CN1485413A - Process of desulfurizing and eliminating aromatic hydrocarbons deeply for diesel oil - Google Patents
Process of desulfurizing and eliminating aromatic hydrocarbons deeply for diesel oil Download PDFInfo
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Abstract
A process of removing sulfur and aromatic hydrocarbons from diesel oil. It comprises, mixing diesel oil and circulating hydrogen, and entering the first reactor for hydrogenating and removing sulfur and nitrogen, hydrogenating and saturating olefins and aromatic hydrocarbons, the effluent entering a high-temperature high-pressure gas stripping tower for gas stripping to remove H2S and NH3, then mixing the effluent and circulating hydrogen, entering the second hydrogenation refining reactor; the effluent of the reactor entering in sequence a high-pressure separator, a low-pressure separator and a fractionating tower, the fractionating tower separating naphtha and diesel fractions; gas enriched in hydrogen from the high-temperature high-pressure gas stripping tower entering a water-washing tank, to remove H2S and NH3, then mixing with gas enriched in hydrogen from the high-pressure separator, compressing and circulating to the first and the second reactor. The method could greatly reduce impurities in diesel oil, such as sulfur and nitrogen.
Description
Technical field
The invention belongs in the method that has refining hydrocarbon ils under the situation of hydrogen, more particularly, is the method that belongs to a kind of diesel oil hydrofining.
Background technology
Because the cry of environment protection increases day by day, countries in the world have been revised its diesel oil specification one after another, require oil refining enterprise production environment close friend's fuel.1998, by " world's fuel oil standard " that three big Automobile Associationss initiate to formulate the diesel product standard is divided for I class, II class, III class, increased the IV class recently again newly.In the new diesel oil specification, changing bigger is sulphur content, aromaticity content and these several indexs of cetane value.Wherein II class diesel oil requires: sulphur content is not more than 300ppm, and total aromaticity content is not higher than 25 weight %, and polycyclic aromatic hydrocarbon content is not higher than 5 weight %, and cetane index is not less than 50; III class diesel oil requires: sulphur content is not more than 30ppm, and total aromaticity content is not higher than 15 weight %, and polycyclic aromatic hydrocarbon content is not higher than 2 weight %, and cetane index is not less than 52.This specification is as world's standard, and the formulation of the new diesel oil standard in various countries is being produced deep effect.
By transforming existing hydro-refining unit (5.0～6.0 MPa pressure rating), as reduce air speed or improve temperature of reaction, the active higher means such as catalyst for refining of replacing, from intermediate distillates particularly catalytic diesel oil produce above-mentioned II class diesel oil, can make sulphur content reach requirement, but the aromaticity content that reduces in the product is an a great problem.Because the restriction of the saturated thermodynamics speciality of aromatic hydrogenation, under common hydrofining condition aromatic hydrogenation saturated be very difficult.
US5114562 discloses a kind of technology of utilizing two-stage hydrogenation technology to produce the low fragrant product of low-sulfur from intermediate distillates.Its technological process is removed H for the liquid product that comes out from first section reactor through hydrogen stripped
2S and NH
3After, heat up through heat exchange again, enter into second section reactor.Load finishing agent in first section reactor, filling is to H in second section reactor
2The noble metal catalyst that S concentration is very sensitive.Compare with first section, second section pressure and air speed are higher, and temperature is lower.
US5183556 has announced a kind of two-stage hydrogenation technology of producing fine-quality diesel oil from diesel oil distillate, and reactor is placed in-line in this technology.During operation, hydrogen and liquid phase feeding also flow to into first section reactor, and the liquid-phase product that comes out from first section reactor contacts with hydrogen is reverse second section reactor.The used reactor of this technology is fixed-bed reactor, and first section is base metal catalysts, and second section can be noble metal catalyst, also the available bases metal catalyst.
" Upgrading Light Cycle Oil to Diesel Using the Engelhard-WashingtonREDAR Process " (calendar year 2001 NPRA meeting AM-01-23) has been introduced the technology of utilizing REDAR technology catalytic cracking light cycle oil upgrading to be become diesel oil.This technology realizes in the two reactor system, and what first section hydrofining reactor used is base metal catalysts, and what second section reforming reactor used is the noble metal catalyst of anti-sulphur and nitrogen.In the middle of two reactors, the hydrogen stripped tower is set, to take off the hydrogen sulfide (H of first reactor effluent
2S) and ammonia (NH
3), the gas phase series connection of second section and first section, the gas after refining no longer directly enters first section through handling earlier by second section from second section gas that comes out, and makes the hydrogen dividing potential drop of upgrading section be higher than hydrogen dividing potential drop 15 crust (213psi) of refining section.
Above-mentioned prior art all adopts the operational path of noble metal catalyst, and the subject matter of existence is the increase greatly of tooling cost.
CN1156752A has announced a kind of two-stage hydrogenation technology of producing fine-quality diesel oil with diesel oil distillate, and this invention is two sections integrated techniques, has added water washing device between two reactor, removes one section H in the effluent
2S and NH
3The used reactor of this technology is fixed-bed reactor, and first section is base metal catalysts, and second section for containing the base metal catalysts of molecular sieve.But this method energy consumption is higher, and the washing between two sections easily causes environmental pollution.
Summary of the invention
The purpose of this invention is to provide the processing method that a kind of desulfurizing and dearomatizing diesel oil deeply is provided on the basis of existing technology.
Method provided by the invention comprises: diesel raw material and circulating hydrogen are mixed into first section reactor and carry out hydrogenating desulfurization, hydrodenitrification, saturated, the aromatic hydrogenation saturated reaction of hydrogenation of olefins, and reaction effluent enters the High Temperature High Pressure stripping tower and removes H through new hydrogen stripping
2S, NH
3After be mixed into second section hydrofining reactor again with hydrogen, the effluent of this reactor enters high-pressure separator, light pressure separator and separation column in proper order, separation column is divided into petroleum naphtha and diesel oil distillate with reaction product; The hydrogen rich gas that comes out from the High Temperature High Pressure stripping tower cleaning of evaporator of intaking mutually removes H wherein
2S, NH
3Deng behind the impurity with mix from the isolated hydrogen rich stream of high-pressure separator, be circulated to first section and second section reactor after compression.
Method provided by the invention can reduce the sulphur and the aromaticity content of diesel oil significantly, and the sulphur content of diesel oil is reduced to below the 10ppm, and aromaticity content satisfies II class or III class diesel oil standard; Owing to adopt of the technical process of new hydrogen, thereby reduced the severity of water washing tank, can suitably reduce plant investment, process cost and difficulty as the high-pressure stripper stripping gas.
Description of drawings
Accompanying drawing is the processing method synoptic diagram of desulfurizing and dearomatizing diesel oil deeply provided by the invention.
Embodiment
Method provided by the invention is so concrete enforcement:
Diesel raw material and circulating hydrogen are mixed into first section reactor and carry out hydrogenating desulfurization, hydrodenitrification, saturated, the aromatic hydrogenation saturated reaction of hydrogenation of olefins, and reaction effluent enters the High Temperature High Pressure stripping tower and removes H through new hydrogen stripping
2S, NH
3After be mixed into second section hydrofining reactor again with hydrogen, the effluent of this reactor enters high-pressure separator, light pressure separator and separation column in proper order, separation column is divided into petroleum naphtha and diesel oil distillate with reaction product; The hydrogen rich gas that comes out from the High Temperature High Pressure stripping tower cleaning of evaporator of intaking mutually removes H wherein
2S, NH
3Deng behind the impurity with mix from the isolated hydrogen rich stream of high-pressure separator, be circulated to first section and second section reactor after compression.
This technology is 180～400 ℃ diesel raw material applicable to boiling range, and its sulphur content is not more than 3wt% and preferably is not more than 2.0wt%, and nitrogen content is not more than 0.2wt% and preferably is not more than 0.1wt%.Used diesel raw material is catalytic cracking diesel oil, straight-run diesel oil, coker gas oil, visbreaking diesel oil or its mixing oil.
Processing method condition of the present invention is as follows: hydrogen dividing potential drop 4.0～10.0MPa, 300～450 ℃ of temperature of reaction, liquid hourly space velocity 0.1～20h
-1, hydrogen-oil ratio 300～2000v/v.
First section is adopted hydrofining agent or modifying catalyst, and second section is adopted conventional Hydrobon catalyst.Catalyst for hydro-upgrading is VIA or the VIII family base metal catalysts that contains on unformed aluminum oxide of loading on of a certain amount of molecular sieve or the silica-alumina supports, and Hydrobon catalyst is VIA or the VIII family base metal catalysts that loads on unformed aluminum oxide or the silica-alumina supports.Because conventional hydrofining or modifying catalyst have strict requirement to charging; when feed properties is abominable; need to add an amount of protective material at its top; protective material is VIA or the VIII family base metal catalysts that loads on unformed aluminum oxide or the silica-alumina supports; preferred group becomes the gamma-aluminium oxide carrier that diplopore distributes that has of 1.0～5.0 heavy % nickel oxide, 5.5～10.0 heavy % molybdenum oxides and surplus, and the volume ratio of protective material and Hydrobon catalyst or catalyst for hydro-upgrading is 0.03～0.3.
Below in conjunction with accompanying drawing method provided by the present invention is further detailed.
Accompanying drawing is the processing method synoptic diagram of desulfurizing and dearomatizing diesel oil deeply provided by the invention.Many essential equipment, facility have been omitted among the figure, as process furnace, pump, the gas sweetening measure of high-pressure stripper top, waterflood pump and pipeline etc.
Flow process is described in detail as follows: diesel raw material is after pipeline 1 incoming stock pump 3 boosts to reaction pressure, through pipeline 37 with after hydrogen-rich gas from pipeline 35 mixes, enter first section reactor 5 through pipeline 4, by contacting with beds, remove impurity such as sulphur in the stock oil and nitrogen, reaction is strong exothermal reaction, needs to inject cold hydrogen at the reactor beds interlayer through pipeline 36, with the conditioned reaction temperature distribution.The effluent of first section reactor 5 through pipeline 6 with from the stripping of pipeline 8 after logistics in interchanger 7 after the heat exchange, enter the hydrogen stripped tower 10 of High Temperature High Pressure through pipeline 38, used stripping hydrogen enters from stripping tower 10 bottoms through pipeline 31, gaseous stream behind the stripping enters water washing tank 12 through pipeline 11, and the gas phase after the washing is through 13 times hydrogen gas circulating systems of pipeline; Liquid phase stream behind the stripping is through the effluent heat exchange of pipeline 8 with reactor 5, mix with hydrogen-rich gas through pipeline 16 then from pipeline 33, enter second section hydrofining reactor 17, because second section what mainly carry out is aromatic hydrogenation reaction, belong to strong exothermal reaction, need to inject cold hydrogen through pipeline 34 to second section reactor beds interlayer, to improve reaction temperature profile, the effluent of reactor 17 enters high-pressure separator 19 through pipeline 18 through heat exchange, in high-pressure separator, be separated into two bursts of logistics, wherein liquid phase stream enters light pressure separator 22 through pipeline 21, the lighter hydrocarbons that remove go out light pressure separator 22 through pipeline 23, light pressure separator bottom effluent enters separation column 25 through pipeline 24, the petroleum naphtha that fractionates out, diesel oil distillate is respectively through pipeline 28,29 go out device, and the lighter hydrocarbons at separation column top mix after pipeline 27 enters refinery's low pressure gas pipe network with lighter hydrocarbons from pipeline 23 through pipeline 26.
Gaseous stream behind the stripping enters water washing tank 12 through pipeline 11, gas phase after the washing comes out to be divided into two portions through pipeline 13, wherein a part is delivered to the ingress of new hydrogen supercharger 9 through pipeline 30, another part is with after hydrogen-rich stream from pipeline 20 mixes, enter recycle compressor 14 through pipeline 15, gas after the compression comes out to be divided into three parts through pipeline 32, wherein first part is through between the bed of pipeline 34 as cold hydrogen injecting reactor 17, second section through pipeline 33 with enter reactor 17 after liquid phase stream from pipeline 16 mixes, third part is successively through pipeline 35, between the bed of 36 injecting reactors 5, or through pipeline 35 with mix from the diesel raw material of pipeline 37 after, loop back reactor 5 through pipeline 4.
New hydrogen through pipeline 2 with mix from the gas phase of pipeline 30 after, enter new hydrogen supercharger 9, the gas after the supercharging enters as stripping gas from stripping tower 10 bottoms through pipeline 31.
Processing method of the present invention is set up the High Temperature High Pressure stripping tower in the middle of two reactors, new hydrogen is as the stripping gas of High Temperature High Pressure stripping tower, the gas phase of coming out from the High Temperature High Pressure stripping tower is done taken off H
2S, NH
3Handle, so not only reduced the treatment capacity of water washing tank, and make and contain a spot of hydrogen sulfide in the hydrogen of second section reactor into, can slow down the mistake sulphur of its sulphided state catalyzer.
Processing method of the present invention all adopts non-precious metal catalyst for two sections, compares with adopting the noble metal catalyst two-stage process, and it is low to have a production cost, insensitive to impurity, advantages such as easy handling.
For reducing running cost and difficulty, the present invention all adopts and flow process in gas phase and liquid phase.Gas phase flow process in parallel is to enter two reactors respectively from the circulation gas that compressor comes out because and flow process simpler, be used for two sections technologies of all using base metal catalysts, can reduce operation easier.And gas phase crossfire technology is complicated, is unfavorable for operation, and this flow process mainly is in order to improve the hydrogen dividing potential drop of second stage reactor, thus this process using routine and flow flow process.Liquid phase adopts also stream flow process, and promptly liquid phase and hydrogen pass through fixed-bed reactor with equidirectional, and activity is subject to H the precious metal because base metal catalysts does not resemble
2The influence of S concentration, and the cost of adverse current fixed-bed reactor will be far above general fixed-bed reactor.
Another characteristics of the present invention are to make the stripping gas of High Temperature High Pressure stripping tower of new hydrogen, and behind stripping tower the water receiving cleaning of evaporator, remove the H in the stripping tower gas phase
2S, NH
3Deng impurity, owing to do not comprised two sections gas phase by gas washing, thereby reduced the treatment capacity of water washing tank effectively, reduce investment outlay and process cost.Enter simultaneously in the hydrogen of second stage reactor and contain a spot of H
2S can suppress post vulcanization attitude catalyzer and lose sulphur.For reducing to draw a side line from the outlet of depriving hydrogen sulphide jar and enter the mouth to new hydrogen supercharger owing to of the influence of new hydrogen quantitative changeization to stripping tower.
Method provided by the invention can reduce the sulphur and the aromaticity content of diesel oil significantly, and the sulphur content of diesel oil is reduced to below the 10ppm, and aromaticity content satisfies II class or III class diesel oil standard.
The following examples will give further instruction to present method, but therefore not limit present method.
First reactor and the used catalyzer of second reactor are Hydrobon catalyst among the embodiment, and the trade mark is respectively RN-10 and RJW-2, produce by Changling Refinery Chemical Industry Co., Ltd. of China Petrochemical Industry catalyst plant.
Test raw material is catalytic cracking diesel oil A, stock oil character, processing condition and product property are listed in table 1, table 2 respectively, as seen from the table, this feed sulphur content is higher, aromaticity content is moderate, and under than the demulcent operational condition, every index of the product that obtains can satisfy the requirement of " world's fuel oil standard " II class diesel oil, not only reach the purpose that deep desulfuration takes off virtue, also reached the purpose that satisfies " world's fuel oil standard " II class diesel oil with the catalytic cracking diesel oil direct production.
Test raw material is catalytic cracking diesel oil B, and stock oil character, processing condition and product property are listed in table 1, table 2 respectively.As seen from the table, this raw material aromaticity content is very high, sulphur content is moderate, under harsh operational condition, the product sulphur content that obtains is very low, aromaticity content can satisfy the requirement of " world's fuel oil standard " II class diesel oil, reached the purpose that deep desulfuration takes off virtue, and density reduces significantly with cetane value and increases substantially simultaneously.
Table 1
| | | |
| Feedstock property | Catalytic cracking diesel oil A | Catalytic cracking diesel oil B |
| Density (20 ℃), g/cm 3 | ????0.891 | ????0.920 |
| S, weight % | ????0.85 | ????0.41 |
| N，ppm | ????940 | ????500 |
| Total aromaticity content, weight % | ????55.1 | ????71.5 |
| Polycyclic aromatic hydrocarbon content, weight % | ????29.3 | ????43.5 |
| Boiling range (ASTM D-86), ℃ | ||
| Initial boiling point/10% | ????214/222 | ????203/226 |
| ????50％/90％ | ????284/352 | ????278/341 |
| Do | ????368 | ????362 |
| Cetane index (D4737) | ????36 | ????22 |
Table 2
| | | |
| Processing condition | ||
| The hydrogen dividing potential drop, MPa | ????6.4 | ????8.0 |
| Temperature of reaction, ℃ | ||
| First section | ????350 | ????350 |
| Second section | ????350 | ????350 |
| Volume space velocity, h -1 | ||
| First section | ????1.0 | ????1.0 |
| Second section | ????1.0 | ????1.0 |
| Hydrogen-oil ratio, Nm 3/m 3 | ||
| First section | ????500 | ????500 |
| Second section | ????500 | ????500 |
| Diesel product character | ||
| Yield, weight % | ????98.2 | ????99.0 |
| Density (20 ℃), g/cm 3 | ????0.835 | ????0.8577 |
| ?S，ppm | ????＜10 | ????＜10 |
| Total aromaticity content, weight % | ????19.6 | ????17.2 |
| Polycyclic aromatic hydrocarbon content, weight % | ????2.4 | ????2.9 |
| Boiling range (ASTM D-86), ℃ | ||
| Initial boiling point/10% | ????192/214 | ????181/210 |
| ????50％/90％ | ????268/348 | ????253/332 |
| Do | ????365 | ????362 |
| Cetane index (D4737) | ????52 | ????42 |
Claims (7)
1, a kind of processing method of desulfurizing and dearomatizing diesel oil deeply, it is characterized in that diesel raw material and circulating hydrogen are mixed into first section reactor and carry out hydrogenating desulfurization, hydrodenitrification, saturated, the aromatic hydrogenation saturated reaction of hydrogenation of olefins, reaction effluent enters the High Temperature High Pressure stripping tower and removes H through new hydrogen stripping
2S, NH
3After be mixed into second section hydrofining reactor again with hydrogen, the effluent of this reactor enters high-pressure separator, light pressure separator and separation column in proper order, separation column is divided into petroleum naphtha and diesel oil distillate with reaction product; The hydrogen rich gas that comes out from the High Temperature High Pressure stripping tower cleaning of evaporator of intaking mutually removes wherein behind the impurity and mixes from the isolated hydrogen rich stream of high-pressure separator, is circulated to first section and second section reactor after compression.
2, according to the method for claim 1, it is characterized in that described diesel raw material is catalytic cracking diesel oil, straight-run diesel oil, coker gas oil, visbreaking diesel oil or its mixture, boiling range is 180～400 ℃.
3, according to the method for claim 1, it is characterized in that processing condition are: hydrogen dividing potential drop 4.0～10.0MPa, 300～450 ℃ of temperature of reaction, liquid hourly space velocity 0.1～20h
-1, hydrogen-oil ratio 300～2000v/v.
4,, it is characterized in that first section is adopted hydrofining agent or modifying catalyst according to the method for claim 1.
5,, it is characterized in that described second section is adopted conventional Hydrobon catalyst according to the method for claim 1.
6,, it is characterized in that described Hydrobon catalyst is VIA or the VIII family base metal catalysts that loads on unformed aluminum oxide or the silica-alumina supports according to the method for claim 4 or 5.
7,, it is characterized in that described catalyst for hydro-upgrading is VIA or the VIII family base metal catalysts that contains on unformed aluminum oxide of loading on of a certain amount of molecular sieve or the silica-alumina supports according to the method for claim 4
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