CN102643670B - Combined processing method of heavy oil raw material - Google Patents
Combined processing method of heavy oil raw material Download PDFInfo
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- CN102643670B CN102643670B CN201110039568.0A CN201110039568A CN102643670B CN 102643670 B CN102643670 B CN 102643670B CN 201110039568 A CN201110039568 A CN 201110039568A CN 102643670 B CN102643670 B CN 102643670B
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Abstract
A combined processing method of heavy oil raw materials. According to the invention, a proper amount of radical terminators are added into heavy oil raw materials, and the mixture is introduced into a thermal conversion reactor for mild thermal conversion; the material flow after thermal conversion enters a contact cracking reactor for a contact cracking reaction to obtain a oil gas product. After mild thermal conversion, the heavy raw oil with the added radical terminator has a decreased molecule size and reduced viscosity, and thus when the heavy oil enters the contact cracking reactor, better contact with contact agents is realized, and product distribution is improved. In addition, the addition of the radical terminator into the heavy oil raw materials increases the yield of liquid products of the mild thermal conversion, and reduces the coke yield.
Description
Technical field
The present invention relates to a kind of in the situation that not there is not hydrogen, the combined method of the thermal non-catalytic cracking of hydrocarbon ils and catalytic thermal cracking.
Background technology
Along with the develop rapidly of world economy, the demand of oils is increased fast, and crude oil heaviness, in poor quality increasingly, the increasingly stringent of environmental requirement simultaneously, has proposed new challenge to refining of petroleum industry.
It is the key that improves crude oil yield of light oil that heavy oil is processed.In heavy oil upgrading technique, there are hydrogenation and decarburization two schemes, no matter be hydrogen addition technology or decarburization technique, its object is all the hydrocarbon ratio changing in heavy oil, make hydrocarbon reconfiguring, become by the lower heavy oil upgrading of hydrogen richness the light-end products that hydrogen richness is higher, meet the needs of national economy.The degree of saturation of hydrogenation products obtained therefrom is high, good security, but the source of cheap hydrogen is one of bottleneck of its development of puzzlement always.And for decarbonization process, heavy oil fluid catalytic cracking has requirement for the content of carbon residue, metal in raw material; There is the shortcomings such as liquid receipts are low, poor product quality in delayed coking.
The fluid coking of Exxon Neftegas Limited's exploitation and flexicoking technique are the process of fluidized decarbonization, this process liquids product yield is than the obvious height of delayed coking process, coke yield is 1.1～1.3 times of carbon residue, but exist the size distribution of coke granule inhomogeneous, easily produce compared with the problem such as megalump and finely-ground coke.
CN1504404A discloses the processing method that a kind of oil refining combines with gasification, and the method comprises the following steps: (1) petroleum hydrocarbon contacts, reacts with coke transfer agent in reactor; (2) separate the reaction oil gas generating and the coke transfer agent that reacts rear carbon deposit, reaction oil gas is sent into follow-up hydrocarbon products separation system, and the coke transfer agent of carbon deposit is delivered to vapourizing furnace after stripping; (3) in vapourizing furnace, the coke transfer agent of carbon deposit contacts with oxygen-containing gas with water vapour under gasification condition, to produce synthetic gas, makes the coke transfer agent of carbon deposit be regenerated simultaneously; (4) coke transfer agent after step (3) regeneration returns in the described reactor of step (1) and recycles.
Yield of light oil is low, coke yield height is the existing subject matter of prior art.
Summary of the invention
The object of the invention is on the basis of existing technology, a kind of heavy oil feedstock working method that improves liquid product yield is provided, the low problem of liquid product yield when technical problem to be solved is the very high inferior heavy oil of processing carbon residue.
Method provided by the invention comprises:
(1) in heavy oil feedstock, add free radical terminator, this logistics enters to relax in thermal conversion reaction device carries out thermal conversion reaction, obtains the product logistics after thermal transition,
(2) the product logistics after thermal transition enters contact cracking case, under contact cracking reaction condition, under the effect of contact substance, reacts, and obtains oil gas product and spent agent,
(3) the oil gas product of step (2) gained, through fractionation, obtains gas, gasoline fraction, diesel oil distillate and wax oil cut.
The Con. carbon (CCR) of the described heavy oil feedstock of step (1) is 5～40 % by weight, and 100 DEG C of viscosity are 50～4000mm2/s.The Con. carbon (CCR) of the described heavy oil feedstock of preferred steps (1) is 15～40 % by weight.Described heavy oil feedstock is selected from one or more in oil at the bottom of heavy crude, acid-containing raw oil, shale oil, long residuum, vacuum residuum, decompressed wax oil, wax tailings, deasphalted oil, hydrocracking tail oil, tank, coal tar, coal liquefaction residue oil or other secondary processing distillate.
Heavy oil feedstock viscosity of the present invention is large, atomization is difficult, if while directly entering contact cracking case without pre-treatment, macromolecular colloid, bituminous matter class material are not gasified totally, that part contacts with contact substance with the form of liquid phase, cause a large amount of condensation green cokes of macromole in heavy oil feedstock, liquid product yield is low.Method provided by the invention is before heavy oil feedstock enters contact cracking case, sets up and relaxes thermal conversion reaction device.Through relaxing after thermal transition, heavy oil feedstock molecule diminishes, reduced viscosity, thereby while making heavy oil feedstock enter contact cracking case, can react with contact substance better, improves products distribution, improves liquid product yield.
More particularly, heavy oil feedstock is through relaxing after thermal transition, and saturated point in heavy oil feedstock mainly generates cracked oil; And bituminous matter is many rings polycondensation aromatic hydrocarbons with many short-side chains, generate gas so be easy to occur side chain chain rupture; Fragrance point, colloid are between the intermediate component between saturated point and bituminous matter, can produce respectively gas, liquid hydrocarbon.Therefore, after relaxing thermal transition, heavy oil feedstock is decomposed into small molecules by macromole, and long side chain is fractured into short-side chain, makes the reduced viscosity of heavy oil feedstock, can optimize the contact of finish in the time of heavy oil feedstock cracking.
The free radical of free radical saturated hydrocarbon ratio or the free radical of alkene of aromatic hydrocarbons, resin and asphalt are more stable, more easily generate, therefore, the present invention is in thermal conversion processes, employing provides the method for free radical terminator to make aromatic hydrocarbons free radical, colloid free radical and bituminous matter free radical generate saturated molecule, reduce the bitum reactive behavior of green coke precursor simultaneously, stop the gathering between larger free radical.Thereby, heat scission reaction and condensation reaction are stopped before going too far, do not produce too much coke and gas, improve the effect of the shallow degree thermal transition of heavy oil feedstock.
Free radical terminator described in step (1) refers to and can form stable resultant by the Free Radical preferentially and in system, the material of retardance free chain reaction.Described free radical terminator is selected from one or more in hydrogen donor type free radical terminator, electron acceptor(EA) type free radical terminator and stabilized free fundamental mode free radical terminator.Hydrogen donor type free radical terminator is with active hydrogen atom, the mode shifting by chain, free radical in system is captured reactive hydrogen from terminator molecule, newly-generated Sequence of Relative Stability of Free Radicals is very strong, lost the ability that causes chain reaction, preferably hydrogen donor type free radical terminator is selected from one or more in phenol, pyrocatechol, quinhydrones, mercaptan, aniline, oxime, azanol and organic sulfonic acid.Electron acceptor(EA) type free radical terminator contains grips structure altogether, living radical in system can be first and its generation addition reaction, then coupling or disproportionation termination, preferred electron receptor type free radical terminator is selected from nitrophenyl phenolic compounds, zinc dialkyl dithiophosphate and quinones with and derivative in one or more, as 2, 2, 4-dinitrophenol, 2, 4-dinitrobenzene p-cresol, 2-sec-butyl-4, 6-dinitrophenol(DNP), N-{4-{ (1, 3-dimethylbutyl) imido grpup }-2, 5-cyclohexadiene }, 2, 6-di-t-butyl-4-benzylidene-hexamethylene-2, 5-dienone etc.The free radical of stabilized free fundamental mode free radical terminator in can stabilising system, can not trigger monomer, but can stop with living radical double-basis, preferably stabilized free fundamental mode free radical terminator is selected from one or more that are subject in resistance type compound oxygen radical of nitrogen and piperidine nitroxide free-radical compound, as 1,1-phenylbenzene-2-picryl hydrazine.
Taking heavy oil feedstock as benchmark, described in step (1), the add-on of free radical terminator is 5～5000 μ g/g, is preferably 20～500 μ g/g.
Described in step (1), relax the operational condition of thermal conversion reaction device: temperature is 350～490 DEG C, pressure (gauge pressure) is 0～1.5MPa, and the residence time is 5～120min.The preferred operational condition that relaxes thermal conversion reaction device: temperature is 380～440 DEG C, and pressure (gauge pressure) is 0.1～0.3MPa, and the residence time is 10～40min.
Described in step (2), contact cracking case form and be selected from riser reactor, fluidized-bed reactor, moving-burden bed reactor or downer reactor, or be two or more reactor combining in them.Described riser reactor and downer reactor are isodiametric or straighten footpath.
In step (2), contact reacts condition is: temperature of reaction is 300～700 DEG C, reaction times is 0.5～180 second, the weight ratio of contact substance and heavy oil feedstock is 3～25: 1, the weight ratio of water vapor and heavy oil feedstock is 0.02～0.40: 1, and reaction pressure (gauge pressure) is 0～1.0MPa.Heavy oil feedstock in contact cracking case with contact substance contact reacts, can realize the lighting of the larger degree of depth, and decarburization, demetalization.The oil gas product of gained, through fractionation, obtains gas, gasoline fraction, diesel oil distillate and wax oil cut.
Described in step (2), contact substance contains silica-alumina material, and micro-activity (is measured by standard A STM D3907-87) between 2～80, and particle size range is between 0～2000 μ m, and median size is between 70～150 μ m.Described silica-alumina material is selected from one or more in molecular sieve, amorphous silicon aluminium, carclazyte, kaolin, montmorillonite, rectorite leng, illite, chlorite, aluminum oxide, quartz sand, silicon sol.Described contact substance is a kind of good hydrothermal stability, has the spheroidal particle of certain catalytic cracking activity.Can be dried or method of agglomeration preparation by spraying.
Compared with prior art, advantage of the present invention is mainly reflected in the following aspects:
The first, add the heavy oil feedstock of free radical terminator through relaxing after thermal transition, reduced viscosity, while making heavy oil enter contact cracking case, atomizing effect improves, and has optimized finish contact; After part heavy oil macromole diminishes, boiling point lowering, enters after contact cracking case, and after contacting with contact substance, gasification rapidly, has prevented the macromolecular a large amount of green cokes of liquid.The second, this technique can utilize the idle plant modification in refinery for relaxing heat conversion device, does not need to increase large equipment, invests less.The 3rd, the free radical terminator adding can significantly reduce the generation that relaxes thermal transition coke, and can improve the reaction depth that relaxes thermal transition.The 4th, the add-on of free radical terminator is less, but larger on the impact of products distribution, can greatly improve the benefit of refinery.
Embodiment
The following examples will be further described method provided by the invention, but therefore not make the present invention be subject to any restriction.
Embodiment 1
The present embodiment adopts stock oil A as raw material, and its character is in table 1.The free radical terminator adopting is 2,6 ditertiary butyl p cresol, and taking stock oil A as benchmark, add-on is 300 μ g/g.Stock oil A and 2,6 ditertiary butyl p cresol are joined in thermal conversion reaction device and relax thermal conversion reaction, and its operational condition is: temperature of reaction is 430 DEG C, and the residence time is 20min, and reaction pressure (gauge pressure) is 0.2MPa.Stock oil A is after relaxing thermal transition, and the distribution of reaction product is as shown in table 2, and after reaction, raw material oil properties is as shown in table 3.
As can be seen from Table 3, stock oil A is greatly improved through the character that relaxes thermal transition after product, and the kinematic viscosity 100 DEG C time is by 926mm
2/ s reduces to 386mm
2/ s, average molecular mass reduces to 534 by 650.That is to say, the heavy oil feedstock oil that adds free radical terminator is after relaxing thermal transition, and reduced viscosity, molecular-weight average reduce, character be improved significantly, and can obtain higher liquid product yield and lower coke yield.
Comparative example 1
As different from Example 1, this comparative example does not add free radical terminator to raw material, but directly stock oil A is joined in thermal conversion reaction device, is 430 DEG C in temperature of reaction, the residence time is 20min, under the condition that reaction pressure (gauge pressure) is 0.2MPa, relaxes thermal transition.Stock oil A is after relaxing thermal transition, and the distribution of reaction product is as shown in table 2, and the character of reaction product is as shown in table 3.
As can be seen from Table 2, the coke yield of embodiment 1 is 0.9 % by weight, and liquid product yield is 96.4 % by weight.And coke yield in comparative example 1 is 2.5 % by weight, liquid product yield is 94.2 % by weight.So adopt method of the present invention, in heavy raw oil, add free radical terminator can make stock oil relax the liquid product yield raising of thermal transition, coke yield reduces.
As can be seen from Table 3, compared with comparative example 1, add the stock oil A of free radical terminator in embodiment 1 after relaxing thermal transition, it is more that viscosity, relative molecular mass reduce, more excellent to heavy-oil modified effect.
Embodiment 2
The raw material that the present embodiment adopts is stock oil B, and its character is in table 1.The free radical terminator adopting is zinc dialkyl dithiophosphate, and taking stock oil B as benchmark, its add-on is 300 μ g/g.Stock oil B and zinc dialkyl dithiophosphate are joined to generation mitigation thermal conversion reaction in thermal conversion reaction device, its operational condition: temperature of reaction is 430 DEG C, the residence time is 30min, reaction pressure (gauge pressure) is 0.2MPa.Logistics after thermal transition is sent in fluidized-bed contact cracking case, contact, react with the semi-synthetic sial contact substance that adopts spray drying technology to produce, the micro-activity of this semi-synthetic sial contact substance is 16.7 (measuring by standard A STM D3907-87), particle size range is 45～150 μ m, and median size is 94 μ m.Its operational condition: temperature of reaction is 500 DEG C, agent-oil ratio is 7, and water-oil ratio is 0.15, and weight hourly space velocity is 8h-1.As shown in table 4 through above-mentioned products distribution after treatment.As can be seen from Table 4, add the stock oil B of zinc dialkyl dithiophosphate through relaxing thermal transition and contacting after cracking, the liquid product yield obtaining is 66.00 % by weight, and coke yield is 22.46 % by weight.
Comparative example 2
As different from Example 2, stock oil B does not add zinc dialkyl dithiophosphate, and without relaxing thermal transition, but directly entering fluidized-bed contact cracking case, the contact substance identical with embodiment 2 contacts and reacts.Operational condition is: temperature of reaction is 500 DEG C, and agent-oil ratio is 7, and water-oil ratio is 0.15, and weight hourly space velocity is 8h-1.Its products distribution is as shown in table 4.Compared with embodiment 2, liquid product yield has reduced by 4.17 percentage points, and coke yield has risen 5.34 percentage points.
Table 1
| Project | Stock oil A | Stock oil B |
| Density (20 DEG C), g/cm 3 | 1.0121 | 1.0296 |
| Kinematic viscosity (100 DEG C), mm 2/s | 926 | 648 |
| Carbon residue, % by weight | 19.2 | 23.2 |
| Average molecular mass (VPO) | 650 | 735 |
| Four components, % by weight | ||
| Saturated point | 23.0 | 9.3 |
| Fragrance point | 34.7 | 53.6 |
| Colloid | 26.3 | 24.4 |
| Bituminous matter | 16.0 | 12.7 |
| Element, % by weight | ||
| C | 85.14 | 83.87 |
| H | 10.58 | 9.98 |
| S | 3.10 | 4.90 |
| N | 0.77 | 0.34 |
Table 2
| Project | Embodiment 1 | Comparative example 1 |
| Products distribution, % by weight | ||
| Gas | 2.7 | 3.3 |
| Gasoline | 3.7 | 4.2 |
| Diesel oil | 7.3 | 7.9 |
| 350～500 DEG C of cuts | 17.8 | 14.9 |
| 500 DEG C of cuts of > | 67.6 | 67.2 |
| Coke | 0.9 | 2.5 |
| Product liquid | 96.4 | 94.2 |
Table 3
| Project | Embodiment 1 | Comparative example 1 |
| Density (20 DEG C), g/cm 3 | 1.0034 | 1.0078 |
| Kinematic viscosity (100 DEG C), mm 2/s | 386 | 482 |
| Carbon residue, % by weight | 20.1 | 19.8 |
| Average molecular mass (VPO) | 534 | 559 |
Table 4
| Project | Embodiment 2 | Comparative example 2 |
| Products distribution, % by weight | ||
| Dry gas | 3.68 | 3.48 |
| Liquefied gas | 7.86 | 6.89 |
| Gasoline | 16.89 | 16.26 |
| Diesel oil | 21.82 | 21.68 |
| Wax oil | 27.29 | 23.89 |
| Coke | 22.46 | 27.80 |
| Product liquid | 66.00 | 61.83 |
Claims (12)
1. a combinational processing method for heavy oil feedstock, comprising:
(1) in heavy oil feedstock, add free radical terminator, this logistics enters to relax in thermal conversion reaction device carries out thermal conversion reaction, obtain the product logistics after thermal transition, the operational condition of described mitigation thermal conversion reaction device: temperature is 350～490 DEG C, pressure gauge pressure is 0～1.5MPa, the residence time is 5～120min, the Con. carbon CCR of described heavy oil feedstock is 15～40 % by weight, taking heavy oil feedstock as benchmark, the add-on of described free radical terminator is 20～500 μ g/g
(2) the product logistics after thermal transition enters contact cracking case, under contact cracking reaction condition, under the effect of contact substance, reacts, and obtains oil gas product and spent agent,
(3) the oil gas product of step (2) gained, through fractionation, obtains gas, gasoline fraction, diesel oil distillate and wax oil cut.
2. in accordance with the method for claim 1, it is characterized in that, 100 DEG C of viscosity of the described heavy oil feedstock of step (1) are 50～4000mm
2/ s.
3. in accordance with the method for claim 1, it is characterized in that, described heavy oil feedstock is selected from one or more in oil at the bottom of heavy crude, acid-containing raw oil, shale oil, long residuum, vacuum residuum, decompressed wax oil, wax tailings, deasphalted oil, hydrocracking tail oil, tank, coal tar, coal liquefaction residue oil or other secondary processing distillate.
4. in accordance with the method for claim 1, it is characterized in that, described in step (1), relax the operational condition of thermal conversion reaction device: temperature is 380～440 DEG C, pressure (gauge pressure-) is 0.1～0.3MPa, and the residence time is 10～40min.
5. in accordance with the method for claim 1, it is characterized in that, free radical terminator described in step (1) refers to and can form stable resultant by the Free Radical preferentially and in system, the material of retardance free chain reaction.
6. in accordance with the method for claim 5, it is characterized in that, free radical terminator described in step (1) is selected from one or more in hydrogen donor type free radical terminator, electron acceptor(EA) type free radical terminator and stabilized free fundamental mode free radical terminator.
7. in accordance with the method for claim 6, it is characterized in that, hydrogen donor type free radical terminator is selected from one or more in phenol, pyrocatechol, quinhydrones, mercaptan, aniline, oxime, azanol and organic sulfonic acid; Electron acceptor(EA) type free radical terminator be selected from nitrophenyl phenolic compounds, zinc dialkyl dithiophosphate and quinones with and derivative in one or more; Stabilized free fundamental mode free radical terminator is selected from one or more that are subject in resistance type compound oxygen radical of nitrogen and piperidine nitroxide free-radical compound.
8. in accordance with the method for claim 1, it is characterized in that, described in step (2), contact cracking case form and be selected from riser reactor, fluidized-bed reactor, moving-burden bed reactor or downer reactor, or be two or more reactor combining in them.
9. in accordance with the method for claim 8, it is characterized in that, described riser reactor and downer reactor are isodiametric or straighten footpath.
10. in accordance with the method for claim 1, it is characterized in that, in step (2), contact reacts condition is: temperature of reaction is 300～700 DEG C, reaction times is 0.5～180 second, the weight ratio of contact substance and heavy oil feedstock is 3～25: 1, the weight ratio of water vapor and heavy oil feedstock is 0.02～0.40: 1, and reaction pressure gauge pressure is 0～1.0MPa.
11. according to the method for claim 1, it is characterized in that, described in step (2), contact substance contains silica-alumina material, and micro-activity is measured by standard A STM D3907-87 between 2～80, particle size range is between 0～2000 μ m, and median size is between 70～150 μ m.
12. according to the method for claim 11, it is characterized in that described silica-alumina material is selected from one or more in molecular sieve, amorphous silicon aluminium, carclazyte, kaolin, montmorillonite, rectorite leng, illite, chlorite, aluminum oxide, quartz sand, silicon sol.
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| US10596583B2 (en) * | 2016-05-11 | 2020-03-24 | General Electric Technology Gmbh | System and method for regulating the viscosity of a fluid prior to atomization |
| CN110607188B (en) * | 2018-06-15 | 2021-05-14 | 中国石油化工股份有限公司 | Pretreating agent and pretreating method for heavy oil fluidized processing raw material |
| CN110607189B (en) * | 2018-06-15 | 2021-05-14 | 中国石油化工股份有限公司 | Pretreating agent and pretreating method for heavy oil fluidized processing raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4378288A (en) * | 1981-02-09 | 1983-03-29 | Mobil Oil Corporation | Coking process by addition of free radical inhibitors |
| CN1827744A (en) * | 2005-03-03 | 2006-09-06 | 中国石油化工股份有限公司 | Method for processing crude oil with high acid value |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4378288A (en) * | 1981-02-09 | 1983-03-29 | Mobil Oil Corporation | Coking process by addition of free radical inhibitors |
| CN1827744A (en) * | 2005-03-03 | 2006-09-06 | 中国石油化工股份有限公司 | Method for processing crude oil with high acid value |
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