CN109022008A - A kind of preparation method of high yield acicular petroleum coke - Google Patents
A kind of preparation method of high yield acicular petroleum coke Download PDFInfo
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- 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
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Abstract
The present invention provides a kind of preparation method of high yield acicular petroleum coke, first by FCC slurry and alkyl halide (iodomethane or iodoethane), polyalcohol (polyethylene glycol, polypropylene glycol, trimethylolpropane) and boron trifluoride, with oil ratio for 0.01~0.07g/g, the ratio of 0.03~0.08g/g and 0.001~0.02g/g is uniformly mixed, catalyzed polycondensation, which is carried out, through 4~6h at a certain temperature couples either shallow alkylated reaction, it is higher to generate molecular weight, the higher carbene mixture of aromaticity, improve the degree of cross linking and the degree of coupling of polycyclic aromatic compounds, then by resulting carbene mixture, 10~14h of carbonization reaction obtains Raw needle coke at 550~600 DEG C, most acicular petroleum coke is obtained through high-temperature calcination at 1500 DEG C afterwards.The method of the present invention is alkylation coupling-carbonization reaction group technology, have the characteristics that intermediate molecule amount and aromaticity is controllable, easily controllable carbonization reaction depth and interphase formation, gained needle coke has the advantages that yield is high, thermal expansion coefficient is low, general yield >=70%, thermal expansion coefficient can be down to 0.9 × 10‑6~1.6 × 10‑6/℃。
Description
Technical field
The present invention relates to a kind of preparation methods of high yield acicular petroleum coke, belong to carbon material technical field.
Background technique
Acicular petroleum coke be the 1970s occur high quality carbon kind, because its thermal expansion coefficient is low, the high and low sulphur of density,
The characteristics such as low ash point, low-metal content and conductivity height, be production ultra-high power graphite electrode, extraordinary carbon material, Carbon fibe and its
The raw material of the high-end carbon product such as composite material.According to statistics, China needs about 200,000 tons of needle coke or so every year, but domestic at present
In the actual production of petroleum needle coke, needle coke quality is not sufficiently stable, there are coke strenth is low and the problems such as coke breeze is more, these
Problem all seriously constrains the processing capacity of needle coke quality and device, be still unable to continuous production high quality can be used for manufacturing it is super
The needle coke of high power graphite electrode goes back partial dependency import, it is seen that needle coke has good market prospects.
Quantity due to carrying out the acicular petroleum coke raw material of autothermal cracking plant cannot meet the needs of production.Currently, needle-shaped
It is burnt mainly to be produced by pretreatment of raw material, delayed coking, calcine technology.It can have been used on delayed coking unit now
Raw material appropriate and technique produce needle coke, and production procedure is similar with general coke, but operating condition is extremely harsh, and yield is lower.By
In the good value of needle coke, there are many people to study it.
A kind of method using crosslinking agent preparation interphase, this method operation letter are provided in Chinese patent CN1185491
Single, high-quality mesophase pitch high income, easily designed and control interphase forming process and composed structure, interphase obtained drip
Green softening point is low, and optical anisotropy is flourishing and content is high, and rheological property is excellent, and H/C is than high, but the patent is only for modelling
Object is closed, cost is high, and it is not applicable to petroleum system, temporarily without wide range of industrial applications.It is disclosed in Chinese patent CN103642511A
A kind of preparation method of high-quality needle-shape coke raw material, this method passes through heat filtering first and carries out purified treatment to coal tar, then passes through
Vacuum distillation and catalytic hydrogenation handle the heavy component coal tar pitch modification in coal tar, the delayed coking of gained asphalitine and forging
It burns and obtains needle coke.Prepared needle coke resistivity is low, bulk density is big, thermal expansion coefficient is small, has reached high-quality needle coke
Requirement.Although the needle coke function admirable of this method preparation, is related to a variety of production technologies, and hydrogenation reaction risk compared with
Greatly, it is unfavorable for industrial practical application.
Summary of the invention
The present invention provides a kind of methods for improving delayed coking acicular petroleum coke yield.This method is lower by aromaticity
Oil product synthesize high interphase at a lower temperature containing needle-type coke, the yield of acicular petroleum coke can be improved, and reaction process is held
It is easy to control.
The invention adopts the following technical scheme:
A kind of preparation method of high yield acicular petroleum coke, include the following steps: by feedstock oil and alkyl halide, polyalcohol and
Boron trifluoride is respectively the ratio mixing of 0.01~0.07g/g, 0.03~0.08g/g and 0.001~0.02g/g with oil ratio
Homogeneous reaction generates that average molecular weight is larger, the higher carbene mixture of aromaticity；Then, by resulting carbene mixture
10~14h of delayed coking obtains Raw needle coke at 550~600 DEG C, most obtains needle-shaped stone through high-temperature calcination at 1500 DEG C afterwards
Oil coke.
Further, the feedstock oil is FCC slurry.
Further, after catalyzed polycondensation coupling either shallow alkylated reaction, the property of obtained carbene mixture are as follows: average mark
Son amount is 600~800, cycloalkanes number of rings 2~5, aromatic ring number 2~6, aromatic carbon rate 0.6~0.8, alkyl carbon rate 0.2~0.4.
The alkyl halide is iodomethane and/or iodoethane；The polyalcohol is polyethylene glycol, polypropylene glycol, three hydroxyls
One of methylpropane is a variety of；The catalyst is boron trifluoride.
Catalyzed polycondensation coupling either shallow alkylation process needs to be filled with nitrogen and is protected, and pressure is 0.1~0.5MPa, with halogen
Be alkylating agent for hydrocarbon, polyalcohol is couplant, reaction temperature is 200~250 DEG C, reacts 4~6h.
Gained acicular petroleum coke yield >=70%, the acicular petroleum coke product of generation have the fine fibre of height uniaxial orientation
Shape interphase optical texture, interphase content >=90%, real density > 2.15g/cm3, thermal expansion coefficient CTE≤1.5 × 10-6/
DEG C, volatile matter < 0.6.
More specific technical solution is as follows: a kind of preparation method of high yield acicular petroleum coke includes the following steps: (1)
In high temperature and high pressure kettle, according to the oil ratio of 0.01~0.07g/g, 0.03~0.08g/g, by a certain amount of alkylating agent ---
Halogenated hydrocarbons, couplant --- polyalcohol and the mixing of a certain amount of FCC slurry, and it is urging for 0.001~0.02g/g that oil ratio, which is added,
Agent boron trifluoride；(2) it is replaced after sealing through nitrogen, is filled with the nitrogen of 0.1~0.5MPa, and keep pressure constant；Alkane is added
After base agent, reaction temperature is 200~250 DEG C；Alkylation 4~6h of coupling, keep during the reaction revolving speed 250~
350r/min；(3) in the carbene mixture investment coking furnace generated reaction, in the nitrogen gas that pressure is 0.1~0.9mpa
10~14h is reacted in atmosphere at 550~600 DEG C, obtains green coke.Green coke calcines 2~6h at 1500 DEG C of high temperature in an inert atmosphere,
Obtain acicular petroleum coke, acicular petroleum coke yield >=70%.
The acicular petroleum coke of the preparation method preparation of above-mentioned high yield acicular petroleum coke is also claimed in the present invention；It generates
Acicular petroleum coke product has the fine-fibrous interphase optical texture of height uniaxial orientation, interphase content >=90%, very close
Degree > 2.15g/cm3, thermal expansion coefficient CTE≤1.5 × 10-6/ DEG C, volatile matter < 0.6.
The purposes of the acicular petroleum coke is also claimed in the present invention, for producing ultra-high power graphite electrode, extraordinary charcoal element
Material, Carbon fiber and carbon fiber composites.
It for the reason of catalyst is its low boiling point that the present invention, which selects boron fluoride, is easy to steam from reactant, can recycle
It uses；Can the formation such as same alcohol, ether or phenols there is the complex compound of catalytic activity, side reaction is few.Alkylating agent is halogenated hydrocarbons, coupling
The reason of mixture is polyalcohol be, this catalyzed polycondensation coupling either shallow alkylated reaction is electrophilic substitution reaction, in the presence of catalyst,
Alkylating agent polarizes strongly becomes electrophilic particle vivaciously, and electrophilic particle attack reactant generates б-complex compound, this is complexed later
Object sloughs proton and generates alkylate；In the present invention, alkyl halide makes the alkyl in feedstock by alkylated reaction
Increase with alkyl side chain, improves the reactivity of raw material；Meanwhile polyol molecule is made in feedstock oil by alkylated reaction
Aromatic hydrocarbon molecule between intercouple, generate the biggish heavy aromatics molecule of molecular weight, improve the aromaticity and coupling of raw material,
Under the effect of the multiple chemical of halogenated hydrocarbons and polyalcohol, the carbene mixture with certain alkyl charcoal rate, high aromaticity is generated.
During next high temperature pyrolysis, modified feedstock oil generates a large amount of living radicals by dealkylation, and activation energy
It can be reduced due to the presence of alkyl chain, be conducive to the steady progress of condensation reaction, lattice defect is less, is graphitized journey conducive to generating
Higher, the preferable mesophase pitch of optical texture is spent, then forms acicular petroleum coke after high temperature carbonization.
Alkylating agent is required to be mixed with FCC slurry according to certain oil ratio in the method for the present invention, alkylating agent
Dosage affects the composed structure of polymer, if the dosage of alkylating agent is excessive, will lead to the alkylation of carbene mixture excessively,
Reactivity is larger, further heat treatment when, will lead to violent carbonization reaction so that reaction process cannot steadily into
Row, influences the shaping and development of mesophase pitch, while will lead to and produce the unstable of gas in carbonization process, reduces the product of needle coke
Matter.
The present invention will rationally control temperature and the reaction time of Macroscopic single crystal.Reaction temperature is excessively high, and the reaction time is too long,
It can cause more side reaction, heteroatomic introducing improves system heat reactivity energy, and the rule for being unfavorable for mesophase pitch takes
To, easily formation mosaic texture；Simultaneous reactions temperature is too low, and the reaction time is too short, will lead to alkylation it is insufficient, reduce electrophilic
Substitution reaction rate influences the yield of acicular petroleum coke.
Dosage the present invention claims control catalyzed polycondensation coupling either shallow catalyst for alkylation reaction is 0.001~0.02g/g,
The dosage of catalyst increases, and can reaction rate be greatly improved, and the degree of polymerization increases, boron trifluoride when making catalyst, due to
It can dissociate fluorine ion, so that alkylating agent is generated ion pair or ionic complex under heat effect, advantageous as electrophilic
The biggish position of cloud density of reagent attack aromatic hydrocarbon molecule, accelerates electrophilic substitution reaction.
Method of the invention has the advantage that compared with prior art
1, the method that mainly a kind of delayed coking acicular petroleum coke of the present invention improves yield, is coupled shallow by catalyzed polycondensation
The method for spending alkylated reaction, can be improved the aromaticity of raw material, to improve the carbonization yield of green coke, improves FCC slurry
Utilization rate increases its added value.
2, it is easy to control the structure and composition of needle-shape coke raw material, by controlling alkylating agent type, dosage, alkyl
Change the conditions such as temperature, reaction time, controls reaction depth, and avoid the excessive pyrolysis of asphaltene molecule, it is poly- so as to control
Condensation degree, the secondary quinoline insolubles content etc. of object are closed, carbonization reaction design is carried out, is conducive to high-quality acicular petroleum coke raw material
Design preparation.
3, complete optical anisotropy, optically anisotropic mesophase pitch can be prepared, this mesophase pitch is after
Continuous delayed coking can prepare that fibrous structure is more, the lower high-quality acicular petroleum coke of thermal expansion coefficient.
4, operation of the present invention is simple, is not related to complicated production equipment, and raw material and production technology cost are lower, and maximum to the greatest extent can
It has been avoided that the corrosivity to equipment, has been conducive to promote its industrial application.
Specific embodiment
In order to which a kind of technical solution of method for improving delayed coking needle coke of the present invention is more clearly understood,
With reference to embodiment to we it is bright in technical solution be further described.
Embodiment 1:
By FCC slurry at 1MPa nitrogen atmosphere, 560 DEG C delayed coking 10h, obtain green coke.By obtained green coke
6h is calcined at nitrogen atmosphere, 1500 DEG C, obtains real density 2.23g/cm3, thermal expansion coefficient 1.93 × 10-6/ DEG C, volatile matter
The acicular petroleum coke of 0.54wt%, yield 59.3%.
Embodiment 2:
FCC slurry 1000g is taken, after mixing with 55g iodomethane, 50g trimethylolpropane, 5g catalyst boron trifluoride
It is fitted into corrosion resistant high temperature and high pressure kettle, temperature reaction is carried out under 0.5MPa nitrogen protection and 300r/min stirring, until 240
DEG C, constant temperature 5h obtains solid shaped polymer, after which is crushed, washs 2~3 times, drying for standby through clear water, completes catalysis
Polycondensation couples either shallow alkylated reaction.Then pass through delayed coking, by the polymer-asphalt in the nitrogen atmosphere that pressure is 1MPa
Under in 560 DEG C of Coke-oven 10h, obtain green coke.High-temperature calcination is carried out later, by green coke 1500 DEG C of calcining 3h in a nitrogen atmosphere,
The wherein property of carbene mixture: average molecular weight 650, aromatic ring number are 5, and cycloalkanes number of rings is 3, and aromatic carbon rate is 0.6, alkyl carbon
Rate is 0.4.Obtain real density 2.18g/cm3, thermal expansion coefficient 1.11 × 10-6/ DEG C, volatile matter 0.46wt%, yield 79.5%
Acicular petroleum coke.
Embodiment 3:
Take FCC slurry 1000g, with 55g iodomethane, 50g polyethylene glycol and 5g catalyst to boron trifluoride after mixing
It is fitted into corrosion resistant high temperature and high pressure kettle, temperature reaction is carried out under 0.5MPa nitrogen protection and 300r/min stirring, until 240
DEG C, constant temperature 5h obtains solid shaped polymer, after which is crushed, washs 2~3 times, drying for standby through clear water, completes catalysis
Polycondensation couples either shallow alkylated reaction.Then delayed coking is carried out, by the polymer-asphalt in the nitrogen atmosphere that pressure is 1MPa
Under in 560 DEG C of Coke-oven 10h, obtain green coke.High-temperature calcination is carried out later, by green coke 1500 DEG C of calcining 3h in a nitrogen atmosphere,
The wherein property of carbene mixture: average molecular weight 700, aromatic ring number are 4, and cycloalkanes number of rings is 2, and aromatic carbon rate is 0.8, alkyl carbon
Rate is 0.2.Obtain real density 2.52g/cm3, thermal expansion coefficient 1.21 × 10-6/ DEG C, volatile matter 0.32wt%, yield 72.5%
Acicular petroleum coke.
Embodiment 4:
FCC slurry 1000g is taken, is uniformly mixed with 60g iodoethane, 50g trimethylolpropane and 5g catalyst boron trifluoride
After be fitted into corrosion resistant high temperature and high pressure kettle, 0.5MPa nitrogen protection and 300r/min stirring under carry out temperature reaction, until 240
DEG C, constant temperature 5h obtains solid shaped polymer, after which is crushed, washs 2~3 times, drying for standby through clear water, completes catalysis
Polycondensation couples either shallow alkylated reaction.Then delayed coking is carried out, by the polymer-asphalt in the nitrogen atmosphere that pressure is 1MPa
Under in 560 DEG C of Coke-oven 10h, obtain green coke.High-temperature calcination is carried out later, by green coke 1500 DEG C of calcining 3h in a nitrogen atmosphere,
The wherein property of carbene mixture: average molecular weight 700, aromatic ring number are 5, and cycloalkanes number of rings is 3, and aromatic carbon rate is 0.6, alkyl carbon
Rate is 0.4.Obtain real density 2.36g/cm3, thermal expansion coefficient 1.42 × 10-6/ DEG C, volatile matter 0.41wt%, yield 70.9%
Acicular petroleum coke.
Embodiment 5:
FCC slurry 1000g is taken, is filled after mixing with 60g iodoethane, 50g polyethylene glycol and 5g catalyst boron trifluoride
Enter in corrosion resistant high temperature and high pressure kettle, carries out temperature reaction under 0.5MPa nitrogen protection and 300r/min stirring, until 180 DEG C,
Constant temperature 5h obtains solid shaped polymer, after which is crushed, washs 2~3 times through clear water, drying for standby, completes catalysis contracting
Poly- coupling either shallow alkylated reaction.Then delayed coking is carried out, by the polymer-asphalt in the case where pressure is the nitrogen atmosphere of 1MPa
In 560 DEG C of Coke-oven 10h, green coke is obtained, carries out high-temperature calcination later, by green coke 1500 DEG C of calcining 3h in a nitrogen atmosphere,
The property of middle carbene mixture: average molecular weight 780, aromatic ring number are 4, and cycloalkanes number of rings is 3, and aromatic carbon rate is 0.7, alkyl carbon rate
It is 0.3.Obtain real density 2.43g/cm3, thermal expansion coefficient 1.02 × 10-6/ DEG C, volatile matter 0.47wt%, yield 75.9%
Acicular petroleum coke.
The foregoing is only a preferred embodiment of the present invention, these specific embodiments are all based on the present invention
Different implementations under general idea, and scope of protection of the present invention is not limited thereto, it is any to be familiar with the art
Technical staff in the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all cover of the invention
Within protection scope.Therefore, the scope of protection of the invention shall be subject to the scope of protection specified in the patent claim.
Claims (10)
1. a kind of preparation method of high yield acicular petroleum coke, which comprises the steps of: by feedstock oil with it is halogenated
Alkane, polyalcohol and boron trifluoride are respectively 0.01~0.07g/g, 0.03~0.08g/g and 0.001~0.02g/g with oil ratio
Ratio be uniformly mixed reaction and generate that average molecular weight is larger, the higher carbene mixture of aromaticity；Then, by resulting carbon
Green matter mixture 10~14h of delayed coking at 550~600 DEG C obtains Raw needle coke, most afterwards through high-temperature calcination at 1500 DEG C
Obtain acicular petroleum coke.
2. a kind of preparation method of high yield acicular petroleum coke according to claim 1, it is characterised in that: the raw material
Oil is FCC slurry.
3. a kind of preparation method of high yield acicular petroleum coke according to claim 1, it is characterised in that: the carbon is green
The property of matter mixture are as follows: average molecular weight is 600~800, cycloalkanes number of rings 2~5, aromatic ring number 2~6, aromatic carbon rate 0.6~0.8,
Alkyl carbon rate 0.2~0.4.
4. a kind of preparation method of high yield acicular petroleum coke according to claim 1, it is characterised in that: described is halogenated
Alkane is iodomethane or iodoethane；The polyalcohol is one of polyethylene glycol, polypropylene glycol, trimethylolpropane or more
Kind；The catalyst is boron trifluoride.
5. a kind of preparation method of high yield acicular petroleum coke according to claim 1, it is characterised in that: catalyzed polycondensation coupling
It closes either shallow alkylation process to need to be filled with nitrogen and protected, pressure is 0.1~0.5MPa, using halogenated hydrocarbons as alkylating agent, more
First alcohol is couplant, and reaction temperature is 200~250 DEG C, reacts 4~6h.
6. a kind of preparation method of high yield acicular petroleum coke according to claim 1, it is characterised in that: the needle-shaped stone of gained
Oil coke yield >=70%, the acicular petroleum coke product of generation have height uniaxial orientation fine-fibrous interphase optical texture,
Interphase content >=90%, real density > 2.15g/cm3, thermal expansion coefficient CTE≤1.5 × 10-6/ DEG C, volatile matter < 0.6.
7. a kind of preparation method of high yield acicular petroleum coke according to claim 1-6, which is characterized in that institute
State preparation method specific steps are as follows: (1) in high temperature and high pressure kettle, according to the agent oil of 0.01~0.07g/g, 0.03~0.08g/g
--- halogenated hydrocarbons, couplant --- polyalcohol and FCC slurry mixing than by a certain amount of alkylating agent, and oil ratio is added and is
The catalyst boron trifluoride of 0.001~0.02g/g；(2) it is replaced after sealing through nitrogen, is filled with the nitrogen of 0.1~0.5MPa, and protect
It is constant to hold pressure；After alkylating agent is added, reaction temperature is 200~250 DEG C；Alkylation 4~6h of coupling, during the reaction
Keep revolving speed in 250~350r/min；(3) will reaction generate carbene mixture investment coking furnace in, pressure be 0.1~
10~14h is reacted in the nitrogen atmosphere of 0.9mpa at 550~600 DEG C, obtains green coke；(4) green coke high temperature in an inert atmosphere
2~6h is calcined at 1500 DEG C, obtains acicular petroleum coke.
8. a kind of described in any item acicular petroleum cokes of the preparation method preparation of high yield acicular petroleum coke of claim 1-7.
9. acicular petroleum coke according to claim 8, it is characterised in that: the acicular petroleum coke product of generation has height list
Fine-fibrous interphase optical texture, interphase content >=90%, real density > 2.15g/cm of axis orientation3, thermal expansion coefficient
CTE≤1.5×10-6/ DEG C, volatile matter < 0.6.
10. the purposes of the described in any item acicular petroleum cokes of claim 8-9, it is characterised in that: production ultra-high power graphite electrode, spy
Kind carbon material.
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| CN113621393A (en) * | 2021-07-21 | 2021-11-09 | 武汉钢铁有限公司 | Classification matching method for coking coal with volatile content of 18-22% |
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