CN1351125A - Hydrogenating process for reducing viscosity of heavy oil or residual oil - Google Patents
Hydrogenating process for reducing viscosity of heavy oil or residual oil Download PDFInfo
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- CN1351125A CN1351125A CN 00123147 CN00123147A CN1351125A CN 1351125 A CN1351125 A CN 1351125A CN 00123147 CN00123147 CN 00123147 CN 00123147 A CN00123147 A CN 00123147A CN 1351125 A CN1351125 A CN 1351125A
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Abstract
A hydrogenating process for reducing viscosity of heavy or residual oil in the existance of hydrogen-contained gas and dispersion-type catalyst is prepared through heating said heavy or residual oil and catalyst uniformly dispersed in it, adding it along with hydrogen-contained gas to reactor, and cracking reaction at 360-460 deg.C and 1-15 MPa to produce low-viscosity fuel oil or light fractional oil with low boiling point.
Description
The present invention relates to the hydrogenation visbreaking processing method of a kind of thickness weight, residual oil.
Because the minimizing of low-density oil resource, the refinery is faced with increasing heavy of processing and viscous crude oil.How economical and efficient ground is the major issue that refinery faces with the product that thickness heavy oil or residual oil become high value, and viscosity breaking is with these heavy oil lightings or directly becomes an important method of product.Another purpose of visbreaking technology is to produce heavy fuel oil.Many boilers that aim at combusting heavy oil and design are arranged in operation all over the world, especially large ship is main fuel especially with the heavy fuel oil.
The subject matter of visbreaking process is that residual oil also condensation reaction will take place when scission reaction takes place, if cracking severity increases, then condensation reaction also increases, and stops up boiler tube and reactor until green coke.In addition, even do not worry device running period, a large amount of green coke precursors (available toluene insolubles measurement) that cracking and condensation reaction produce also cause the visbreaking unstable products, make oil fuel store and transportation in layering even precipitate.Therefore the visbreaking process must carefully be controlled reaction depth with the minimizing green coke, and the low visbreaking purpose that do not reach of reaction depth.
For, residual oil heavy from thickness obtain low viscous steady fuel oil production as much as possible or benzoline, many oil companies are all in the technology of studying and improve viscosity breaking, except traditional hot visbreaking and delayed heat visbreaking, there are a variety of hydrovisbreakings and hydrogenation viscosity breaking technology method to carry again.
In order to improve the severity of visbreaking operation, Lummus Crest company proposes the heavy constituent in the visbreaking product are gone out through solvent extraction or centrifugation about 15% in U.S. Pat 4773986, tell after the heavy constituent the visbreaking product again through the dilution of blending light oil to reach the fixed viscosity requirement of merchantable fuels fuel oil meter.Improve depth of conversion under the condition of not mending hydrogen, it is relatively more current way that Jiao that condensation in the product is obtained and heavy constituent are separated to obtain uniform visbreaking product.
The Mobil oil company proposes a kind ofly to make the catalysis visbreaking process of catalyzer with tin anhydride in U.S. Pat 5057204, it is said that the hydrogen that can change the residual oil molecule distributes.Residual oil is under the viscosity breaking operational condition, and part hydrogen is shifted out the unstable molecule fragment reaction that produces with cracking from the residual oil transfer, thereby makes these unsettled crackates stable.The hydrogen that adding tin anhydride catalyzer can make the residual oil transfer be shifted out during the visbreaking reaction obviously increases, thereby can suppress the green coke process, increases the reaction depth of process under the prerequisite that does not shorten on-stream time.Because the tin anhydride catalyzer of Mobil company must be supported on the solid carriers such as coal, coke or carclazyte, and these solid particulates very easily become the green coke carrier, the reaction of catalyzer and carrier thereof itself and absorption generates burnt, all caused ash and insolubles increase in the visbreaking product, made unstable products.
The Phillips oil company proposes to do with the diphenol compounds of molybdenum the hydrovisbreaking process of catalyzer in U.S. Pat 4802972, when catalyzer add-on (in molybdenum) is 40～50 μ g/g, long residuum carries out hydrogenation viscosity breaking reaction under 427 ℃, 13.7MPa (2000psig) hydrogen pressure, 10% when the product coking yield can be from catalyst-free reduces to 2.9%.
Up to the present, also there be not both can improving the visbreaking operating severity by a relatively large margin and not reduce the viscosity breaking improvement project in operational cycle substantially and putting forward of a kind of economy.
The objective of the invention is to find a kind of can under higher conversion, the operation (high severe this degree) and the process hydrogenation viscosity breaking method of green coke (growing the operational cycle) not substantially.
Another object of the present invention is to find a kind of method with refinery low value raw material production low-sulfur heavy fuel oil.Adopt this method can make full-bodied raw material under than the demulcent reaction conditions, react the oil fuel product that production meets the requirement of oil fuel viscosity index, mix a large amount of diesel oil and regulate viscosity satisfying index request and need not return, thereby reduce the production cost of oil fuel.
Be suitable for heavy oil of the present invention and residual oil and comprise various normal pressures or vacuum residuum, topping heavy oil, solvent deoiling pitch, oil sands bitumen, shale wet goods.
The present invention includes the following aspects: water-soluble disperse type catalyzer or other efficient disperse type catalyzer that will have hydrogenation activity are dispersed in the visbreaking stock oil.
Be heated to the viscosity breaking temperature of reaction after the uniform visbreaking raw material of catalyst mix mixes hydrogen in process furnace, the upper reaches enters the visbreaking reactor reaction then.Viscosity breaking and hydrogenation reaction take place in heavier feedstocks oil in reactor.The processing condition of hydrogenation visbreaking are: reaction pressure is 1～15MPa, better is 2～10MPa; Temperature of reaction is 360～460 ℃, better is 380～450 ℃; Reaction time is 20 minutes to 3 hours; Hydrogen to oil volume ratio (under the standard pressure) is 100～1000.
Catalyzer can be oil-soluble, it also can be solid fines, also can be the aqueous solution of metal-salt, the water-soluble disperse type catalyzer that preferably adopts the contriver to propose in Chinese patent CN 1045307B and U.S. Pat 5948721,6004454 contains elements such as Mo, Ni, P in the aqueous catalyst solution, Mo content is 2～15w%, better be 5～10w%, Ni is 0.1～1w%, better is 0.2～1w%, and P is that 0.2～2w% better is 0.2～1w%.
The visbreaking reactor can be with similarly installing with the hydrogenation of residual oil suspended bed reactor, and the visbreaking raw material of mixed catalyzer and hydrogen enters from reactor bottom, and reactor is passed through at the upper reaches.Because residual oil is evenly distributed in the stirring action of hydrogen, reactor, the local mistake can occur and react and the hyporeactive problem of part material.
Be that example is further introduced technical scheme of the present invention with two concrete viscosity breaking flow processs below.Fig. 1 is the hydrogenation visbreaking unit schematic flow sheet of low temperature charging; Fig. 2 is the hydrogenation visbreaking unit schematic flow sheet of high temperature charging, specifically is described below below in conjunction with accompanying drawing:
Residual oil raw material and disperse type catalyzer enter blender 3 from pipeline 1 and 2 respectively. Blender 3 can be An agitator tank also can be a colloid mill or static mixer or other conventional mixing apparatus, will Residual oil and catalyst mix are even. If material viscosity is especially big, be difficult to below 100 ℃ with routine side The method mixing also can be earlier mixes catalyst with a small amount of low viscosity residual oil, and then with full-bodied charging Mix. Charging after mixing enters heater 8 through pipeline 4 and pump 5, pipeline 7, and hydrogen is via pipeline 6 Enter system. Charging is heated to 430 ℃ in heating furnace 8, enter reactor 10 through pipeline 9 then. Reaction Product enters high-pressure separator 12 via pipeline 11, tells gas and degass through pipeline 14 that body reclaims and segregative line System 15, hydrogen can loop back reactor by pipeline 16 behind washing, purifying, and light oil goes out device through pipeline 17. The liquid material that high-pressure separator 12 is told goes to separate (production light distillate) or concocts (living through pipeline 13 Produce the low viscosity heavy fuel oil) system.
When processing directly the high-temperature feeding from upstream device, adopt and directly in feeding line, inject catalysis The method of agent, Fig. 2 is seen in the flow process signal. From the warm sludge oil of pipeline 4 introducings from upstream device. Catalyst water Solution is squeezed into by pump 3, through a distributor 5 aqueous solution is spurted in the residual oil, and residual oil is at flow process The catalyst neutralisation aqueous solution. High pressure hydrogen mixes rear being sent into by pipeline 7 by pipeline 6 introducings and adds with residual oil Hot device 8, the charging that is heated to reaction temperature is carried out the hydrogenation visbreaking by pipeline 9 introducing reactors 10. Reaction is produced Thing enters high-pressure separator 12 by pipeline 11, tells gas and degass through pipeline 14 that body reclaims and piece-rate system 15, hydrogen loops back reactor by pipeline 16 behind washing, purifying, and light oil goes out device through pipeline 17. High pressure The liquid material that separator 12 is told goes separation (production light distillate) or blending (to produce low through pipeline 13 The viscosity heavy fuel oil) system.
If the visbreaking purpose is in order to obtain low-viscosity fuel oil, then to react to advance under than the mitigation condition OK, for example 380～430 ℃ of reaction temperatures, reaction pressure 1～5MPa. If the visbreaking purpose is Big limit obtains light distillate, and then reaction can be than carrying out under the harsh conditions, and for example 420～460 ℃, 8～15MPa.
Advantage of the present invention is:
1 high-activity hydrogenation catalyst that has adopted the present invention to propose, reaction exists and hydroconversion condition at hydrogen Under carry out so that the unstable molecule fragment that thickness residual oil produces in cracking process is saturated by hydrogenation, the contracting The tendency of closing with green coke is suppressed in a large number, the green coke not thereby visbreaking can carry out under higher conversion, Device can the long period smooth operation.
2 owing to the water-dispersion type high activated catalyst that has adopted the present invention to propose, so that the catalyst addition Can be down to 100 μ g/g even lower. Because the catalyst addition is few, again without the solid carrier, basically Do not increase ash content and insolubles content in the visbreaking residue, thereby avoided separating heavy from the visbreaking product The problem of component and solid particle.
For further specifying all main points of the present invention, enumerate following examples, but be not limited to each specific embodiment.
Load weighted industrial molybdenum oxide, basic nickel carbonate, phosphoric acid are put into reactor, and adding water, to be modulated into containing metal Mo and Ni total amount be that 7.6% the disperse type catalyzer aqueous solution is standby.Wherein the weight ratio of various elements is Ni: Mo: P=0.07: 0.04: 1.0.
Embodiment metal water more than 2 dissolubility Preparation of catalysts
Load weighted molybdenum oxide, phospho-wolframic acid, cobaltous acetate, basic nickel carbonate, phosphoric acid are put into reactor, and adding water, to be modulated into the multi-metal dispersive catalyst aqueous solution of total metal contents in soil 9.5w% standby.Wherein the weight ratio of various metallic elements is Ni: W: Co: P: Mo=0.09: 0.9: 0.05: 0.07: 1.0.
In the autoclave that a 700mL band stirs, put in the Ah (a kind of typical sulphur-bearing crude that originates in the Middle East) vacuum residuum (4.85%, 100 ℃ of viscosity 3100mm of sulphur content
2/ s) 150g adds the aqueous catalyst solution of a certain amount of embodiment 1 preparation.Closed reactor carries out hydrogenation viscosity breaking reaction 1 hour under hydrogen pressure 1～5MPa, 360～430 ℃ of conditions.Reaction product is surveyed the toluene insolubles productive rate respectively, gasoline fraction and fraction of diesel oil yield, 537 ℃
+Transformation efficiency and full cut generate oil viscosity, test conditions and the results are shown in Table 1.
Table 1 in Ah vacuum residuum visbreaking test-results example embodiment 3 embodiment 4 embodiment 5 embodiment 6 Comparative Examples 1 test conditions: temperature of reaction ℃ 380 400 420 435 435 reaction pressure MPa, 14355 catalyzer, μ g/g 70 50 250 100 0 visbreaking product characteristicses:
Toluene insolubles, w% 0.07 0.07 0.18 0.74 10.60
＜180℃，w％ 0.7 2.1 4.5 10.0 17.7
Fraction of diesel oil, w% 2.1 6.3 12.0 19.7 32.1
537 ℃
+Transform, w% 8.0 16.8 40.4 58.1 79.2
Full cut generates oil viscosity, and 100 ℃, 610 366 29.8 10.9 have coke button, inhomogeneous
mm
2/s
Full cut generates oily sulphur content, and w% 2.48 2.16 1.78 1.67 3.97
Compare with the hot visbreaking of hydrogen (Comparative Examples 1) that faces that does not add catalyzer, can under the situation at green coke not raw material residual oil be converted into benzoline in a large number at residual oil viscosity breaking method of the present invention under identical temperature of reaction and the hydrogen pressure, the viscosity of product and sulphur content have also obtained significantly reducing.In addition, when (as embodiment 4) operated under the higher conversion condition, the toluene insolubles content of visbreaking product did not have coke to generate still less than 1%.
The hydrogenation visbreaking of embodiment 7～9 several homemade residual oil
In the autoclave that a 700mL band stirs, put into 150g residual oil, add a certain amount of disperse type catalyzer.Closed reactor carries out hydrogenation viscosity breaking reaction under hydrogen pressure 2～8MPa, 380～430 ℃ of conditions.Reaction product is surveyed the toluene insolubles productive rate respectively, gasoline fraction and fraction of diesel oil yield, 537 ℃
+Transformation efficiency and full cut generate oil viscosity, and operational condition and reaction result see Table 2.
VR Xinjiang, the viscosity breaking acetonideexample 789 stock oil Liaohe River VR isolated island VR stock oil viscosity of table 2 different material residual oil, 100 ℃, mm
2/ s 3,600 1,600 1300 reaction conditionss: reaction pressure, MPa 832 reaction times, h 321 temperature, ℃ 430 420 385 catalyst rings alkanoic acid Mo examples 2 preparation examples 1 preparation catalyzer add-on, μ g/g 150 80 30 product characteristicses: toluene insolubles, 0.98 0.41 0.37＜180 ℃ of w%, 6.5 4.5 3.2180～350 ℃ of w%, w% 16.3 15.0 10.5 full cuts generate oil viscosity, 100 ℃, 9.6 26 38mm
2/ s537 ℃
+Transform, w% 61.1 43.4 36.1
The residual hydrogenation viscosity breaking reaction that embodiment 10～12 explanations are carried out on continuous apparatus.Fig. 1 is seen in the signal of residual hydrogenation visbreaking continuous apparatus.Residual oil raw material oil (matter crude oil subtracts slag and Iran and subtracts slag and mix in the Saudi Arabia, and weight ratio is 1: 1) and embodiment 1 prepared aqueous catalyst solution mix in mixing tank 3.Charging after mixing enters well heater 8 through pipeline 4 and pump 5, pipeline 7, and hydrogen enters system via pipeline 6.Charging is heated in process furnace to fixed temperature, enters reactor 10 through pipeline 9 then.Reaction product enters high-pressure separator 12 via pipeline 11, tells gas and degass through pipeline 14 that body reclaims and separation system 15, and hydrogen loops back reactor by pipeline 16 behind washing, purifying.The liquid material that high-pressure separator is told goes out system through pipeline 13.Survey each cut productive rate and toluene insolubles.Operational condition and reaction result see Table 3.
Viscosity breaking acetonideexample 89 10 reaction conditionss of table 3 residual oil on the continous way visbreaking unit:
Reaction pressure, MPa 555
Reaction time, h 322
Temperature, ℃ 400 420 435
Hydrogen-oil ratio, v/v 300 500 700
The catalyzer add-on, μ g/g 100 50 200 product characteristicses:
Toluene insolubles, w% 0.05 0.11 0.94
＜180℃，w％ 3.5 4.5 9.2
180～350℃，w％ 10.3 15.0 20.5
537 ℃
+Transform, w% 26.1 48.4 72.1
Under the high temperature and the high severity in long reaction times, operate 537 ℃
+The heavy constituent transformation efficiency was up to 72% o'clock, and the toluene insolubles content in the product shows that still less than 1% viscosity breaking method of the present invention not only can reduce residual oil viscosity significantly, can also obtain the lower boiling benzoline in a large number.
Claims (9)
1. a weight, residual hydrogenation viscosity breaking method, it is characterized in that the upper reaches enters visbreaking reactor after weight, residual oil and decentralized hydrogenation catalyst as the visbreaking raw material and the hydrogen-containing gas Hybrid Heating carries out viscosity breaking and hydrogenation reaction, and reaction product obtains benzoline, low-viscosity fuel oil ingredient or directly as low-viscosity fuel oil through separation.
2. according to the described hydrogenation viscosity breaking method of claim 1, it is characterized in that the processing condition of hydrogenation visbreaking are: reaction pressure is 1～15MPa; Temperature of reaction is 360～460 ℃; The reaction solution hourly space velocity is 0.2～1.5h
-1Hydrogen to oil volume ratio is 100～1000.
3. according to the described hydrogenation viscosity breaking method of claim 2, it is characterized in that the processing condition of hydrogenation visbreaking are: reaction pressure is 2～10MPa; Temperature of reaction is 380～450 ℃; The reaction solution hourly space velocity is 0.2～1.0h
-1Hydrogen to oil volume ratio is 100～1000.
4. according to the described hydrogenation viscosity breaking method of claim 1, it is characterized in that said disperse type catalyzer is water-soluble disperse type catalyzer.
5. according to the described hydrogenation viscosity breaking method of claim 1, it is characterized in that said catalyzer is a kind of water-soluble disperse type catalyzer, contains Mo, Ni, P element in the aqueous catalyst solution.
6. according to the described hydrogenation viscosity breaking method of claim 5, it is characterized in that said Mo content is 2～15w%, Ni is 0.1～1w%, and P is 0.2～2w%.
7. according to the described hydrogenation viscosity breaking method of claim 5, it is characterized in that said Mo content is 5～10w%, Ni is 0.2～1w%, and P is 0.2～1w%.
8. according to the described hydrogenation viscosity breaking method of claim 2, the catalyst levels that it is characterized in that the floating bed hydrogenation process is 10～5000 μ g/g.
9. according to the described hydrogenation viscosity breaking method of claim 1, the catalyst levels that it is characterized in that the floating bed hydrogenation process is 10～500 μ g/g.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618324A (en) * | 2011-01-27 | 2012-08-01 | 中国石油化工股份有限公司 | Combination method for processing heavy oil raw material |
| CN103102934A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Pretreatment method for inferior heavy oil |
| CN103102984A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Hydrogenation combined process for inferior heavy oil |
| CN106147836A (en) * | 2015-03-27 | 2016-11-23 | 中国石油天然气股份有限公司 | Heavy oil modifying and viscosity reducing method and application |
| CN108587675A (en) * | 2018-03-29 | 2018-09-28 | 南京大学连云港高新技术研究院 | A kind of method of heavy oil visbreaking |
| CN110218581A (en) * | 2018-03-02 | 2019-09-10 | 中国海洋石油集团有限公司 | A kind of method for modifying of oil sands bitumen |
| CN111417702A (en) * | 2017-08-21 | 2020-07-14 | 沙特阿拉伯石油公司 | Removal of asphaltenes from crude oil using solid heteropoly compounds without the use of solvents |
-
2000
- 2000-10-26 CN CN 00123147 patent/CN1123633C/en not_active Expired - Lifetime
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618324A (en) * | 2011-01-27 | 2012-08-01 | 中国石油化工股份有限公司 | Combination method for processing heavy oil raw material |
| CN103102934A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Pretreatment method for inferior heavy oil |
| CN103102984A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Hydrogenation combined process for inferior heavy oil |
| CN103102984B (en) * | 2011-11-10 | 2015-04-01 | 中国石油化工股份有限公司 | Hydrogenation combined process for inferior heavy oil |
| CN103102934B (en) * | 2011-11-10 | 2015-04-15 | 中国石油化工股份有限公司 | Pretreatment method for inferior heavy oil |
| CN106147836A (en) * | 2015-03-27 | 2016-11-23 | 中国石油天然气股份有限公司 | Heavy oil modifying and viscosity reducing method and application |
| CN111417702A (en) * | 2017-08-21 | 2020-07-14 | 沙特阿拉伯石油公司 | Removal of asphaltenes from crude oil using solid heteropoly compounds without the use of solvents |
| CN110218581A (en) * | 2018-03-02 | 2019-09-10 | 中国海洋石油集团有限公司 | A kind of method for modifying of oil sands bitumen |
| CN110218581B (en) * | 2018-03-02 | 2021-07-20 | 中国海洋石油集团有限公司 | Modification method of oil sand asphalt |
| CN108587675A (en) * | 2018-03-29 | 2018-09-28 | 南京大学连云港高新技术研究院 | A kind of method of heavy oil visbreaking |
| CN108587675B (en) * | 2018-03-29 | 2020-06-09 | 南京大学连云港高新技术研究院 | Heavy oil viscosity reducing method |
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