CN110079354A - A kind of delayed coking raw material and its preprocess method and petroleum coke and preparation method thereof - Google Patents
A kind of delayed coking raw material and its preprocess method and petroleum coke and preparation method thereof Download PDFInfo
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- CN110079354A CN110079354A CN201910470721.1A CN201910470721A CN110079354A CN 110079354 A CN110079354 A CN 110079354A CN 201910470721 A CN201910470721 A CN 201910470721A CN 110079354 A CN110079354 A CN 110079354A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/20—Refining by chemical means inorganic or organic compounds
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Abstract
The invention discloses a kind of delayed coking raw material and its preprocess methods and petroleum coke and preparation method thereof, the following steps are included: carrying out cavitation oxidation processes to delayed coking raw material using oxidant-catalyst, it is handled again through dehesion, the difficult sulphur decomposed in delayed coking raw material is made to be converted into labile sulfone and oxysulfide gas.The present invention realizes petroleum coke production progress synchronous with desulfurization in delay coking process, enormously simplifies existing desulfurizing petrol coke technique, effectively overcomes the high cost problem that desulfurization is re-refined in first production.
Description
Technical field
The present invention relates to technical field of petrochemical industry, and in particular to a kind of delayed coking raw material and its preprocess method with
And petroleum coke and preparation method thereof.
Background technique
Petroleum coke can be divided into low-sulfur burnt (sulfur content is lower than 2%), middle sulphur coke (sulfur content 2%- according to sulfur content therein
And three kinds of Behavior of High-sulfur Petroleum Coke (sulfur content be higher than 4%) 4%).The content of sulfur in petroleum coke determines the final use of petroleum coke, Behavior of High-sulfur Petroleum Coke
It is mainly used to do fuel.Low sulfur petroleum coke trains anode mainly for the production of electrolytic aluminium in advance, needs as electrolysis aluminum feedstock petroleum coke
Its physicochemical property and electrical property are improved by calcining.
The main thiophene of sulphur content contained in petroleum coke and benzothiophenes, in order to which the sulphur reduced in petroleum coke contains
Amount, many domestic and foreign scholars propose some research methods, mainly use solvent extraction process desulfurization, chemical oxidization method desulfurization, alkali
Metallic compound doctor treatment, high-temperature calcination doctor treatment.
Currently, the research emphasis of desulfurizing petrol coke technique be all catalyst, reducing agent improvement on, in petroleum coke high temperature
Reducibility gas or mixed catalyst are passed through in calcination process to achieve the purpose that desulfurization, still without using to coking raw material into
The method report of pretreatment desulfurizing before row delayed coking, being particularly suitable for industrialization pretreatment reduces the side of petroleum coke sulfur content
There is not been reported for method.
Summary of the invention
The purpose of the present invention is to provide a kind of delayed coking raw material and its preprocess method and petroleum coke and its preparations
Method, solve current desulfurizing petrol coke technique research emphasis be all catalyst, reducing agent improvement on, in petroleum coke height
Reducibility gas or mixed catalyst are passed through in warm calcination process to reach the low efficiency in sweetening process, at high cost ask
Topic, and existing desulfurizing petrol coke technique is enormously simplified, effectively overcome the high cost problem that desulfurization is re-refined in first production.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention provides a kind of method for reducing petroleum coke sulfur content, comprising the following steps: uses oxidant-catalyst pair
Delayed coking raw material carries out cavitation oxidation processes, then handles through dehesion, is converted into the difficult sulphur decomposed in delayed coking raw material easily
The sulfone and oxysulfide gas of decomposition.
The present invention also provides a kind of delayed coking raw materials handled by above-mentioned preprocess method.
The present invention also provides a kind of preparation methods of petroleum coke comprising: pass through the above-mentioned pre- place to delayed coking raw material
Reason method pre-processes delayed coking raw material, then the delayed coking raw material obtained after pretreatment is carried out coking processing.
The present invention also provides a kind of petroleum cokes that the preparation method by above-mentioned petroleum coke is prepared.
The beneficial effects of the present invention are:
The present invention provides a kind of delayed coking raw material and its preprocess methods and petroleum coke and preparation method thereof, pass through
Cavitation reinforcement oxidation-dehesion processing is carried out to delayed coking raw material, by delayed coking raw material in cavitation processes at oxidation
It manages, the thiophenic sulfur of more difficult decomposition is converted into labile sulfoxide or sulfone in raw material, and part organic sulfur is in the process with dioxy
The form for changing sulphur is removed, then handles reduction through dehesion, and the chain rupture for labile sulfoxide or sulfone C-S key provides more heat
Amount, to change the sulphur distribution situation of delayed coking product, from the sulfur content reduced in raw material on source, again by above-mentioned raw materials
The petroleum coke handled through coking, the sulfur content in the petroleum coke is low, and the quality of petroleum coke product is high, it is easy to accomplish industrialization
Production, meets high-quality consumer demand.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to a kind of delayed coking raw material provided in an embodiment of the present invention and its preprocess method and petroleum coke and its
Preparation method is specifically described.
The embodiment of the invention provides a kind of preprocess methods of delayed coking raw material, comprising the following steps: using oxidation
Agent-catalyst carries out cavitation oxidation processes to delayed coking raw material, then handles through dehesion, makes difficult decomposition in delayed coking raw material
Sulphur is converted into labile sulfone and oxysulfide gas.
The embodiment of the invention provides a kind of preprocess methods of delayed coking raw material, this method comprises: to delayed coking
Raw material carries out cavitation reinforcement oxidation-dehesion processing processing, on the one hand passes through generated extreme condition in cavitation processes: high temperature,
The enhanced oxidations process such as high pressure, high shear force so that in raw material the thiophenic sulfur of more difficult decomposition be converted into labile sulfoxide or
Sulfone, on the other hand the chain rupture using visbreaking invigoration effect for labile sulfoxide or sulfone C-S key provides more heats, thus
The sulphur distribution situation for changing delayed coking product makes in delayed coking raw material the difficult sulphur decomposed be converted into labile sulfone and a small amount of
Oxysulfide gas, reduce the sulfur content of petroleum coke, effectively overcome delayed coking raw material hydrodesulfurization hydrogen consumption with
And hydrogen source it is at high cost the problems such as.
In some embodiments, delayed coking raw material includes reduced crude, decompression residuum, coal tar, solvent release drip
At least one of green oil.
In some embodiments, oxidant includes tert-butyl hydroperoxide, cumyl hydroperoxide, in hydrogen peroxide
At least one, catalyst include formic acid, acetic acid, the carboxylic acid of trifluoroacetic acid class, phosphotungstic acid, at least one of phosphomolybdic acid.
In some embodiments, the respective additional amount of catalyst and oxidant is the 1%- of delayed coking material quality
10%, and the molar ratio of catalyst and oxidant is 1:1-1:8.
In some embodiments, cavitation apparatus used in cavitation oxidation processes includes venturi-type, the liquid whistle
Formula, throttle orifice be board-like or at least one of jet pipe type cavitation apparatus, and dehesion processing carries out in dehesion reactor.
In some embodiments, the pressure in cavitation oxidation processes is 2-10Mpa, preferably 4-8Mpa, and temperature is
90-150℃。
A kind of preprocess method of delayed coking raw material provided in an embodiment of the present invention first carries out delayed coking raw material
Cavitation oxidation processes, comprising: the mixing of catalyst, oxidant and coking raw material is first carried out Cavitation enhanced oxidation process,
High temperature, high pressure and the microjet that can be mainly generated in little space using the cavitation-shock wave generated in cavitation processes, can
To greatly promote oxidizing agent solution and delayed coking raw material oil water contact, be conducive to the oxidation of thiophene, while cavitation processes generate
High-energy can provide the high temperature of thousands of degree on microcosmic and can effectively facilitate the fracture of C-S key, make small part sulfoxide or sulfone
It decomposes and generates sulfur dioxide.
In some embodiments, the temperature of dehesion processing is 330-450 DEG C, and preferably 370-410 DEG C, the time is
0.5h-1h。
A kind of preprocess method of delayed coking raw material provided in an embodiment of the present invention, will be after cavitation oxidation processes
Material carries out visbreaking pretreatment again, all-radiant furnace of the small hydrocarbon molecules on the one hand low temperature visbreaking process being utilized to generate in delayed coking
Interior endothermic gasification provides more energy for depth thermal cracking, is more advantageous to and provides more energy for C-S fracture, on the other hand
Visbreaking process temperature compared with coking is lower, slows down condensation reaction, effectively prevents sulfoxide or sulfone pyrolytic goes out
Sulphur content swept along and can not be removed in petroleum coke, further reduced the sulfur content of petroleum coke.
The embodiment of the present invention also provides a kind of delayed coking raw material handled by above-mentioned preprocess method.
The embodiment of the present invention also provides a kind of preparation method of petroleum coke comprising: by above-mentioned to delayed coking raw material
Preprocess method delayed coking raw material is pre-processed, then will the delayed coking raw material that obtained after pretreatment carry out coking at
Reason.
The embodiment of the present invention provides also a kind of preparation method of petroleum coke, will be after cavitation oxidation-dehesion processing
Substance carries out delayed coking processing again, since the dehesion treatment process in cavitation oxidation-dehesion treatment process avoids under high temperature
Coking raw material is condensed rapidly, and the volatile sulphur content that part sulfoxide or sulfone decomposite is swept along the process that can not be removed, and is strengthened
Sulfoxide or sulfone decompose the process for generating sulfur dioxide in delayed coking, drop the sulfur content in petroleum coke further
Low, delayed coking reaction process is consistent with conventional coking process.
The embodiment of the present invention also provides a kind of petroleum coke being prepared by above-mentioned petroleum coke preparation method.
Feature and performance of the invention are described in further detail with reference to embodiments.
Oxidant used in the embodiment of the present invention is hydrogen peroxide, and catalyst is acetic acid.
Embodiment 1
A method of reducing petroleum coke sulfur content, comprising the following steps: using oxidant-catalyst to delayed coking original
Material carries out cavitation oxidation processes, then handles through dehesion, and Conventional delayed coking processing obtains petroleum coke, wherein
Cavitation oxidation processes reaction condition are as follows: 90 DEG C of cavitation temperature, cavitation pressure 4Mpa, the addition of catalyst and oxidant
Amount is the 1% of coking raw material quality, molar ratio 1:3, the condition of dehesion processing are as follows: 370 DEG C of visbreaking temperature, the visbreaking time
0.5h, the condition of coking processing are as follows: coking is conventional delayed coking, and obtained petroleum coke sulfur content is 3.32%.
Embodiment 2
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: 90 DEG C of cavitation temperature, cavitation pressure 4Mpa, the additional amount of catalyst and oxidant is the 1% of coking raw material quality, molar ratio
For 1:3, the condition of dehesion processing are as follows: 370 DEG C of visbreaking temperature, visbreaking time 1h, the condition of coking processing are as follows: coking is normal
The delayed coking of rule, obtained petroleum coke sulfur content are 3.05%.
Embodiment 3
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: 150 DEG C of cavitation temperature, cavitation pressure 4Mpa, the additional amount of catalyst and oxidant is the 1% of coking raw material quality, mole
Than for 1:3, the condition of dehesion processing are as follows: 370 DEG C of visbreaking temperature, visbreaking time 1h, the condition of coking processing are as follows: coking is
Conventional delayed coking, obtained petroleum coke sulfur content are 2.96%.
Embodiment 4
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: 90 DEG C of cavitation temperature, cavitation pressure 4Mpa, the additional amount of catalyst and oxidant is the 1% of coking raw material quality, molar ratio
For 1:3, the condition of dehesion processing are as follows: 390 DEG C of visbreaking temperature, visbreaking time 1h, the condition of coking processing are as follows: coking is normal
The delayed coking of rule, obtained petroleum coke sulfur content are 2.66%.
Embodiment 5
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: 90 DEG C of cavitation temperature, cavitation pressure 8Mpa, the additional amount of catalyst and oxidant is the 1% of coking raw material quality, molar ratio
For 1:3, the condition of dehesion processing are as follows: 390 DEG C of visbreaking temperature, visbreaking time 1h, the condition of coking processing are as follows: coking is normal
The delayed coking of rule, obtained petroleum coke sulfur content are 2.35%.
Embodiment 6
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: 90 DEG C of cavitation temperature, cavitation pressure 8Mpa, the additional amount of catalyst and oxidant is the 1% of coking raw material quality, molar ratio
For 1:5, the condition of dehesion processing are as follows: 410 DEG C of visbreaking temperature, visbreaking time 1h, the condition of coking processing are as follows: coking is normal
The delayed coking of rule, obtained petroleum coke sulfur content are 2.15%.
Embodiment 7
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: 90 DEG C of cavitation temperature, cavitation pressure 8Mpa, the additional amount of catalyst and oxidant is the 3% of coking raw material quality, molar ratio
For 1:5, the condition of dehesion processing are as follows: 410 DEG C of visbreaking temperature, visbreaking time 1h, the condition of coking processing are as follows: coking is normal
The delayed coking of rule, obtained petroleum coke sulfur content are 1.98%.
Embodiment 8
Experimental procedure is same as Example 1, is only that the parameter in reaction process is different, cavitation oxidation processes reaction condition
Are as follows: reaction condition are as follows: 90 DEG C of cavitation temperature, cavitation pressure 8Mpa, the additional amount of catalyst and oxidant is coking raw material quality
5%, molar ratio 1:5, dehesion processing condition are as follows: 410 DEG C of visbreaking temperature, visbreaking time 1h, coking processing condition are as follows:
Coking is conventional delayed coking, and obtained petroleum coke sulfur content is 1.95%.
Comparative example 1
Zhenghai refinery decompression residuum with property such as table 1 is coking raw material, and coking raw material does not carry out under any disposition,
It is only 4.12% through the Conventional delayed coking sulfur content for handling obtained petroleum coke.
The main character of 1 decompression residuum of table
Comparative example 2
It is hydrogen peroxide that oxidant is implemented in this experiment, and catalyst is acetic acid；Reaction condition are as follows: 90 DEG C of cavitation temperature, cavitation pressure
The additional amount of power 4Mpa, catalyst and oxidant is the 1% of coking raw material quality, and molar ratio 1:3, coking is conventional prolong
Slow coking processing, petroleum coke sulfur content are 3.54%.
Test result
Following table 2 is the petroleum coke sulfur content table that 1-8 of the embodiment of the present invention and comparative example 1-2 are obtained.
The petroleum coke sulfur content table that 2 1-8 of the embodiment of the present invention of table and comparative example 1-2 are obtained
By above-mentioned table 2 it can be seen that since the coking raw material in comparative example 1 does not carry out under any disposition, in raw material
Containing a large amount of sulfur-containing compound, after the above-mentioned raw material handled without cavitation oxidation processes-dehesion directly carries out coking processing,
Still contain a large amount of sulfur-containing compound in obtained product petroleum coke, be compared to comparative example 1, the raw material warp in comparative example 2
Cross cavitation oxidation processes, can it is a degree of reduce petroleum coke in sulfur-containing compound content, be compared to 1 He of comparative example
For raw material in 2,1-8 of the embodiment of the present invention by cavitation oxidation processes-dehesion processing, the desulfurization degree of obtained petroleum coke is much high
In comparative example 1 and 2, sulfur content is well below comparative example 1 and 2, it is seen then that by carrying out at cavitation oxidation to delayed coking raw material
Reason, then handled through dehesion, the difficult sulphur decomposed in delayed coking raw material can be made to be converted into labile sulfone and oxysulfide gas,
The sulfur content being substantially reduced in product.
As seen through the above analysis, the embodiment of the present invention provide a kind of delayed coking raw material and its preprocess method with
And petroleum coke and preparation method thereof, cavitation oxidation processes are carried out to delayed coking raw material first, then handle through dehesion, makes delay coke
Change the difficult sulphur decomposed in raw material and is converted into labile sulfone and oxysulfide gas, delayed coking raw material after the above treatments
Sulfur content therein is significantly reduced, and delayed coking raw material not only avoids high temperature Coke-oven raw material after viscosity reduction processing
Condensation rapidly, the volatile sulphur content that part sulfoxide or sulfone decomposite is swept along the process that can not be removed, and is enhanced and prolonged
Sulfoxide or sulfone decompose the process for generating sulfur dioxide in slow coking, so that the sulphur in delayed coking raw material is before coking
It is removed, realizes petroleum coke production progress synchronous with desulfurization in delay coking process, it is de- to enormously simplify existing petroleum coke
Sulphur technique effectively overcomes the high cost problem that desulfurization is re-refined in first production.Comparative example through inventive embodiments and comparative example
As can be seen that the removing process in the present invention is stripped of sulphur ingredient therein from source, so that in the petroleum coke that coking obtains
Sulfur content is substantially reduced, hence it is evident that improves the quality of petroleum coke product.
Compared with prior art, the embodiment of the present invention have it is below the utility model has the advantages that
1), preparation method realizes petroleum coke production and the same stepping of desulfurization in delay coking process in the embodiment of the present invention
Row, enormously simplifies existing desulfurizing petrol coke technique, effectively overcomes the high cost problem that desulfurization is re-refined in first production.
2), simple process provided in an embodiment of the present invention, cavitation apparatus is simple, and low energy consumption, maintenance cost is low, Yi Shi
Now industrialize.
3), the technique in the embodiment of the present invention is aoxidized in cavitation processes, not only enhances catalyst, oxidant
Oxidation efficiency is improved with effectively contacting for coking raw material, and the extreme high-energy generated promotes the fracture of C-S key, enhances
The reaction efficiency of desulfurization.
4), the coking in the embodiment of the present invention is using visbreaking-delayed coking, compared with direct delay coking,
Visbreaking process avoids high temperature Coke-oven raw material and is condensed rapidly, and the volatile sulphur content that part sulfoxide or sulfone decomposite is swept along
The process that can not be removed enhances sulfoxide or sulfone in delayed coking and decomposes the process for generating sulfur dioxide.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preprocess method of delayed coking raw material, which comprises the following steps: use oxidant-catalyst
Cavitation oxidation processes are carried out to delayed coking raw material, then are handled through dehesion, the difficult sulphur decomposed in delayed coking raw material is converted into
Labile sulfone and oxysulfide gas.
2. preprocess method according to claim 1, which is characterized in that the delayed coking raw material include reduced crude,
At least one of decompression residuum, coal tar, solvent release coal tar.
3. preprocess method according to claim 1, which is characterized in that the oxidant include tert-butyl hydroperoxide,
At least one of cumyl hydroperoxide, hydrogen peroxide, the catalyst include formic acid, acetic acid, the carboxylic acid of trifluoroacetic acid class,
Phosphotungstic acid, at least one of phosphomolybdic acid.
4. preprocess method according to claim 1, which is characterized in that the catalyst and the respective of the oxidant add
Enter the 1%-10% that amount is the delayed coking material quality, and the molar ratio of the catalyst and the oxidant is 1:1-
1:8。
5. preprocess method according to claim 1, which is characterized in that sky used in the cavitation oxidation processes
Makeup is set including venturi-type, liquid whistle formula, throttle orifice are board-like or at least one of jet pipe type cavitation apparatus, the dehesion
Processing carries out in dehesion reactor.
6. preprocess method according to claim 1, which is characterized in that the pressure in the cavitation oxidation processes is
2-10Mpa, preferably 4-8Mpa, temperature are 90-150 DEG C.
7. preprocess method according to claim 1, which is characterized in that the temperature of the dehesion processing is 330-450 DEG C,
Preferably 370-410 DEG C, time 0.5h-1h.
8. a kind of delayed coking raw material, which is characterized in that it is pre- by the described in any item delayed coking raw materials of claim 1-7
Processing method handles to obtain.
9. a kind of preparation method of petroleum coke, characterized in that it comprises: pass through the described in any item delays of claim 1-7
The preprocess method of coking raw material pre-processes the delayed coking raw material, then the delay coke that will be obtained after pretreatment
Change raw material and carries out delayed coking processing.
10. a kind of petroleum coke, which is characterized in that it is prepared by the preparation method of petroleum coke as claimed in claim 9.
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| CN113862033A (en) * | 2021-09-18 | 2021-12-31 | 中国石油大学(华东) | Method for preparing needle coke with low thermal expansion coefficient by combining fluid coking and delayed coking |
| RU2768163C1 (en) * | 2020-10-09 | 2022-03-23 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт нефтехимического синтеза им. А.В. Топчиева Российской академии наук (ИНХС РАН) | Method for producing coke with low sulfur content (embodiments) |
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| CN112742476A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Catalyst, preparation method thereof and method for producing low-sulfur petroleum coke |
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| CN113862033A (en) * | 2021-09-18 | 2021-12-31 | 中国石油大学(华东) | Method for preparing needle coke with low thermal expansion coefficient by combining fluid coking and delayed coking |
| CN113862033B (en) * | 2021-09-18 | 2023-01-13 | 中国石油大学(华东) | Method for preparing needle coke with low thermal expansion coefficient by combining fluid coking and delayed coking |
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Application publication date: 20190802 |