CN109370629B - A kind of production method of coal-based needle coke - Google Patents
A kind of production method of coal-based needle coke Download PDFInfo
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- CN109370629B CN109370629B CN201811205547.XA CN201811205547A CN109370629B CN 109370629 B CN109370629 B CN 109370629B CN 201811205547 A CN201811205547 A CN 201811205547A CN 109370629 B CN109370629 B CN 109370629B
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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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- 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
- C10C1/04—Working-up tar by distillation
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Abstract
The invention belongs to needle coke preparation technical fields, disclose a kind of production method of coal-based needle coke, the method mixes coal tar asphalt and solvent, it is isolated to light phase and heavy phase, solvent in removal light phase is purified coal tar asphalt, coking is carried out to purification coal tar asphalt to handle to obtain coal-based needle coke, the solvent that the method uses is the mixture of aromatic hydrocarbon solvent and aliphatic solvent, it contains more≤200 DEG C of light fraction, the density of solvent is lower, after it is mixed with coal tar asphalt, the light phase of formation is easier to separate with heavy phase, and because containing a large amount of light fraction in solvent, the solvent is easier to separate with purification coal tar asphalt when separating the solvent in light phase, reduce the recycling energy consumption of solvent, improve the rate of recovery of solvent, reduce production cost.
Description
Technical field
The invention belongs to needle coke preparation technical fields, are related to the production method of needle coke, and in particular to a kind of coal measures needle
The production method of shape coke.
Background technique
Needle coke is a kind of high-quality carbon materials, due to gaining the name after crushing in elongated acicular texture, its favorable orientation,
Conduction, heating conduction are strong, are the primary raw materials for manufacturing advanced graphite electrode, have with the ultra high power graphite electrode that needle coke produces
Have the advantages that resistivity is low, bulk density is big, high mechanical strength, thermal expansion coefficient is small, thermal shock resistance is good.Needle coke graphitization
Product is widely used in the fields such as electric furnace steel making electrode, nuclear reactor decelerating material and rocketry.
The needle coke produced at present can be divided into petroleum needle coke and coal-based needle coke using the difference of raw material according to it
Two major classes.Wherein, petroleum needle coke is produced by raw material of petroleum heavy oil, coal-based needle coke be then with coal tar asphalt and
Its fraction is raw material production.In needle coke producing initial stage, petroleum needle coke is occupied an leading position, thereafter since oil price occupies height
Not lower and PETROLEUM PROCESSING lighting increasingly, causes petroleum needle-shape coke raw material to reduce, then from the 1970s later period
Start, broad development has been prepared in coal-based needle coke.The formation of coal-based needle coke must undergo unstable mesophasespherule
Formation and spherular growth and melt and process, and the toluene insoluble in coal tar pitch raw material-quinoline soluble matter (QS-
TI) and quinoline insolubles (QI) can hinder further growing up and melting simultaneously for mesophasespherule, so that fibre structure cannot be formed
Good coal-based needle coke.Therefore, the coal-based needle coke of high-quality in order to obtain it may first have to the coal of production coal-based needle coke
Tar asphalt is pre-processed to remove QS-TI and QI ingredient therein, is then carried out to obtained purification coal tar asphalt burnt
Change processing.As Chinese patent literature CN103509572A discloses a kind of work using solvent method preparation high-quality coal-based needle coke
Skill, the technique mix coal measures raw material with solvent, remove quinoline insolubles by physical separation, carry out after separation to clarified solution
Distillation carries out hydrotreating to the heavy end after distillation, and then coking obtains coal-based needle coke.However, being used in the technique
Its heavy end of solvent content it is high, solvent density is larger, after mixing with coal measures raw material, is not readily separated, increases solvent recovery
Difficulty, improve high production cost；In addition, not comprehensively utilizing to insoluble matter in the technique, coal measures raw material is reduced
Overall utilization rate, be unfavorable for improve environmental economical profit.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is that overcoming the existing technique for preparing coal-based needle coke, there are solvents to return
It is big and the problem of do not comprehensively utilize to raw material to receive difficulty, low energy consumption, rate of recovery height to provide a kind of solvent recovery, and to coal
The production method for the coal-based needle coke that the full fraction of tar is comprehensively utilized.
In order to solve the above technical problems, the present invention provides a kind of production method of coal-based needle coke, including coal tar drip
The coking step of green purifying step and purification coal tar asphalt, the purification of the coal tar asphalt include the following steps:
(1) coal tar asphalt and solvent are mixed, obtains the mixture of coal tar asphalt and solvent；
(2) mixture for separating the coal tar asphalt and solvent, obtains light phase and heavy phase；
(3) light phase and the heavy phase are discharged respectively；
(4) solvent in the light phase is removed, coal tar asphalt is purified；
Wherein, the solvent includes aromatic hydrocarbon solvent and aliphatic solvent, the aromatic hydrocarbon solvent be Doak Tar Oil and/
Or 150~270 DEG C of fractions that coking oil gas obtains, total aromatic hydrocarbons account for 70~80% by weight；The aliphatic solvent is to steam
It evaporates product that 270~360 DEG C of fractions that coal tar and/or coking oil gas obtain obtain through hydrogenated processing and is again fractionated and obtain
130~310 DEG C of fractions, or be fractionated obtained 130~310 DEG C of petroleum distillate, total saturated hydrocarbons accounts for 95 by weight~
99%.
Further, the mass ratio of the aromatic hydrocarbon solvent and the aliphatic solvent is 5:5~7:3.
Further, the mass ratio of the solvent and the coal tar asphalt is (0.8~1.2): 1.
Further, step (1) coal tar asphalt and the temperature of solvent mixing are 100~140 DEG C.
Further, step (2) is described is separated into sedimentation separation, and the temperature of the sedimentation is 60~100 DEG C, sedimentation when
Between be 4~10h.
Further, the mass ratio (17~19) of step (2) light phase and heavy phase: 1.
Further, step (4) is described is separated into vacuum distillation.
Further, further include the steps that handling the heavy phase after the step (3), it is described to heavy phase at
Reason includes the following steps:
It is evaporated under reduced pressure the heavy phase, the solvent that recycling is obtained makees obtained residue as solvent in step (1)
For binder pitch.
It further, further include that the coal tar asphalt is pre- before step (1) mixes the coal tar asphalt and solvent
The step of heat is to 120~150 DEG C.
Further, the production method further includes the solvent in the light phase that will be removed as in step (1)
The step of solvent.
Further, the production method further includes the coking that will be generated in the coking step of the purification coal tar asphalt
The step of oil gas is as the raw material for preparing the solvent.
Herein, the TS is xylene solubles, and QS-TI is toluene insoluble quinoline soluble matter, and QI is quinoline insolubles.
Technical solution of the present invention has the advantages that
1. the production method of coal-based needle coke provided by the invention, after the method mixes coal tar asphalt and solvent,
It is isolated to light phase and heavy phase, the solvent removed in light phase is purified coal tar asphalt, carries out to purification coal tar asphalt
Coking handles to obtain coal-based needle coke, and the solvent that the method uses is the mixture of aromatic hydrocarbon solvent and aliphatic solvent,
Containing more≤200 DEG C of light fraction, compared to the solvent containing a large amount of heavy ends, solvent density of the invention is lower, will
After it is mixed with coal tar asphalt, the light phase of formation is easier to separate with heavy phase, and because containing a large amount of light fraction in solvent, goes
The solvent is easier to separate with purification coal tar asphalt when except solvent in light phase, reduces the recycling energy consumption of solvent, improves
The rate of recovery of solvent, reduces production cost.
The solvent of the invention is coal measures solvent, by the by-product during coal tar and/or coal tar production needle coke
Coking oil gas is obtained through processing, is improved the overall utilization rate of coal tar, is reduced production cost, has good environmental economy
Benefit.
2. the production method of coal-based needle coke provided by the invention, the method is defined the fragrant rouge ratio of solvent, with
Make the solvent moderate viscosity to be formed, not only there is stronger material asphalt solvability, makes the rate of recovery for purifying coal tar asphalt
Height, QI and QS-TI content is few, improves the quality of coal-based needle coke, and the solvent is also easy to recycle, high financial profit.
3. the production method of coal-based needle coke provided by the invention carries out the mass ratio of the solvent and coal tar asphalt
It limits, on the one hand avoids the too small restricted T S dissolution of mass ratio, the yield of purification coal tar asphalt is reduced, so that it is needle-shaped to reduce coal measures
On the other hand burnt yield also avoids solute amount than the excessive waste for leading to solvent.
4. the production method of coal-based needle coke provided by the invention, to the mixing temperature of the coal tar asphalt and solvent into
Row limits, and is the too low dissolution for being unfavorable for coal tar asphalt of temperature because mixed, while also resulting in the coal tar drip of dissolution
Blueness deposition is precipitated, and is unfavorable for continuous and stable production；And mixed temperature is excessively high, and it is excessively high to will lead to energy consumption, and solvent loss is serious.
5. the production method of coal-based needle coke provided by the invention limits the sedimentation temperature of the coal tar and solvent mixture
The segregation ratio of degree and time and light phase and heavy phase guarantees the product quality and yield of purification coal tar asphalt, to produce Gao Pin
Matter coal-based needle coke provides good precondition.
6. the production method of coal-based needle coke provided by the invention further includes handling the heavy phase, will recycle
To solvent recycle, using obtained residue as binder pitch, proposed for the high quinoline insolubles residue of by-product clear
Utilization orientation, substantially increase the overall utilization rate of coal tar, significantly increase the added value of coal tar, have apparent ring
Border economic benefit.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the production technological process of coal-based needle coke of the present invention.
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
In following embodiment, middle coalite tar is provided by Shaanxi Coal Chemical Industry Group Shenmu Tianyuan Chemical Co., Ltd,
Using the middle coalite tar it is previous as be preheated to 50~60 DEG C；Coking oil gas forms needle-shaped for coal tar asphalt coking
The oil gas generated during burnt.Specific experiment step or condition are not specified in embodiment, is retouched according to the literature in the art
The operation for the routine experiment step stated or condition can carry out.
Embodiment 1
After middle coalite tar and coking oil gas are mixed, it is sent into the first fractionating column air-distillation after preheating, is fractionated to obtain tower
Oil gas, the first survey line distillate (150~270 DEG C), the second survey line distillate (270~360 DEG C), coal tar asphalt are pushed up, is collected
First survey line distillate measures its total aromatic hydrocarbons by weight 70~80% to get aromatic solvent, according to hydro carbons composing method.
After tower top oil gas is mixed with the second survey line distillate (270~360 DEG C), hydrogenator is sent into after preheating, setting temperature is
320 DEG C, pressure 14MPa, hydrotreating is carried out to the mixture of tower top oil gas and the second survey line distillate, after hydrotreating
Obtained product is sent into the air-distillation of after-fractionating tower, and 130~310 DEG C of distillates being fractionated are aliphatic solvent, root
Its total saturated hydrocarbons by weight 95~99% is measured according to hydro carbons composing method.Above-mentioned aromatic solvent is pressed with aliphatic solvent
On-line mixing is carried out according to mass ratio 7:3, obtains the solvent for preparing coal-based needle coke.
Above-mentioned solvent is preheated to 110 DEG C, coal tar asphalt is preheated to 140 DEG C, is then 1:1 mixing with mass ratio, obtains
To the mixture of coal tar asphalt and solvent.Stirring is cooled to 90 DEG C until coal tar asphalt sufficiently dissolves at 130 DEG C,
Standing sedimentation, isolated light phase and heavy phase collect light phase and heavy phase, for use respectively.In the present embodiment, time of repose 4h,
The segregation ratio of light phase and heavy phase is 17:1.Light phase is evaporated under reduced pressure, removes the solvent in light phase up to the purification coal
Tar asphalt recycles resulting solvent and enters solvent tank, recycles.Above-mentioned purification coal tar asphalt is sent into coking tower, if
The temperature for setting coking is 460 DEG C, and the pressure of coking is 0.15MPa, up to the coal-based needle coke product after pyrogenetic reaction, together
When, the coking oil gas that coking is generated is sent into the first fractionating column, molten collectively as coal-based needle coke is prepared with middle coalite tar
The raw material of agent.Heavy phase is evaporated under reduced pressure, the solvent removed in heavy phase obtains asphaltic residue, it is used as binder pitch,
It recycles resulting solvent and enters solvent tank, recycle.
Embodiment 2
After middle coalite tar and coking oil gas are mixed, it is sent into the first fractionating column air-distillation after preheating, is fractionated to obtain tower
Oil gas, the first survey line distillate (150~270 DEG C), the second survey line distillate (270~360 DEG C), coal tar asphalt are pushed up, is collected
First survey line distillate measures its total aromatic hydrocarbons by weight 70~80% to get aromatic solvent, according to hydro carbons composing method.
After tower top oil gas is mixed with the second survey line distillate (270~360 DEG C), hydrogenator is sent into after preheating, setting temperature is
250 DEG C, pressure 15MPa, hydrotreating is carried out to the mixture of tower top oil gas and the second survey line distillate, after hydrotreating
Obtained product is sent into the air-distillation of after-fractionating tower, and 130~310 DEG C of distillates being fractionated are aliphatic solvent, root
Its total saturated hydrocarbons by weight 95~99% is measured according to hydro carbons composing method.Above-mentioned aromatic solvent is pressed with aliphatic solvent
On-line mixing is carried out according to mass ratio 6:4, obtains the solvent for preparing coal-based needle coke.
Above-mentioned solvent is preheated to 120 DEG C, then it is 0.8:1 mixing with mass ratio that coal tar asphalt, which is preheated to 150 DEG C,
Obtain the mixture of coal tar asphalt and solvent.Stirring is cooled to 100 until coal tar asphalt sufficiently dissolves at 140 DEG C
DEG C, standing sedimentation, isolated light phase and heavy phase collect light phase and heavy phase, for use respectively.In the present embodiment, time of repose is
The segregation ratio of 6h, light phase and heavy phase is 18:1.Light phase is evaporated under reduced pressure, removes the solvent in light phase up to the purification
Coal tar asphalt recycles resulting solvent and enters solvent tank, recycles.Above-mentioned purification coal tar asphalt is sent into coking tower,
The temperature that coking is arranged is 460 DEG C, and the pressure of coking is 0.15MPa, up to the coal-based needle coke product after pyrogenetic reaction, together
When, the coking oil gas that coking is generated is sent into the first fractionating column, molten collectively as coal-based needle coke is prepared with middle coalite tar
The raw material of agent.Heavy phase is evaporated under reduced pressure, the solvent removed in heavy phase obtains asphaltic residue, it is used as binder pitch,
It recycles resulting solvent and enters solvent tank, recycle.
Embodiment 3
After middle coalite tar and coking oil gas are mixed, it is sent into the first fractionating column air-distillation after preheating, is fractionated to obtain tower
Oil gas, the first survey line distillate (150~270 DEG C), the second survey line distillate (270~360 DEG C), coal tar asphalt are pushed up, is collected
First survey line distillate measures its total aromatic hydrocarbons by weight 70~80% to get aromatic solvent, according to hydro carbons composing method.
After tower top oil gas is mixed with the second survey line distillate (270~360 DEG C), hydrogenator is sent into after preheating, setting temperature is
390 DEG C, pressure 12MPa, hydrotreating is carried out to the mixture of tower top oil gas and the second survey line distillate, after hydrotreating
Obtained product is sent into the air-distillation of after-fractionating tower, and 130~310 DEG C of distillates being fractionated are aliphatic solvent, root
Its total saturated hydrocarbons by weight 95~99% is measured according to hydro carbons composing method.Above-mentioned aromatic solvent is pressed with aliphatic solvent
Be stirred in tank according to mass ratio 6:4, obtains the solvent for preparing coal-based needle coke.
Above-mentioned solvent is preheated to 100 DEG C, then it is 1.2:1 mixing with mass ratio that coal tar asphalt, which is preheated to 140 DEG C,
Obtain the mixture of coal tar asphalt and solvent.Stirring is cooled to 80 until coal tar asphalt sufficiently dissolves at 120 DEG C
DEG C, standing sedimentation, isolated light phase and heavy phase collect light phase and heavy phase, for use respectively.In the present embodiment, time of repose is
The segregation ratio of 8h, light phase and heavy phase is 18:1.Light phase is evaporated under reduced pressure, removes the solvent in light phase up to the purification
Coal tar asphalt recycles resulting solvent and enters solvent tank, recycles.Above-mentioned purification coal tar asphalt is sent into coking tower,
The temperature that coking is arranged is 460 DEG C, and the pressure of coking is 0.15MPa, up to the coal-based needle coke product after pyrogenetic reaction, together
When, the coking oil gas that coking is generated is sent into the first fractionating column, molten collectively as coal-based needle coke is prepared with middle coalite tar
The raw material of agent.Heavy phase is evaporated under reduced pressure, the solvent removed in heavy phase obtains asphaltic residue, it is used as binder pitch,
It recycles resulting solvent and enters solvent tank, recycle.
Embodiment 4
Will middle coalite tar preheating after be sent into the first fractionating column air-distillation, be fractionated tower top oil gas, the first survey line evaporate
Divide oily (150~270 DEG C), the second survey line distillate (270~360 DEG C), coal tar asphalt, collects the first survey line distillate, i.e.,
Aromatic solvent is obtained, its total aromatic hydrocarbons by weight 70~80% is measured according to hydro carbons composing method.After the preheating of tower top oil gas
It is sent into hydrogenator, setting temperature is 390 DEG C, pressure 12MPa, hydrotreating is carried out to tower top oil gas, by hydrotreating
The product obtained afterwards is sent into the air-distillation of after-fractionating tower, and 130~310 DEG C of distillates being fractionated are aliphatic solvent,
Its total saturated hydrocarbons by weight 95~99% is measured according to hydro carbons composing method.By above-mentioned aromatic solvent and aliphatic solvent
Be stirred in tank according to mass ratio 5:5, obtains the solvent for preparing coal-based needle coke.
Above-mentioned solvent is preheated to 100 DEG C, then it is 1.2:1 mixing with mass ratio that coal tar asphalt, which is preheated to 120 DEG C,
Obtain the mixture of coal tar asphalt and solvent.Stirring is cooled to 60 until coal tar asphalt sufficiently dissolves at 100 DEG C
DEG C, standing sedimentation, isolated light phase and heavy phase collect light phase and heavy phase, for use respectively.In the present embodiment, time of repose is
The segregation ratio of 10h, light phase and heavy phase is 19:1.Light phase is evaporated under reduced pressure, removes the solvent in light phase up to described net
Change coal tar asphalt, recycles resulting solvent and enter solvent tank, recycle.Above-mentioned purification coal tar asphalt is sent into coking
Tower, the temperature that coking is arranged is 460 DEG C, and the pressure of coking is 0.15MPa, is produced after pyrogenetic reaction up to the coal-based needle coke
Product, meanwhile, the coking oil gas that coking is generated is sent into the first fractionating column, needle-shaped collectively as coal measures is prepared with middle coalite tar
The raw material of burnt solvent.Heavy phase is evaporated under reduced pressure, the solvent removed in heavy phase obtains asphaltic residue, makes as binder pitch
With recycling resulting solvent and enter solvent tank, recycle.
Embodiment 5
After middle coalite tar and coking oil gas are mixed, it is sent into the first fractionating column air-distillation after preheating, is fractionated to obtain tower
Oil gas, the first survey line distillate (150~270 DEG C), the second survey line distillate (270~360 DEG C), coal tar asphalt are pushed up, is collected
First survey line distillate measures its total aromatic hydrocarbons by weight 70~80% to get aromatic solvent, according to hydro carbons composing method.
Air-distillation petroleum raw material, 130~310 DEG C of distillates being fractionated are aliphatic solvent, according to hydro carbons composing method
Measure its total saturated hydrocarbons by weight 95~99%.By above-mentioned aromatic solvent and aliphatic solvent according to mass ratio 6:4 into
It is stirred in row tank, obtains the solvent for preparing coal-based needle coke.
Above-mentioned solvent is preheated to 100 DEG C, then it is 1.2:1 mixing with mass ratio that coal tar asphalt, which is preheated to 130 DEG C,
Obtain the mixture of coal tar asphalt and solvent.Stirring is cooled to 80 until coal tar asphalt sufficiently dissolves at 120 DEG C
DEG C, standing sedimentation, isolated light phase and heavy phase collect light phase and heavy phase, for use respectively.In the present embodiment, time of repose is
The segregation ratio of 8h, light phase and heavy phase is 18:1.Light phase is evaporated under reduced pressure, removes the solvent in light phase up to the purification
Coal tar asphalt recycles resulting solvent and enters solvent tank, recycles.Above-mentioned purification coal tar asphalt is sent into coking tower,
The temperature that coking is arranged is 460 DEG C, and the pressure of coking is 0.15MPa, up to the coal-based needle coke product after pyrogenetic reaction, together
When, the coking oil gas that coking is generated is sent into the first fractionating column, molten collectively as coal-based needle coke is prepared with middle coalite tar
The raw material of agent.Heavy phase is evaporated under reduced pressure, the solvent removed in heavy phase obtains asphaltic residue, it is used as binder pitch,
It recycles resulting solvent and enters solvent tank, recycle.
Comparative example 1
Coal-based needle coke is prepared according to the method that Chinese patent literature CN103509572A embodiment 4 provides.
Comparative example 2
Coal-based needle coke is prepared according to the method that comparative example 1 provides, the difference is that, in this comparative example, solvent
It is mixed with coal tar asphalt according to mass ratio for 1.2:1.
Comparative example 3
Coal-based needle coke is prepared according to the method for the embodiment of the present invention 3, the difference is that, it is molten in this comparative example
Agent is that 2:1 is mixed according to mass ratio with coal tar asphalt.
Comparative example 4
Coal-based needle coke is prepared according to the method for the embodiment of the present invention 3, the difference is that, it is molten in this comparative example
Agent is that 0.5:1 is mixed according to mass ratio with coal tar asphalt.
Comparative example 5
Coal-based needle coke is prepared according to the method for the embodiment of the present invention 3, the difference is that, in this comparative example, institute
Solvent is stated by the way that aromatic solvent and aliphatic solvent to be mixed to get according to mass ratio 4:1.
Comparative example 6
Coal-based needle coke is prepared according to the method for the embodiment of the present invention 3, the difference is that, in this comparative example, gently
It is mutually 21:1 with the segregation ratio of heavy phase.
Comparative example 7
Coal-based needle coke is prepared according to the method for the embodiment of the present invention 3, the difference is that, in this comparative example, gently
It is mutually 15:1 with the segregation ratio of heavy phase.
Experimental example 1
The present invention is determined the boiling range of solvent in embodiment 1-5, initial boiling point >=130 DEG C under normal pressure, and 200
Quantity of distillate >=45% (w/w) before DEG C, quantity of distillate >=95% (w/w) before 300 DEG C.Meanwhile we are bright also to embodiment 1-5 and comparison
Solvent density is determined respectively in example 1-5, and measurement result is as shown in table 1 below.
The density case of the various solvents of table 1
| Density (g/cm3) | |
| Embodiment 1 | 0.86~0.92 |
| Embodiment 2 | 0.86~0.92 |
| Embodiment 3 | 0.86~0.92 |
| Embodiment 4 | 0.86~0.92 |
| Embodiment 5 | 0.86~0.92 |
| Comparative example 1 | 1.05~1.12 |
| Comparative example 2 | 1.05~1.12 |
| Comparative example 3 | 0.86~0.92 |
| Comparative example 4 | 0.86~0.92 |
| Comparative example 5 | 0.88~0.95 |
Experimental example 2
In order to reduce production cost, the overall utilization rate of coal tar is improved, the present invention is by embodiment 1-5 and comparative example 1-
Solvent after handling coal tar asphalt in 7 is recycled, and calculates separately the corresponding rate of recovery, as a result as shown in table 2 below.
The rate of recovery of the various solvents of table 2
Experimental example 3
In order to confirm technical effect of the invention, the present invention is first to the quinoline non-soluble in the coal tar asphalt before solvent processing
Object (QI), toluene insoluble-quinoline soluble matter (QS-TI) percentage composition are measured, and as a result respectively 1.2% and 5.79%, so
Afterwards to quinoline in the purification coal tar asphalt handled respectively with the solvent in above-described embodiment 1-5 and comparative example 1-7
Insoluble moiety object (QI), toluene insoluble-quinoline soluble matter (QS-TI) percentage composition are measured respectively, measurement result such as the following table 3 institute
Show.
QI and QS-TI content in the various purification coal tar asphaltes of table 3
Experimental example 4
Obtained purification coal after measuring the coal tar asphalt of embodiment 1-5 and comparative example 1-7 respectively and being handled with solvent
The quality of tar asphalt, calculates the yield of the purification coal tar asphalt, and result is as shown in table 4 below.
The yield of coal tar asphalt is purified under the various methods of table 4
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (9)
1. a kind of production method of coal-based needle coke, the coking of purifying step and purification coal tar asphalt including coal tar asphalt
The purification of step, the coal tar asphalt includes the following steps:
(1) coal tar asphalt and solvent are mixed, obtains the mixture of coal tar asphalt and solvent；
(2) mixture for separating the coal tar asphalt and solvent, obtains light phase and heavy phase；
(3) light phase and the heavy phase are discharged respectively；
(4) solvent in the light phase is removed, coal tar asphalt is purified；
It is characterized in that, the solvent includes aromatic hydrocarbon solvent and aliphatic solvent, the aromatic hydrocarbon solvent and the aliphatic hydrocarbon
The mass ratio of solvent is 6:4~7:3；The aromatic hydrocarbon solvent is 150~270 that Doak Tar Oil and/or coking oil gas obtain
DEG C fraction, total aromatic hydrocarbons account for 70~80% by weight；The aliphatic solvent is that Doak Tar Oil and/or coking oil gas obtain
The product that obtains through hydrogenated processing of 270~360 DEG C of fractions be fractionated 130~310 DEG C of obtained fractions again, or be fractionated and obtain
130~310 DEG C of petroleum distillate, total saturated hydrocarbons accounts for 95~99% by weight.
2. production method according to claim 1, which is characterized in that the mass ratio of the solvent and the coal tar asphalt
For (0.8~1.2): 1.
3. production method according to claim 1 or 2, which is characterized in that step (1) coal tar asphalt and solvent are mixed
The temperature of conjunction is 100~140 DEG C.
4. production method according to claim 1 or 2, which is characterized in that step (2) is described to be separated into sedimentation separation, institute
The temperature for stating sedimentation is 60~100 DEG C, and the time of sedimentation is 4~10h.
5. production method according to claim 1 or 2, which is characterized in that the mass ratio of step (2) light phase and heavy phase
For (17~19): 1.
6. production method according to claim 1 or 2, which is characterized in that after the step (3) further include to the heavy phase
The step of being handled, it is described to heavy phase carry out processing include the following steps:
It is evaporated under reduced pressure the heavy phase, the solvent that recycling is obtained is as solvent in step (1), using obtained residue as viscous
Tie agent pitch.
7. production method according to claim 1 or 2, which is characterized in that step (1) is by the coal tar asphalt and solvent
Further include the steps that the coal tar asphalt being preheated to 120~150 DEG C before mixing.
8. production method according to claim 1 or 2, which is characterized in that further include the institute in the light phase that will be removed
Solvent is stated as in step (1) the step of solvent.
9. production method according to claim 1 or 2, which is characterized in that further include by the purification coal tar asphalt
The step of coking oil gas generated in coking step is as the raw material for preparing the solvent.
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| CN102676196A (en) * | 2011-03-18 | 2012-09-19 | 北京三聚创洁科技发展有限公司 | Coal tar pitch for preparing needle coke, method for preparing same and solvent used in preparation process of coal tar pitch |
| CN103509574A (en) * | 2012-06-19 | 2014-01-15 | 北京宝塔三聚能源科技有限公司 | Process for preparing high-quality coal-series needle-coke |
| CN103509572A (en) * | 2012-06-19 | 2014-01-15 | 北京宝塔三聚能源科技有限公司 | Solvent process for preparation of high-quality coal-based needle coke |
| CN103509575A (en) * | 2012-06-19 | 2014-01-15 | 北京宝塔三聚能源科技有限公司 | Solvent used for preparation of high-quality coal-based needle coke |
| CN107892937A (en) * | 2017-12-01 | 2018-04-10 | 枣庄矿业集团煤化工研究院有限公司 | A kind of efficient solvent preparation method of refined bitumen |
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|---|---|---|---|---|
| CN102676196A (en) * | 2011-03-18 | 2012-09-19 | 北京三聚创洁科技发展有限公司 | Coal tar pitch for preparing needle coke, method for preparing same and solvent used in preparation process of coal tar pitch |
| CN103509574A (en) * | 2012-06-19 | 2014-01-15 | 北京宝塔三聚能源科技有限公司 | Process for preparing high-quality coal-series needle-coke |
| CN103509572A (en) * | 2012-06-19 | 2014-01-15 | 北京宝塔三聚能源科技有限公司 | Solvent process for preparation of high-quality coal-based needle coke |
| CN103509575A (en) * | 2012-06-19 | 2014-01-15 | 北京宝塔三聚能源科技有限公司 | Solvent used for preparation of high-quality coal-based needle coke |
| CN107892937A (en) * | 2017-12-01 | 2018-04-10 | 枣庄矿业集团煤化工研究院有限公司 | A kind of efficient solvent preparation method of refined bitumen |
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