KR101764712B1 - Method and apparatus for producing binder for coke - Google Patents

Method and apparatus for producing binder for coke Download PDF

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Publication number
KR101764712B1
KR101764712B1 KR1020150186331A KR20150186331A KR101764712B1 KR 101764712 B1 KR101764712 B1 KR 101764712B1 KR 1020150186331 A KR1020150186331 A KR 1020150186331A KR 20150186331 A KR20150186331 A KR 20150186331A KR 101764712 B1 KR101764712 B1 KR 101764712B1
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South Korea
Prior art keywords
coal
solvent
mixer
additive
additional solvent
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KR1020150186331A
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Korean (ko)
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KR20170076275A (en
Inventor
김희수
이승재
박상현
이상온
박정준
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주식회사 포스코
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Priority to KR1020150186331A priority Critical patent/KR101764712B1/en
Priority to CN201680071502.0A priority patent/CN108368430A/en
Priority to AU2016376254A priority patent/AU2016376254A1/en
Priority to PCT/KR2016/012865 priority patent/WO2017111301A1/en
Priority to BR112018012474-5A priority patent/BR112018012474A2/en
Publication of KR20170076275A publication Critical patent/KR20170076275A/en
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Publication of KR101764712B1 publication Critical patent/KR101764712B1/en
Priority to AU2020202042A priority patent/AU2020202042A1/en

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B57/00Other carbonising or coking processes; Features of destructive distillation processes in general
    • C10B57/04Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition
    • C10B57/06Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition containing additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D35/00Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/02Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00Disintegrating plant with or without drying of the material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B57/00Other carbonising or coking processes; Features of destructive distillation processes in general
    • C10B57/04Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition
    • B01F2215/0075

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

In order to maximize the solid-liquid separation efficiency with respect to the viscous liquefied slurry in the preparation of the additive for coke, a feed step of supplying an additional solvent to the liquefied product, a mixing step of lowering the viscosity of the liquefied product by mixing the liquefied product and the further solvent And a filtration step of subjecting the liquefied product to solid-liquid separation.

Description

TECHNICAL FIELD [0001] The present invention relates to an additive for coke,

A manufacturing method and an apparatus for manufacturing an additive for coke used for improving coke strength are disclosed.

Generally, coke is produced through a coke making process using coking coal. The coking coal used to manufacture the coke is classified as hard-boiled and un-boiled, depending on the degree of cohesion. For stable operation of large blast furnaces, the use of high-strength coke is required. In order to produce a high-strength coke, it is advantageous to use strong coals having excellent cohesiveness or to use a large amount of coals compared to uncoated coals. In the meantime, a large amount of high-priced, high-priced strong coals has been used in the production of coke.

However, due to the rapid increase in demand for coking coal for metallurgical use globally and the limited reserves of hard-boiled coals, it has become increasingly difficult to secure strong coals, which has led to a surge in prices. Accordingly, the development of a technique for manufacturing high-strength coke while using low-cost and low-cost coking coal such as bituminous coal or lignite as coking coal is actively under way.

For example, a technique has been developed for producing a quality improving agent for coke production through a sales method in which a low-grade raw material is dissolved in an expensive supercritical solvent under a high-temperature and high-pressure condition to extract a cohesive substance.

However, nowadays, the focus is mainly on the production of oil from coal, so there is no optimized process for the extraction of additives, which is insufficient to produce additives effectively. In addition, there is a problem that the economical efficiency in production of additives is inferior due to frequent breakdown and new operating know-how by using existing coal direct liquefaction type process.

Accordingly, it is required to develop an optimized and differentiated technique capable of effectively producing additive for coke.

A method and an apparatus for manufacturing an additive for coke which are capable of more effectively separating additives for coke and residues in manufacturing additives for coke.

The present invention also provides a method and apparatus for manufacturing an additive for coke which can maximize the solid-liquid separation efficiency with respect to a viscous liquefied slurry.

The additive manufacturing method of this embodiment includes: a coal pretreatment step of dispersing coal into a slurry by dispersing it in a solvent; A step of adding a dispersed iron catalyst during the pretreatment of coal; A coal liquefaction process for liquefying coal slurry by reacting coal slurry with cracking gas; A step of supplying COG and / or LNG with a cracking gas during a coal liquefaction process; A separation step of separating the additive from the liquefied product; And a recycle process in which the liquid oil obtained in the separation process is supplied to the coal pretreatment process and used as a solvent.

The coal pretreatment step may further include pulverizing coal and drying the pulverized coal.

The coal may comprise lignite or sub-bituminous coal.

In the coal pulverization step, the coal may be pulverized to a size of 60 mesh or less.

The step of drying the coal may include drying the coal so that the moisture content of the coal is 10 wt% or less.

The coal pretreatment may be performed by mixing the dried coal with the solvent at a weight ratio of 1/1 to 1/4 to form a slurry.

The dispersed iron catalyst may be Fe 2 O 3 .

The dispersed iron catalyst may be added in an amount of 0.5 to 3.0 parts by weight based on 100 parts by weight of coal.

The coal liquefaction process may be performed at a temperature of 250 to 450 DEG C and a pressure of 30 to 120 bar.

The coal liquefaction process may be performed by heating the cracking gas at 400 to 600 ° C.

The separation step includes a separating step of separating the gas component from the liquefied product, a filtration step of separating the liquid material and the solid matter, and a fractionation step of distilling the liquid material separated in the filtration step to separate the additive can do.

The recycle process may be such that the oil separated from the additive in the fractional distillation step is supplied to the coal pretreatment process.

The filtration step may be performed at a temperature of 120 to 400 ° C.

The fractionation step may be carried out at a temperature of from 350 to 450 < 0 > C.

The filtration step may further comprise a feeding step of supplying an additional solvent to the liquefied product, and a mixing step of mixing the liquefied product and the further solvent to lower the viscosity of the liquefied product.

The filtration step may further include a recovery step of recovering only the additional solvent from the liquid material after solid-liquid separation.

The filtration step may further include a reuse step of transferring and supplying the additional solvent recovered in the recovery step to the mixing step.

The additional solvent may be a solution having a different boiling point compared to the solvent mixed in the liquefied product.

The additional solvent may be any one selected from toluene, nucleic acid, and alcohol.

The apparatus for producing an additive according to this embodiment comprises a mixer for mixing a pretreated coal and a solvent into a slurry, a catalyst supply unit for supplying the dispersed iron catalyst to the mixer, a reactor for liquefying the coal slurry through the mixer, A separator for separating the additive from the liquefied product generated from the reactor, a separator connected between the separator and the mixer for supplying the oil separated from the separator to the mixer as a solvent, And a supply line for supplying the supply voltage.

The separator includes a separator for separating the gas component from the liquefaction process product, a filter device connected to the separator for separating the liquid material and the solid material, and a separator for separating the additive from the liquid material, And an oil separator connected to the mixer through the oil separator and supplying the oil separated from the additive to the mixer.

The filter device includes a filter unit for solid-liquid separating a liquefied product into a liquid material and a solid material, a mixer connected to the inlet of the filter unit for mixing an additional solvent into a liquefied product and supplying the mixture to a filter unit, and a supply unit for supplying an additional solvent to the mixer .

The filter device may further include a recovery tower connected to the filter outlet side for recovering the additional solvent from the liquid material separated in the filter unit.

And a recovery line connected between the recovery tower and the mixer for re-supplying the recovered additional solvent to the mixer.

The additional solvent may be any one selected from toluene, nucleic acid, and alcohol.

The manufacturing apparatus may further include a crusher for crushing coal for pretreatment of coal, and a drier for drying the crushed coal.

The coal may comprise lignite or sub-bituminous coal.

The pulverizer can pulverize coal to a size of 60 mesh or less.

The dryer may be configured to dry the coal so that the moisture content of the coal is 10 wt% or less.

The catalyst supply unit may be configured to supply Fe 2 O 3 as a dispersed iron catalyst.

The catalyst supply unit may be charged with 0.5 to 3.0 parts by weight of the dispersed iron catalyst per 100 parts by weight of coal.

As described above, according to this embodiment, by adding a solvent to the liquefied slurry and lowering the viscosity, the solid-liquid separation operation can be performed more easily.

In addition, productivity of the coke additive can be increased by performing the filtration work more effectively while minimizing clogging of the filter with respect to the viscous liquefied slurry.

1 is a schematic structural view showing an apparatus for producing additive for coke according to this embodiment.
2 is a schematic view showing a filter device of an apparatus for producing additive for coke according to this embodiment.
FIG. 3 is a graph showing the content of additives and oil remaining in the solid material separated through the separation step according to the present embodiment, in comparison with the conventional method.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention. The singular forms as used herein include plural forms as long as the phrases do not expressly express the opposite meaning thereto. Means that a particular feature, region, integer, step, operation, element and / or component is specified, and that other specific features, regions, integers, steps, operations, elements, components, and / And the like.

Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. Accordingly, the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.

Fig. 1 schematically shows the construction of an apparatus for producing additive for coke according to this embodiment.

As shown in FIG. 1, the additive manufacturing apparatus of the present embodiment includes a mixer 10 for mixing a pretreated coal and a solvent into a slurry, a catalyst supply unit 20 for supplying a dispersion catalyst to the mixer 10, A reactor 30 for liquefying a coal slurry through the reactor 10, a gas supply 32 for supplying a cracking gas to the reactor 30, a separator 30 for separating the additive from the liquefied product generated from the reactor 30, And a supply line 50 connected between the separator 40 and the mixer 10 to supply the oil separated from the separator to the mixer 10 as a solvent.

The manufacturing apparatus may further include a crusher 12 for crushing coal and a drier 14 for drying the crushed coal to pretreat coal.

In this embodiment, the raw material for the additive manufacturing coal may include low-grade non-coking coal such as lignite and sub-bituminous coal. Low-grade carbon such as lignite and bituminous coal has low physical properties such as cohesiveness, but it is rich in resources and low in cost, so that it is possible to lower the production cost when manufacturing additive for coke.

The mixer 10 mixes the pretreated coal with a solvent to form a coal slurry.

In the present embodiment, the solvent introduced into the mixer 10 is structured such that the additive is finally separated through the separator 40 and the remaining oil is utilized.

To this end, the feed line 50 is connected between the separator 40 and the mixer 10 so that the oil remaining after the additive separation is recycled as solvent to the mixer 10 via the feed line 50.

As described above, the liquid oil separated through the separator 40 is directly supplied to the mixer 10 and recycled as a solvent, so that the facility can be simplified, and the process can be simplified to reduce the cost of producing the additive.

The catalyst supply unit 20 is connected to the mixer 10 to supply a dispersed iron catalyst. Thus, the dispersed iron catalyst is evenly mixed with the coal and the solvent in the mixer 10.

In this embodiment, the dispersed iron catalyst may be Fe 2 O 3 . By adding the dispersed iron catalyst to the coal slurry in this way, the reactivity in the liquefaction reaction can be increased. Accordingly, even when COG or LNG is used as the cracking gas in the liquefaction reaction, the dispersed iron catalyst can increase the reactivity and can obtain a sufficient reaction effect for the production of the additive.

The mixed coal slurry in the mixer 10 is conveyed to the reactor 30 by a high-pressure pump. The coal slurry is supplied to the coal slurry through the heating unit 16 provided between the mixer 10 and the reactor 30 in the process of transferring the coal slurry from the mixer 10 to the reactor 30, can do.

The reactor 30 is a vessel which is sufficiently resistant to high temperature and high pressure and has a reaction space therein, and liquefies the coal slurry under high temperature and high pressure.

A heater or the like for applying thermal energy to the reactor 30 is installed outside the reactor 30, and an agitator may be installed therein. The gas supply unit 32 is connected to one side of the reactor 30 to supply a cracking gas to the reactor 30. In the present embodiment, the gas supply unit 32 supplies COG (Coke Oven Gas), LNG (Liquefied Natural Gas), or a combination thereof as a cracking gas.

Thus, by using COG or LNG as the cracking gas, the apparatus of this embodiment does not need to be provided with a conventional hydrogen production facility. The hydrogen production facility is very complicated as it is known. The construction cost is 1/4 of the total installation cost and the operation cost is also high. Therefore, in the case of this embodiment, since it is not necessary to construct a hydrogen production facility, the entire plant scale can be reduced and the production cost of the additive can be greatly reduced.

The separation unit 40 includes a separator 42 for separating the gas component from the liquefied product, a filter device 44 connected to the separator for separating the liquid material and the solid material, And a distiller 46 for separating the coke additive (B) by distillation.

The distiller 46 of the separator 40 is connected to the mixer 10 via a supply line 50. Thus, the oil separated from the additive via the still 46 is supplied to the mixer 10 through the feed line. The distiller (46) may be a fractionator which separates the additive using the difference in boiling point. Thus, the apparatus can finally produce the coke additive (B) through the separator (40).

In the apparatus for producing a coke additive having the above-described structure, the filter unit 44 of the separating unit is configured to filter the liquefied product while minimizing the filter clogging, thereby separating the solid product and the liquid product more effectively.

Fig. 2 illustrates the structure of the filter device according to the present embodiment. Hereinafter, the structure of the filter device of this embodiment will be described with reference to FIG.

Coal liquefied products are very slurry and very viscous and have solid residue which is an indefinite un-liquefied coal scrap, making it difficult to divide easily into liquid and solid, to block the filter, and to block piping during transport Lt; / RTI >

Thus, the filter device 44 of the present embodiment has a structure in which an additional solvent is separately added to the liquefied product having a high viscosity to lower the viscosity of the liquefied product to be subjected to solid-liquid separation and to increase the amount of the solvent, have.

To this end, the filter device 44 of the present embodiment includes a filter device 441 having a filter (not shown) therein to solid-liquid separate the liquefied product into liquid and solid materials, A mixer for mixing the liquid product with an additional solvent and supplying the mixture to the filter unit 441, and a supply unit for supplying additional solvent to the mixer.

The filter device may further include a recovery tower 447 connected to the outside of the filter unit 441 to recover additional solvent from the liquid material separated at the filter unit 441.

Thus, the liquefied product in which the gas is separated while passing through the separator 42 of the separator is mixed with the additional solvent via the mixer 443, thereby lowering the viscosity and increasing the amount of the solvent. Thereafter, It is possible to reduce the burden on the filter and separate the solid matter and the liquid matter more easily.

The filter unit 441 may have a pore size of 5 to 10 탆. The filter unit 441 passes only the liquid material and the solvent in a liquid state smaller than the hole size of the filter. The residue of coal, which is larger than the pore size, can not pass through the filter and is solid-liquid separated as it is filtered.

The mixer 443 is installed between the separator 42 of the separator and the filter unit 441. The mixer 443 may be a structure for evenly stirring the liquefaction product and the additional solvent. For example, the mixer 443 may include a stirring blade for mixing the liquefaction product and the additional solvent, and a driving motor for rotating the stirring blade. The mixer 443 is applicable to both the liquefied product and the structure that evenly stirs the additional solvent.

And a supply unit 445 for supplying additional solvent is connected to the mixer 443. The supply unit 445 puts an appropriate amount of the additional solvent into the mixer 443. In this embodiment, the supply portion 445 may be a structure for supplying a solution having a boiling point different from that of the mixed solvent to the liquefied product as an additional solvent. As mentioned above, the liquefied product is mixed with the coal and the solvent through the mixer 443 in a slurry state.

In this embodiment, the additional solvent has a boiling point different from that of the solvent mixed with the liquefied product. By using the boiling point of the solution in the later recovery tower 447, it is possible to easily recover only the additional solvent except for the solvent by mixing the liquefied product with the additional solvent having different boiling points as compared with the solvent of the liquefied product.

In this embodiment, the additional solvent may be any one selected from toluene, nucleic acids and alcohols having a relatively lower boiling point than the solvent mixed in the liquefied product.

The recovery tower 447 is a structure for separating and recovering only the additional solvent from the liquid mixture using the difference in boiling point, for example, a fractionation still can be used. The recovery tower 447 is connected between the filter unit 441 and the still unit 46 of the separation unit to recover additional solvent from the liquid material separated through the filter unit 441. The liquid material passing through the recovery tower 447 is transferred to the still.

Between the recovery tower 447 and the mixer 443, a recovery line 449 for re-supplying the additional solvent recovered from the recovery tower 447 to the mixer 443 may be installed. Thus, the additional solvent separated from the recovery tower 447 is supplied to the mixer 443 through the recovery line 449 and reused.

The additional solvent is recovered in the recovery tower 447 and supplied to the mixer 443 through the recovery line 449 so that the supply part 445 is not completely recovered in the recovery tower 447 and is passed to the post- It can be supplied to the mixer 443 only by the amount of the additional solvent.

As described above, the filter device 44 of the present embodiment lowers the viscosity of the liquefied product and increases the amount of the solvent, thereby reducing the clogging of the filter in the process of passing through the filter device 441, . ≪ / RTI >

Hereinafter, a process for producing an additive according to this embodiment will be described.

The process for preparing the additive includes a coal pretreatment process in which coal is dispersed in a solvent to form a slurry, a process of adding a dispersed iron catalyst in coal pretreatment, a coal liquefaction process in which coal slurry is reacted with cracking gas to liquefy coal slurry, A process of supplying COG and / or LNG with a cracking gas during the liquefaction process, a process of separating the additive from the liquefied product, and a recirculation process of supplying the liquid oil obtained in the separation process to the coal pretreatment process and using it as a solvent do.

The coal pretreatment process is a process of preparing coal as a raw material for the preparation of additives by pulverizing the coal and then drying the pulverized coal.

Coal as raw material is low tin (or low grade) coal with low or no cohesion and low price, and lignite, bituminous coal can be used. Low-grade coal such as lignite and bituminous coal is crushed through a crusher. The pulverization of the coal can be carried out, for example, to a size of 60 meshes or less.

The pulverized coal is subjected to a drying process to remove moisture. Moisture of coal interferes with the mixing of coal and solvent and makes reactor pressure unstable, which lowers reaction efficiency. In this embodiment, the coal is dried so as to have a water content of 10 wt% or less through the coal drying process. When the water content of the coal exceeds 10 wt%, the process efficiency is lowered and additional waste gas treatment steps are required.

The pulverized and dried coal is mixed with a solvent and slurried. In this embodiment, the coal dried for the solvent is mixed at a weight ratio of 1/1 to 1/4.

When the ratio of coal to the solvent is larger than 1/1, the amount of the solvent is small and the coal slurry is not well formed. Thus, the conversion rate of coal in the reactor is also lowered. When the ratio of coal to solvent is lower than 1/4, the viscosity of the coal slurry is lowered by adding too much solvent, and the throughput is increased in each step, thereby increasing the scale of the equipment. As a result, equipment costs and utility usage are increased, resulting in cost problems.

Here, the solvent may be an oil remaining after the additive is finally separated through an additive manufacturing process.

The dispersed iron catalyst may be added during the coal pretreatment.

In this embodiment, the dispersed iron catalyst may be Fe 2 O 3 . As described above, by adding the dispersed iron catalyst and mixing it with the coal slurry, the reactivity in the liquefaction reaction can be increased.

The dispersed iron catalyst may be added in an amount of 0.5 to 3.0 parts by weight based on 100 parts by weight of coal.

When the amount of the dispersed iron catalyst is less than the above range, the catalyst can not be used as a catalyst. If the amount exceeds the above range, it is difficult to regenerate the catalyst and the catalyst is adversely affected.

The coal slurried through the above process is transferred to the reactor and subjected to a coal liquefaction process. The coal slurry is heated to the desired temperature through the heating process during the transfer to the liquefaction process.

The coal liquefaction process is a process of liquefying the coal slurried at a sufficiently high temperature in the pretreatment process. The coal slurry and the cracking gas are introduced into the reactor and the liquefaction reaction is carried out under the set temperature and pressure.

In this embodiment, the coal liquefaction process can be carried out at a temperature of 250 to 450 DEG C and a pressure of 30 to 120 bar. The pressure inside the reactor can be controlled by adjusting the supply flow rate of the cracking gas.

As the inside of the reactor is set to the above temperature and pressure range, a liquefaction reaction proceeds in a mixture of coal and a solvent, that is, a coal slurry. At this time, the supplied cracking gas not only regulates the pressure inside the reactor, but also serves to liquefy the broken loop between the carbon atoms constituting the coal.

When the temperature is lower than 250 ° C in the coal liquefaction process, the coal is not melted and the liquefaction process does not proceed. When the temperature exceeds 450 ° C, the coal is caulked and the coal is hardened and hardened.

Also, when the reaction pressure is less than 30 bar in the liquefaction process of coal, the pressure in the reactor is low so that donation of hydrogen to coal does not occur. If the pressure exceeds 120 bar, hydrogen will be excessively supplied to the coal, resulting in a reduction in the final production of coke additive, and an increase in the production of undesirable materials such as oil.

In the coal liquefaction step, COG, LNG, or a mixed gas thereof may be supplied as the cracking gas.

Depending on the process conditions, either COG or LNG can be selectively used in the reactor, or both COG and LNG can be used to feed the reactor.

Thus, by using COG or LNG, the production amount of liquefied oil is reduced and the amount of additive produced is increased in the coal liquefaction process.

The cracking gas may be supplied by heating at 400 to 600 ° C in accordance with the internal temperature of the reactor in which the coal liquefaction reaction is performed. Therefore, when the cracking gas is introduced, the change in the temperature inside the reactor is minimized, and the degradation of reactivity can be prevented.

The product produced in the coal liquefaction process can be separated into coke additive, which is the final target through the separation process.

In this embodiment, the separation step is a step of separating the gas components sequentially from the liquefaction process product, a filtration step of separating the liquid material and the solid matter, and a step of distilling the liquid material separated in the filtration step, And a fractional distillation step of separating the mixture.

The products liquefied through the coal liquefaction process include both solid products, liquid products and gaseous products. The liquid product includes an additive for coke and an oil, and the gaseous product may include fuel gas, sulfur, ammonia, and the like.

The separation step is to separate from the rating of the light gas component (C1 to C5, H 2 S, NH 3 , H 2 , etc.) the product of the substance produced through the coal liquefaction process. In the filtration step, the product is separated into a solid product and a liquid product.

Here, the filtration step may further include a supplying step of supplying an additional solvent to the liquefied product, and a mixing step of mixing the liquefied product and the additional solvent to lower the viscosity of the liquefied product.

The filtration step may further include a recovery step of recovering only the additional solvent from the liquid material after solid-liquid separation. The filtration step may further include a reuse step of transferring the additional solvent recovered in the recovery step to the mixing step and re-supplying the additional solvent.

The liquefied product separated from the gaseous components by the separating process is mixed with the additional solvent supplied before the filtration step, so that the viscosity becomes lower and the amount of the solvent becomes larger and becomes more diluted. Thus, it is possible to more effectively perform the solid-liquid separation while reducing the burden on the filter in the subsequent filtration process.

The additional solvent added to the liquefied product in this embodiment may be a lower boiling point solution, such as toluene, nucleic acid, or alcohol, as compared to the solvent mixed with the liquefied product. The additional solvent has a boiling point lower than that of the solvent mixed in the liquefied product, so that it is possible to more easily recover additional solvent in the subsequent recovery process.

After filtration, the liquefied product is separated into solid and liquid materials.

The separated liquid material is subjected to fractional distillation and recovered before the additive is separated to recover the additional solvent. Since the boiling point of the solvent contained in the liquid material and the additional solvent differ in the recovery process, the liquid material is heated in accordance with the boiling point temperature of the additional solvent, so that only the additional solvent can be distilled and recovered. The recovered additional solvent is transferred to the mixing stage and reused as an additional solvent to be mixed with the liquefied product. The additional solvent is recovered and the remaining liquid material is finally subjected to fractional distillation to finally be made into an additive for coke.

FIG. 3 shows the contents of additives and oil remaining in the solid material separated through the separation step according to the present embodiment, in comparison with the prior art.

3, the additive and the oil content remaining in the solid material after the separation process by mixing an additional solvent with the liquefied product as mentioned above are shown, and the comparative example shows that the addition product And the remaining additives and oil content in the solid material after the separation process.

Toluene was used as an additional solvent in the examples.

As a result, as shown in FIG. 3, in the comparative example, the additive remaining in the solid material and the oil content were 33% at a temperature lower than 260 ° C., indicating that the solid-liquid separation was not effectively performed. On the other hand, in the case of Examples, the additive remaining in the solid material and the oil component were reduced to 4% at a temperature of less than 260 ° C, and it was confirmed that the solid-liquid separation was very effective.

Therefore, in the conventional structure as in the comparative example, the solid-liquid separation efficiency is as low as 67%, whereas in the structure in which the liquefied product is diluted with the additional solvent as in the embodiment, the solid-liquid separation efficiency can be increased to 96%.

In this embodiment, the filtration step may be performed at a temperature of 120 to 400 ° C.

The coke additive has a softening point of about 120 캜. Therefore, when the temperature is lower than 120 캜 in the filtration step, the additive for coke is present as a solid product, and since the solid product and the additive for coke are mixed, only the additive for coke can not be separated. The filtration step is performed at a temperature of 120 ° C or higher in consideration of the softening point of the additive for coke.

Also, as mentioned above, since the coal liquefaction process is performed at a temperature of 250 to 450 ° C., the initial product produced in the coal liquefaction process is present at a high temperature of 120 to 400 ° C., unless it is cooled. Therefore, when the filtration step is performed immediately after the coal liquefaction process without further heating the product in the filtration step, the filtration process can be performed at a temperature of 120 ° C or higher using the heat of the product. Therefore, in this embodiment, it is necessary to perform the filtration step immediately before the temperature of the product is lowered below 120 캜 immediately after the coal liquefaction process.

The fractionation step following the filtration step is to distill off the liquid product separated in the filtration step, finally obtaining the coke additive separately.

In the fractional distillation step, the liquid product separated through the filtration step is distilled using a distiller to obtain an additive for coke.

As mentioned above, the liquid product separated in the filtration step contains oil as well as additives for coke, and it may further include some fuel gas, sulfur, ammonia and the like depending on the temperature.

Fractional distillation which is usually used in the above fractionation stage can be used.

In this embodiment, the fractional distillation step may be carried out at a temperature of from 350 to 450 < 0 > C. Since the oil of the liquid product has a boiling point lower than 350 to 450 ° C, the oil is separated and removed from the liquid product by fractional distillation to obtain an additive for coke. That is, when the liquid product is heated at a temperature of 350 ° C to 450 ° C in the fractional distillation step, the oil is evaporated and only the additive for coke can be separated from the residue. The oil is then separated through a fractional distillation step to finally obtain an additive for coke.

The recycle process recycles the oil obtained in the separation process to the coal pretreatment process so that the oil is used as a solvent in the coal slurry process.

In this embodiment, the recycle process is to feed the oil obtained through the fractional distillation step directly to the mixer of the coal pretreatment process. Thus, the oil separated in the separation step can be recycled directly to the coal pretreatment process, thereby simplifying the process.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, Of course.

10: mixer 12: crusher
14: dryer 20: catalyst supplier
30: Reactor 32: Gas supply part
40: separator 42: separator
44: Filter device 46: Distiller
50: supply line 441: filter unit
443: Mixer 445:
447: Recovery tower 449: Recovery line

Claims (19)

A coal pretreatment step of dispersing coal into a slurry by dispersing it in a solvent; A step of adding a dispersed iron catalyst during the pretreatment of coal; A coal liquefaction process for liquefying coal slurry by reacting coal slurry with cracking gas; A step of supplying COG and / or LNG with a cracking gas during a coal liquefaction process; A separation step of separating the additive from the liquefied product; And a recycle process in which the liquid oil obtained in the separation process is supplied to the coal pretreatment process and used as a solvent,
The separation step includes a separating step of separating the gas component from the liquefied product, a filtration step of separating the liquid material and the solid matter, and a fractionation step of distilling the liquid material separated in the filtration step to separate the additive In addition,
Wherein the filtering step further comprises a feeding step of supplying an additional solvent to the liquefied product and a mixing step of mixing the liquefied product with an additional solvent to lower the viscosity of the liquefied product.
The method according to claim 1,
Wherein the additional solvent is a solution having a different boiling point compared to the solvent mixed in the liquefied product.
3. The method of claim 2,
Wherein the additional solvent is any one selected from toluene, nucleic acid, and alcohol.
4. The method according to any one of claims 1 to 3,
Wherein the filtration step further comprises a recovery step of recovering only the additional solvent from the liquid material after solid-liquid separation.
5. The method of claim 4,
Wherein the filtration step further comprises a reuse step of transferring and re-supplying the additional solvent recovered in the recovery step to the mixing step.
5. The method of claim 4,
Wherein the recycle step comprises feeding the oil separated from the additive in the fractional distillation step to the coal pretreatment step.
5. The method of claim 4,
Wherein the coal pretreatment step comprises mixing the dried coal to the solvent at a weight ratio of 1/1 to 1/4.
5. The method of claim 4,
Wherein the dispersed iron catalyst is Fe 2 O 3 .
8. The method of claim 7,
Wherein the dispersed iron catalyst is added in an amount of 0.5 to 3.0 parts by weight based on 100 parts by weight of coal.
5. The method of claim 4,
Wherein the filtration step is performed at a temperature of 120 to 400 ° C.
5. The method of claim 4,
Wherein the coal pretreatment step further comprises pulverizing coal and drying the pulverized coal.
12. The method of claim 11,
Wherein the step of drying the coal is performed so that the water content of the coal is 10 wt% or less.
5. The method of claim 4,
Wherein the coal liquefaction process is performed by heating the cracking gas at 400 to 600 ° C.
A mixer for mixing the pretreated coal and the solvent to form a slurry, a catalyst supply unit for supplying the dispersed iron catalyst to the mixer, a reactor for liquefying the coal slurry through the mixer, and a COG and / or LNG A separator for separating the additive from the liquefied product generated from the reactor, and a supply line connected between the separator and the mixer for supplying the oil separated from the separator to the mixer as a solvent,
The separator includes a separator for separating the gas component from the liquefaction process product, a filter device connected to the separator for separating the liquid material and the solid material, and a separator for separating the additive from the liquid material, And a distiller connected to the mixer through an inlet and an outlet to supply the additive and the separated oil to the mixer,
The filter device includes a filter unit for solid-liquid separating a liquefied product into a liquid material and a solid material, a mixer connected to the inlet of the filter unit for mixing an additional solvent into a liquefied product and supplying the mixture to a filter unit, and a supply unit for supplying an additional solvent to the mixer Containing additive.
15. The method of claim 14,
Wherein the filter device further comprises a recovery tower connected to the filter outlet to recover additional solvent from the liquid material separated in the filter unit.
16. The method of claim 15,
Further comprising a recovery line connected between the recovery tower and the mixer for re-supplying the recovered additional solvent to the mixer.
17. The method according to any one of claims 14 to 16,
Wherein the additional solvent is any one selected from toluene, nucleic acid, and alcohol.
18. The method of claim 17,
A pulverizer for pulverizing coal for pretreatment of coal, and a dryer for drying the pulverized coal.
18. The method of claim 17,
Wherein the catalyst supply unit supplies Fe 2 O 3 as a dispersed iron catalyst.
KR1020150186331A 2015-12-21 2015-12-24 Method and apparatus for producing binder for coke KR101764712B1 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
KR1020150186331A KR101764712B1 (en) 2015-12-24 2015-12-24 Method and apparatus for producing binder for coke
CN201680071502.0A CN108368430A (en) 2015-12-21 2016-11-09 The manufacturing method and manufacturing device of coking additire
AU2016376254A AU2016376254A1 (en) 2015-12-21 2016-11-09 Method and apparatus for preparing additive for coke
PCT/KR2016/012865 WO2017111301A1 (en) 2015-12-21 2016-11-09 Method and apparatus for preparing additive for coke
BR112018012474-5A BR112018012474A2 (en) 2015-12-21 2016-11-09 method and apparatus for preparing coke additive
AU2020202042A AU2020202042A1 (en) 2015-12-21 2020-03-20 Method and apparatus for preparing additive for coke

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KR101764712B1 true KR101764712B1 (en) 2017-08-03

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