CN210915939U - Air oxidation device for preparing coal tar pitch with high softening point - Google Patents
Air oxidation device for preparing coal tar pitch with high softening point Download PDFInfo
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- CN210915939U CN210915939U CN201921805602.9U CN201921805602U CN210915939U CN 210915939 U CN210915939 U CN 210915939U CN 201921805602 U CN201921805602 U CN 201921805602U CN 210915939 U CN210915939 U CN 210915939U
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Abstract
The utility model discloses an air oxidation device for preparing coal tar pitch with high softening point. The device comprises: the horizontal multi-shaft oxidation reactor with the jacket is filled with heat conducting oil, two ends of the side wall of the reactor are provided with a heat conducting oil inlet and a heat conducting oil outlet, the bottom of the reactor is provided with a discharge hole, at least 3 sets of stirrers are arranged in a direction which is vertical to the radial direction of the reactor, the stirrers are arranged in parallel and uniformly, and the top of the reactor is provided with at least 3 sets of air inlets, a tail gas vacuumizing outlet and a medium-temperature coal tar feeding hole; each air inlet is connected with an air inlet pipe and a distributor, the air inlet pipes are communicated with each other, and the bottom of the air distributor is connected with the reactor through a support piece; and a liquid level sensor is arranged on each medium-temperature coal pitch feeding hole. The utility model discloses, simple structure, easy operation, the quinoline insoluble and the toluene soluble content of the high softening point pitch of making moreover are low and have fine rheology under the liquefaction state.
Description
Technical Field
The utility model relates to an air oxidation device for preparing coal tar pitch with high softening point.
Background
China is a country rich in coal and poor in oil, and the coal coking industry generates at least 2000 million tons of coal tar every year. In recent decades, the coal tar is used as a raw material to be deeply processed to prepare anthracene oil, wash oil, refined naphthalene, medium-temperature coal pitch and other industrial products, but the productivity of the domestic products is far higher than the current market capacity, so that the domestic products have unreasonable structures and harsh market competition, particularly medium-temperature coal pitch products. Meanwhile, the industries of pitch-based carbon fiber, pitch-based spherical active carbon, coating materials of graphite cathode materials of lithium ion batteries, electrolytic aluminum anodes, magnesia carbon bricks and the like also put urgent demands on high-softening-point coal pitch with high softening point (180-290 ℃), high residual carbon rate (63-78%) and good rheological property, and the high-softening-point coal pitch prepared by the domestic problem of the oxidation device of medium-temperature coal pitch is difficult to meet the performance requirements of the fields. Therefore, the preparation of high-softening-point coal pitch from medium-temperature coal pitch has been a research focus in recent years.
The air oxidation method is a conventional method for preparing high-softening-point coal pitch by using medium-temperature coal pitch as a raw material. Namely, a tank reactor shown in figure 1 is adopted, medium-temperature coal pitch is used as a raw material, air is used as an oxidant, and oxidation is carried out for 2-12 hours at the temperature of 280-350 ℃. By using the oxidation apparatus shown in FIG. 1, it is possible to obtain a high softening point coal tar pitch having a softening point of 180 to 290 ℃. The oxidation device has the advantages that: 1) the influence of the uneven distribution of the thermal field on the reaction temperature of the reactants is reduced by improving the length/diameter ratio of the reaction kettle; 2) the dispersion of air in reactants is improved and the contact area between the air and asphalt is improved by adopting a stirring mode; 3) air is introduced from the upper end of the reaction kettle and flows out from the bottom, so that the problem of blockage of an air inlet pipe is avoided, and the reaction time between the air and the asphalt can be prolonged; 4) the medium temperature coal pitch is fed from the top and discharged from the bottom of the reaction kettle, and the operation is easy. However, the high-softening-point coal pitch prepared by the oxidation device has high quinoline insoluble content and toluene soluble content, so that the rheological property of the high-softening-point coal pitch in a liquefied state is poor, the carbon residue rate is low due to wide molecular weight distribution, and the practical application and popularization of the high-softening-point coal pitch in downstream products such as pitch-based carbon fibers are limited. The fundamental reason for the poor quality of high softening point coal tar pitch is that such tank reactors suffer from the following serious disadvantages. 1) The oxidation reaction between the medium-temperature coal pitch and the air is an exothermic reaction, which causes a large temperature difference along the radial direction of the reaction kettle, and the temperature difference affects the uniformity and stability of the quality of the high-softening-point coal pitch; 2) the medium-temperature coal pitch has low heat conductivity coefficient, and the pitch matrix has large temperature difference along the axial direction in the heating or reaction process, and the temperature difference can also influence the uniformity and stability of the quality of the high-softening-point coal pitch; 3) at the temperature of 280-350 ℃, partial aliphatic hydrocarbon with low aromaticity is subjected to thermal cracking reaction and forms free radicals while the medium-temperature coal pitch is subjected to oxidation reaction with oxygen, and further the free radical thermal polymerization reaction is performed, so that the quinoline insoluble substance content of the prepared high-softening-point coal pitch is up to 30-54%; 4) when the oxidation reaction reaches a certain degree, the softening point of the asphalt rises, the viscosity increases, and the oxidation reaction can only be continued under the condition of a lower stirring speed, which directly influences the uniformity of the quality of the coal asphalt with a high softening point, so that the content of the toluene soluble substances is increased, the molecular weight distribution is wider, and the carbon residue rate is reduced. In view of the above situation, researchers have proposed that oxidation is performed by a three-stage heating method, i.e., heating with heat transfer oil, and three independent heat transfer oil heating and circulating systems are designed in the jackets of the upper, middle and lower parts of the reaction kettle. The method can properly reduce the adverse effect caused by reaction heat by controlling the temperature of different parts, but the increase of the heating system and the heat-conducting oil auxiliary circulating system can undoubtedly greatly improve the power consumption in the production process.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model designs an I-shaped horizontal multi-axial oxidation reactor which is used for improving the defects of high softening point coal tar pitch in the oxidation process. The oxidation device not only can effectively reduce the content of quinoline insoluble substances and toluene soluble substances of the high-softening-point coal pitch, but also fully avoids the influence of factors such as reaction heat, a temperature field, gas distribution and the like on the uniformity and stability of the product quality.
The utility model discloses to improving the quality of high softening point coal tar pitch, promote the development of high softening point coal tar pitch and low reaches industrial chain to have very important effect, also have the significance to the development that promotes china's pitch-based carbon trade and relevant trade.
The utility model aims at providing an air oxidation device of preparation high softening point coal pitch.
The purpose of the utility model can be implemented by the following technical scheme:
an air oxidation unit for producing high softening point coal tar pitch, the unit comprising: the horizontal multi-shaft oxidation reactor is provided with a jacket, heat conducting oil is filled in the jacket, a heat conducting oil inlet is formed in the front end of the side wall of the reactor, a heat conducting oil outlet is formed in the rear end of the side wall of the reactor, 1 discharge hole is formed in the bottom of the reactor, at least 3 sets of stirrers are arranged in the reactor in a direction perpendicular to the radial direction of the reactor, the stirrers are arranged in parallel and uniformly, and at least 3 sets of air inlets, a tail gas vacuumizing outlet and a medium-temperature coal pitch feed hole are formed in the top of the reactor; each air inlet is connected in parallel through a pipeline and is connected with an air inlet pipe and an air distributor below the air inlet pipe, the air inlet pipes are communicated with each other, and the bottom of the air distributor is connected with the reactor through a support piece; each vacuumizing outlet is connected in parallel through a pipeline; all the medium temperature coal tar pitch feed inlets are connected in parallel through pipelines, and a liquid level sensor is arranged on each medium temperature coal tar pitch feed inlet.
The number of the air inlets, the middle-temperature coal pitch feed inlets and the tail gas vacuumizing outlets is the same as that of the stirrers.
And a baffle is arranged between the stirrers and is a porous plate.
The lower part of the air inlet pipe is provided with air distribution holes.
The utility model has the advantages as follows: 1) by adopting the air oxidation device, the high-softening-point coal pitch with the softening point of 180-290 ℃ and the carbon residue rate of 63-78% can be prepared, and the content of quinoline insoluble substances in the prepared high-softening-point coal pitch can be reduced to be within 10%; 2) by adopting the air oxidation device, the molecular weight distribution of the prepared high-softening-point coal pitch is narrow, and the content of toluene soluble substances can be reduced to be within 5 percent; 3) by adopting the air oxidation device, the coal pitch with high softening point and good rheological property in a liquefied state can be prepared; 4) by adopting the air oxidation device, the properties of the prepared high-softening-point coal pitch have good uniformity and stability.
Drawings
FIG. 1 shows a conventional oxidation apparatus for domestic production of high softening point coal tar pitch.
FIG. 2 is a schematic diagram of an oxidation apparatus for high-softening-point coal pitch. Wherein: a, a reactor inner layer; b, a jacket layer of the reactor; c1-3, a stirrer; d1-3, an air inlet pipe; e1-2, baffles; f, an inner cavity of the reactor; g, a gas distributor; a1-3, air interface; b1-3, a vacuum-pumping outlet; c1-3, a feed inlet of medium-temperature coal tar pitch; d1, an inlet for conduction oil; d2, an outlet for conduction oil; e, discharging a material outlet; f1-3, support of gas distributor; g1-3, a liquid level sensor.
FIG. 3 is a structural diagram of a horizontal multi-axial oxidation reactor. Wherein: a, a reactor inner layer; b, a jacket layer of the reactor; c1-3, a stirrer; e1-2, baffles; a1-3, air interface; b1-3, a vacuum-pumping outlet; c1-3, a feed inlet of medium-temperature coal tar pitch; d1, an inlet for conduction oil; d2, an outlet for conduction oil; and e, discharging the materials.
Fig. 4 is a structural view of an air intake system of the air oxidizing device. Wherein: a, a reactor inner layer; b, a jacket layer of the reactor; d1-3, an air inlet pipe; f, an inner cavity of the reactor; g, a gas distributor; a1-3, air interface; f1-3, support of gas distributor.
FIG. 5 is a block diagram of a medium temperature coal tar pitch feed system of an air oxidation unit. Wherein, A, the inner layer of the reactor; b, a jacket layer of the reactor; c1-3, feed inlet of medium temperature coal tar pitch.
FIG. 6 is a schematic view of a vacuum system of the air oxidation apparatus. Wherein, A, the inner layer of the reactor; b, a jacket layer of the reactor; b1-3, and a vacuum outlet is pumped.
FIG. 7 is a block diagram of a liquid level control system of the oxygen air oxidation apparatus. Wherein, A, the inner layer of the reactor; b, a jacket layer of the reactor; c1-3, a feed inlet of medium-temperature coal tar pitch; g1-3, a liquid level sensor.
Detailed Description
The invention will now be further illustrated by the following figures and examples.
The air oxidation device of the coal tar pitch with high softening point of the utility model is shown as the attached figure 2. The horizontal multi-shaft oxidation reactor (see figure 3) is a horizontal multi-shaft reaction kettle. A baffle is arranged between the stirrers and is a porous plate, so that liquid or quasi-liquid can pass through the baffle; the air inlet pipes are arranged in the reactor according to the structure shown in figure 4, are communicated with each other and can regulate and control the distribution state of air in the reactor by controlling the flow; a plurality of feed inlets are arranged, and the number of the feed inlets is the same as that of the stirrers; the stability of the liquid level of the reactant is ensured by adjusting the flow of each feed inlet, and the stability of the product quality is finally ensured. In order to improve the distribution and mass transfer of air in the liquefied asphalt, the whole reaction process is negative pressure operation; regulating the content of toluene soluble substances of the coal pitch with high softening point by controlling the vacuum degree in the reaction kettle; the tail gas is discharged in time through negative pressure operation and then treated. Timely detecting the liquid level of the liquefied asphalt in the reactor through a liquid level sensor; the feedback signal is transmitted to the automatic regulating valve through the sensor, the medium temperature coal pitch is supplemented properly to keep the stability of the liquid level in the kettle, and the stability of the quality of the high softening point coal pitch can be ensured to a certain extent.
Examples
The implementation process comprises the following steps: 1) heating the medium-temperature coal pitch to about 150 ℃ for liquefaction treatment; 2) closing an outlet d2 of the heat transfer oil, and injecting the heat transfer oil into a jacket B of the reactor from d 1; 3) closing the discharge hole e, and heating the heat conduction oil to 280-350 ℃; 4) starting a liquid delivery pump, and injecting the liquefied medium-temperature coal pitch into the reactor from c1, c2 and c3 through the liquid delivery pump; 5) starting a motor of the stirring device to stir the medium-temperature coal pitch in the reactor; 6) starting a circulating pump of a heat conduction oil heating system to heat the medium-temperature coal pitch in the reactor until the required oxidation reaction temperature is reached; 7) opening valves of air ports a1, a2 and a3, allowing air to enter the reactor through an air inlet pipe and a gas distributor at a certain flow rate, and performing oxidation reaction with medium-temperature coal pitch; 9) starting a vacuum pump of the vacuum system to exhaust tail gas from the interfaces b1, b2 and b 3; 10) in order to ensure the stability of the quality of the coal pitch with high softening point, liquefied medium-temperature coal pitch needs to be supplemented timely through liquid level sensors g1, g2 and g3 in the reactor from time to time; 11) after reacting for a certain time, discharging the prepared high-softening-point coal pitch from a discharge hole e, and repeating the preparation of the next batch of high-softening-point coal pitch.
Claims (4)
1. An air oxidation unit for producing high softening point coal tar pitch, the unit comprising: the horizontal multi-shaft oxidation reactor is provided with a jacket, heat conducting oil is filled in the jacket, a heat conducting oil inlet is formed in the front end of the side wall of the reactor, a heat conducting oil outlet is formed in the rear end of the side wall of the reactor, 1 discharge hole is formed in the bottom of the reactor, at least 3 sets of stirrers are arranged in the reactor in a direction perpendicular to the radial direction of the reactor, the stirrers are arranged in parallel and uniformly, and at least 3 sets of air inlets, a tail gas vacuumizing outlet and a medium-temperature coal pitch feed hole are formed in the top of the reactor; each air inlet is connected in parallel through a pipeline and is connected with an air inlet pipe and an air distributor below the air inlet pipe, the air inlet pipes are communicated with each other, and the bottom of the air distributor is connected with the reactor through a support piece; each vacuumizing outlet is connected in parallel through a pipeline; all the medium temperature coal tar pitch feed inlets are connected in parallel through pipelines, and a liquid level sensor is arranged on each medium temperature coal tar pitch feed inlet.
2. The air oxidation apparatus as set forth in claim 1, wherein the number of said air inlets, said medium temperature coal tar pitch feed ports and said tail gas evacuation outlets is the same as the number of said agitators.
3. The air oxidation apparatus as set forth in claim 1, wherein a baffle plate is provided between said agitators, said baffle plate being a perforated plate.
4. The air oxidation apparatus as set forth in claim 1, wherein the lower portion of the inlet pipe is configured with gas distribution holes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921805602.9U CN210915939U (en) | 2019-10-25 | 2019-10-25 | Air oxidation device for preparing coal tar pitch with high softening point |
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| CN201921805602.9U CN210915939U (en) | 2019-10-25 | 2019-10-25 | Air oxidation device for preparing coal tar pitch with high softening point |
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| CN210915939U true CN210915939U (en) | 2020-07-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426852A (en) * | 2022-01-05 | 2022-05-03 | 中国石油化工股份有限公司 | High-softening-point asphalt and preparation method and application thereof |
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2019
- 2019-10-25 CN CN201921805602.9U patent/CN210915939U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426852A (en) * | 2022-01-05 | 2022-05-03 | 中国石油化工股份有限公司 | High-softening-point asphalt and preparation method and application thereof |
| CN114426852B (en) * | 2022-01-05 | 2023-03-10 | 中国石油化工股份有限公司 | High-softening-point asphalt and preparation method and application thereof |
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