CN103540352A - Coal tar processing method for increasing yield of light oils - Google Patents
Coal tar processing method for increasing yield of light oils Download PDFInfo
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- CN103540352A CN103540352A CN201210241135.8A CN201210241135A CN103540352A CN 103540352 A CN103540352 A CN 103540352A CN 201210241135 A CN201210241135 A CN 201210241135A CN 103540352 A CN103540352 A CN 103540352A
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Abstract
The invention relates to a coal tar processing method for increasing the yield of light liquid. According to the method, all distillates of coal tar are distilled and are divided into distillates which are lower than or equal to 350 DEG C and distillates higher than 350 DEG C, the coal tar distillates higher than 350 DEG C are mixed with hydrogen gas and distillate oil and then enter a slurry-bed hydrogenation device for reaction, partial hydrogenated tail oil of a product is circulated to a slurry-bed reactor, and part of the tail oil (350-450 DEG C) is subjected to solid particle removal and then is conveyed to a fixed-bed residue oil hydrogenation device; the coal tar distillates which are lower than or equal to 350 DEG C are mixed with hydrogen gas, the hydrogenated tail oil and the distillate oil and then enter the fixed-bed residue oil hydrogenation device for reaction. The method has the advantages that slurry-bed hydrotreating and fixed-bed hydrotreating processes are organically combined, so that all the distillates of the coal tar can be processed, and the utilization rate of the coal tar is increased; the distillate oil is added into light and heavy ingredients of the coal tar, so that the conversion ratio of raw materials is increased, the yield of the light liquid is increased, the coking of a hydrogenation catalyst can be delayed, and the operating cycle of the devices is prolonged.
Description
Technical field
The present invention relates to process with hydroprocessing technique the method for coal tar, say more specifically and in coal tar weight component, add distillate and fixed bed hydrogenation technique is organically combined and processes coal tar with slurry state bed hydroprocessing technique, improve the method for light oil yield.
Background technology
21 century, the feature of petroleum industry was: oil price is higher, and that crude oil constantly becomes is heavy, quality becomes bad, and the ratio of non-conventional crude oil (as viscous crude, super viscous crude and oil sands bitumen etc.) is more and more higher.Therefore, residual oil deep processing is more and more paid attention to.Due to increasing and the increasingly stringent of environmental regulation of distillate demand between city's field alignment, make residual hydrogenation technology obtain very fast development.
In the lightening method of residual oil, patent US4,713,221, the residual oil hydrogenation-catalytic cracking combined technological of CN1262306A, CN1119397C, CN101210200A report, in residual oil, add distillate as catalytically cracked oil steam thing, heavy catalytic cycle oil enters residual hydrogenation equipment, can improve the quality of residual hydrocracking, extends the operational cycle of residual hydrocracking, can also increase the yield of catalytic cracking light oil, and improve the treatment capacity of catalytic cracking unit.Combination process just low value by product, as catalytically cracked oil etc. is converted into high-value product, significantly improves the economic benefit of petroleum chemical enterprise.
Due to political factor and prospective oil and exploitation quantitative limitation, crude oil price is high, and this needs petroleum chemical enterprise's degree of depth to tap the latent power or finds other cheap substitute energy.Coal tar is the byproduct of coking technology, no matter from boiling range, still forms, and coal tar and stone oil composition approach.The foreign matter contents such as coal tar oil composition be take aromatic hydrocarbon as main, and polycyclic aromatic hydrocarbon content is high, sulphur nitrogen oxygen are high.The method of current coal tar hydrogenating, wherein:
US4,855,037 disclose a kind of catalyzer and the method that coal tar hydrogenating is processed.The method be by the coal tar after hydrotreatment for delayed coking, hydrogenation technique is to occur as the pretreatment technology of delay coking of coal tar, not the object product such as direct production light-end products.The method is mainly processed heavy coal tar, and working pressure is high, invests larger.
CN101768465A discloses a kind of method for preparing clean diesel and products thereof.The mixing raw material that the method is prepared diesel oil distillate and vegetables oil and/or animal grease by coal is that raw material prepares clean diesel cut.
CN1464031 discloses a kind of coal tar hydrogenation process and catalyzer.This patent is used special-purpose catalyst, and flow process is common processing process.The method is only carried out upgrading to raw material, in its special-purpose catalyst, contains molecular sieve, and the water that coal tar hydrogenating is generated is very responsive, the work-ing life of having reduced like this catalyzer, serious destruction catalyzer and cause bed pressure drop to rise, caused device to stop work.
CN1351130A discloses a kind of method that coal tar hydrogenating is produced diesel oil.The method is mainly that first coal tar pass through fractionation, the last running obtaining is not as the raw material of hydrotreatment, just the light ends in coal tar is carried out to hydrotreatment, owing to not using hydrocracking catalyst, the course of processing obtains diesel oil distillate can only be as the blend component of diesel product, and coal tar is not utilized completely, cause the whole yield of light-end products greatly to reduce.
CN101962571A discloses a kind of coal tar heavy fractioning suspension bed hydrocracking method and system.The method can make coal tar heavy fractioning lighting, effectively improves the productive rate that coal tar hydrogenating generates fuel oil.But only the last running of coal tar is processed, also coal tar is not utilized completely.
CN101724461A discloses a kind of catalystic hydrogenation of coal tar treatment process of productive, lightweight and clean fuel oil though.The method by coal tar through prefractionation, except heavy constituent and heavy metallic salt and solid impurities etc. such as deasphaltings, cut be respectively less than 300 ℃ and 300-380 ℃ cut as hydrogenating materials oil, two kinds of cuts enter different reactor reaction.This method is not utilized coal tar completely yet.
Therefore, need to improve and to utilize existing hydrogenation technique, for the comprehensive and reasonable utilization of coal tar provides a kind of feasible scheme, improve the utilization ratio of coal tar, the life cycle that simultaneously extends fixed bed hydrogenation device, improves the yield of light-end products.
Summary of the invention
The object of the invention is by adding distillate, improve the conversion of coal tar, coal tar is fully used, improve slurry state bed hydroprocessing and the fixed bed hydrogenation combined technical method of light oil yield.
The technical scheme of the hydrogenation combination technique of processing coal tar of the present invention is:
The full cut distillation of feed coal tar is divided into the lightweight coal tar fraction that is less than or equal to 350 ℃ and the heavy coal tar fraction that is greater than 350 ℃; Coal tar heavy fractioning (being greater than 350 ℃) is mixed with distillate, catalyzer and vulcanizing agent, carry out catalyst vulcanization under the effect of hydrogen, the mixture after sulfuration carries out preheating, then enters paste state bed reactor and carries out hydrocracking reaction; By paste state bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Partial hydrogenation tail oil turns back to paste state bed reactor as circulation tail oil, and partial hydrogenation tail oil (350-450 ℃) adopts one or more methods in filtration, distillation, rotating separation etc. to remove and in tail oil, after solid particulate, is delivered to fixed bed hydrogenation device.
Under the condition that the lighting end of coal tar and distillate exist at hydrogen with the hydrogenation tail oil being come by paste state bed reactor, entering fixed bed hydrogenation device contacts with hydrogenation catalyst and carries out hydrotreatment reaction; Hydrogenation catalyst be comprise protective material, metal remover, sweetening agent three classes or more than; different catalysts is divided into different bed fillings; can be seated in a reactor or a plurality of reactor, protective material can be contained in up-flow reactor or fixed-bed reactor.By fixed-bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.
Method provided by the invention is described as follows:
(1) slurry state bed hydroprocessing part
In the present invention, the reaction of slurry state bed hydroprocessing is carried out under the condition relatively relaxing, and the transformation efficiency of controlling the reaction of slurry state bed hydroprocessing is 20-80%, preferably 25-65%.Reaction conditions is: reactive hydrogen dividing potential drop is 8-24MPa, preferably 8-20MPa; Temperature of reaction is 320-450 ℃, preferably 370-420 ℃; Liquid hourly space velocity is 0.1-3h
-1, preferred 0.3-2h
-1; Hydrogen to oil volume ratio is 300-3000, preferably 400-2500.Catalyzer can be water-soluble catalyst, oil-soluble catalyst, solid powder th-1 catalyst etc., in catalyzer, there are one or more in the elements such as Mo, Ni, Co, Fe or Ti, catalyzer add-on (take metal) is 50-5000 μ g/g, preferably 100-500 μ g/g.Described vulcanizing agent is various S-contained substances, as one or more in sulphur, dithiocarbonic anhydride, dimethyl thioether, dimethyl disulphide etc., the add-on of vulcanizing agent is 0.1%-0.9%, and being preferably 0.1-0.6%(, to take the quality of coal tar heavy fractioning (being greater than 350 ℃) be calculating standard).Catalyzer can adopt any kind catalyzer in slurry state bed hydroprocessing technique.Coal tar heavy fractioning is mixed with distillate, catalyzer and vulcanizing agent, carry out catalyst vulcanization under the effect of hydrogen, the mixture after sulfuration carries out preheating, then enters paste state bed reactor and carries out hydrocracking reaction; By paste state bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Partial hydrogenation tail oil turns back to paste state bed reactor as circulation tail oil, and part tail oil adopts one or more methods in filtration, distillation, rotating separation etc. to remove and in tail oil, after solid particulate, is delivered to fixed bed residual hydrogenation equipment.
(2) fixed bed hydrogenation part
The raw material that device is used is slurry state bed hydroprocessing tail oil and coal tar lighting end (being less than or equal to 350 ℃).Adopt the catalyzer grating of fixed bed residual hydrogenation equipment, filling simultaneously comprises three classes or the above catalyzer of three classes of protective material, metal remover, sweetening agent.Different catalysts is divided bed filling, can be contained in a reactor, also can be contained in a plurality of reactors.Catalyzer be generally take porous inorganic oxide as aluminum oxide be carrier, group VIB and VIII family metal oxide as the oxide compound of W, Mo, Co, Ni etc. be active ingredient.Protective material bed can adopt fixed-bed reactor, also can adopt up-flow reactor, and other beds adopts fixed-bed reactor.
Operational condition is: hydrogen partial pressure 10-22MPa, preferably 14-20MPa; Temperature of reaction is 300 ~ 435 ℃, preferably 360-420 ℃; Volume space velocity 0.1～6.5hr
-1, preferred 0.5-5hr
-1; Hydrogen to oil volume ratio is 500～2000.By weight, distillate (catalytically cracked oil, vegetables oil) by mass percentage, is the 0.5%-35% of feed coal tar lighting end.Distillate and coal tar lighting end (being less than or equal to 350 ℃) are reacted from the first reactor feed mouth access to plant, and reaction product can be separated into dry gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenated residue.
In the light and heavy fractions of coal tar, add distillate, can reduce raw material oil viscosity on the one hand, improve diffusibility and the impurity removal speed of reaction molecular in catalyzer duct, in coal distillate, be rich on the other hand polycyclic aromatic hydrocarbons and strengthen the bitum effect that can play hydrogen supply agent simultaneously of dissolving, reduce green coke precursor green coke on catalyzer, thereby improve the light weight fluid yield of high added value, the running period of extension fixture.
Accompanying drawing explanation
The hydrogenation combination technique schematic flow sheet of Fig. 1 processing coal tar of the present invention and residual oil.
Embodiment
Coal tar distillation is divided into the lightweight coal tar fraction that is less than or equal to 350 ℃ and the heavy coal tar fraction that is greater than 350 ℃; Coal tar heavy fractioning (being greater than 350 ℃) is mixed with distillate, catalyzer and vulcanizing agent, carry out catalyst vulcanization under the effect of hydrogen, the mixture after sulfuration carries out preheating, then enters paste state bed reactor and carries out hydrocracking reaction; By paste state bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Partial hydrogenation tail oil returns to paste state bed reactor as circulation tail oil, and part tail oil is delivered to fixed bed residual hydrogenation equipment after removing solid particulate.Under the condition that the lighting end of coal tar (being less than 350 ℃) and distillate exist at hydrogen with the hydrogenation tail oil being come by paste state bed reactor, enter fixed bed residual hydrogenation equipment and contact with residual oil hydrocatalyst and carry out hydrotreatment reaction, by fixed-bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.
Embodiment 1
The present embodiment adopts hydrogenation combination technique of the present invention, and the character of coal tar, coal tar light and heavy fractions and distillate (catalytically cracked oil) is in Table 1.
Table 1 feedstock property
Coal tar distillation is divided into the lightweight coal tar fraction that is less than 350 ℃ and the heavy coal tar fraction that is greater than 350 ℃; By coal tar heavy fractioning (being greater than 350 ℃), 3:1, catalyzer and vulcanizing agent mix in mass ratio with distillate, under the effect of hydrogen, carry out catalyst vulcanization, mixture after sulfuration carries out preheating, then enters paste state bed reactor and carries out hydrocracking reaction; By paste state bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Under the lighting end of coal tar (being less than 350 ℃) and the distillate condition that 4:1 exists at hydrogen in mass ratio, enter fixed bed residual hydrogenation equipment and contact with residual oil hydrocatalyst and carry out hydrotreatment reaction, by fixed-bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Product distribution and reaction conditions are in Table 2.
Embodiment 2
Coal tar distillation is divided into the lightweight coal tar fraction that is less than 350 ℃ and the heavy coal tar fraction that is greater than 350 ℃; Coal tar heavy fractioning (being greater than 350 ℃) is mixed with distillate mass ratio 1:1, catalyzer and vulcanizing agent, under the effect of hydrogen, carry out catalyst vulcanization, mixture after sulfuration carries out preheating, then enters paste state bed reactor and carries out hydrocracking reaction; By paste state bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil; Part hydrogenation tail oil turns back to recycle in preliminary heating device as circulation tail oil, and another part (350-450 ℃) is delivered to fixed bed residual hydrogenation equipment.Under the condition that the lighting end (being less than 350 ℃) of hydrogenation tail oil and coal tar exists at hydrogen with distillate mass ratio 1:4:1, enter fixed bed residual hydrogenation equipment and contact with residual oil hydrocatalyst and carry out hydrotreatment reaction, by fixed-bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenated residue.Move after 3000 hours that product distributes and reaction conditions in Table 2.Comparative example
Coal tar distillation is divided into the lightweight coal tar fraction that is less than 350 ℃ and the heavy coal tar fraction that is greater than 350 ℃; Coal tar heavy fractioning (being greater than 350 ℃) is mixed with catalyzer and vulcanizing agent, carry out catalyst vulcanization under the effect of hydrogen, the mixture after sulfuration carries out preheating, then enters paste state bed reactor and carries out hydrocracking reaction; By paste state bed reactor product out, through fractionation, obtain gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Coal tar gently heats up in a steamer and under the condition existing at hydrogen, enters fixed bed residual hydrogenation equipment and contact with residual oil hydrocatalyst and carry out hydrotreatment reaction, by fixed-bed reactor product out, through fractionation, obtains gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil.Move after 3000 hours that product distributes and reaction conditions in Table 2.
Table 2 product distributes and reaction conditions
By table 2 contrast, we can know, move after 3000 hours, the carbon deposit on sweetening agent HDS1, the HDS2 in embodiment 1,2 and de-carbon residue HDCCR is starkly lower than comparative example, and expectation comparative example runtime is high 3 months and 2 months; In embodiment, diesel yield is higher 1.1 and 0.7 percentage points respectively than comparative example; S in embodiment, N decreasing ratio will be higher than comparative example.
Claims (6)
1. a coal tar processing method that improves light oil yield, is characterized in that:
(1) coal tar distillation is divided into the lightweight coal tar fraction that is less than or equal to 350 ℃ and the heavy coal tar fraction that is greater than 350 ℃;
(2) the heavy coal tar fraction and distillate, hydrogen, catalyzer and the vulcanizing agent that in step (1), are greater than 350 ℃ are mixed into slurry state bed hydroprocessing reactor reaction, reaction product is isolated to dry gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenation tail oil, partial hydrogenation tail oil is circulated to paste state bed reactor, and 350-450 ℃ of cut fraction hydrogenation tail oil is delivered to fixed bed residual hydrogenation equipment after removing after filtration solid particulate; Slurry reactor condition is: reactive hydrogen dividing potential drop is 8-24MPa; Temperature of reaction is 320-450 ℃; Liquid hourly space velocity is 0.1-3h
-1; Hydrogen to oil volume ratio is 300-3000;
(3) the lightweight coal tar fraction that is less than or equal to 350 ℃ in step (1) is entered to fixed bed residual hydrogenation equipment with distillate and hydrogen, hydrogenation tail oil by device raw material mouth and react, reaction product separation obtains dry gas, hydrotreated naphtha, hydrogenated diesel oil and hydrogenated residue; Fixed bed hydrogenation condition is: hydrogen dividing potential drop 10-22MPa, and temperature of reaction is 340 ℃-435 ℃, volume space velocity is 0.1-5.5hr
-1, hydrogen to oil volume ratio 500-2000.
2. method according to claim 1, it is characterized in that, fixed bed residual hydrogenation equipment described in step (3) is one or more combination of reactors, adopts catalyzer grading loading technology, filling protective material, metal remover, sweetening agent, de-carbon residue catalyzer; Different catalysts is divided bed filling, is seated in one or more reactors, and protective material bed adopts fixed-bed reactor or up-flow reactor.
3. method according to claim 1, is characterized in that, the described used for slurry bed catalyzer of step (2) is oil-soluble catalyst or water-soluble catalyst or solid powder th-1 catalyst.
4. method according to claim 1, is characterized in that, described hydrogenation tail oil removes solid particulate and adopts one or more methods in filtration, distillation, rotating separation.
5. method according to claim 1, is characterized in that, described distillate is one or both the mixture in catalytically cracked oil, vegetables oil.
6. method according to claim 1, is characterized in that, the described distillate of step (3) by weight percentage, is the 0.5%-35% of raw material coal tar heavy fractioning.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479739A (en) * | 2014-12-03 | 2015-04-01 | 宁波市化工研究设计院有限公司 | Method for producing fuel oil by hydrogenation of fraction oil of high-temperature coal tar |
| CN104479737A (en) * | 2014-12-12 | 2015-04-01 | 宁波市化工研究设计院有限公司 | High-temperature coal tar distillate oil hydrogenation device with low aromatic oil circulation |
| CN105623703A (en) * | 2016-01-19 | 2016-06-01 | 何巨堂 | Thermal high-pressure dissociating gas dust removal method for three-phase product of hydrocarbon material hydrogenation reaction |
| CN105038852B (en) * | 2015-08-14 | 2016-08-31 | 北京宝塔三聚能源科技有限公司 | A kind of hydrogenation technique of ethylene bottom oil |
| CN110317637A (en) * | 2019-07-17 | 2019-10-11 | 华东理工大学 | Handle the combined hydrogenation method of residual oil and sludge pyrolytic oil |
| CN112175668A (en) * | 2020-09-24 | 2021-01-05 | 济安永蓝(北京)工程技术开发有限公司 | Double-circulation slurry bed hydrocracking method |
| CN113249137A (en) * | 2021-04-15 | 2021-08-13 | 甘肃宏汇能源化工有限公司 | Process for prolonging service life of catalyst in coal tar hydrogenation technology |
| CN116948683A (en) * | 2023-09-15 | 2023-10-27 | 克拉玛依市先能科创重油开发有限公司 | Slurry bed reaction on-line switching method using cycloalkyl residual oil and ethylene cracking tar as raw materials |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479739A (en) * | 2014-12-03 | 2015-04-01 | 宁波市化工研究设计院有限公司 | Method for producing fuel oil by hydrogenation of fraction oil of high-temperature coal tar |
| CN104479737A (en) * | 2014-12-12 | 2015-04-01 | 宁波市化工研究设计院有限公司 | High-temperature coal tar distillate oil hydrogenation device with low aromatic oil circulation |
| CN104479737B (en) * | 2014-12-12 | 2017-06-20 | 宁波市化工研究设计院有限公司 | High temperature coal-tar distillate hydrogenation device with the circulation of low aromatic naphtha |
| CN105038852B (en) * | 2015-08-14 | 2016-08-31 | 北京宝塔三聚能源科技有限公司 | A kind of hydrogenation technique of ethylene bottom oil |
| CN105623703A (en) * | 2016-01-19 | 2016-06-01 | 何巨堂 | Thermal high-pressure dissociating gas dust removal method for three-phase product of hydrocarbon material hydrogenation reaction |
| CN110317637A (en) * | 2019-07-17 | 2019-10-11 | 华东理工大学 | Handle the combined hydrogenation method of residual oil and sludge pyrolytic oil |
| CN112175668A (en) * | 2020-09-24 | 2021-01-05 | 济安永蓝(北京)工程技术开发有限公司 | Double-circulation slurry bed hydrocracking method |
| CN113249137A (en) * | 2021-04-15 | 2021-08-13 | 甘肃宏汇能源化工有限公司 | Process for prolonging service life of catalyst in coal tar hydrogenation technology |
| CN116948683A (en) * | 2023-09-15 | 2023-10-27 | 克拉玛依市先能科创重油开发有限公司 | Slurry bed reaction on-line switching method using cycloalkyl residual oil and ethylene cracking tar as raw materials |
| CN116948683B (en) * | 2023-09-15 | 2023-12-12 | 克拉玛依市先能科创重油开发有限公司 | Slurry bed reaction on-line switching method using cycloalkyl residual oil and ethylene cracking tar as raw materials |
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Application publication date: 20140129 |