CN108130121B - Method for recovering extractant from coal-based oil residue extraction residues through vacuum film drying - Google Patents
Method for recovering extractant from coal-based oil residue extraction residues through vacuum film drying Download PDFInfo
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- CN108130121B CN108130121B CN201810001316.0A CN201810001316A CN108130121B CN 108130121 B CN108130121 B CN 108130121B CN 201810001316 A CN201810001316 A CN 201810001316A CN 108130121 B CN108130121 B CN 108130121B
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- 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
- C10G21/28—Recovery of used solvent
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Abstract
The invention relates to a method for recovering an extractant from coal-based oil residue raffinate through vacuum film drying, which comprises the following steps of adding ⑴ asphalt-like oil residue containing wash oil into a primary film drying machine for indirect heating to respectively obtain oil residue and light oil steam with the wash oil content of 5-20%, adding ⑵ oil residue with the wash oil content of 5-20% into a secondary film drying machine for indirect heating to respectively obtain oil residue and heavy oil steam with the wash oil content of 5-0.5%, cooling the light oil steam and injecting the light oil steam to obtain uncondensed steam and a small amount of dust A, cooling ⑶ the oil residue with the wash oil content of 5-0.5% to obtain the oil residue with the temperature of 30-100 ℃, cooling and injecting the heavy oil steam to obtain uncondensed light oil steam and a small amount of dust B, mixing ⑷ the uncondensed light oil steam and the small amount of dust A with the uncondensed steam and the small amount of dust B to form mixed wash oil steam, cooling to obtain condensed wash oil, and cooling the wash oil at the temperature of ⑸ to obtain small investment benefit of the invention.
Description
Technical Field
The invention relates to the technical field of coal chemical industry, in particular to a method for recovering an extracting agent from coal-based oil residue extraction residues by vacuum film drying.
Background
With the increase of the demand of energy and chemical products in China, the coal chemical industry has an important position in the field, and the development of the coal chemical industry has a supplementary effect on relieving the contradiction between supply and demand of high-quality energy such as petroleum, natural gas and the like in China. The coal liquefaction technology is an effective technical approach for solving the contradiction and realizing sustainable energy development in China.
The coal-based oil residue is a solid-liquid mixed residue obtained by carrying out reduced pressure distillation on a coal hydrogenation liquefaction product, and accounts for about 20-30% of the total coal input. The residue contains heavy liquefied oil, asphalt substances and unconverted coal, wherein the content of the heavy oil and the asphalt substances accounts for about 50% of the total oil residue. Usually, the organic solvent extraction method is adopted to recover the part of the oil product. More than 20% of the extraction solvent remains in the oil residue after the extraction and filtration treatment. The part of the extractant is recycled, the usage amount of the extractant can be saved, the oil residue post-treatment cost is reduced, the pollution problem caused by the subsequent process is avoided, and the operability and the economic feasibility of the oil residue extraction separation process can be improved. The general extractant is wash oil, which is an organic solvent with wide boiling range and high boiling point and very complex components.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for recovering an extracting agent in coal-based oil residue raffinate by vacuum film drying, which has the advantages of low investment, easy implementation and high benefit.
In order to solve the problems, the method for recovering the extractant in the coal-based oil residue raffinate by vacuum film drying comprises the following steps:
⑴ adding the asphalt-like oil residue containing washing oil into a primary film dryer through a feeding system I, and introducing heat conducting oil into a central shaft and a shell of the primary film dryer for indirect heating, wherein the light oil component in the oil residue is evaporated under the vacuum condition to respectively obtain oil residue with washing oil content of 5-20% and light oil steam;
⑵ adding the oil residue with washing oil content of 5-20% into a secondary film dryer through a feeding system II, and introducing heat conducting oil into a central shaft and a shell of the secondary film dryer for indirect heating;
the light oil steam is sent to a light oil washing tower through an obliquely arranged pipeline A with a spray function, meanwhile, cooling water A is introduced into the light oil washing tower through a heat exchanger I and a light oil washing pump to cool the light oil steam, a large amount of dust is removed through the injection effect of a Venturi tube in the tower, and uncondensed light oil steam, a small amount of dust A and light oil liquid are obtained respectively; the uncondensed light oil steam and a small amount of dust A enter the spray tower from the bottom of the tower under the suction action of the vacuum pump; pumping the light oil liquid by the light oil washing pump, and cooling the light oil liquid by the heat exchanger I to obtain light oil at the temperature of 30-100 ℃, wherein one part of the light oil at the temperature of 30-100 ℃ is used as the top spray liquid of the light oil washing tower, and the other part of the light oil is sent to the top of the heavy oil washing tower to be used as the spray liquid of the heavy oil washing tower;
⑶, directly discharging the oil residue with the washing oil content of 5-0.5% into an intermediate storage bin, and sending the oil residue into a film cooler through a gas locking valve I, meanwhile, introducing cooling water B into the film cooler to cool the oil residue with the washing oil content of 5-0.5% to obtain the oil residue with the temperature of 30-100 ℃, and discharging the oil residue with the temperature of 30-100 ℃ through a gas locking valve II to enter a subsequent process;
the heavy oil steam is sent to the heavy oil washing tower through an obliquely arranged pipeline B with a spray, meanwhile, cooling water C is introduced into the heavy oil washing tower through a heat exchanger II and a heavy oil washing pump to cool the heavy oil steam, a large amount of dust is removed through the injection effect of a venturi tube in the tower, and uncondensed light oil steam, a small amount of dust B and heavy oil liquid are respectively obtained; the uncondensed light oil steam and a small amount of dust B enter the spray tower from the bottom of the tower under the suction action of the vacuum pump; the heavy oil liquid is pumped out by the heavy oil washing pump and cooled by the heat exchanger II to obtain heavy oil at the temperature of 30-100 ℃, one part of the heavy oil at the temperature of 30-100 ℃ is used as the tower top spray liquid of the heavy oil washing tower, and the other part of the heavy oil is discharged to be used as a washing oil product and sent to a subsequent working section;
⑷ mixing the uncondensed light oil steam and a small amount of dust A with the uncondensed light oil steam and a small amount of dust B in the spray tower to form mixed wash oil steam, simultaneously, cooling water D enters from the top of the spray tower and is directly contacted with the mixed steam to respectively obtain condensed wash oil and non-condensable gas, and the non-condensable gas is evacuated by the vacuum pump;
⑸, pumping the condensed washing oil from the bottom of the spray tower by a spray pump, sending the oil to a heat exchanger III for further cooling to obtain washing oil at the temperature of 30-100 ℃, sending one part of the washing oil at the temperature of 30-100 ℃ to the top of the spray tower to be used as spray liquid, and discharging the other part of the washing oil to be used as a washing oil product and sending the washing oil product to a subsequent working section.
The operation pressure of the primary film dryer is-10 to-90 KPa, and the operation temperature is 120 to 240 ℃.
The operation pressure of the secondary film dryer is-15 to-95 KPa, and the operation temperature is 120 to 270 ℃.
And heating media of the primary film dryer and the secondary film dryer are both steam or heat conduction oil.
The light oil washing tower and the heavy oil washing tower are single-spraying or multi-spraying Venturi injection towers.
The spray tower refers to one of a perforated plate tower, a packed tower or a spray tower.
The heat exchanger I, the heat exchanger II and the heat exchanger III are all spiral plate type heat exchangers or floating head type tube heat exchangers.
: the operation pressure of the light oil washing tower, the heavy oil washing tower and the spray tower is-10 to-95 KPa.
The feeding system I and the feeding system II refer to one or more of a plunger pump, a screw pump or a screw conveyer.
Compared with the prior art, the invention has the following advantages:
1. the material entering the film dryer strengthens heat transfer and mass transfer under the rotating and stirring action of the hot shaft of the dryer, so that the material is easy to dry, volatile matters are easy to volatilize, and the drying time is short.
2. The drying machine and other dynamic equipment adopted by the invention are all operated under negative pressure, so that the leakage of dust and toxic gas is effectively prevented.
3. The dry light steam contains fine dust and high viscosity, and is easy to block the light oil steam conveying pipeline, so that the light oil steam conveying pipeline is obliquely arranged and provided with pipeline spraying, and the blockage of a pipeline is effectively prevented.
4. The thin film dryer adopted by the invention can mix and dry materials to the maximum extent, the heat medium smoothly enters and exits, no dead zone is generated, the stirring and mixing are uniform, the shaft power is low, and the heat efficiency of the dryer is greatly improved.
5. The invention has the advantages of small investment, easy implementation and high benefit.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of the present invention.
In the figure: 1-a feeding system I; 2-first-level film dryer; 3-a feeding system II; 4-second level film dryer; 5-an intermediate storage bin; 6-air locking valve I; 7-film cooler; 8-air locking valve II; 9-light oil wash column; 10-heat exchanger I; 11-light oil wash pump; 12-a heavy oil wash column; 13-heat exchanger II; 14-heavy oil washing pump; 15-a vacuum pump; 16-heat exchanger iii; 17-a spray tower; 18-spray pump.
Detailed Description
As shown in fig. 1, a method for recovering an extractant from coal-based oil residue raffinate by vacuum membrane drying comprises the following steps:
⑴ the asphalt-like oil residue containing washing oil is added into the primary film dryer 2 through the feeding system I1, meanwhile, heat conducting oil is introduced into the central shaft and the shell of the primary film dryer 2 for indirect heating, and light oil components in the oil residue are evaporated under the condition that the vacuum degree is-60 KPa, so that the oil residue and light oil steam with the washing oil content of 5% -20% are obtained respectively.
Wherein: the operation pressure of the primary film dryer 2 (patent number: 201420010597.3) is-10 to-90 KPa, the operation temperature is 120 to 240 ℃, and the heating medium is steam or heat conducting oil.
The feeding system I1 refers to one or more of a plunger pump, a screw pump or a screw conveyer.
⑵ oil residue with washing oil content of 5-20% is added into a secondary film dryer 4 through a feeding system II 3, meanwhile, heat conducting oil is introduced into a central shaft and a shell of the secondary film dryer 4 for indirect heating, heavy oil components in the oil residue are evaporated under the condition that the vacuum degree is-60 KPa, and oil residue with washing oil content of 5-0.5% and heavy oil steam are respectively obtained, wherein the operating pressure of the secondary film dryer 4 (patent number: 201420010597.3) is-15 to-95 KPa, the operating temperature is 120-270 ℃, and a heating medium is steam or heat conducting oil, and the feeding system II 3 refers to one or more of a plunger pump, a screw pump or a screw conveyor.
The light oil steam is sent to a light oil washing tower 9 through an obliquely arranged pipeline A with a spray, meanwhile, cooling water A is introduced into the light oil washing tower 9 through a heat exchanger I10 and a light oil washing pump 11 to cool the light oil steam, a large amount of dust is removed through the injection effect of a Venturi tube in the tower, and uncondensed light oil steam, a small amount of dust A and light oil liquid are respectively obtained; the uncondensed light oil steam and a small amount of dust A enter the spray tower 17 from the bottom of the tower under the suction action of the vacuum pump 15; and pumping the light oil liquid by a light oil washing pump 11, cooling the light oil liquid by a heat exchanger I10 to obtain light oil with the temperature of 30-100 ℃, wherein one part of the light oil with the temperature of 30-100 ℃ is used as the top spray liquid of the light oil washing tower 9, and the other part of the light oil is sent to the top of the heavy oil washing tower 12 to be used as the spray liquid of the heavy oil washing tower 12.
⑶ the oil residue with washing oil content of 5-0.5% is directly discharged into the intermediate storage bin 5 and sent into the film cooling machine 7 through the air locking valve I6, meanwhile, cooling water B is introduced into the film cooling machine 7 to cool the oil residue with washing oil content of 5-0.5% to obtain the oil residue with the temperature of 30-100 ℃, and the oil residue with the temperature of 30-100 ℃ is discharged through the air locking valve II 8 to enter the subsequent process, wherein the film cooling machine 7 (patent number: 201420010597.3).
Heavy oil steam is sent to a heavy oil washing tower 12 through an obliquely arranged pipeline B with a spray, meanwhile, cooling water C is introduced into the heavy oil washing tower 12 through a heat exchanger II 13 and a heavy oil washing pump 14 to cool the heavy oil steam, a large amount of dust is removed through the injection effect of a venturi tube in the tower, and uncondensed light oil steam, a small amount of dust B and heavy oil liquid are respectively obtained; the uncondensed light oil steam and a small amount of dust B enter the spray tower 17 from the bottom of the tower under the suction action of the vacuum pump 15; and pumping the heavy oil liquid by a heavy oil washing pump 14, cooling by a heat exchanger II 13 to obtain the heavy oil with the temperature of 30-100 ℃, wherein one part of the heavy oil with the temperature of 30-100 ℃ is used as the tower top spray liquid of the heavy oil washing tower 12, and the other part is discharged as a washing oil product and sent to a subsequent working section.
⑷ mixing the uncondensed light oil steam and a small amount of dust A with the uncondensed light oil steam and a small amount of dust B in the spray tower 17 to form mixed washing oil steam, simultaneously, cooling water D enters from the top of the spray tower 17 and is directly contacted with the mixed steam to respectively obtain condensed washing oil and non-condensable gas, and the non-condensable gas is evacuated by the vacuum pump 15;
⑸, pumping the condensed washing oil from the bottom of the spray tower 17 by a spray pump 18, sending the oil to a heat exchanger III 16 for further cooling to obtain washing oil at 30-100 ℃, wherein one part of the washing oil at 30-100 ℃ is sent to the top of the spray tower 17 to be used as spray liquid, and the other part is discharged to be used as a washing oil product and sent to a subsequent working section.
In the invention, the light oil washing tower 9 and the heavy oil washing tower 12 are both single-spray or multi-spray Venturi injection towers.
The spray tower 17 refers to one of a perforated plate tower, a packed tower or a spray tower.
The operation pressure of the light oil washing tower 9, the heavy oil washing tower 12 and the spray tower 17 is-10 to-95 KPa.
The heat exchanger I10, the heat exchanger II 13 and the heat exchanger III 16 are all spiral plate type heat exchangers or floating head type tube heat exchangers.
Claims (9)
1. A method for recovering an extractant from coal-based oil residue raffinate by vacuum film drying comprises the following steps:
⑴ adding the asphalt-like oil residue containing washing oil into a primary film dryer (2) through a feeding system I (1), and simultaneously introducing heat conducting oil into a central shaft and a shell of the primary film dryer (2) for indirect heating, evaporating light oil components in the oil residue under the vacuum condition to respectively obtain the oil residue with the washing oil content of 5-20% and light oil steam;
⑵ adding the oil residue with washing oil content of 5-20% into a secondary film dryer (4) through a feeding system II (3), and simultaneously introducing heat conduction oil into a central shaft and a shell of the secondary film dryer (4) for indirect heating, evaporating heavy oil components in the oil residue under a vacuum condition to respectively obtain the oil residue with washing oil content of 5-0.5% and heavy oil steam;
the light oil steam is sent to a light oil washing tower (9) through an obliquely arranged pipeline A with a spray, meanwhile, cooling water A is introduced into the light oil washing tower (9) through a heat exchanger I (10) and a light oil washing pump (11) to cool the light oil steam, a large amount of dust is removed through the injection effect of a Venturi tube in the tower, and uncondensed light oil steam, a small amount of dust A and light oil liquid are respectively obtained; the uncondensed light oil steam and a small amount of dust A enter a spray tower (17) from the bottom of the tower under the suction action of a vacuum pump (15); the light oil liquid is pumped out by the light oil washing pump (11) and cooled by the heat exchanger I (10) to obtain light oil with the temperature of 30-100 ℃, one part of the light oil with the temperature of 30-100 ℃ is used as the top spray liquid of the light oil washing tower (9), and the other part of the light oil is sent to the top of the heavy oil washing tower (12) to be used as the spray liquid of the heavy oil washing tower (12);
⑶, directly discharging the oil residue with the washing oil content of 5-0.5% into an intermediate storage bin (5), and sending the oil residue into a film cooler (7) through an air locking valve I (6), meanwhile, introducing cooling water B into the film cooler (7) to cool the oil residue with the washing oil content of 5-0.5% to obtain the oil residue with the temperature of 30-100 ℃, and discharging the oil residue with the temperature of 30-100 ℃ through an air locking valve II (8) to enter a subsequent process;
the heavy oil steam is sent to the heavy oil washing tower (12) through an obliquely arranged pipeline B with a spray, meanwhile, cooling water C is introduced into the heavy oil washing tower (12) through a heat exchanger II (13) and a heavy oil washing pump (14) to cool the heavy oil steam, a large amount of dust is removed through the injection effect of a venturi tube in the tower, and uncondensed light oil steam, a small amount of dust B and heavy oil liquid are respectively obtained; the uncondensed light oil steam and a small amount of dust B enter a spray tower (17) from the bottom of the tower under the suction action of the vacuum pump (15); the heavy oil liquid is pumped out by the heavy oil washing pump (14) and cooled by the heat exchanger II (13), so that heavy oil with the temperature of 30-100 ℃ is obtained, one part of the heavy oil with the temperature of 30-100 ℃ is used as the tower top spray liquid of the heavy oil washing tower (12), and the other part of the heavy oil is discharged to be used as a washing oil product and sent to a subsequent working section;
⑷ mixing the uncondensed light oil steam and a small amount of dust A with the uncondensed light oil steam and a small amount of dust B in the spray tower (17) to form mixed washing oil steam, simultaneously, cooling water D enters from the top of the spray tower (17) and is directly contacted with the mixed washing oil steam to respectively obtain condensed washing oil and non-condensable gas, wherein the non-condensable gas is evacuated by the vacuum pump (15);
⑸, pumping the condensed washing oil from the bottom of the spray tower (17) by a spray pump (18), sending the condensed washing oil to a heat exchanger III (16) for further cooling to obtain washing oil at 30-100 ℃, wherein one part of the washing oil at 30-100 ℃ is sent to the top of the spray tower (17) to be used as spray liquid, and the other part is discharged to be used as a washing oil product and sent to a subsequent working section.
2. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the operation pressure of the primary film dryer (2) is-10 to-90 KPa, and the operation temperature is 120 to 240 ℃.
3. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the operation pressure of the secondary film dryer (4) is-15 to-95 KPa, and the operation temperature is 120 to 270 ℃.
4. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: and heating media of the primary film dryer (2) and the secondary film dryer (4) are both steam or heat conduction oil.
5. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the light oil washing tower (9) and the heavy oil washing tower (12) are single-spray or multi-spray Venturi injection towers.
6. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the spray tower (17) refers to one of a perforated plate tower, a packed tower or a spray tower.
7. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the heat exchanger I (10), the heat exchanger II (13) and the heat exchanger III (16) are both spiral plate type heat exchangers or floating head type tube heat exchangers.
8. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the operation pressure of the light oil washing tower (9), the operation pressure of the heavy oil washing tower (12) and the operation pressure of the spraying tower (17) are all-10 to-95 KPa.
9. The method for recovering the extractant in the coal-based oil residue raffinate through vacuum film drying as claimed in claim 1, wherein the method comprises the following steps: the feeding system I (1) and the feeding system II (3) refer to one or more of a plunger pump, a screw pump or a screw conveyer.
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| CN1314788C (en) * | 2002-10-24 | 2007-05-09 | 皇冠制铁公司 | Two stage device for removing solvent from food granular powder |
| CN103242881B (en) * | 2013-05-30 | 2015-08-12 | 神华集团有限责任公司 | The method of separate bitumen class material from coal directly-liquefied residue |
| CN104560121B (en) * | 2013-10-10 | 2016-09-21 | 天华化工机械及自动化研究设计院有限公司 | The recovery method of extractant and equipment in coal base oil slag extraction leftover |
| CN205925038U (en) * | 2016-08-19 | 2017-02-08 | 河南省亚临界生物技术有限公司 | Continuous vaporization system of subcritical extract |
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