CN105950206A - Device and method for simulating carbon-base macromolecule delayed coking process to achieve quick coking and coke forming - Google Patents
Device and method for simulating carbon-base macromolecule delayed coking process to achieve quick coking and coke forming Download PDFInfo
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- CN105950206A CN105950206A CN201610411629.4A CN201610411629A CN105950206A CN 105950206 A CN105950206 A CN 105950206A CN 201610411629 A CN201610411629 A CN 201610411629A CN 105950206 A CN105950206 A CN 105950206A
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- 238000004939 coking Methods 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000571 coke Substances 0.000 title abstract description 20
- 229920002521 macromolecule Polymers 0.000 title abstract 4
- 230000008569 process Effects 0.000 title description 10
- 230000003111 delayed effect Effects 0.000 title description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 78
- 239000000463 material Substances 0.000 claims description 19
- 230000000694 effects Effects 0.000 claims description 16
- 230000008859 change Effects 0.000 claims description 15
- 238000004088 simulation Methods 0.000 claims description 12
- 230000035939 shock Effects 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000003546 flue gas Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229910052756 noble gas Inorganic materials 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 39
- 235000019198 oils Nutrition 0.000 description 38
- 239000000295 fuel oil Substances 0.000 description 11
- 238000012545 processing Methods 0.000 description 7
- 239000011331 needle coke Substances 0.000 description 6
- 238000007670 refining Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 241000772415 Neovison vison Species 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000116 mitigating effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 206010020843 Hyperthermia Diseases 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000036031 hyperthermia Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002006 petroleum coke Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005491 wire drawing Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical group [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000002010 green coke Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000009491 slugging Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G9/00—Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G9/005—Coking (in order to produce liquid products mainly)
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a device for simulating quick preparation of coke samples by means of carbon-base macromolecules under different coking conditions. The device comprises a reaction still and a heating furnace, wherein the reaction still is located in a cavity of the heating furnace, a reaction still cover used for sealing the reaction still is arranged at the upper end of the reaction still, and an air outlet is formed in the reaction still cover and connected with a backpressure valve through an air outlet pipeline; a raw material inlet and a circulation oil inlet are formed in the annular wall of the reaction still and connected with a raw oil tank and a circulation oil tank through pipelines respectively; an air inlet is formed in a bottom cover of the reaction still and connected with an air supply system through an air inlet pipeline; the heating furnace is connected with a program temperature controller. The invention further discloses a method for simulating preparation of coke samples by means of carbon-base macromolecules under different coking conditions with the device. By the adoption of the device and method, quick preparation of coke samples from carbon-base macromolecules can be achieved under different conditions, and the influence of different coking conditions on coking morphology of coke samples can be researched.
Description
Technical field
The invention belongs to mink cell focus technical field of hot working, be specifically related to a kind of simulation carbonaceous macromole delayed coking the most burnt
The device and method of coking is prepared in change.
Background technology
World's crude resources heaviness day by day and in poor quality, especially add the cost advantage that processing heavy crude is brought, lead
Global petrochemical industry refining enterprise (U.S.: even as high as 2/3 refining enterprise) that there are about 42% of cause is tended to raising and is processed raw material middle heavy
The ratio of matter crude oil, the heavy oils quantity such as the residual oil of output, FCC slurry, ethylene bottom oil is also inevitable therewith increases therewith.This
A little heavy oilses or tenor height, hetero atom (sulfur, nitrogen, oxygen) content height；Rich in aromatic hydrocarbons, alkene structures, surely
Qualitative difference, broadly falls into the inferior heavy oil that difficulty of processing is bigger.One of significant challenge that petrochemical industry refining enterprise of China currently faces is
These inferior heavy oil of processing and utilization the most to greatest extent, improve the level of resources utilization, increase Business Economic Benefit, therefore, high
Effect converts the process technology of heavy oils becomes each big refining enterprise and the unprecedented focus of attention of international energy company.The U.S.'s " stone
Oil the epoch " comment Heavy Oil Processing Technology time point out, a new generation oil refining process mainly have three kinds, i.e. RFCC, delay coke
Change and heavy-oil hydrogenation.Wherein delay coking process is as heavy oil degree of depth hot-working process, is particularly suitable for processing heavy oil material.
Using heavy crude oil residue as raw material, delayed coking (abbreviation coking) is used to be processed, while producing lightweight oil plant
Can the substantial amounts of petroleum coke of by-product.The petroleum coke that coking typically produces is spongy, thus is referred to as sponge coke.But
In the actual course of processing, along with asphaltene in vacuum residues and the increase of tenor, it is a kind of special also to generate in coking
Coking coking form shot coke.Shot coke is a kind of the most special, the most not of uniform size, diameter Distribution 1-4mm it
Between, fine and close low space, smooth surface less porous, the most spherical or ellipticity burnt ball group of shape such as BB bullet connect and form, therefore be called
Shot coke.During coking heavy oil, the generation of shot coke can bring a series of production and safety problem: during coke drum dismounting bottom,
The loose structure of shot coke makes the process of coming down in torrents be difficult to control；Shot coke is main green coke bed cooling difficulty, after cold Jiao still
There is the situation that local temperature is too high；Site operation personnel is deposited by the accident landslide in coke-removing procedure and the high-temperature material in focus layer
At bigger security threat；Make coke drum produce " slugging " phenomenon in process of production, cause that tower body is improper to be rocked, formation
Potential safety hazard.
The additionally the most widely used coking technology of energy enterprise, processes FCC slurry, ethylene bottom oil raw material, produces needle coke.Needle-like
Afocal is seen as silver gray, is had the porosu solid of metallic luster, and its structure has the texture that substantially flows, and hole is greatly and less and slightly in ellipse
Shape, granule has bigger length-width ratio, just like the texture trend of threadiness or needle-like, therefore gains the name.
In general, the characteristic of heavy oils coking coking is to affect delayed coking changing effect, processing cost, product classification
One of key factor, the priority research areas of the study on regulation of coking coking characteristic current energy industry especially.Become in coking at present
In the research of burnt characteristic, the method for preparation coking coking sample is mainly reacted by autoclave or medium-sized coking plant is carried out.Adopt
The method preparing Jiao's sample by autoclave simulation coking thermal process, it main problem is that and actual delay coking deviation strengthens,
Such as, autoclave is difficult to control to the pressure of conversion process, it is impossible to air-flow ease bigger on the impact of coking characteristic in simulation coking
Go out, shear, stir and shock effect, the recycle oil in heavy oils coking can not be implemented and inject.Use medium-sized coking
Method is the most loaded down with trivial details, prepares a coking sample and not only takes time and effort, is difficult to accomplish quickly to prepare, in order to after fast carrying out
Continuous analysis and characterization, the most uneconomical.Therefore, a kind of carbonaceous macromole of simulating is developed under different coking conditions
The quickly device and method of the burnt sample of preparation, the research for different coking condition Coke-oven sample coking performances has highly important
Meaning.
Summary of the invention
For above-mentioned prior art, it is an object of the invention to provide and a kind of simulate carbonaceous macromole under different coking conditions quickly
The device and method of the burnt sample of preparation, it is possible to achieve under different condition, carbonaceous macromole quickly prepares coking sample, is used for studying different Jiao
The impact on coking sample coking pattern of the change condition.
For achieving the above object, the present invention adopts the following technical scheme that
According to the first aspect of the invention, it is provided that a kind of carbonaceous macromole of simulating quickly prepares burnt sample under different coking conditions
Device, including: reactor and heating furnace；
Described reactor is positioned at the cavity of heating furnace, and the upper end of reactor is provided with the reaction kettle cover for sealed reactor, described
Reactor lid is provided with gas outlet, is connected with back pressure valve by outlet gas line, for the pressure setting and controlling in reactor
Power；
The ring wall of reactor is provided with material inlet and recycle oil charging aperture, respectively by pipeline and material tank and circulation oil tank phase
Even；The interpolation of oil can be circulated while raw material reaction, change the structure composition of reaction raw materials, for specific form coking
Necessary condition is provided.
The bottom of reactor is provided with air inlet, is connected with air supply system by gas feed pipeline；Existed by gas flow change
In reactor simulation formed varying strength gas shock, escape, shear, agitation effects.
Described heating furnace is connected with programmable temperature control device, is effectively controlled the temperature in body of heater by programmable temperature control device.
Further, described outlet gas line is additionally provided with condenser, uses the oil gas that circulating water condensing coking produces, it is to avoid
Damage back pressure valve.
Further, on described outlet gas line, it is additionally provided with Pressure gauge after the condenser, for monitoring the pressure in reactor
Power.
Further, described gas feed pipeline is provided with effusion meter, is used for measuring gas injection flow velocity.
Further, the pipeline between material tank and material inlet is provided with first flow pump, circulation oil tank and recycle oil charging
Pipeline between Kou is provided with second flow pump；Pass through first flow pump and second flow pump respectively to the raw material in pipeline and circulation
Fluid rate of flow of fluid regulates and controls.
Further, described air supply system includes that oxidizing gas feeder, reducibility gas feeder and noble gas supply
Device of air.Preferably, described oxidizing gas feeder is oxygen feeder；Described reducibility gas feeder is hydrogen
Gas or carbon monoxide feeder；Described noble gas feeder is nitrogen feeder.
Preferably, the temperature of reaction unit in the range of described heating furnace uses medium/low frequency electromagnetic oscillation effect fast lifting solenoid
Degree, its energy energy produced acts on inside metallic reactors within a short period of time, temperature in maximum quick-lift attachreactor,
Improve heat transfer efficiency, reduce reaction raw materials scorch time.
Further, the outside of described heating furnace is provided with heat-insulation layer, is used for reflecting hyperthermia radiation energy, completely cuts off thermal convection current, reduces
Heat loss.
Further, described programmable temperature control device includes thermocouple and controls terminal；Programmable temperature control device design temperature program can be passed through
Change sequence, make reaction temperature according to arranging change (including linear temperature increase, constant temperature etc.), in order to reflect coking temperature.
According to the second aspect of the invention, it is provided that one utilizes said apparatus simulation carbonaceous macromole the most quickly to prepare
The method of burnt sample, step is as follows:
(1) heating furnace is opened, the air in emptying reactor, set back pressure valve steady pressure value, make reacting kettle inner pressure tie up
Hold at preset value, in order to reflect pressure in coking plant；Open programmable temperature control device, design temperature change of program sequence, make reaction
Temperature is according to arranging change, in order to reflect coking temperature；
(2) reach to preset after reaction temperature, by gas injection in gas inlet tube alignment reactor, after preventing reaction raw materials from injecting from
Leaking at gas feed, open first flow pump, inject reaction raw materials, raw material is rapidly heated to instead at reaction kettle body inner bottom part
Answer temperature, pyrogenetic reaction occurs；
(3) in course of reaction, control gas inlet and outlet gas speed, by injecting gas, simulate the gas shock of varying strength, ease
Go out, shear, agitation effects；
(4), when prepared by specific coking coking, need, after injecting reaction raw materials, to open second flow pump, inject recycle oil and participate in
Reaction；
(5), after the molding of coking coking completes, bakee 2～4 hours, utilize simultaneously gas feed inject inert gas purge flue gas and
Oil gas, the rapidly burnt sample of cooling.
Said method, in step (1), the preset value of described reacting kettle inner pressure is preferably-0.1MPa～1MPa.
Said method, in step (1), coking temperature is preferably 150 DEG C～650 DEG C.
Said method, in step (3), injects the range of flow of gas at 0.1L/min～4L/min.
Beneficial effects of the present invention:
(1) assembly of the invention simple in construction, it is possible to simulate different coking temperature, coking pressure, recycle oil, gas shock
Condition, and the time needed for preparing coking Jiao's sample is short, quickly can provide basis coking sample for industrial optimization reaction condition
Product.
(2) present invention can simulated atmosphere condition wide, all can use under oxidisability, reproducibility, inert conditions, use atmosphere
It is passed through the effect that can play stirring continuously, inert gas cold shock focus layer after reaction, heat can be taken away rapidly, shorten the system burnt time,
And the impact effect that air-flow in coking escapes, impacts, shears the burnt pattern of focusing chemical conversion can be simulated, also can at reaction mass relatively
For washing away formation wire drawing or needle-like macrostructure by orientation time sticky, be conducive to generating the sample of class needle coke.
(3) present invention selectable coking temperature scope is wide, and temperature programmed control can analog linearity intensification, constant temperature, alternating temperature operation
Condition.
(4) applicable raw materials scope of the present invention is wide, it is adaptable to high molecular polymer, coal liquefaction products, biomass pyrolysis oil, oil
And the preparation of the multiple carbonaceous macromole coking coking such as derivant, important coking material data can not only be provided for petroleum industry,
Can also prepare suitable condition offer basic data for exploration coking Morphological control, needle coke, the evaluation for follow-up burnt sample quickly provides
Sample.
Accompanying drawing explanation
The structural representation of Fig. 1: apparatus of the present invention；
Fig. 2: the sample of the shot coke obtained under harsh conditions；
Fig. 3: the sample of the sponge coke obtained under the conditions of mitigation；
The sample being similar to needle coke that Fig. 4: alternating temperature obtains under the conditions of becoming circulation variable pressure；
Wherein: 1. heating furnace, 2. heat-insulation layer, 3. reaction kettle cover, 4. reactor, 5. circulation oil tank, 6. first flow pump, 7. control
Terminal processed, 8. thermocouple, 9. reactor bottom, 10. air supply system (gas cylinder), 11. gas feed pipelines, 12. gas inlet tubes
Linear flow rate meter 13. second flow pump, 14. material tanks, 15. outlet gas lines, 16. back pressure valve, 17. Pressure gauges, 18. is cold
Condenser.
Detailed description of the invention
The present invention is further illustrated in conjunction with the embodiments, it should explanation, the description below merely to explain the present invention,
Its content is not defined.
Embodiment 1: simulation carbonaceous macromole quickly prepares the device of burnt sample under different coking conditions
A kind of carbonaceous macromole of simulating quickly prepares the device of burnt sample under different coking conditions, and its structure is as it is shown in figure 1, wrap
Include: reactor 4 and heating furnace 1；Described reactor 4 is positioned at the cavity of heating furnace 1, by support (being not drawn in figure)
Support is in the central authorities of the cavity of heating furnace 1.The upper end of reactor 4 is provided with the reaction kettle cover 3 for sealed reactor 4, with reaction
Still 4 is connected by flange and bolt；Described reaction kettle cover 3 is provided with gas outlet, for emergent gas product；Gas outlet is passed through
Outlet gas line 15 is connected with back pressure valve 16, for the pressure setting and controlling in reactor；On outlet gas line 15
Also being sequentially provided with condenser 18 and Pressure gauge 17, wherein, condenser 18 uses the oil gas that circulating water condensing coking produces, it is to avoid
Damage counterbalance valve；Pressure gauge 17 is for monitoring the pressure in reactor.
The ring wall of reactor 4 is provided with material inlet and recycle oil charging aperture, respectively by pipeline and material tank 14 and recycle oil
Tank 5 is connected；Pipeline between material tank 14 and material inlet is provided with first flow pump 6, and circulation oil tank 5 and recycle oil enter
Pipeline between material mouth is provided with second flow pump 13；Pass through first flow pump 6 and second flow pump 13 respectively in pipeline
Raw material and recycle oil flow rate of liquid regulate and control.The interpolation of oil can be circulated while raw material reaction, change reaction raw materials
Structure composition, provide necessary condition for specific form coking.
The bottom of reactor 4 is provided with air inlet, for being passed through of respective reaction atmosphere, by gas feed pipeline and gas cylinder 10
It is connected；By gas flow change gas shock of simulation formation varying strength reactor 4 in, escape, shear, stir effect
Should.Gas feed pipeline 11 is provided with effusion meter 12, is used for measuring gas injection flow velocity.
Described heating furnace 1 is connected with programmable temperature control device, and this programmable temperature control device includes thermocouple 8 and controls terminal 7, passes through program
Temperature in body of heater is effectively controlled by temperature controller.There is a cuboid cavity in described heating furnace 1, use medium/low frequency electromagnetism
The temperature of reaction unit in the range of concussion effect fast lifting solenoid, its energy energy produced acts on gold within a short period of time
Belong to inside reactor, temperature in maximum quick-lift attachreactor, improve heat transfer efficiency, reduce reaction raw materials scorch time.
The outside of described heating furnace 1 is provided with heat-insulation layer 2, is used for reflecting hyperthermia radiation energy, completely cuts off thermal convection current, reduces heat loss.
Embodiment 2: simulation carbonaceous macromole the most quickly prepares the method for burnt sample
(1) open heating furnace 1, mounted reactor 4 and reaction kettle cover 3 are placed on fixing point therein, then will be anti-
Answering kettle 4 and material feeding tube, recycle oil feed pipe, gas inlet tube, gas outlet tube is bolted connection, so
After shut the door of heating furnace 1.
(2) valve 16 on outlet gas line, feedstock pipeline, recycle oil feeding line and pump 6,13 are closed, from
Gas feed pipeline is passed through the required atmosphere of reaction, reaches to close during certain pressure the valve of gas cylinder 10, opens outlet gas line
Valve 16 on 15, the gas in emptying reactor 4, the most repeatedly for three times, discharge air therein.
(3) after air-out, setting counterbalance valve 16 steady pressure value, in maintaining reactor 4, pressure maintains preset value, uses
With pressure in reflection coking plant；Open temperature control system 7, design temperature change of program sequence, make reaction temperature according to setting
Put change (including linear temperature increase, constant temperature etc.), in order to reflect coking temperature.
(4) after reaching to preset reaction temperature.First open gas inlet valve, keep a certain amount of gas injection, prevent reaction raw materials from injecting
After leak at gas feed.Turn-on flow rate pump 13, injects reaction raw materials from material inlet pipeline according to setting flow, and raw material exists
Reaction kettle body inner bottom part is rapidly heated to reaction temperature, and pyrogenetic reaction occurs.
(5) in course of reaction, control gas inlet and outlet gas speed, by injecting gas, simulate the gas shock of varying strength, ease
Go out, shear, agitation effects.
(6) preparation of specific coking coking needs to add recycle oil, after needing the time injected to reach, opens recycle oil inlet valve,
Inject recycle oil by flow pump 5 according to certain flow and participate in reaction.
(7), after the molding of coking coking completes, bakee 2～4 hours, utilize simultaneously gas feed inject inert gas purge flue gas and
Oil gas, cools down rapidly, in time being down to 50 DEG C, closes the valve 16 on the pipeline of gas import/export, opens heating furnace 1, by each bar
Pipeline dismounting is complete, takes out reactor 4, obtains coking gained coking.
Embodiment 3: simulation preparation class shot coke Jiao's sample
Use the device of embodiment 1, prepare the method for burnt sample by embodiment 2 and carry out burnt sample and prepare, be 500 DEG C in temperature, pressure
Power is 0.1MPa, and without recycle oil, gas speed, under the harsh coking condition of 1.5L/min (intense impact effect), uses mink cell focus
Crude distillation residue oil implements coking as coking raw material, and gained Jiao's sample is bullet shape, may be regarded as class technical grade shot coke Jiao's sample,
The pattern of burnt sample is as shown in Figure 2.
Embodiment 4: simulation preparation class sponge coke Jiao's sample
Use the device of embodiment 1, prepare the method for burnt sample by embodiment 2 and carry out burnt sample and prepare, be 480 DEG C in temperature, pressure
Power is 0.15MPa, recycle oil (recycle ratio 0.2), and gas is fast under the mitigation coking condition of 0.5L/min (airflow stirring effect),
Using mink cell focus crude distillation residue oil to implement coking as coking raw material, gained Jiao's sample is spongy, may be regarded as class technical grade sea
Continuous burnt sample, the pattern of burnt sample is as shown in Figure 3.
Embodiment 5: simulation preparation class needle coke sample
Using the device of embodiment 1, prepare the method for burnt sample by embodiment 2 and carry out burnt sample and prepare, point two sections of alternating temperature transformations become to be followed
Ring pyrogenetic reaction, the first stage: temperature is 430 DEG C, pressure is 1.0MPa, and without recycle oil, gas speed is at 0.1L/min (air-flow
Gentle agitation effect) mitigation coking condition under, use catalytic cracked oil pulp as coking raw material implement tentatively relax coking；The
Two-stage: temperature is 480 DEG C, pressure is 0.8MPa, recycle oil (recycle ratio 1.5), and at 0.8L/min, (air-flow orients gas speed
Wire drawing effect) coking condition under gained Jiao's sample be needle-like, may be regarded as class needle coke sample, the pattern of burnt sample is as shown in Figure 4.
Claims (10)
1. simulate carbonaceous macromole device of the burnt sample of quick preparation under different coking conditions for one kind, it is characterised in that including:
Reactor and heating furnace；
Described reactor is positioned at the cavity of heating furnace, and the upper end of reactor is provided with the reaction kettle cover for sealed reactor, described
Reactor lid is provided with gas outlet, is connected with back pressure valve by outlet gas line；
The ring wall of reactor is provided with material inlet and recycle oil charging aperture, respectively by pipeline and material tank and circulation oil tank phase
Even；
The bottom of reactor is provided with air inlet, is connected with air supply system by gas feed pipeline；
Described heating furnace is connected with programmable temperature control device.
2. device as claimed in claim 1, it is characterised in that be also sequentially provided with condenser and pressure on described outlet gas line
Power table.
3. device as claimed in claim 1, it is characterised in that described gas feed pipeline is provided with effusion meter.
4. device as claimed in claim 1, it is characterised in that the pipeline between material tank and material inlet is provided with first
Flow pump, the pipeline between circulation oil tank and recycle oil charging aperture is provided with second flow pump.
5. device as claimed in claim 1, it is characterised in that described air supply system includes oxidizing gas feeder, goes back
Originality gas feeder and noble gas feeder.
6. device as claimed in claim 1, it is characterised in that the outside of described heating furnace is provided with heat-insulation layer.
7. the unit simulation carbonaceous macromole that a kind utilizes described in any one of claim 1-6 the most quickly prepares burnt sample
Method, step is as follows:
(1) heating furnace is opened, the air in emptying reactor, set counterbalance valve steady pressure value, make reacting kettle inner pressure maintain
At preset value, in order to reflect pressure in coking plant；Open programmable temperature control device, design temperature change of program sequence, make reaction temperature
Degree is according to arranging change, in order to reflect coking temperature；
(2) after reaching to preset reaction temperature, by gas injection in gas inlet tube alignment reactor, open first flow pump, inject
Reaction raw materials, raw material is rapidly heated to reaction temperature at reaction kettle body inner bottom part, and pyrogenetic reaction occurs；
(3) in course of reaction, control gas inlet and outlet gas speed, by injecting gas, simulate the gas shock of varying strength, ease
Go out, shear, agitation effects；
(4), when prepared by specific coking coking, need, after injecting reaction raw materials, to open second flow pump, inject recycle oil and participate in
Reaction；
(5), after the molding of coking coking completes, bakee 2～4 hours, utilize simultaneously gas feed inject inert gas purge flue gas and
Oil gas, the burnt sample of cooling.
8. method as claimed in claim 7, it is characterised in that in step (1), the preset value of described reacting kettle inner pressure
It is preferably-0.1MPa～1MPa.
9. method as claimed in claim 7, it is characterised in that in step (1), coking temperature is 150 DEG C～650 DEG C.
10. method as claimed in claim 7, it is characterised in that in step (3), the range of flow injecting gas exists
0.1L/min～4L/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342213A (en) * | 2018-01-16 | 2018-07-31 | 华中科技大学 | A kind of device and method preparing Nano carbon ball using biomass |
| CN108342220A (en) * | 2018-01-22 | 2018-07-31 | 华中科技大学 | A kind of system that the bio oil based on component separation is used using method with it |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942314A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Technology for producing needle coke by kettle-type coking |
| CN102965132A (en) * | 2012-08-23 | 2013-03-13 | 方大炭素新材料科技股份有限公司 | Method for preparing needle coke by magnetization reaction kettle |
| CN205856394U (en) * | 2016-06-13 | 2017-01-04 | 中国石油大学(华东) | The device of coking is prepared in the simulation carbonaceous quick coking of macromole delayed coking |
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2016
- 2016-06-13 CN CN201610411629.4A patent/CN105950206B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942314A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Technology for producing needle coke by kettle-type coking |
| CN102965132A (en) * | 2012-08-23 | 2013-03-13 | 方大炭素新材料科技股份有限公司 | Method for preparing needle coke by magnetization reaction kettle |
| CN205856394U (en) * | 2016-06-13 | 2017-01-04 | 中国石油大学(华东) | The device of coking is prepared in the simulation carbonaceous quick coking of macromole delayed coking |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342213A (en) * | 2018-01-16 | 2018-07-31 | 华中科技大学 | A kind of device and method preparing Nano carbon ball using biomass |
| CN108342213B (en) * | 2018-01-16 | 2019-11-08 | 华中科技大学 | A kind of device and method preparing Nano carbon ball using biomass |
| CN108342220A (en) * | 2018-01-22 | 2018-07-31 | 华中科技大学 | A kind of system that the bio oil based on component separation is used using method with it |
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