CN212152198U - Coal tar segmentation preprocessing device - Google Patents
Coal tar segmentation preprocessing device Download PDFInfo
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- CN212152198U CN212152198U CN202020713139.1U CN202020713139U CN212152198U CN 212152198 U CN212152198 U CN 212152198U CN 202020713139 U CN202020713139 U CN 202020713139U CN 212152198 U CN212152198 U CN 212152198U
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Abstract
The utility model provides a coal tar segmentation preprocessing device, the device is including the one-level solid-liquid separation unit, second grade solid-liquid separation unit that connect gradually and add the hydrogenation reaction unit in advance, the second grade solid-liquid separation unit is including the mixing arrangement and the separator that connect gradually, it includes the ebullated bed hydrogenation ware to add the hydrogenation reaction unit in advance. The device is at first with heterogeneous impurity segmentation desorption in the coal tar, desorption quinoline insoluble, metallic impurity in proper order, can reduce the use amount of hydrogenation pretreatment catalyst by a wide margin, adopts fluidized bed hydrogenation ware to carry out the desorption of easy coking unsaturated hydrocarbons such as alkadiene afterwards, and device operation cycle is long, and the catalyst need not online loading and unloading.
Description
Technical Field
The utility model belongs to the technical field of the coal industry, a coal tar segmentation preprocessing device is related to.
Background
Coal is used as an important fossil fuel, the components are complex, the varieties of coal chemical products are various, coal tar byproducts are generated in the processes of coal coking, dry distillation, gasification and the like, for example, bituminous coal and lignite are used as raw materials, one of the byproducts generated in the process of producing semicoke is coal tar, and the yield of the coal tar is about 10% of the yield of the semicoke.
The coal tar has complex composition, high content of polycyclic aromatic hydrocarbon, colloid and asphaltene, and simultaneously contains a large amount of oxygen-containing polar substances, a certain amount of unsaturated hydrocarbon, sulfur, nitrogen, metal and other impurities.
The quinoline insoluble substances are components insoluble in quinoline in coal tar or coal tar pitch, wherein the content of the quinoline insoluble substances is one of main indexes for representing the properties of the coal tar, the quinoline insoluble substances generally mainly comprise inorganic impurity particles such as ash in the coal tar and organic substances formed by condensed ring aromatic hydrocarbon condensates, part of the quinoline insoluble substances have small granularity and are uniformly dispersed in the coal tar under the action of polar substances, and the quinoline insoluble substances are difficult to remove by a conventional separation means; and due to the existence of solid-phase impurities and metals in the coal tar, the solid-phase impurities and the metals are easy to deposit on the outer surface and in pore channels of the catalyst in the hydrogenation production process, and cover the active center, so that the catalyst is poisoned and inactivated, and bed pressure drop is generated at the same time, so that the operation period of the device is influenced.
CN 105505453A discloses a coal tar anhydrous desalting and demetallizing method, which sequentially comprises heating treatment, first additive mixing, first-stage solid-liquid separation, second additive mixing and second-stage solid-liquid separation, wherein impurities such as metals and quinoline insoluble substances are removed by stirring and mixing through adding an auxiliary agent, but the impurities such as unsaturated hydrocarbons and other substances which are easy to generate coke in the coal tar are not effectively removed, and when subsequent hydrogenation operation is carried out, the pressure drop of a bed layer rises too fast, the utilization rate of a catalyst is low, and the long-period continuous operation of the device cannot be ensured.
CN 101240193A discloses a coal tar multistage hydrogenation treatment process, which comprises the steps of feeding coal tar distillate oil or whole fraction with high contents of impurities, colloid, asphaltene, oxygen elements and the like into a pre-hydrogenation reactor, carrying out reactions such as olefin hydrogenation, raw material descaling, partial metal removal and the like, and then carrying out steps such as solid particle separation, hydrodemetallization, deep hydrogenation refining and the like, but the coal tar has high contents of metal and carbon residue, the consumption of a catalyst required by pre-hydrogenation treatment is high, the cost is high, and the catalyst is easily deactivated by metal.
CN 103695036A discloses a full-range processing technique of medium-low temperature coal tar, the pretreatment of the technique is through electric desalting and fractionation dehydration, insoluble substances of metal and quinoline in the coal tar are removed through a fluidized bed hydrogenation reactor, and the catalyst is loaded and unloaded on line, although the problems that the catalyst in the traditional fixed bed hydrogenation reactor is quickly deactivated, the pressure drop of the bed layer is quickly increased, and the catalyst needs to be shut down and replaced can be solved, the problems that the deactivation of the fluidized bed hydrogenation catalyst is quick and the cost for processing the coal tar is high are not fundamentally solved.
In summary, for the pretreatment of coal tar, especially full-range coal tar, it is necessary to first remove different types of impurities such as quinoline insoluble substances and metal impurities, respectively, to reduce the consumption of the subsequent hydrogenation catalyst, and then remove unsaturated hydrocarbons by using a suitable hydrogenation pretreatment reactor, so as to prolong the continuous operation period of the device.
SUMMERY OF THE UTILITY MODEL
Problem to prior art existence, the utility model aims to provide a coal tar segmentation preprocessing device, the device is through the impurity segmentation desorption with different kinds in the coal tar, desorption quinoline insoluble and metallic impurity in proper order earlier, carries out the desorption of unsaturated hydrocarbon again to avoid impurity such as metal, quinoline insoluble to the influence of hydrogenation pretreatment catalyst, reduce the quantity of catalyst, prolong the life cycle of catalyst.
To achieve the purpose, the utility model adopts the following technical proposal:
the utility model provides a coal tar segmentation preprocessing device, the device is including the one-level solid-liquid separation unit, second grade solid-liquid separation unit that connect gradually and add the hydrogenation reaction unit in advance, the second grade solid-liquid separation unit is including the mixing arrangement and the separator that connect gradually, it includes the ebullated bed hydrogenation ware to add the hydrogenation reaction unit in advance.
In the utility model, because the coal tar is complex in composition and more in impurity type, impurities need to be removed before refining treatment, and through the arrangement of the pretreatment device, impurities such as quinoline insoluble substances, metals and unsaturated hydrocarbons in the coal tar are removed in sequence, so that when the catalyst is removed in common use, the impurities such as metals influence the activity of the catalyst, the catalyst is easy to be inactivated, and the bed pressure drop is easy to increase due to the quinoline insoluble substances and the metal impurities, so that the operation period of the device is influenced; therefore, most of quinoline insoluble substances and metals are removed in advance by a simple method, the using amount of the catalyst can be effectively reduced, and the difficulty of coal tar purification treatment is reduced.
Following conduct the utility model discloses preferred technical scheme, nevertheless do not conduct the utility model provides a technical scheme's restriction, through following technical scheme, can reach and realize better the utility model discloses a technical purpose and beneficial effect.
As the preferred technical scheme of the utility model, one-level solid-liquid separation unit includes centrifuge.
The utility model discloses in, because the particle diameter of quinoline insoluble substance granule is often less, it is great to adopt static solid-liquid separation operation separation degree of difficulty, consequently adopts centrifugal separation's mode, most quinoline insoluble substance in the desorption coal tar.
As the utility model discloses preferred technical scheme, the device still includes chemical auxiliary agent and adds the device, chemical auxiliary agent adds the entry that the device and mixing arrangement link to each other.
As the preferable technical proposal of the utility model, the mixing device is a stirring reaction device with a jacket.
The utility model discloses in, to metallic impurity's desorption, generally adopt to add chemical auxiliary agent and the mode that the metal carries out the chemical complexation, at least one of quaternary ammonium salt, phosphate or polyphosphate is generally selected to the chemical auxiliary agent, and the coal tar mixes the stirring with the chemical auxiliary agent, reacts under the certain temperature condition, consequently can heat mixed liquid, if adopt the device to press from both sides the mode of cover or heat and get into the device again after rising temperature, the temperature generally selects 100 ~ 200 ℃, for example 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃ or 200 ℃ etc. but not only limited to the numerical value enumerated, other numerical values not enumerated in this numerical value range are equally suitable for.
As the preferred technical scheme of the utility model, separator includes filter equipment.
The utility model discloses in, after metallic impurity and chemical auxiliary complex reacted, formed solid particle thing, the filterable mode separation of accessible, metallic impurity's desorption rate can reach more than 90%.
As the preferred technical scheme of the utility model, the device still includes the hydrogen supply device, the hydrogen supply device is connected to the connecting pipeline of separator and ebullated bed hydrogenation ware.
As the utility model discloses preferred technical scheme, ebullated bed hydrogenation reactor is equipped with two exports, and an export is connected to ebullated bed hydrogenation reactor's entry through return line, and another export links to each other with subsequent hydrofining reactor.
As the utility model discloses preferred technical scheme, the device still includes the circulating pump, the circulating pump sets up on the return line of ebullated bed hydrogenation ware.
The utility model discloses in, hydrogenation pretreatment reactor adopts ebullated bed reactor, is mainly based on the coal tar is adopting fixed bed reactor to carry out hydrogenation pretreatment in-process, and the raw materials entry is the easy section that blocks up to the reaction section apart from the about 1/3 of entry, and the catalyst just has to park the catalyst of changing the top in the pre-hydrogenation reactor completely not inactivation this moment, influences the operation cycle of reactor, consequently adopts ebullated bed, and the catalyst is in the fluidization state, need not to change on line, carries out disposable loading before the start-up and can carry out the complete consumption till.
The solid catalyst mainly comprising transition metal compound as active component, such as Mo-Ni composite catalyst and W-Mo-Ni-Co composite catalyst, is loaded on a carrier, and the carrier is usually Al2O3、SiO2Etc.; the catalyst has a diameter of 0.6 to 2mm, for example 0.6mm, 0.8mm, 1mm, 1.2mm, 1.4mm, 1.6mm, 1.8mm or2mm, etc., but are not limited to the recited values, and other values not recited within the numerical range are also applicable.
According to the ebullated bed hydrogenation process, unsaturated hydrocarbons which are easy to coke in coal tar are subjected to high-pressure hydrogenation saturation, and meanwhile, a small amount of residual metal and quinoline insoluble substances in the coal tar are further removed, so that purified coal tar is obtained, and a high-quality raw material is provided for subsequent hydrorefining.
The reaction pressure of the fluidized bed hydrogenation reactor is 10-18 MPaG, such as 10MPaG, 11MPaG, 12MPaG, 13MPaG, 14MPaG, 15MPaG, 16MPaG, 17MPaG or 18 MPaG; the reaction temperature is 160-230 ℃, such as 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃ or 230 ℃ and the like; the hydrogen-oil ratio is 300-800, such as 300, 400, 500, 600, 700 or 800; the volume airspeed is 1-10 h-1E.g. 1h-1、2h-1、3h-1、4h-1、5h-1、6h-1、8h-1Or 10h-1Etc.; a recycle ratio of 0.5 to 5, for example 0.5, 1, 1.5, 2, 2.5, 3, 4 or 5; the above-mentioned numerical values are not limited to the enumerated numerical values, and other numerical values not enumerated within the respective numerical ranges are also applicable.
Wherein, most of the metal and quinoline insoluble substances are removed, and the reaction of unsaturated hydrocarbon is mainly carried out during hydrogenation, so that a larger space velocity can be achieved; the circulation ratio is a volume ratio of a circulation amount of the circulation pump to a fresh feed amount, and the circulation operation can effectively maintain a fluidized state of the catalyst and also contribute to sufficient reaction of a coke-prone substance such as unsaturated hydrocarbon.
The utility model discloses in, through adopting physical filtration, chemical reaction + filterable operation method, most quinoline insoluble and metallic impurity of desorption reduce follow-up hydrogenation catalyst's consumption, adopt suitable hydrogenation pretreatment reactor pattern to carry out the desorption of unsaturated hydrocarbon simultaneously, extension fixture's continuous operation cycle.
Compared with the prior art, the utility model discloses following beneficial effect has:
(1) the device of the utility model removes the impurities of different types in the coal tar in sections, and removes the quinoline insoluble substances, the metal impurities and the unsaturated hydrocarbons in sequence, so as to avoid the influence of the impurities such as the metal, the quinoline insoluble substances and the like on the hydrogenation pretreatment catalyst, and reduce the dosage of the hydrogenation pretreatment catalyst;
(2) the device adopts the fluidized bed hydrogenation reactor to remove easily coked unsaturated hydrocarbons such as alkadiene and the like, and prolongs the operation period of the device;
(3) the fluidized bed hydrogenation reactor catalyst does not need to be loaded and unloaded on line.
Drawings
FIG. 1 is a schematic structural diagram of a coal tar segment pretreatment device provided in embodiment 1 of the present invention;
wherein, the method comprises the steps of 1-a centrifugal machine, 2-a mixing device, 3-a separating device, 4-a fluidized bed hydrogenation reactor and 5-a circulating pump.
Detailed Description
To better explain the technical solution of the present invention, it is convenient to understand the technical solution of the present invention, and the following is further detailed description of the present invention, but the following embodiments are only simple examples of the present invention, and do not represent or limit the protection scope of the present invention, and the protection scope of the present invention is subject to the claims.
The utility model discloses embodiment mode part provides a coal tar segmentation preprocessing device, the device is including the one-level solid-liquid separation unit, second grade solid-liquid separation unit that connect gradually and add the hydrogenation reaction unit in advance, second grade solid-liquid separation unit is including the mixing arrangement 2 and the separator 3 that connect gradually, it includes boiling bed hydrogenation ware 4 to add the hydrogenation reaction unit in advance.
The following are typical but non-limiting examples of the present invention:
example 1:
the embodiment provides a coal tar segmentation pretreatment device, the structural schematic diagram of the device is shown in fig. 1, and the device comprises a first-stage solid-liquid separation unit, a second-stage solid-liquid separation unit and a pre-hydrogenation reaction unit which are sequentially connected, wherein the second-stage solid-liquid separation unit comprises a mixing device 2 and a separation device 3 which are sequentially connected, and the pre-hydrogenation reaction unit comprises a fluidized bed hydrogenation reactor 4.
The primary solid-liquid separation unit comprises a centrifuge 1.
The device also comprises a chemical additive adding device, and the chemical additive adding device is connected with the inlet of the mixing device 2; the chemical auxiliary agent selects quaternary ammonium salt and phosphate with the mass ratio of 1: 1.
The mixing device 2 is a stirring reaction device with a jacket.
The separation device 3 comprises a filter device.
The device also comprises a hydrogen supply device which is connected to a connecting pipeline of the separation device 3 and the fluidized bed hydrogenation reactor 4.
The boiling bed hydrogenation reactor 4 is provided with two outlets, one outlet is connected to the inlet of the boiling bed hydrogenation reactor 4 through a return pipeline, and the other outlet is connected with a subsequent hydrofining reactor.
The device also comprises a circulating pump 5, wherein the circulating pump 5 is arranged on a return pipeline of the fluidized bed hydrogenation reactor 4.
Wherein, the reaction conditions of the ebullated-bed hydrogenation reactor 4 are as follows: the reaction pressure is 15MPaG, the reaction temperature is 200 ℃, the hydrogen-oil ratio is 500, and the volume space velocity is 1.5h-1The recycle ratio was 2.
Example 2:
the embodiment provides a coal tar segmentation preprocessing device, the device is including the one-level solid-liquid separation unit, second grade solid-liquid separation unit and the pre-hydrogenation reaction unit that connect gradually, second grade solid-liquid separation unit is including the mixing arrangement 2 and the separator 3 that connect gradually, the pre-hydrogenation reaction unit includes ebullated bed hydrogenation ware 4.
The primary solid-liquid separation unit comprises a centrifuge 1.
The device also comprises a chemical additive adding device, and the chemical additive adding device is connected with the inlet of the mixing device 2; the chemical auxiliary agent is selected from quaternary ammonium salt and polyphosphate with the mass ratio of 1: 1.
The mixing device 2 is a stirring reaction device with a jacket.
The separation device 3 comprises a filter device.
The device also comprises a hydrogen supply device which is connected to a connecting pipeline of the separation device 3 and the fluidized bed hydrogenation reactor 4.
The boiling bed hydrogenation reactor 4 is provided with two outlets, one outlet is connected to the inlet of the boiling bed hydrogenation reactor 4 through a return pipeline, and the other outlet is connected with a subsequent hydrofining reactor.
The device also comprises a circulating pump 5, wherein the circulating pump 5 is arranged on a return pipeline of the fluidized bed hydrogenation reactor 4.
Wherein, the reaction conditions of the ebullated-bed hydrogenation reactor 4 are as follows: the reaction pressure is 18MPaG, the reaction temperature is 230 ℃, the hydrogen-oil ratio is 800, and the volume space velocity is 5h-1The recycle ratio was 0.5.
Example 3:
the embodiment provides a coal tar segmentation preprocessing device, the device is including the one-level solid-liquid separation unit, second grade solid-liquid separation unit and the pre-hydrogenation reaction unit that connect gradually, second grade solid-liquid separation unit is including the mixing arrangement 2 and the separator 3 that connect gradually, the pre-hydrogenation reaction unit includes ebullated bed hydrogenation ware 4.
The primary solid-liquid separation unit comprises a centrifuge 1.
The device also comprises a chemical additive adding device, and the chemical additive adding device is connected with the inlet of the mixing device 2; the chemical auxiliary agent is selected from quaternary ammonium salt, phosphate and polyphosphate with the mass ratio of 4:3: 3.
A heat exchanger is arranged between the centrifuge 1 and the mixing device 2, and the mixing device 2 is a stirring reaction device.
The separation device 3 comprises a filter device.
The device also comprises a hydrogen supply device which is connected to a connecting pipeline of the separation device 3 and the fluidized bed hydrogenation reactor 4.
The boiling bed hydrogenation reactor 4 is provided with two outlets, one outlet is connected to the inlet of the boiling bed hydrogenation reactor 4 through a return pipeline, and the other outlet is connected with a subsequent hydrofining reactor.
The device also comprises a circulating pump 5, wherein the circulating pump 5 is arranged on a return pipeline of the fluidized bed hydrogenation reactor 4.
Wherein, the reaction conditions of the ebullated-bed hydrogenation reactor 4 are as follows: the reaction pressure is 10MPaG, the reaction temperature is 160 ℃, the hydrogen-oil ratio is 300, and the volume space velocity is 8h-1The recycle ratio was 1.
In the embodiment, the device is used for pretreating the coal tar, and the pretreatment is mainly divided into three steps, wherein firstly, the coal tar is subjected to solid-liquid separation by a centrifugal machine, and most of quinoline insoluble substances in the coal tar are removed; then the separated liquid phase is heated and stirred and mixed with a chemical auxiliary agent to generate chemical complex reaction, metal impurities are converted into solid particles, coal tar with low metal content is obtained through solid-liquid separation, and the removal rate of the metal reaches more than 90%; the treated coal tar is mixed with hydrogen and then enters a fluidized bed hydrogenation reactor to carry out hydrogenation reaction of unsaturated hydrocarbon, the removal rate of unsaturated diene can reach more than 99 percent, simultaneously, the remaining metal and quinoline insoluble substances are further removed, and the reaction effluent is subjected to deep hydrogenation refining reaction.
Comparative example 1:
this comparative example provides a coal tar pretreatment apparatus, which is comparable to the apparatus of example 1, except that: the device does not comprise a primary solid-liquid separation unit and a secondary solid-liquid separation unit, namely the device is directly introduced into the fluidized bed hydrogenation reactor 4, and the volume space velocity of the fluidized bed hydrogenation reactor 4 is 0.5h-1。
In the comparative example, the coal tar is not subjected to quinoline insoluble substances and metal impurities in advance, but is subjected to combined removal during hydrogenation pretreatment, and the content of impurities such as metal, quinoline insoluble substances and the like is high, so that the catalyst is low in airspeed and large in initial loading amount; quinoline insoluble substances are easy to adsorb in a hydrogenation catalyst pore passage to reduce the activity of the catalyst, metal components are easy to cause catalyst poisoning and inactivation to influence the service life of the catalyst, 1% of the catalyst in a reactor needs to be replaced on line every day of operation on average, the consumption of each ton of coal tar catalyst is about 8-10 times of that in the embodiment, and the pretreatment cost of the coal tar is greatly improved.
It can be seen from the above examples and comparative examples that the device of the utility model removes quinoline insoluble substances, metal impurities and unsaturated hydrocarbons in sequence by removing different impurities in the coal tar in sections so as to avoid the influence of the impurities such as metal and quinoline insoluble substances on the hydrogenation pretreatment catalyst and reduce the dosage of the hydrogenation pretreatment catalyst; the device adopts a fluidized bed hydrogenation reactor to remove diolefins and other easily-coked unsaturated hydrocarbons, and the operation period of the device is prolonged; the ebullated bed hydrogenation reactor catalyst does not need to be loaded and unloaded online.
The applicant states that the present invention is described in the above embodiments, but the present invention is not limited to the above detailed device, i.e. the present invention must not be implemented by relying on the above detailed device. It should be clear to those skilled in the art that any improvement of the present invention, to the addition of the equivalent replacement and auxiliary devices of the present invention, the selection of the specific mode, etc., all fall within the scope of protection and disclosure of the present invention.
Claims (8)
1. The coal tar segmentation pretreatment device is characterized by comprising a first-stage solid-liquid separation unit, a second-stage solid-liquid separation unit and a pre-hydrogenation reaction unit which are sequentially connected, wherein the second-stage solid-liquid separation unit comprises a mixing device and a separation device which are sequentially connected, and the pre-hydrogenation reaction unit comprises a fluidized bed hydrogenation reactor.
2. The coal tar staged pretreatment device according to claim 1, wherein the ebullated bed hydrogenation reactor is provided with two outlets, one outlet is connected to the inlet of the ebullated bed hydrogenation reactor through a return line, and the other outlet is connected to a subsequent hydrofining reactor.
3. The coal tar staged pretreatment device of claim 2, further comprising a circulation pump disposed on a return line of the ebullated bed hydrogenation reactor.
4. The coal tar staged pretreatment device of claim 1, wherein the primary solid-liquid separation unit comprises a centrifuge.
5. The coal tar staged pretreatment device of claim 1, further comprising a chemical additive addition device, wherein the chemical additive addition device is connected to an inlet of the mixing device.
6. The coal tar staged pretreatment device of claim 1, wherein the mixing device is a jacketed stirred tank reactor.
7. The coal tar staged pretreatment device of claim 1, wherein the separation device comprises a filtration device.
8. The coal tar staged pretreatment device of claim 1, further comprising a hydrogen supply device connected to the connection line between the separation device and the ebullated bed hydrogenation reactor.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020713139.1U CN212152198U (en) | 2020-04-30 | 2020-04-30 | Coal tar segmentation preprocessing device |
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| CN202020713139.1U CN212152198U (en) | 2020-04-30 | 2020-04-30 | Coal tar segmentation preprocessing device |
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| CN212152198U true CN212152198U (en) | 2020-12-15 |
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