CN1276059C - Process for producing chemical industry products and fuel oil from coal tar - Google Patents
Process for producing chemical industry products and fuel oil from coal tar Download PDFInfo
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- CN1276059C CN1276059C CN 200410012455 CN200410012455A CN1276059C CN 1276059 C CN1276059 C CN 1276059C CN 200410012455 CN200410012455 CN 200410012455 CN 200410012455 A CN200410012455 A CN 200410012455A CN 1276059 C CN1276059 C CN 1276059C
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Abstract
The present invention relates to a method of producing chemical products and fuel oil from coal tar, which belongs to the field of the processing and the use of coal tar. The present invention relates to the method of producing chemical products and fuel oil including vehicle fuel oil from coal tar, and is characterized in that the coal tar is fractionated into a light fraction and a heavy fraction, wherein the light fraction is light coal tar and tar pitch, and is produced into light products by hydrofining or upgrading; if the processing technique of tar asphalt is combined with a coke oven or with delayed coking, more chemical products of phenol, naphthalene and gasoline, diesel oil or light fuel oil, etc. can be produced, and the quality of coke in the coke oven can be improved, or coke with less ashes can be directly produced; if an inhibitor is added simultaneously, coking in a furnace tube or a reactor is inhibited or alleviated so as to ensure that devices can run for long cycles.
Description
One, technical field
The present invention belongs to the processing and utilization field of coal tar from the method for coal tar production chemicals and oil fuel, and it relates to from coal tar production chemical product and oil fuel, comprises the method for vehicle fuel oil.
Two, technical background
The processing of coal tar, the past mainly concentrates on production chemical product aspect, as it being divided into several close-cut fractions and tar-bitumens such as light oil, carbolic oil, naphtalene oil, washing oil, carbolineum by distillation.From different close-cut fractions, isolate thick chemicals or smart chemicals then, industrialized kind reaches more than 100, along with petroleum resources face exhaustion, and the increase of diesel oil demand, produce each fuel oils, particularly diesel oil by coal tar and be subjected to great attention again.Currently, account for the utilization that coal tar is formed the heavy bitumen more than 50%, also be in the development phase, it is important key for the processing economy of coal tar.
Number of patent application 02122573.7 uses hydrofining or modification technology carries out hydrogenation production petroleum naphtha and diesel oil to lightweight coal tar (＜350 ℃).Then need adopt suspension bed hydrogenation process to the full fraction hydrogenating of coal tar, China does not still have the industrialization practice at present.Publication CN1351130A has proposed the method that a kind of coal tar is produced diesel oil, and it mainly is that lightweight coal tar is carried out hydrofining, is the raising diesel cetane-number, after the hydrofining, again through dearomatization catalyst, to reduce aromaticity content in the product.CN1012503B has proposed the heavy bitumen of coal tar is carried out the hydrogenation method of coking production needle coke more after treatment.
Three, summary of the invention
The present invention produces the method for chemicals and oil fuel from coal tar, it is raw material with coal tar that its purpose is to disclose a kind of, hydrofining technology, coke making process or delay coking process are made up, and cooperate to add a kind of production chemicals of the green coke inhibitor that prevents furnace tubing and reactor bed carbon deposit and the method for oil fuel.
A kind of method of producing chemicals and oil fuel from coal tar of the present invention, it is characterized in that, with low temperature, middle gentle coal-tar heavy oil and from them extraction unit divide residue blending fraction oil behind the chemical industry raw material, comprise that light, heavy coal tar is raw material, hydrofining technology and delay coking process are made up, and cooperate to add the method that a kind of production chemicals phenol, naphthalene and oil fuel that prevents the green coke inhibitor of furnace tubing and reactor bed carbon deposit comprises solvent oil, diesel oil or light-weight fuel oil;
Its concrete processing step method is:
I, feed coal tar is told less than 360 ℃ lightweight coal tar with greater than 360 ℃ tar-bitumen through distillation, cut 170～210 ℃ and 210～230 ℃ of two fractions in the coal tar on the lenient side simultaneously, go manufacture phenol and NAPTHALENE FLAKES. (INDUSTRIAL GRADE respectively;
II, will produce phenol and the remaining fraction of naphthalene, the tar light oil that other tar light oil and delayed coking generate mixes as hydrorefined raw material, its Hydrobon catalyst is molybdenum, nickel, phosphorus type or tungsten nickel type, carrier is aluminum oxide or aluminum oxide and titanium dioxide composition, hydrogenator is typical trickle-bed reactor, and catalyzer adopts classification filling technology, and reactor operating pressure is 8.0～12Mpa, temperature of reaction is 350～380 ℃, and volume space velocity is 0.5～1.2h
-1, hydrogen to oil volume ratio is 800～1500, above-mentioned raw materials obtains solvent oil, diesel oil or light-weight fuel oil through hydrofining;
III, be benchmark with the weight percent, the coal-tar middle oil pitch ash oontent of above-mentioned I is 0.5～1.0%, volatile matter is up to more than 50%, tar-bitumen is as the raw material of delayed coking, at temperature of reaction 450-550 ℃, the residence time is 8～24h, produces more tar light oils and high grade coke through cracking and polycondensation;
Add a kind of in IV, the fraction that behind coal tar hydrogenating, generates in order to prevent process furnace and beds carbon deposit, obstruction, the generation of energy good restraining free radical, can make the green coke inhibitor of device long period safe operation, the effective ingredient of this inhibitor is: naphthane 0.4～4%, perhydronaphthalene 0.3～3%, dihydroanthracene 1.3～8%, with the weight percent is that benchmark their content in hydrogenated oil is 2～15%, the injection rate that with the weight percent is this inhibitor of benchmark is 5～30%, and the stock oil temperature when injecting this green coke inhibitor is 180～360 ℃.
Further specify the present invention below in conjunction with accompanying drawing:
Figure-1 is hydrofining and coking combinations produce purpose goods batch figure.Atmospheric distillation plant 1 is made up of one or more towers among the figure.Feed coal tar is divided into less than 170 ℃ of fractions, 170～210 ℃, 210～230 ℃ other fractions that reach less than 360 ℃, tells tar-bitumen at the bottom of the tower.Wherein 170～210 ℃ and 210～230 ℃ of fractions reclaim phenol and naphthalene respectively in equipment 2,3, and the residue fraction and other fraction oil that reclaim behind phenol and the naphthalene are mixed into fixed bed hydrogenation reactor 4.The catalyzer of hydrofining or upgrading is housed in the reactor, under hydrogen pressure and certain temperature, it is saturated to carry out hydrogenating desulfurization, denitrogenation, alkene, and aromatic hydrocarbons fractional saturation and remove reaction such as part colloid makes oil product decolouring, deodorization or part cracking generate the lower generation oil of boiling point.This generation oil just can obtain the light-weight fuel oil of solvent oil or all size or vapour, diesel oil on demand through normal pressure distillation 5 again.
Figure-2 hydrofinings and delayed coking combinations produce purpose goods batch figure are further with more light fraction of tar-bitumen processing and useful coke, to increase economic efficiency on the basis of figure-1.The hydrogenation of figure in-2 and naphthalene recovery etc. with scheme-1 identically, repeat no more for this reason.Figure-2 increases by a cover delayed coking unit 6 on flow process, replaced the pit kiln among the figure-1.Enter coke drum from atmospheric unit 1 effusive pitch after the tubular oven heating and react, cracking and polycondensation take place at this in pitch, generate low molecular dry gas, tar light oil, heavy tar and coke.Its pyrogenic reaction conditions is pressure 0.15～0.2Mpa, and 490～510 ℃ of furnace outlet temperature make the whole or overwhelming majority circulation of tar heavy oil (＞360 ℃), reduce the output of tar heavy oil as far as possible.The yield of tar light oil accounts for 40～50% of charging, and coking yield is 30～50%, and dry gas accounts for 8～12%.The tar light oil that generates is unsettled thick product, and it will enter the chemical utilization of hydrogenation unit coal tar in the lump with the lightweight coal tar mixing of atmospheric distillation plant 1 and the production of oil fuel combines, and reaches the optimizing utilization of each component.Combine with producing diesel oil as from coal tar, producing phenol and naphthalene etc., both obtained the phenol of high added value and naphthalene etc., can significantly improve the cetane value of hydrogenated diesel oil again.
Four, description of drawings: figure-1 hydrofining and coking combinations produce purpose goods batch figure
Label among the figure is respectively:
1 atmospheric distillation plant, 2 phenol recovery systems, 3 naphthalene recovery systems
4 hydro-refining units, 5 product distillation plants, 6 pit kiln
7 variable-pressure adsorption equipments, 8 thick solvent oil 9 carbolic oil
10 technical phenols, 11 naphtalene oils, 12 NAPTHALENE FLAKES. (INDUSTRIAL GRADE
13 washing oil, 14 hydrogenated oils, 15 solvent oils
16 diesel oil (thin fuel oil), 17 coking coal, 18 tar-bitumens
19 coal tar, 20 coke, 21 coke(oven)gas
22 hydrogen
Figure-2 hydrofinings and delayed coking combinations produce purpose goods batch figure
Label among the figure is respectively:
1 atmospheric distillation plant, 2 phenol recovery systems, 3 naphthalene recovery systems
4 hydro-refining units, 5 product distillation plants, 6 delayed coking units
7 variable-pressure adsorption equipments, 8 thick solvent oil 9 carbolic oil
10 technical phenols, 11 naphtalene oils, 12 NAPTHALENE FLAKES. (INDUSTRIAL GRADE
13 washing oil, 14 hydrogenated oils, 15 solvent oils
16 diesel oil (thin fuel oil), 17 coal tar, 18 tar-bitumens
19 tar light oils, 20 coke, 21 coke(oven)gas
22 hydrogen
Five, embodiment
Embodiment one:
I, feed coal tar is told less than 360 ℃ lightweight coal tar with greater than 360 ℃ tar-bitumen through distillation, cut 170～210 ℃ and 210～230 ℃ of two fractions in the coal tar on the lenient side simultaneously, go manufacture phenol and NAPTHALENE FLAKES. (INDUSTRIAL GRADE respectively;
II, will produce phenol and the remaining fraction of naphthalene, the tar light oil that other tar light oil and delayed coking generate mixes as hydrorefined raw material, its Hydrobon catalyst is molybdenum, Nie, Ling type or tungsten nickel type, carrier is aluminum oxide or aluminum oxide and titanium dioxide composition, hydrogenator is typical trickle-bed reactor, and catalyzer adopts classification filling technology, and reactor operating pressure is 8.0Mpa, temperature of reaction is 350 ℃, and volume space velocity is 0.5h
-1, hydrogen to oil volume ratio is 800～1500, above-mentioned raw materials obtains solvent oil, diesel oil or light-weight fuel oil through hydrofining;
The coal-tar middle oil pitch ash oontent of III, above-mentioned I is 0.5%, and volatile matter is up to more than 50%, and tar-bitumen can also be as the raw material of delayed coking, and 450 ℃ of temperature of reaction, the residence time is 8h, produces more tar light oils and high grade coke through cracking and polycondensation;
Add a kind of in IV, the fraction that behind coal tar hydrogenating, generates in order to prevent process furnace and beds carbon deposit, obstruction, the generation of energy good restraining free radical, can make the green coke inhibitor of device long period safe operation, this inhibitor be present in present method described as: its effective ingredient mainly is: naphthane 0.4%, perhydronaphthalene 0.3%, dihydroanthracene 1.3%, their content is 2% in hydrogenated oil, the injection rate of this inhibitor is 5%, 180 ℃ of temperature.
Experiment sees Table-1 with coal tar character.Through distillation cut＜360 ℃ of fractions go hydrofining, the pitch that fractionates out (＞360 ℃) loops back pit kiln.For investigating the testing apparatus of the ad hoc meter one cover simulation process of coking of the variation of this pitch under the coking condition, to get the above-mentioned pitch of 1000g and under the coking condition, carry out coking test, it the results are shown in Table-2.
Table-1 coal tar character
| Boiling range scope ℃ | Yield % |
| ＜170 170～210 210～230 230～300 300～330 330～360 ＞360 | 0.7 2.4 10.8 6.4 16.3 5.3 58.1 |
Table-2 pitch coking test-results
| Reaction conditions | Pressure Mpa temperature ℃ reaction times h | 0.12 500 8 |
| Product distribution % | | 9 34 57 |
The generation tar density of above-mentioned test-results is 0.994g/cm
3, yield is 34%.Coke ash is 0.6%.
Embodiment two:
I, feed coal tar is told less than 360 ℃ lightweight coal tar with greater than 360 ℃ tar-bitumen through distillation, cut 210 ℃ and 230 ℃ of two fractions in the coal tar on the lenient side simultaneously, go manufacture phenol and NAPTHALENE FLAKES. (INDUSTRIAL GRADE respectively;
II, will produce phenol and the remaining fraction of naphthalene, the tar light oil that other tar light oil and delayed coking generate mixes as hydrorefined raw material, its Hydrobon catalyst is molybdenum, Nie, Ling type or tungsten nickel type, carrier is aluminum oxide or aluminum oxide and titanium dioxide composition, hydrogenator is typical trickle-bed reactor, and catalyzer adopts classification filling technology, and reactor operating pressure is 12Mpa, temperature of reaction is 380 ℃, and volume space velocity is 1.2h
-1, hydrogen to oil volume ratio is 1500, above-mentioned raw materials obtains solvent oil, diesel oil or light-weight fuel oil through hydrofining;
The coal-tar middle oil pitch ash oontent of III, above-mentioned I is 1.0%, and volatile matter is up to more than 50%, and tar-bitumen can also be as the raw material of delayed coking, and 550 ℃ of temperature of reaction, the residence time is 24h, produces more tar light oils and high grade coke through cracking and polycondensation;
Add a kind of in IV, the fraction that behind coal tar hydrogenating, generates in order to prevent process furnace and beds carbon deposit, obstruction, the generation of energy good restraining free radical, can make the green coke inhibitor of device long period safe operation, this inhibitor be present in present method described as: its effective ingredient mainly is: naphthane 4%, perhydronaphthalene 3%, dihydroanthracene 8%, their content is 15% in hydrogenated oil, the injection rate of this inhibitor is 30%, 360 ℃ of temperature.
Test coal tar character sees Table-1, and cuts that remaining blending fraction is a raw material behind 230 ℃ of fractions, is mimic diagram-2 boiling range, make coal tar＜360 ℃ generate oil with delayed coking and go hydrofining in the lump.Coal tar＞360 a ℃ fraction goes delayed coking, and test-results sees Table-3, and the solvent oil, the diesel oil main character that generate through hydrogenation see Table-4.
Table-3 hydrogenation and delayed coking test-results
| Hydropyrolysis experiment | The delayed coking test |
| Test conditions | Pressure Mpa temperature ℃ air speed h -1Hydrogen/oily V circulation | 8.0 370 1.0 1000 | 0.12 500＞360 ℃ of recycle to extinctions |
| Product distributes *％ | Gas generates oil and generates the water coke | 1.6 98.6 2.4 | 12 40 48 |
*Product distributes and all is as the criterion with charging separately
The main character of table-4 products
| Solvent oil | Diesel oil | |
| Boiling range scope ℃ density g/cm 3Sulphur content μ g/g nitrogen content μ g/g octane value RON cetane value condensation point ℃ | ＜180 0.7450 80 41 76 | 180～360 0.8428 320 68 44 -6 |
Embodiment three:
I, feed coal tar is told less than 360 ℃ lightweight coal tar with greater than 360 ℃ tar-bitumen through distillation, cut 170～210 ℃ and 210～230 ℃ of two fractions in the coal tar on the lenient side simultaneously, go manufacture phenol and NAPTHALENE FLAKES. (INDUSTRIAL GRADE respectively;
II, will produce phenol and the remaining fraction of naphthalene, the tar light oil that other tar light oil and delayed coking generate mixes as hydrorefined raw material, its Hydrobon catalyst is molybdenum, Nie, Ling type or tungsten nickel type, carrier is aluminum oxide or aluminum oxide and titanium dioxide composition, hydrogenator is typical trickle-bed reactor, and catalyzer adopts classification filling technology, and reactor operating pressure is 10Mpa, temperature of reaction is 360 ℃, and volume space velocity is 0.9h
-1, hydrogen to oil volume ratio is 1000, above-mentioned raw materials obtains solvent oil, diesel oil or light-weight fuel oil through hydrofining;
The coal-tar middle oil pitch ash oontent of III, above-mentioned I is 0.8%, and volatile matter is up to more than 50%, and tar-bitumen can also be as the raw material of delayed coking, and 500 ℃ of temperature of reaction, the residence time is 16h, produces more tar light oils and high grade coke through cracking and polycondensation;
Add a kind of in IV, the fraction that behind coal tar hydrogenating, generates in order to prevent process furnace and beds carbon deposit, obstruction, the generation of energy good restraining free radical, can make the green coke inhibitor of device long period safe operation, this inhibitor be present in present method described as: its effective ingredient mainly is: naphthane 3%, perhydronaphthalene 2%, dihydroanthracene 7%, their content is 12% in hydrogenated oil, the injection rate of this inhibitor is 20%, 260 ℃ of temperature.
For verifying the effect of green coke inhibitor of the present invention, the spy does following test, does reactor with 14 * 2mm stainless steel tube, and 60 order aluminium sesquioxides are adorned in the electrically heated of external application tile in the device.To show coal tar injecting reactor in-1 with pump, and measure bed layer pressure and fall, stop test when reaching 0.3Mpa when pressure falls.With the coke forming property that adds and do not add above-mentioned inhibitor of how much passing judgment on of oil inlet quantity, it is defined as:
The oil inlet quantity of the oil inlet quantity/inhibiting of inhibiting of coke forming property=not
Obviously should be worth less than 1, the more little expression coke forming property of numeral is low more, and it is good more to suppress effect.The green coke inhibitor is a certain fraction in the hydrogenated oil of the present invention.Test-results sees Table-5, as can be seen when add this inhibitor account for raw material 10% the time can reach uniform pressure and fall the time, can increase treatment capacity 35%.When adding 30%, the treatment capacity that can double almost.
The test of table-5 inhibitor
| Test conditions | Pressure MPa temperature ℃ air speed h -1Hydrogen/oily V allows pressure reduction MPa | Normal pressure 370 1.0 1,000 0.3 | |||
| Inhibitor add-on % coke forming property | 0 1 | 10 0.74 | 20 0.62 | 30 0.48 | |
Claims (1)
1. method of producing chemicals and oil fuel from coal tar, it is characterized in that, with low temperature, middle gentle coal-tar heavy oil and from them extraction unit divide residue blending fraction oil behind the chemical industry raw material, comprise that light, heavy coal tar is raw material, hydrofining technology and delay coking process are made up, and cooperate to add the method that a kind of production chemicals phenol, naphthalene and oil fuel that prevents the green coke inhibitor of furnace tubing and reactor bed carbon deposit comprises solvent oil, diesel oil or light-weight fuel oil;
Its concrete processing step method is:
I, feed coal tar is told less than 360 ℃ lightweight coal tar with greater than 360 ℃ tar-bitumen through distillation, cut 170～210 ℃ and 210～230 ℃ of two fractions in the coal tar on the lenient side simultaneously, go manufacture phenol and NAPTHALENE FLAKES. (INDUSTRIAL GRADE respectively;
II, will produce phenol and the remaining fraction of naphthalene, the tar light oil that other tar light oil and delayed coking generate mixes as hydrorefined raw material, its Hydrobon catalyst is molybdenum, nickel, phosphorus type or tungsten nickel type, carrier is aluminum oxide or aluminum oxide and titanium dioxide composition, hydrogenator is typical trickle-bed reactor, and catalyzer adopts classification filling technology, and reactor operating pressure is 8.0～12Mpa, temperature of reaction is 350～380 ℃, and volume space velocity is 0.5～1.2h
-1, hydrogen to oil volume ratio is 800～1500, above-mentioned raw materials obtains solvent oil, diesel oil or light-weight fuel oil through hydrofining;
III, be benchmark with the weight percent, the coal-tar middle oil pitch ash oontent of above-mentioned I is 0.5～1.0%, volatile matter is up to more than 50%, tar-bitumen is as the raw material of delayed coking, at temperature of reaction 450-550 ℃, the residence time is 8～24h, produces more tar light oils and high grade coke through cracking and polycondensation;
Add a kind of in IV, the fraction that behind coal tar hydrogenating, generates in order to prevent process furnace and beds carbon deposit, obstruction, the generation of energy good restraining free radical, can make the green coke inhibitor of device long period safe operation, the effective ingredient of this inhibitor is: naphthane 0.4～4%, perhydronaphthalene 0.3～3%, dihydroanthracene 1.3～8%, with the weight percent is that benchmark their content in hydrogenated oil is 2～15%, the injection rate that with the weight percent is this inhibitor of benchmark is 5～30%, and the stock oil temperature when injecting this green coke inhibitor is 180～360 ℃.
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Cited By (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747925A (en) * | 2009-12-26 | 2010-06-23 | 何巨堂 | Method for coking heavy oil of coal tar |
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