CN215312409U - Rotary thermal polycondensation reaction device and mesophase pitch preparation system - Google Patents
Rotary thermal polycondensation reaction device and mesophase pitch preparation system Download PDFInfo
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- CN215312409U CN215312409U CN202121826914.5U CN202121826914U CN215312409U CN 215312409 U CN215312409 U CN 215312409U CN 202121826914 U CN202121826914 U CN 202121826914U CN 215312409 U CN215312409 U CN 215312409U
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Abstract
The utility model provides a rotary thermal polycondensation reaction device and a mesophase pitch preparation system. The rotary thermal polycondensation reaction apparatus comprises: a rotation driving mechanism including a rotation portion that is reciprocally rotatable; the sleeve is fixedly connected with the rotating part, and is provided with a plurality of centrifugal holes which are circumferentially distributed at intervals around a central shaft of the sleeve; the reaction kettle is detachably arranged in the centrifugal hole and is used for containing feed liquid; the heater is arranged on the sleeve and used for heating the sleeve; and a heating power supply unit which is in contact with and electrically conducted to the heater and supplies power to the heater. The mesophase pitch preparation system comprises the rotary thermal polycondensation reaction device. The rotary thermal polycondensation reaction device provided by the utility model mixes the reaction system through centrifugal acting force, is uniformly heated, and is not easy to hang on the wall and coke. The intermediate phase asphalt preparation system can reduce impurities such as quinoline insoluble substances in the asphalt and prepare high-quality intermediate phase asphalt.
Description
Technical Field
The utility model relates to the technical field of chemical equipment, in particular to a rotary thermal polycondensation reaction device and a mesophase pitch preparation system.
Background
The carbon fiber is a high-strength and high-modulus fiber with a carbon content of more than 90%, and can be divided into Polyacrylonitrile (PAN) system and Pitch (Pitch) system according to the parent material of the raw material. The carbon fiber of pitch system is widely used in high-end fields of aerospace industry, unmanned planes, military, racing car, etc. because of its advantages of high strength, ultrahigh tensile modulus, ultrahigh thermal conductivity, light weight, excellent electrical conductivity, excellent electromagnetic shielding effectiveness, etc.
The asphalt raw material has low cost, and has the characteristics of high carbon content, moderate carbon-to-hydrogen ratio, high aromatic degree, easy polymerization, partially saturated aromatic rings, branched alkanes with different carbon numbers on the aromatic rings and the like. However, ordinary pitch is not suitable for direct use in the manufacture of high-end carbon fiber products and requires processing into anisotropic mesophase pitch. The high-quality mesophase pitch meets the requirements that the content of the mesophase is more than 98 percent under a polarizing microscope, has wide-area morphology, proper softening temperature and the like.
The thermal polycondensation reaction is an important step in the process of preparing mesophase pitch, and the existing thermal polycondensation reaction equipment has the problems of easy wall hanging blockage, uneven heating, different reaction intensity, insufficient growth of condensed ring molecules, easy coking of the inner wall of a high-temperature heating reactor and the like.
SUMMERY OF THE UTILITY MODEL
In view of the above, it is necessary to provide a rotary thermal polycondensation reaction apparatus which mixes a reaction system by centrifugal force, heats the reaction system uniformly, is less prone to wall hanging and coking, and contributes to a polymerization reaction in a molten state of asphalt.
A rotary thermal polycondensation reaction apparatus comprising:
a rotation driving mechanism including a rotation portion that is reciprocally rotatable;
the sleeve is fixedly connected with the rotating part, a plurality of centrifugal holes are formed in the sleeve, and the centrifugal holes are circumferentially distributed at intervals around a central shaft of the sleeve;
the reaction kettle is detachably arranged in the centrifugal hole and is used for containing feed liquid;
the heater is arranged on the sleeve and used for heating the sleeve; and
and a heating power supply unit that is in contact with and electrically conducted with the heater and supplies power to the heater.
Above-mentioned rotation type thermal polycondensation reaction unit heats the sleeve through the heater, and then heats reation kettle and material wherein (like pitch), and reation kettle compares in the agitator diameter littleer, is heated more evenly, avoids the wall built-up, and the reciprocal rotatory centrifugation of rotation of rotary driving mechanism drive sleeve, and the feed liquid is difficult to the coking, helps the feed liquid to react in reation kettle.
In one embodiment, the rotating part is a rotating base, and the bottom of the rotating base is connected with a rotating driving motor.
In one embodiment, the sleeve is fixedly connected with the rotating base in the circumferential direction.
In one embodiment, a mounting groove is formed in the rotating base, a limiting strip is arranged in the mounting groove, a limiting groove matched with the limiting strip is formed in the sleeve, and the limiting strip is clamped and fixed in the limiting groove.
In one embodiment, the sleeve is a ceramic sleeve.
In one embodiment, the heater is a ceramic heater rod.
In one embodiment, the reaction kettle comprises a container body, an upper cover and a lower cover which are vertically communicated, the upper cover is in threaded connection with one end of the container body, the lower cover is in threaded connection with the other end of the container body, and a closed accommodating cavity is formed among the container body, the upper cover and the lower cover. The reaction kettle with the structure can be opened vertically, and is favorable for feeding or discharging.
In one embodiment, the reaction kettle is cylindrical, the outer diameter of the reaction kettle is 5-10 cm, the inner diameter of the reaction kettle is 3-8 cm, and the wall thickness of the reaction kettle is 1-3 cm. The reaction kettle with the size can ensure that the asphalt is heated more uniformly and controllably.
In one embodiment, the reaction vessel is a stainless steel reaction vessel. The reaction kettle is made of stainless steel, such as stainless steel 304 or stainless steel 316.
In one embodiment, the heating power supply is a rotating conductive slip ring.
The utility model also provides a mesophase pitch preparation system, which comprises a supercritical fluid filler extraction tower, a separation kettle, a thin film evaporator, a first molecular distillation apparatus, a second molecular distillation apparatus, a rotary thermal polycondensation reaction device and a third molecular distillation apparatus which are connected in sequence; the rotary thermal polycondensation reaction device is the rotary thermal polycondensation reaction device; the supercritical fluid filler extraction tower is used for extracting and rectifying the asphalt raw material; the first molecular distillation apparatus and the second molecular distillation apparatus are used for separating entrainer and asphalt; the rotary thermal polycondensation reaction device is used for providing a thermal polycondensation reaction site for the asphalt distilled by the second molecular distillation instrument; the third molecular still is used to separate mesophase pitch and impurities.
The intermediate phase asphalt preparation system can reduce impurities such as quinoline insoluble substances in the asphalt and prepare high-quality intermediate phase asphalt.
In one embodiment, the bottom of the supercritical fluid packed extraction tower is connected with a collection kettle, and the collection kettle is used for heavy components in the supercritical fluid packed extraction tower.
Compared with the prior art, the utility model has the following beneficial effects:
according to the rotary thermal polycondensation reaction device, the sleeve is heated through the heater, so that the reaction kettle and materials (such as asphalt) in the reaction kettle are heated, the reaction kettle is smaller in diameter compared with a stirrer and is heated more uniformly, wall hanging is avoided, the rotary driving mechanism drives the sleeve to rotate and centrifuge in a reciprocating mode, feed liquid is not easy to coke, and the reaction of the feed liquid in the reaction kettle is facilitated.
The intermediate phase asphalt preparation system can reduce impurities such as quinoline insoluble substances in the asphalt and prepare high-quality intermediate phase asphalt.
Drawings
FIG. 1 is a schematic view of a rotary thermal polycondensation apparatus in the example.
FIG. 2 is a schematic structural view of the reaction vessel in the example.
FIG. 3 is a schematic diagram showing the movement trend of the feed liquid in the reaction vessel during the reciprocating centrifugation of the rotary thermal polycondensation reaction device in the example.
FIG. 4 is a schematic diagram of a mesophase pitch production system in an example.
In the figure, 1, supercritical fluid packing extraction tower, 2, separation kettle, 3, thin film evaporator, 4, first molecular distillation apparatus, 5, second molecular distillation apparatus, 6, rotary thermal polycondensation reaction device, 7, third molecular distillation apparatus, 8, collection kettle, 100, rotary part, 200, sleeve, 210, centrifugal hole, 300, reaction kettle, 310, container body, 320, upper cover, 330, lower cover, 400, heater, 500, heating power supply part, 600, feed liquid.
Detailed Description
To facilitate an understanding of the utility model, the utility model will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the utility model herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the utility model. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
A rotary thermal polycondensation reaction apparatus, as shown in FIG. 1, comprises a rotary drive mechanism, a sleeve 200, a reaction vessel 300, a heater 400 and a heating power supply part 500. The rotation driving mechanism includes a rotation portion 100 capable of rotating reciprocally, the sleeve 200 is fixedly connected to the rotation portion 100, and the rotation portion 100 can drive the sleeve 200 to rotate reciprocally. The sleeve 200 has a plurality of centrifugal holes 210 at an end thereof away from the rotating portion 100, and the centrifugal holes 210 are circumferentially and uniformly distributed around a central axis of the sleeve 200. The reaction kettle 300 is detachably mounted in the centrifugal hole 210, the reaction kettle 300 is used for containing feed liquid 600, and the feed liquid 600 can be asphalt or other raw materials. When the sleeve 200 rotates reciprocally, the feed liquid 600 in the reaction kettle 300 can be centrifuged reciprocally. The center of the sleeve 200 is also provided with a mounting hole, the heater 400 is circumferentially fixed in the mounting hole, and the heater 400 can heat the sleeve 200 and further heat the reaction kettle 300 and the feed liquid 600 in the reaction kettle 300. The heating power supply unit 500 is in contact with and electrically conducted to the heater 400 to supply power to the heater 400, and specifically, the heating power supply unit 500 employs a rotating conductive slip ring, and the heating power supply unit 500 is fixed in the slip ring, so that power can be supplied to the heater 400 by rotating the conductive slip ring when the heater 400 rotates reciprocally with the rotating unit 100.
Specifically, the rotating portion 100 is a rotating base, and the bottom of the rotating base is connected to a rotation driving motor, and the rotation driving motor drives the rotating base to rotate reciprocally. The rotating base is provided with a circular mounting groove (not shown), a limiting strip is arranged in the mounting groove, a limiting groove matched with the limiting strip is arranged on the sleeve 200, the limiting strip is clamped in the limiting groove, the sleeve 200 is fixedly connected with the rotating base in the circumferential direction, and the sleeve 200 rotates in a reciprocating manner along with the rotating base when the rotating base rotates in a reciprocating manner.
Preferably, the sleeve 200 is a ceramic sleeve, the heater 400 is a ceramic heating rod, and the ceramic material has the advantages of good heat conductivity, strong mechanical property, corrosion resistance and the like.
In order to facilitate feeding and discharging, the reaction kettle 300 includes a container body 310, an upper cover 320 and a lower cover 330 (as shown in fig. 2) which are vertically communicated, the upper cover 320 is in threaded connection with one end of the container body 310, the lower cover 330 is in threaded connection with the other end of the container body 310, and a closed accommodating cavity is formed among the container body 310, the upper cover 320 and the lower cover 330. Preferably, reaction vessel 300 is elongated cylindrical. In a heating closed environment, the pressure inside the reaction kettle 300 is high, and in order to ensure the safety of the reaction, the reaction kettle 300 is made of stainless steel, such as stainless steel 304 or stainless steel 316. A pressure gauge can also be arranged on the upper cover 320 to detect the pressure in the reaction kettle.
The following brief description is made of the method of using and the operation principle of the rotary thermal polycondensation reaction apparatus: the reaction kettle 300 is taken down, the upper cover 320 is unscrewed, asphalt is added, the upper cover 320 is screwed, the quality of the asphalt added in different reaction kettles 300 is basically the same, and the asphalt is symmetrically placed in the centrifugal holes 210 of the sleeve 200, so that the vibration of the device caused by unstable gravity center during rotation is avoided; when centrifugation is needed, the rotary driving mechanism and the heating power supply part 500 are started to carry out rotary reciprocating centrifugation and heating, and the movement trend of asphalt in the reaction kettle 300 during the rotary reciprocating centrifugation is shown in figure 3; when only heating is needed and centrifugation is not needed, the rotation driving mechanism is turned off, and the heating power supply part 500 is turned on. After the reaction is completed, the centrifugation and heating are stopped, the reaction kettle 300 is taken down, and the lower cover 330 is opened for discharging.
Example 2
A mesophase pitch production system, as shown in FIG. 4, comprises a supercritical fluid filler extraction column 1, a separation kettle 2, a thin film evaporator 3, a first molecular distillation apparatus 4, a second molecular distillation apparatus 5, a rotary thermal polycondensation reaction apparatus 6 and a third molecular distillation apparatus 7, which are connected in sequence.
The supercritical fluid filler extraction tower 1 is used for extracting and rectifying asphalt raw materials, wherein the asphalt raw materials can adopt coal tar pitch, the extraction medium adopts supercritical carbon dioxide, and the entrainer adopts a mixture of ethanol, quinoline and toluene. Mixing asphalt raw materials and entrainers, introducing the mixture from the middle section or the upper end of a tower body, introducing an extraction medium from the bottom of the tower, carrying out countercurrent extraction rectification on the asphalt raw materials and the extraction medium in the tower body, allowing light components to flow out of the top of the tower and enter a separation kettle 2, allowing heavy components to flow out of the bottom of the tower and enter a collection kettle 8, mixing the materials in the collection kettle 8 with the asphalt raw materials through a raw material pump, and then allowing the mixed materials to enter a supercritical fluid filler extraction tower 1 for extraction rectification, so that the utilization rate of the raw materials is improved, and the cost is reduced. In the separation kettle 2, carbon dioxide escapes and is recycled, and the rest materials are introduced into the thin film evaporator 3. In the thin film evaporator 3, ethanol and the like are distilled off, and the remaining material is passed into the first molecular still 4. In the first molecular distillation apparatus 4, toluene was distilled off, and the remaining material was passed into the second molecular distillation apparatus 5. Distilling off quinoline in the second molecular distillation apparatus 5, adding the rest materials into a reaction kettle of a rotary thermal polycondensation reaction device 6 in batches, heating and centrifuging the rotary thermal polycondensation reaction device 6 adopting the rotary thermal polycondensation reaction device of example 1 to perform thermal polycondensation reaction, introducing the materials into a third molecular distillation apparatus 7, and performing flash evaporation or reduced pressure distillation to obtain an asphalt intermediate phase.
By adopting the mesophase pitch preparation system of the embodiment, the softening point of the obtained pitch mesophase is 150-250 ℃, quinoline insoluble substances are lower than 5 wt%, toluene insoluble substances are not less than 95 wt%, the content of soluble mesophase is not less than 50%, and the content of the wide-area morphology mesophase is 100%.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the utility model. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A rotary thermal polycondensation reaction apparatus comprising:
a rotation driving mechanism including a rotation portion that is reciprocally rotatable;
the sleeve is fixedly connected with the rotating part, a plurality of centrifugal holes are formed in the sleeve, and the centrifugal holes are circumferentially distributed at intervals around a central shaft of the sleeve;
the reaction kettle is detachably arranged in the centrifugal hole and is used for containing feed liquid;
the heater is arranged on the sleeve and used for heating the sleeve; and
and a heating power supply unit that is in contact with and electrically conducted with the heater and supplies power to the heater.
2. The rotary thermal polycondensation reaction apparatus according to claim 1, wherein the rotary part is a rotary base, and a bottom part of the rotary base is connected to a rotary drive motor.
3. The rotary thermal polycondensation reaction apparatus of claim 2 wherein the sleeve is circumferentially fixed to the rotating base.
4. The rotary thermal polycondensation reaction apparatus according to claim 3, wherein the rotary base has a mounting groove, a position-limiting bar is disposed in the mounting groove, a position-limiting groove is disposed in the sleeve, the position-limiting bar is engaged with the position-limiting bar, and the position-limiting bar is engaged with the position-limiting groove.
5. The rotary thermal polycondensation reaction apparatus of claim 1 wherein the sleeve is a ceramic sleeve and the heater is a ceramic heater rod.
6. The rotary thermal polycondensation reaction apparatus according to claim 1, wherein the reaction vessel comprises a vessel body, an upper lid and a lower lid which are vertically through, the upper lid is in threaded connection with one end of the vessel body, the lower lid is in threaded connection with the other end of the vessel body, and a closed accommodating chamber is formed among the vessel body, the upper lid and the lower lid.
7. The rotary thermal polycondensation reaction apparatus according to claim 1, wherein the reaction vessel has a cylindrical shape, an outer diameter of the reaction vessel is 5 to 10cm, an inner diameter of the reaction vessel is 3 to 8cm, and a wall thickness of the reaction vessel is 1 to 3 cm.
8. The rotary thermal polycondensation reaction apparatus of claim 1 wherein the reaction vessel is a stainless steel reaction vessel.
9. The rotary thermal polycondensation reaction apparatus according to any one of claims 1 to 8, wherein the heating power supply unit is a rotary conductive slip ring.
10. A mesophase pitch preparation system is characterized by comprising a supercritical fluid filler extraction tower, a separation kettle, a thin film evaporator, a first molecular distillation apparatus, a second molecular distillation apparatus, a rotary thermal polycondensation reaction device and a third molecular distillation apparatus which are connected in sequence; the thermal polycondensation reaction apparatus is a rotary thermal polycondensation reaction apparatus according to any one of claims 1 to 9; the supercritical fluid filler extraction tower is used for extracting and rectifying the asphalt raw material; the first molecular distillation apparatus and the second molecular distillation apparatus are used for separating entrainer and asphalt; the rotary thermal polycondensation reaction device is used for providing a thermal polycondensation reaction site for the asphalt distilled by the second molecular distillation instrument; the third molecular still is used to separate mesophase pitch and impurities.
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| CN202121826914.5U CN215312409U (en) | 2021-08-05 | 2021-08-05 | Rotary thermal polycondensation reaction device and mesophase pitch preparation system |
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| CN202121826914.5U CN215312409U (en) | 2021-08-05 | 2021-08-05 | Rotary thermal polycondensation reaction device and mesophase pitch preparation system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023169486A1 (en) * | 2022-03-09 | 2023-09-14 | 中国石油大学 (华东) | Reaction system and method for preparing high-quality mesophase pitch and co-producing spinnable isotropic pitch |
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2021
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023169486A1 (en) * | 2022-03-09 | 2023-09-14 | 中国石油大学 (华东) | Reaction system and method for preparing high-quality mesophase pitch and co-producing spinnable isotropic pitch |
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| CB03 | Change of inventor or designer information |
Inventor after: Zhu Baozhang Inventor after: Feng Zhihao Inventor after: Zhu Di Inventor before: Zhu Li Inventor before: Feng Zhihao Inventor before: Zhu Di Inventor before: Zhu Baozhang |