that feed liquid is uniformly distributed, and the opening and closing state of a vent valve III 34 is determined according to the display parameters of a pressure gauge I22 in the conveying process;
a2, starting a raw material valve I28, starting a feed pump I2, adjusting the flow direction of a three-way valve III 38, and ensuring that a first-stage extraction agent in a raw material tank I12 enters a first-stage extraction kettle 5;
a3, closing the feeding pump I2, opening the gas compression pump 1, adjusting the communication direction of the compressed gas three-way valve 37, opening the gas cut-off valve I39, and filling N 2 Closing the corresponding valves of the gas compression pump 1 and the punching system after the pressure reaches 0.3 MPa;
a4, starting a magnetocaloric controller I3, ensuring that the temperature in the primary extraction kettle 5 is maintained at 30-45 ℃, starting ultrasonic radiation magnetic stirring for extraction, and extracting for 0.3h under the conditions;
a5, after extraction is finished, closing a motor I42, closing an ultrasonic radiation device, opening a gas valve I32, opening a thermal control system to heat to 95 ℃, and recovering an extraction solvent and separating light distillate oil-II from a medium-low temperature coal tar mesophase system;
a6, in the solvent recovery and light distillate oil-II extraction system, the liquid cooled by the condenser I15 enters the alkane buffer tank 22 through the control valve I21, the liquid in the alkane buffer tank 22 is conveyed to the alkane storage tank 10 for storage by the circulating pump II 8, and the pressure in the tank is regulated and controlled by the emptying valve I19;
a7, mixing the solvent in the alkane storage tank 10 and the first-stage extracting agent in the raw material tank I12 in proportion, and then entering the first-stage extraction kettle 5 again for secondary extraction;
a8, repeating the above extraction steps, namely steps a2, a3, a4, a5 and a6 more than twice, in particular, in step a3, charging N by the gas compression pump 1 2 The pressure of the first extraction is maintained at 0.3MPa to a first-stage extraction kettle 5, and the pressure of each cycle of the cyclic extraction is increased by 0.1MPa on the basis of the first extraction; in the step a4, the first extraction time is 0.3h, and the time of each cycle of extraction is increased by 0.1h on the basis of the first time. After the two phases are clearly layered, the discharge valve I26 is opened, the gas cut-off valve I39 and the gas valve I32 are closed by means of the pressure in the kettle, and the enriched crude aromatic hydrocarbon is transferred into the secondary extraction kettle 6.
Step b comprises the following steps:
b1, opening a raw material valve II 40 and a raw material valve III 41, opening a feed pump II 7, adjusting the flow direction of a three-way valve II 30, enabling a raw material tank II 13 to be filled with methanol, a raw material tank III 14 to be filled with ethanol, and then ensuring that solvents in the raw material tank II 13 and the raw material tank III 14 enter the secondary extraction kettle 6 according to the preparation proportion.
b2, adjusting the communication direction of the compressed gas three-way valve 37, sequentially opening the gas compression pump 1 and the gas cut-off valve II 45, observing the change of the pressure gauge II 25, and filling N into the secondary extraction kettle 6 2 After reaching 0.1MPa, the gas compression pump 1 is turned off;
b3, starting a magnetocaloric controller II 4, ensuring that the temperature in the secondary extraction kettle 6 is maintained at 50 ℃, starting ultrasonic radiation magnetic stirring for extraction, and extracting for 0.4h under the conditions;
after the extraction is finished, closing a motor II 43, closing an ultrasonic radiation device, opening a gas valve II 33, opening a thermal control system to heat to 90 ℃, and recovering an extraction solvent and separating intermediate phase phenol oil from the crude aromatic hydrocarbon enrichment system;
b5, the extract and the intermediate phase phenol oil enter a condenser II 16 through a gas valve II 33, the condensate enters a phase separation tank 18 after passing through a control valve III 44, the extract and the intermediate phase phenol oil are separated through phase separation, a control valve II 29 and a feed pump II9 are sequentially opened, the separated extract is conveyed to a graded solvent storage tank 11, the graded solvent storage tank 11 is provided with a vent valve II 20, and the pressure in the tank is controlled;
b6, circulating the extract in the grading solvent storage tank 11 to the secondary extraction kettle 6 through a three-way valve I31, and controlling the component proportion of the grading solvent through calculation of the three-way valve I31;
b7 repeating the above extraction steps, namely steps b1, b2, b3, b4 and b5 more than two times, in particular, in step b2, N is charged by the gas compression pump 1 2 The pressure of the first extraction is maintained at 0.1MPa to a second-stage extraction kettle 6, and the pressure of each cycle of the cyclic extraction is increased by 0.1MPa on the basis of the first extraction; in the step b3, the first extraction time is 0.4h, and the time of each cycle of extraction is increased by 0.1h on the basis of the first time. After the two phases are clearly layered, opening a discharge valve II 27 by means of the pressure in the kettle, closing a gas cut-off valve II 45 and a gas valve II 33, and collecting the product enriched refined aromatic hydrocarbon;
b8, opening or closing the control valve IV 46 according to the liquid level change of the raw material tank III 14 to ensure that the liquid level is kept stable.
Step c comprises the following steps:
c1: in the step a, after the step a4 is finished, a relief valve III 34 is opened to relax N 2 The volatile gas is collected and recycled until the normal pressure is reached, and the separation, recovery and distillation temperature of the extraction solvent and the light distillate oil-II is reduced;
c2: in the step a, in the solvent recovery and light distillate oil-II extraction system, in order to ensure the circulating extraction efficiency, the mass of the circulating solvent entering the circulating extraction solution through the alkane storage tank 10 and the three-way valve III 38 is 95% of the mass of the solvent extracted last time;
c3: in the step b, after the step b4 is finished, the vent valve II 33 is opened, and N is relaxed 2 The mixture is cooled to normal pressure, volatile gas is collected for recycling, and the separation, recovery and distillation temperature of the graded solvent and the intermediate phase phenol oil is reduced;
c4: in the step b, a cooling device is arranged on the phase separation tank 18, and after the temperature is reduced to-10 ℃, the rapid separation of the second-stage extraction agent and the light phenol oil is realized;
c5: fresh extract from outside the boundary is connected with a three-way valve I30 through a control valve IV 46, and enters a raw material tank II 13 and a raw material tank III 14 after being calculated and distributed through the control valve three-way valve I30, so that the extraction proportion of the second-stage extraction agent and the enriched crude aromatic hydrocarbon is ensured.
Detection result:
the light distillate-II, the intermediate phase phenol oil and the enriched refined aromatic components are shown in the attached table 1.
Table 1 example results of light distillate-II, mesophase phenolate and enriched refined aromatics gas chromatography/mass spectrometry combined analysis
Note that: petroleum ether at 30-60 ℃): petroleum ether at 60-90 ℃ is expressed as A: b, a step of preparing a composite material; methanol: ethanol is denoted as C: D.
in conclusion, the intermediate phase of the medium-low temperature coal tar can be obtained by cutting the fraction of the medium-low temperature coal tar, so that the difficult problem that solid inorganic matters in components are difficult to separate is solved, the primary enrichment of aromatic hydrocarbon is realized, and a reliable basis is provided for efficient enrichment of aromatic hydrocarbon in the intermediate phase of the medium-low temperature coal tar. Further, the external field cavitation force of synergistic interaction of extraction/back extraction, stirring and ultrasound is adopted to selectively utilize or destroy the interaction force between the intermediate phase organic matter groups of the medium-low temperature coal tar, namely, the selective destruction utilizes the winding action between alkyl groups of the organic molecule groups, pi-pi interaction between aromatic rings, weak hydrogen bonding, strong hydrogen bonding and strong hydrogen bonding/pi-pi composite action, and the relevance of islands and islands in Dan Youzu science is used as a reference to realize the rapid enrichment of the aromatic ring-enriched organic groups. The organic group rich in aromatic rings can be used for further pressurizing gradient column chromatography, and finely separating high-value fine chemicals such as naphthalene, alkyl naphthalene, anthracene, pyrene, benzo [ ghi ] perylene and the like by fractional recrystallization, and the heavy soluble phase does not contain any small particles, so that the organic group rich in aromatic rings can be used for preparing foam carbon, carbon microspheres, asphalt carbon fibers and anticoagulated road asphalt.
The invention starts from the intermediate-phase organic group component of the medium-low temperature coal tar, the light fraction oil-II which is mainly alkane is obtained by separation in the step a, and the component is mixed with the light fraction oil-I obtained by distillation to be prepared and sold as light oil; the light phenol oil and the enriched refined aromatic hydrocarbon separated in the step b are fine chemicals with high added value, and from the viewpoint of fractional utilization, different high-value fine chemicals such as alkoxyphenol, naphthalene, alkyl naphthalene, anthracene, pyrene, benzo [ ghi ] perylene and the like can be obtained by pressure gradient column chromatography and fractional recrystallization.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The equipment for enriching the aromatic hydrocarbon in the middle-low temperature coal tar intermediate phase is characterized by comprising a raw material tank I (12), a first-stage extraction kettle (5), an alkane storage tank (10), a condenser I (15), an alkane buffer tank (17), a second-stage extraction kettle (6), a raw material tank II (13), a raw material tank III (14), a condenser II (16), a grading solvent storage tank (11) and a phase separation tank (18);
the outlet of the raw material tank I (12) is connected with the inlet of the primary extraction kettle (5) through a pipeline, the first outlet of the primary extraction kettle (5) is connected with the inlet of the secondary extraction kettle (6) through a pipeline, the outlet of the primary extraction kettle (5) is connected with the inlet of the condenser I (15) through a pipeline, the outlet of the condenser I (15) is connected with the inlet of the alkane buffer tank (17) through a pipeline, the outlet of the alkane buffer tank (17) is connected with the inlet of the alkane storage tank (10) through a pipeline, and the outlet of the alkane storage tank (10) is connected with the inlet of the primary extraction kettle (5) through a pipeline;
the outlet of the raw material tank II (13) and the outlet of the raw material tank III (14) are connected with the inlet of the secondary extraction kettle (6) through pipelines, the outlet of the secondary extraction kettle (6) is connected with the inlet of the condenser II (16) through pipelines, the outlet of the condenser II (16) is connected with the inlet of the phase separation tank (18) through pipelines, the outlet of the phase separation tank (18) is connected with the inlet of the grading solvent storage tank (11) through pipelines, and the outlet of the grading solvent storage tank (11) is connected with the inlet of the secondary extraction kettle (6) through pipelines.
2. The middle-low temperature coal tar mesophase enrichment aromatic hydrocarbon device according to claim 1, wherein a discharge valve I (26) is arranged at the bottom of the primary extraction kettle (5), an electric auxiliary heating device and an ultrasonic radiation device are arranged on the outer wall of the primary extraction kettle (5), the electric auxiliary heating device and the ultrasonic radiation device are respectively connected with a magnetocaloric controller I (3), a motor I (42), a pressure gauge I (22) and an emptying valve III (34) are arranged at the top of the primary extraction kettle (5), a stirrer I (23) is arranged at the middle part of the primary extraction kettle (5), and the stirrer I (23) is connected with the motor I (42).
3. The mesophase aromatic hydrocarbon enrichment device for medium and low temperature coal tar according to claim 1, which is characterized by comprising any one or more of the following technical characteristics:
1) The first-stage extraction kettle (5) is connected with the feeding device through a pipeline, and a feed liquid valve I (36) is arranged on the pipeline between the first-stage extraction kettle (5) and the feeding device;
2) The first-stage extraction kettle (5) is connected with the gas compression pump (1) through a pipeline, and a gas cut-off valve I (39) and a compressed gas three-way valve (37) are arranged on the pipeline between the first-stage extraction kettle (5) and the gas compression pump (1);
3) A feeding pump I (1), a raw material valve I (28) and a three-way valve III (38) are arranged on a pipeline between the raw material tank I (12) and the primary extraction kettle (5);
4) A gas valve I (32) is arranged on a pipeline between the primary extraction kettle (5) and the condenser I (15);
5) A control valve I (21) is arranged on a pipeline between the condenser I (15) and the alkane buffer tank (17);
6) A circulating pump (8) is arranged on a pipeline between the alkane buffer tank (17) and the alkane storage tank (10);
7) The bottom of the alkane storage tank (10) is connected with a three-way valve III (38), the top of the alkane storage tank (10) is provided with an emptying valve I (19), and the side wall of the alkane storage tank (10) is provided with a light distillate oil-II extraction outlet.
4. The middle-low temperature coal tar mesophase enrichment aromatic hydrocarbon device according to claim 1, wherein a discharge valve II (27) is arranged at the bottom of the secondary extraction kettle (6), an electric auxiliary heating device and an ultrasonic radiation device are arranged on the outer wall of the secondary extraction kettle (6), the electric auxiliary heating device and the ultrasonic radiation device are respectively connected with a magnetocaloric controller II (4), a motor II (43), a pressure gauge II (25) and an emptying valve IV (35) are arranged at the top of the secondary extraction kettle (6), a stirrer II (24) is arranged at the middle part of the secondary extraction kettle (6), and the stirrer II (24) is connected with the motor II (43).
5. The mesophase aromatic hydrocarbon enrichment device for medium and low temperature coal tar according to claim 3, which comprises any one or more of the following technical features:
1) A discharge valve I (26) is arranged on the pipelines of the second-stage extraction kettle (6) and the first-stage extraction kettle (5);
2) The secondary extraction kettle (6) is connected with a compressed gas three-way valve (37) through a pipeline, and a gas cut-off valve II (45) is arranged on the pipeline of the secondary extraction kettle (6) and the compressed gas three-way valve (37);
3) A gas valve II (33) is arranged on a pipeline between the secondary extraction kettle (6) and the condenser II (16);
4) A control valve III (44) is arranged on a pipeline between the condenser II (16) and the phase separation tank (18);
5) A control valve II (29) and a circulating pump II (9) are arranged on a pipeline between the phase separation tank (18) and the grading solvent storage tank (11);
6) A three-way valve II (31) is arranged on a pipeline between the grading solvent storage tank (11) and the secondary extraction kettle (6);
7) The top of the grading solvent storage tank (11) is provided with a vent valve II (20), the inlet of the grading solvent storage tank (11) is connected with the circulating pump II (9), and the outlet of the grading solvent storage tank (11) is connected with a three-way valve II (31);
8) The material tank II (13) is connected with the three-way valve II (31) through a pipeline, a feeding pump II (7) is arranged on the pipeline between the material tank II (13) and the three-way valve II (31), and a material valve II (40) is arranged on the pipeline between the material tank II (13) and the feeding pump II (7);
9) The raw material tank III (14) is connected with the feed pump II (7) through a pipeline, and a raw material valve III (41) is arranged on the pipeline between the raw material tank III (14) and the feed pump II (7);
10 The material tank II (13) and the material tank III (14) are connected with a three-way valve I (30) through pipelines, the three-way valve I (30) is also connected with a feeding device through a pipeline, and a control valve IV (46) is arranged on the pipeline of the three-way valve I (30) and the feeding device.
6. The intermediate phase arene enriching process for medium and low temperature coal tar includes the following steps:
a: the middle-low temperature coal tar intermediate phase is placed in a first-stage extraction kettle (5) through a conveying system, and the light distillate oil-II in organic components of the middle-low temperature coal tar intermediate phase is removed by adopting a first-stage matched extractant to extract the middle-low temperature coal tar intermediate phase, so that enriched crude aromatic hydrocarbon is obtained;
b: and (3) conveying the second-level extraction agent to a second-level extraction kettle (6) and extracting the mixture to obtain enriched refined aromatic hydrocarbon.
7. The process for enriching aromatic hydrocarbon from the mesophase of low-temperature coal tar according to claim 6, wherein the step a comprises the following steps:
a1 Replacement of residual air in the system by N by a gas compression pump (1) 2 The method comprises the steps of opening a feed liquid valve I (36), metering a medium-low temperature coal tar mesophase and then pumping the medium-low temperature coal tar mesophase into a primary extraction kettle (5), opening a stirring device, adjusting a vent valve III (34) according to a pressure gauge I (22), opening a raw material valve I (28), a feed pump I (2) and a three-way valve III (38), adding a first-stage matched extractant in a raw material tank I (12) into the primary extraction kettle (5), closing the feed pump I (2), opening a gas compression pump (1), a compressed gas three-way valve (37) and a gas interception valve I (39), and ensuring a gas path together with and filling N 2 Starting a magnetocaloric controller I (3), heating the primary extraction kettle (5) to 30-45 ℃, and starting an ultrasonic radiation device to extract for 0.3-0.5h;
a2 The motor I (42) and the ultrasonic radiation device are closed, the gas valve I (32) is opened, the thermal control system is opened to heat the primary extraction kettle (5) to 90-105 ℃ for a certain time, the condenser I (15) is opened, the cooling liquid is conveyed to the alkane buffer tank (22) through the control valve I (21), the liquid in the alkane buffer tank (22) is conveyed to the alkane storage tank (10) for storage by the circulating pump II (8), and the solvent in the alkane storage tank (10) and the first-stage extraction agent in the raw material tank I (12) enter the primary extraction kettle (5) again for secondary extraction;
a3 Repeating the extraction steps for a plurality of times, opening a discharge valve I (26), closing a gas cut-off valve I (39) and a gas valve I (32), and transferring the enriched crude aromatic hydrocarbon into a secondary extraction kettle (6).
8. The process for the mesophase enrichment of aromatic hydrocarbons in medium and low temperature coal tar according to claim 7, wherein the step b comprises the following steps:
b1 Opening a raw material valve II (40), a raw material valve III (41), a feeding pump II (7) and a three-way valve II (30) to ensure that a conveying pipeline is smooth, enabling second-stage extraction agents of a raw material tank II (13) and a raw material tank III (14) to enter a second-stage extraction kettle (6) according to a proportion, sequentially opening a compressed gas three-way valve (37), a gas compression pump (1) and a gas cut-off valve II (45) to ensure gas path communication, and adjusting N in the second-stage extraction kettle (6) according to a pressure gauge II (25) 2 The pressure is 0.1-0.3MPa, then the gas compression pump (1) is closed, the magnetocaloric controller II (4) is started to heat the secondary extraction kettle (6) to 40-55 ℃, and the ultrasonic radiation is started to extract for 0.4-0.6h;
b2 Closing the ultrasonic radiation devices of the motor II (43) and the magnetocaloric controller II (4), opening the gas valve II (33), and heating the secondary extraction kettle (6) to 80-100 ℃;
b3 Opening a gas valve II (33) and a condenser II (16), allowing condensate to enter a phase separation tank (18) after passing through a control valve III (44), separating a second graded extractant and intermediate phase phenol oil after passing through a phase separation, sequentially opening a control valve II (29) and a feed pump II (9), conveying the second graded extractant to a graded solvent storage tank (11), wherein the graded solvent storage tank (11) is provided with an emptying valve II (20), and allowing the second graded extractant in the tank to circulate to a second extraction kettle (6) after passing through a three-way valve I (31);
b4 Repeating the extraction steps for a plurality of times, opening a discharge valve II (27), closing a gas cut-off valve II (45) and a gas valve II (33), and collecting the product enriched refined aromatic hydrocarbon.
9. The process for the mesophase enrichment of aromatic hydrocarbons of low and medium temperature coal tar according to claim 8, further comprising the steps of: c, recovering and re-grading the extraction solvent; step c comprises the following steps:
c1 After step a1 is finished, opening the vent valve III (34) to discharge N 2 The volatile gas is collected and recycled after reaching normal pressure, the circulating solvent enters the circulation through an alkane storage tank (10) and a three-way valve III (38), and the quality of the extraction solution is 95% of that of the previous extraction solvent;
c2 After the step b2 is finished, the phase separation tank (18) is cooled to minus 10 ℃, the second-stage extractant and the light phenol oil are separated, a control valve IV (46) and a three-way valve I (30) are opened, fresh extract is calculated and distributed to enter a raw material tank II (13) and a raw material tank III (14) through the control valve three-way valve I (30), and the extraction ratio of the second-stage extractant to the enriched crude aromatic hydrocarbon is ensured.
10. The intermediate phase aromatic hydrocarbon enrichment process for medium and low temperature coal tar according to claim 8, wherein,
in the step a and the step b, the extraction cycle times are more than or equal to 3;
in step a, the first stage extractant consists of petroleum ether with a boiling range of 30-60 ℃ and petroleum ether with a boiling range of 60-90 ℃ in mass ratio (0.8-1.2): 1, the composition is as follows;
in step b, the second graded extractant consists of methanol and ethanol in a mass ratio of (1.8-2.2): 1.
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| CN202310272158.3A CN116531797A (en) | 2023-03-21 | 2023-03-21 | Equipment and process for enriching aromatic hydrocarbon in intermediate phase of medium-low temperature coal tar |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310272158.3A CN116531797A (en) | 2023-03-21 | 2023-03-21 | Equipment and process for enriching aromatic hydrocarbon in intermediate phase of medium-low temperature coal tar |
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