CN101250433A - Coal tar hydrogenation technique - Google Patents
Coal tar hydrogenation technique Download PDFInfo
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- CN101250433A CN101250433A CNA2008100309541A CN200810030954A CN101250433A CN 101250433 A CN101250433 A CN 101250433A CN A2008100309541 A CNA2008100309541 A CN A2008100309541A CN 200810030954 A CN200810030954 A CN 200810030954A CN 101250433 A CN101250433 A CN 101250433A
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- coal tar
- hydrogenation
- reaction
- bed reactor
- oil
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- 239000011280 coal tar Substances 0.000 title claims abstract description 71
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title abstract description 22
- 239000003921 oil Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000010771 distillate fuel oil Substances 0.000 claims abstract description 5
- 239000003502 gasoline Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000571 coke Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000003112 inhibitor Substances 0.000 claims description 7
- 239000002283 diesel fuel Substances 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000004939 coking Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- 239000000295 fuel oil Substances 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000000084 colloidal system Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000011269 tar Substances 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000010426 asphalt Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LOTCVJJDZFMQGB-UHFFFAOYSA-N [N].[O].[S] Chemical compound [N].[O].[S] LOTCVJJDZFMQGB-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 239000003974 emollient agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- -1 vapour Substances 0.000 description 1
Abstract
The invention discloses a coal tar hydrogenation technique, which comprises the following steps: getting coal tar hydrogenation feed after preprocessing coal tar, the coal tar hydrogenation feed which is got gets into a hydrogenation fixed bed reactor from the upper side to the down side, and the hydrogenation reaction oil which is got gets into a main hydrogenation fixed bed reactor from the upper side to the down side, the main hydrogenation reaction oil which is got gets into a fractionating system, and getting gasoline fraction, diesel fraction and light fuel oil fraction. The coal tar hydrogenation technique adopts an up-flow hydrogenation fixed bed reactor to be connected in series with a down-flow main hydrogenation fixed bed reactor, which changes a material flow direction in the technique, increases the retention time of response logistics on catalyst bed layers, can effectively inhibit or release the coking reaction of coal tar under high temperature, and prolongs the process of continuous operating cycle of the coal tar hydrogenation device.
Description
One, technical field
The invention belongs to the fuel chemical field, be specifically related to a kind of coal tar hydrogenation process.
Two, technical background
As everyone knows, utilize hydrogenation technique can effectively remove impurity such as sulphur nitrogen oxygen very high in the low grade coal tar, and can significantly reduce its density, realize lighting, produce qualified light-end products and oil fuel with this.But because coal tar is very complexity of a kind of composition, the raw material that character is very poor, the hydrogenation process of coal tar is again a pyroprocess simultaneously, unsaturated compound in the coal tar raw material, comprise diolefine, alkene, condensed-nuclei aromatics, the polymer nitride, colloid, bituminous matter at high temperature very easily with coal tar in contained free oxygen complicated polyreaction takes place, generate high polymer, this high polymer is long-pending more big more, adds some solid inorganic salts in the coal tar, carbon residue, metals etc. will be at the interchanger of coal tar hydrogenating unit, process furnace, equipment and the interior coking materials that form complexity of pipeline such as reactor.This coking material structure is tight, adhere firmly, heat exchange efficiency, heat transmission and the material transmission of various device have been had a strong impact on, very easily cause equipment and pipeline to stop up when serious, cause the hydrogenation unit cycle of operation too short, the economic benefit of restriction coal tar hydrogenating and the industrialization promotion of coal tar hydrogenating.
The coal tar hydrogenating technology generally adopts conventional downflow system hydrogenation fixed-bed reactor to carry out the hydro-upgrading of coal tar.Chinese patent CN1147575c cuts into the weight cut with coal tar raw material, utilizes lighting end wherein to be hydrogenating materials, adopts conventional downflow system hydrogenation fixed-bed reactor to carry out hydrofining, obtains the petrol and diesel oil product; It is raw material that Chinese patent CN200510028167.X adopts high temperature, the full cut of middle coalite tar, after pre-treatment such as dehydration, off line tool impurity, adopt the downflow system hydrogenation fixed-bed reactor of one section or two sections routine to carry out the hydrofining of coal tar raw material, obtain light-weight fuel oils such as vapour, diesel oil.These two patents all adopt conventional downflow system hydrogenation fixed-bed reactor, be that coal tar raw material and hydrogen mixture stream passes through reactor from top to bottom, its at high temperature since the high molecular polymer that polyreaction generates very easily attached to become greatly on the beds and gradually, long-pending more thick more, thereby hinder Flow of Goods and Materials, cause reactor pressure decrease to rise, quality product descends and reactor plugs.
Three, summary of the invention
The object of the present invention is to provide a kind of coking reaction that can effectively suppress in the coal tar hydrogenating process, realize the coal tar hydrogenation process of the continuous long-term operation of coal tar hydrogenating unit.
The objective of the invention is to be achieved through the following technical solutions: a kind of coal tar hydrogenation process is characterized in that comprising the steps: that 1. coal tar carries out obtaining the coal tar hydrogenating charging after the pre-treatment; 2. the charging of gained coal tar hydrogenating mixes with hydrogen, enters the pre-hydrogenation fixed-bed reactor of upflowing generation pre-hydrotreating reaction from bottom to top, and its operational condition is: 170~300 ℃ of temperature of reaction, reaction pressure 7.0~18.0Mpa, liquid hourly space velocity 0.8~6.0h
-1, hydrogen-oil ratio 600: 1~2400: 1; 3. the pre-hydrogenated oil of gained enters downflow system master hydrogenation fixed-bed reactor from top to bottom main hydrogenation reaction takes place, and its operational condition is: 300~420 ℃ of temperature of reaction, reaction pressure 7.0~18.0Mpa, liquid hourly space velocity 0.3~2.0h
-1, hydrogen-oil ratio 1000: 1~2400: 1; 4. winner of institute hydrogenated oil enters fractionating system, obtains gasoline fraction, diesel oil distillate and light Fuel oil distillate.
Described step is 2. during pre-hydrotreating reaction, can in the coal tar hydrogenating charging, add coke inhibitor, the coke inhibitor addition is 0~300ppm, and this is because coke inhibitor can prevent or slow down coal tar hydrogenating charging coking reaction at high temperature, prolongs the cycle of operation of hydrogenation unit.
Coal tar raw material of the present invention is the coal tar of the various character that was produced from the coke-oven plant, and comprises that middle coalite tar, lurgi pressure gasification method produce the coal tar of water-gas by-product and one or more the mixture in the coal-tar heavy oil.
Coal tar preprocessing process of the present invention comprises that coal tar removes water and remove mechanical impurity, wherein removes the dehydration that the mode of water has flash distillation, distillation, layering and adds emulsion splitter; The mode that removes mechanical impurity has filtration, layering, solvent extraction, electric desalting and distillation.
The pre-hydrogenator that the present invention adopts is a kind of upflow fixed bed reactor, the reactant flow of coal tar hydrogenating charging and hydrogen is passed through reactor bed from bottom to top, increased the residence time of reactant flow on beds, the hydrogenation saturated reaction takes place in materials such as the diolefine of easy coking, alkene, free oxygen in the reactant flow under the demulcent condition on the one hand; Liquid phase stream from bottom to top can increase the solvability that established high polymer is reacted in gum asphalt in the coal tar and coking greatly on the other hand, avoids or reduces its adhesion on beds, forms burnt dirt and stops up the pre-hydrotreating reaction bed.
In main hydrogenator, the pre-hydrogenated oil of coal tar of having removed most of coking precursor diolefine, alkene, free oxygen etc. passes through beds from top to bottom, the deep hydrogenation reaction taking place under the effect of catalyzer, realize its lighting, obtains light-weight fuel oils such as petrol and diesel oil.
2. during pre-hydrotreating reaction, pre-hydrogenation fixed-bed reactor of upflowing and the pre-hydrogenation fixed-bed reactor of downflow system are roughly the same for described step, and difference is that reaction mixture enters the direction difference of reactor.
The present invention takes the pre-hydrogenation fixed-bed reactor series connection of upflowing downflow system master hydrogenation fixed-bed reactor, changed logistics direction in the technology, increase the residence time of reactant flow on beds, can effectively suppress or slow down coal tar coking reaction at high temperature, the process of prolongation coal tar hydrogenating unit cycle of operation.
Five, embodiment
The invention will be further described below in conjunction with embodiment.
On 100ml coal tar hydrogenating testing apparatus, be raw material with identical coal tar, adopt the present invention and the conventional pre-hydrogenation fixed-bed reactor series connection of downflow system downflow system master hydrogenation fixed-bed reactor technology to carry out hydrogenation reaction respectively, the continuous operation time of pressure drop appears in the character of more pre-hydrogenated oil and coal tar hydrogenating testing apparatus, and particular case is seen following embodiment:
Embodiment 1
With the coalite tar that was produced from certain coke-oven plant is raw material.With the coal tar standing demix, tell moisture and lower floor mechanical impurity and obtain the coal tar hydrogenating charging.The coal tar hydrogenating charging with enter pre-hydrogenation fixed-bed reactor after hydrogen mixes, its reaction conditions is pressure 7.0MPa, 170 ℃ of temperature, hydrogen-oil ratio 600: 1, liquid hourly space velocity 6.0h
-1Pre-hydrogenated oil enters main hydrogenation fixed-bed reactor, and its reaction conditions is pressure 7.0MPa, 300 ℃ of temperature, hydrogen-oil ratio 1000: 1, liquid hourly space velocity 2.0h
-1The character of test raw material and test-results see Table 1 respectively, table 2.As can be seen from the table, for the relatively poor coalite tar raw material of character, adopt hydrogenation desulfurization and denitrogenation effect of the present invention poorer slightly than common process, but the polymer content of gum asphalt and generation will be starkly lower than common process, the continuous operation time that occurs pressure drop to bed is 469h, be almost 4 times of traditional technology, visible the present invention has good inhibition coking reaction effect, can prolong the runtime of coal tar hydrogenating unit greatly.
Table 1 coalite tar raw material properties
Project | The coalite tar raw material |
Density, kg/m 3(20℃) | 932.7 |
Carbon residue, m% | 3.44 |
C/H,m% | 83.29/9.88 |
Total sulfur, m% | 1.76 |
Total nitrogen, m% | 1.19 |
Colloid+bituminous matter, m% | 24.68 |
Polymkeric substance, ppm | 239 |
The pre-hydrogenated oil character of table 2 coalite tar
Project | Technology of the present invention | Common process |
Density, kg/m 3(20℃) | 918.9 | 915.6 |
Carbon residue, m% | 3.66 | 3.71 |
Total sulfur, m% | 1.36 | 1.19 |
Total nitrogen, m% | 1.07 | 0.92 |
Colloid+bituminous matter, m% | 25.78 | 30.64 |
Device continuous operation time when pressure drop appears in bed, h | 469 | 132 |
Embodiment 2
With the coal-tar middle oil that was produced from certain coke-oven plant is raw material, adds the coke inhibitor of 150ppm in the coal tar hydrogenating charging, and enters pre-hydrogenation fixed-bed reactor after hydrogen mixes, its reaction conditions is pressure 12.0MPa, 300 ℃ of temperature, hydrogen-oil ratio 1800: 1, liquid hourly space velocity 3.0h
-1Main hydrogenation conditions is pressure 12.0MPa, 370 ℃ of temperature, hydrogen-oil ratio 1600: 1, liquid hourly space velocity 1.0h
-1Other reaction conditionss and step are with embodiment 1.The character of test raw material and test-results see Table 3 respectively, table 4.As can be seen from the table, for the relatively poor coal-tar middle oil raw material of character, adopt the hydrogenation desulfurization and denitrogenation effect of this technology poorer slightly than common process, but the polymer content of gum asphalt and generation will be starkly lower than common process, the continuous operation time that occurs pressure drop to bed is 472h, be more than 4 times of common process, as seen this technology has good inhibition coking reaction effect, can prolong the runtime of coal tar hydrogenating unit greatly.
Table 3 coal-tar middle oil raw material properties
Project | The coal-tar middle oil raw material |
Density, kg/m 3(20℃) | 989.7 |
Carbon residue, m% | 4.69 |
C/H,m% | 81.29/9.09 |
Total sulfur, m% | 2.02 |
Total nitrogen, m% | 1.56 |
Colloid+bituminous matter, m% | 34.69 |
The pre-hydrogenated oil character of table 4 coal-tar middle oil
Project | Technology of the present invention | Common process |
Density, kg/m 3(20℃) | 968.7 | 957.9 |
Carbon residue, m% | 4.78 | 4.97 |
Total sulfur, m% | 1.71 | 1.58 |
Total nitrogen, m% | 1.23 | 1.11 |
Colloid+bituminous matter, m% | 35.99 | 39.21 |
Polymkeric substance, ppm | 517 | 798 |
Device continuous operation time when pressure drop appears in bed, h | 472 | 117 |
Embodiment 3
With the coal-tar heavy oil that was produced from certain coke-oven plant is raw material, adds the coke inhibitor of 300ppm in the coal tar hydrogenating charging, and enters pre-hydrogenation fixed-bed reactor after hydrogen mixes, its reaction conditions is pressure 18.0MPa, 280 ℃ of temperature, hydrogen-oil ratio 2400: 1, liquid hourly space velocity 0.8h
-1Main hydrogenation conditions is pressure 18.0MPa, 420 ℃ of temperature, hydrogen-oil ratio 2400: 1, liquid hourly space velocity 0.3h
-1Other reaction conditionss and step are with embodiment 1.The character of test raw material and test-results see Table 5 respectively, table 6.As can be seen from the table, for the very poor coal-tar heavy oil raw material of character, adopt the hydrogenation desulfurization and denitrogenation effect of this technology poorer slightly than common process, but the polymer content of gum asphalt and generation will be starkly lower than common process, the continuous operation time that occurs pressure drop to bed is 256h, be more than 5 times of common process, as seen this technology has good inhibition coking reaction effect, can prolong the runtime of coal tar hydrogenating unit greatly.
Table 5 coal-tar heavy oil raw material properties
Project | The coal-tar heavy oil raw material |
Density, kg/m 3(20℃) | 1132.3 |
Carbon residue, m% | 8.69 |
C/H,m% | 79.99/7.89 |
Total sulfur, m% | 4.37 |
Total nitrogen, m% | 2.36 |
Colloid+bituminous matter, m% | 46.78 |
The pre-hydrogenated oil character of table 6 coal-tar heavy oil
Project | Technology of the present invention | Common process |
Density, kg/m 3(20℃) | 1101.3 | 1097.6 |
Carbon residue, m% | 8.88 | 9.02 |
Total sulfur, m% | 3.99 | 3.38 |
Total nitrogen, m% | 2.01 | 1.67 |
Colloid+bituminous matter, m% | 47.12 | 50.36 |
Device continuous operation time when pressure drop appears in bed, h | 256 | 48 |
Claims (2)
1. a coal tar hydrogenation process is characterized in that comprising the steps: that 1. coal tar carries out obtaining the coal tar hydrogenating charging after the pre-treatment; 2. the charging of gained coal tar hydrogenating mixes with hydrogen, enters the pre-hydrogenation fixed-bed reactor of upflowing generation pre-hydrotreating reaction from bottom to top, and its operational condition is: 170~300 ℃ of temperature of reaction, reaction pressure 7.0~18.0Mpa, liquid hourly space velocity 0.8~6.0h
-1, hydrogen-oil ratio 600: 1~2400: 1; 3. the pre-hydrogenated oil of gained enters downflow system master hydrogenation fixed-bed reactor from top to bottom main hydrogenation reaction takes place, and its operational condition is: 300~420 ℃ of temperature of reaction, reaction pressure 7.0~18.0Mpa, liquid hourly space velocity 0.3~2.0h
-1, hydrogen-oil ratio 1000: 1~2400: 1; 4. winner of institute hydrogenated oil enters fractionating system, obtains gasoline fraction, diesel oil distillate and light Fuel oil distillate.
2, according to the described coal tar hydrogenation process of claim 1, it is characterized in that: described step adds coke inhibitor in 2. in the coal tar hydrogenating charging, the coke inhibitor addition is 0~300ppm.
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CN2008100309541A CN101250433B (en) | 2008-03-28 | 2008-03-28 | Coal tar hydrogenation technique |
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CN2008100309541A CN101250433B (en) | 2008-03-28 | 2008-03-28 | Coal tar hydrogenation technique |
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Cited By (8)
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CN102256931A (en) * | 2008-12-22 | 2011-11-23 | 亨茨曼国际有限公司 | Process for production of methylene-bridged polyphenyl polyamines |
CN102443428A (en) * | 2010-10-13 | 2012-05-09 | 中国石油化工股份有限公司 | Heavy-hydrocarbon hydrogenation treatment method |
CN102443434A (en) * | 2010-10-13 | 2012-05-09 | 中国石油化工股份有限公司 | Heavy-hydrocarbon raw material hydrogenation treatment method |
CN101712889B (en) * | 2009-11-26 | 2013-01-09 | 湖南长岭石化科技开发有限公司 | Method for preparing light aromatics from coal tar |
CN103059938A (en) * | 2011-10-21 | 2013-04-24 | 中国石油化工股份有限公司 | Heavy hydrocarbon hydrotreating method |
CN103254928A (en) * | 2013-06-08 | 2013-08-21 | 安徽工业大学 | Method for increasing utilization ratio of additional value of high-temperature coal tar |
CN105001892A (en) * | 2015-07-17 | 2015-10-28 | 程志宇 | Method for co-production of refined maltha through fixed bed-based coal-tar hydrogenation process |
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CN105001892A (en) * | 2015-07-17 | 2015-10-28 | 程志宇 | Method for co-production of refined maltha through fixed bed-based coal-tar hydrogenation process |
CN105001892B (en) * | 2015-07-17 | 2017-05-24 | 程志宇 | Method for co-production of refined maltha through fixed bed-based coal-tar hydrogenation process |
CN108300510A (en) * | 2017-01-12 | 2018-07-20 | 中国石油化工股份有限公司 | A kind of method of preparing fuel oil with coal oil hydrogenation |
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Address after: 414012 Lu Kou Zhen Chang Lian Long Kou, Yunxi District, Yueyang City, Hunan Province (opposite to Chang Lian hospital) Patentee after: Hunan Changlian New Materials Technology Co.,Ltd. Country or region after: China Address before: 414012 Yunxi District, Hunan City, Yueyang Province, Changling Patentee before: HUNAN CHANGLING PETROCHEMICAL TECHNOLOGY DEVELOPMENT Co.,Ltd. Country or region before: China |