CN112973575A - High-pressure tubular reactor and operation method thereof - Google Patents
High-pressure tubular reactor and operation method thereof Download PDFInfo
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- CN112973575A CN112973575A CN202110299663.8A CN202110299663A CN112973575A CN 112973575 A CN112973575 A CN 112973575A CN 202110299663 A CN202110299663 A CN 202110299663A CN 112973575 A CN112973575 A CN 112973575A
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/042—Pressure vessels, e.g. autoclaves in the form of a tube
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
The invention discloses a high-pressure tubular reactor and an operation method thereof, which are characterized in that a structure of a cooling water side of the reactor is improved by adding a fin, a spiral structure and the like at a special part of the outer side pipe wall of the reactor, the contact area of a medium and the surface of the reactor is increased, the change and transmission of the temperature can be faster and more effective, and the heat transfer efficiency of the reactor is improved, so that the temperature in the tubular reactor is more accurately controlled, the decomposition rate of an initiator in the reactor is adjusted, and the purposes of adjusting the production load and the molecular weight distribution of the reactor are achieved. According to the high-pressure tubular LDPE reaction system, the three-dimensional structures such as fins and spirals are added in each zone of the reactor, so that the heat transfer efficiency is improved, the temperature is effectively controlled, the decomposition rate of the initiator is adjusted, the molecular weight distribution of the product is regulated, the product performance can be effectively improved, and the unnecessary loss in the production of polyolefin by the high-pressure tubular LDPE reaction system can be greatly reduced.
Description
Technical Field
The invention relates to a high-pressure tubular reactor, in particular to a mode of increasing the wall surface three-dimensional structure of the reactor, which improves the heat transfer efficiency of the reactor so as to realize more accurate temperature control and higher production load.
Background
Low Density Polyethylene (LDPE), one of the three major polyethylene products, has remained a durable market and has been in a vigorous market since its advent. The tubular high-pressure polyethylene process is the most common high-pressure polyethylene process in the world at present due to the advantages of high conversion per pass, low monomer consumption, long production period, high production capacity, simple and reliable equipment form and the like. At present, dozens of sleeve type LDPE devices in China keep high operating rate so as to meet the vigorous market demand.
The Molecular Weight Distribution (MWD) of LDPE has a crucial influence on the density and crystalline melting point of the product, as well as the physical and mechanical properties of the final product, and the phase equilibrium state in the tubular reactor is closely related to the Molecular Weight Distribution of LDPE, because of the essential characteristics of the polymerization of monomers at high temperature and high pressure in the high pressure polyethylene process, the high pressure polyethylene process itself is also highly dangerous, and the polymerization reaction is an exothermic reaction, if the exothermic reaction cannot be removed in time and accumulates locally, a temperature runaway phenomenon is easily caused, when the temperature reaches above 350 ℃, the decomposition reaction of ethylene occurs, and the most serious condition causes the explosion of the reactor. Meanwhile, due to fluctuation of operating conditions and difference of properties of products with different grades, liquid-liquid phase separation sometimes occurs in homogeneous reaction materials, and a polymer-rich phase is easy to deposit and adhere to the inner wall of a reaction tube due to high viscosity to form a compact polyethylene film, so that the wall adhesion phenomenon of the reactor is caused. The wall sticking causes the heat transfer coefficient between the materials in the reactor and the jacket cooling water to be reduced, so that the heat removal capacity of the reactor is reduced, the yield is reduced, and the stability of the product quality and the long-period stable operation of the device are influenced. For the tubular process, the heat released by the polymerization reaction is removed by cooling water in a heat exchange jacket outside the reaction tube, and the temperature control is also realized by heat transfer through the heat exchange jacket. Thus, the bottleneck in increasing the production of LDPE is the cooling capacity of the heat exchange jacket. The structure of the heat exchange jacket has great influence on the heat transfer effect of the reactor when the device runs, and the heat exchange jacket with excellent structure can obviously improve the heat transfer coefficient of the whole device.
According to the invention, the three-dimensional structure is added on the outer wall surface of the reactor, the flow and the temperature of the cooling medium are regulated and controlled, the temperature of the reactor is better controlled, the molecular weight distribution and the product performance of the polymer are optimized, and the purposes of improving the productivity of the device and reducing the energy consumption are achieved.
Disclosure of Invention
The invention aims to provide a solution for the problems of low initiator decomposition efficiency and poor product performance caused by poor heat dissipation effect and low heat transfer coefficient of a heat exchanger in the tubular LDPE production process.
In order to solve the problems, the technical scheme of the invention is as follows: a high-pressure tubular reactor and its operation method features that the stereo structure is additionally made on the external surface of casing tube reactor to increase the heat transfer efficiency of heat exchange jacket, so effectively controlling the temp in reactor and regulating the decomposition rate of trigger and the molecular weight distribution of product. Tests prove that the production load of the reactor with the three-dimensional structure can be improved by 1-15 percent and can be improved to 20 percent at most.
The invention firstly provides a high-pressure tubular reactor which at least comprises two subareas, wherein the outer wall surface of each subarea is wrapped by at least one heat exchange jacket; at least one spatial structure for enhancing heat exchange is arranged in the outer wall surface area of at least one reactor which exchanges heat with the heat exchange jacket and is divided into at least one subarea.
Further, the subarea is a region in which the wall sticking phenomenon easily occurs in the reaction tube, so that the heat transfer efficiency is low, or a region in which the temperature runaway phenomenon easily occurs at the initiator feed inlet, or both the subareas.
Furthermore, the three-dimensional structure for heat exchange enhancement is a fin or spiral three-dimensional structure for heat exchange enhancement, and the arrangement mode is winding arrangement, so that the heat exchange area between the cooling medium in the heat exchange jacket and the inner side of the heat exchange jacket is increased.
The invention also provides a method for improving the yield and regulating and controlling the molecular weight distribution of the product in the production process of tubular LDPE (Low-Density polyethylene):
selecting at least two partitions on a high-pressure tubular reactor, wherein the outer wall surface of each partition is wrapped by at least one heat exchange jacket;
at least one three-dimensional structure for strengthening heat exchange is arranged on the outer wall surface of at least one high-pressure tubular reactor wrapped by a heat exchange jacket;
the cooling medium in the heat exchange jacket exchanges heat with the reaction materials in the tubular reactor, the flow rate of the cooling medium in the heat exchange jacket is controlled to be 0.2-2m/s, and the temperature of the cooling medium is controlled to be 30-180 ℃.
As a preferred embodiment of the present invention, the flow rate of the cooling medium in the jacket outside the high-pressure tubular reactor is preferably from 0.5 to 1.5m/s and the temperature is preferably from 100 ℃ to 170 ℃. The cooling medium in the heat exchange jacket is preferably flowing liquid water.
As a preferable aspect of the present invention, the three-dimensional structure may be selected from a fin, a spiral, or other members that contribute to enhancing the heat exchange effect, for example, other members that contribute to increasing the heat exchange area, or contribute to improving the heat exchange effect by enhancing the flow state of the cooling medium. The three-dimensional structure may be a single or a combination of one or more different members.
In a preferred embodiment of the present invention, the three-dimensional structure is a protrusion having a certain height on the outer wall surface of the reactor.
As a preferred scheme of the invention, the added three-dimensional structure is selected in a targeted manner from places in the tubular reactor where high-temperature phenomena and wall sticking are easy to happen. As a preferred embodiment of the present invention, each of the zones has a separate initiator feed inlet at the inlet.
As a preferable scheme of the invention, when the three-dimensional structure is selected as the fins, the fins are arranged around the pipe wall in circles at the position where temperature control is needed, wherein each circle is distributed in a scattered point mode, and the number of the fins arranged in each circle ranges from 3 to 10, and is preferably 4 to 8.
As a preferred embodiment of the present invention, when the three-dimensional structure is selected as a spiral, the spiral is spirally arranged around the pipe wall at the position where temperature control is required, and the number of turns of the spiral ranges from 5 to 20 turns, preferably from 6 to 15 turns.
As a preferred embodiment of the present invention, the height of the three-dimensional structure ranges from 2 to 15cm, preferably from 4 to 13 cm.
As a preferable scheme of the invention, the increase range of the heat exchange area of the fins is 10-50%, and the preferable range is 20-35%.
As a preferred scheme of the invention, the increase of the heat exchange area of the screw thread is in the range of 20-75%, preferably 35-65%. As a preferred embodiment of the invention, the high-pressure tubular reactor is a tubular reactor for LDPE in a tubular process.
Drawings
In FIG. 1 is a process flow diagram of an embodiment of the invention for use in a high pressure tubular reactor heat exchanger.
FIG. 2 is a process flow diagram of an embodiment of the use of a high pressure tubular reactor heat exchanger according to the present invention.
FIG. 3 is a process flow diagram of an embodiment of the use of a high pressure tubular reactor heat exchanger according to the present invention.
FIG. 4 is a process flow diagram of an embodiment of the use of a high pressure tubular reactor heat exchanger according to the present invention.
FIG. 5 is a process flow diagram of an embodiment of the use of a high pressure tubular reactor heat exchanger according to the present invention.
In the embodiment of the invention, the material in the inner pipe is a reaction medium, the material in the jacket is a cooling medium, and the heat released by the polymerization reaction is removed by the cooling medium circulating in the jacket. In some preferred embodiments, the cooling medium is cooling water which is in countercurrent heat exchange with the reaction mass for all reaction zones. In some preferred embodiments, the cooling water is in cocurrent heat exchange with the reaction mass for all reaction zones. In some preferred embodiments, the cooling water is in co-current heat exchange with the reaction mass in some zones of the reactor and in counter-current heat exchange with the reaction mass in other zones of the reactor.
Detailed Description
While the invention has been described with reference to exemplary embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will include embodiments falling within the scope of the appended claims.
As shown in FIG. 1, in a specific embodiment of the present invention, the heat exchange process in the high-pressure tubular reactor is a double tube type, the high-pressure tubular reactor comprises a plurality of zones, and each zone has a separate initiator feed inlet at its inlet; the outer wall surface of each partition is wrapped by at least one heat exchange jacket; at least one spatial structure for enhancing heat exchange is arranged in the outer wall surface area of at least one reactor which exchanges heat with the heat exchange jacket and is divided into at least one subarea.
In the embodiment of the invention, for convenience of explanation, each partition corresponds to one heat exchange jacket, and a three-dimensional structure for enhancing heat exchange is arranged in each jacket. In fig. 1, the triangular shaded area indicates the location where modification can be selected (where temperature control is required); 2, a cross-sectional view of the fin structure for reconstruction; and 3, a structural schematic diagram of the thread for reconstruction. Further description is provided below in connection with the selection of a particular retrofit configuration.
As shown in fig. 2, in a preferred embodiment of the present invention, under certain polymerization pressure and temperature conditions, fins are added at the end of each section of heat exchanger, and when circulating water is injected into the heat exchanger and flows through the fin region, the heat exchange efficiency is greatly increased due to the increase of the heat exchange area, and the production load of the reactor is increased. In addition, the temperature of the material at the outlet of the former subarea of the reactor is reduced, so that the initiator in the latter subarea is decomposed at a lower reaction temperature and initiates ethylene polymerization, the number average molecular weight of the LDPE is increased, and the invention also has the effect of improving the molecular weight distribution of the LDPE.
As shown in fig. 3, in a preferred embodiment of the present invention, under certain polymerization pressure and temperature conditions, a fin is added at the front end of each heat exchanger, and after circulating water is injected into the heat exchanger, when water flows through the fin region, the heat exchange efficiency will be greatly improved due to the increase of the heat exchange area, at this time, for the region with large temperature change, the heat transfer speed will be greatly improved, the initiator decomposition rate will be slow, the temperature rise speed of the reaction material in the reactor will be slow, and the effective reaction region will be enlarged, so that the production load of the reactor can be effectively increased, and the molecular weight distribution of LDPE can be improved.
As shown in fig. 4, in a preferred embodiment of the present invention, under certain polymerization pressure and temperature conditions, fins are added at the front and rear ends of each heat exchanger, and after circulating water is injected into the heat exchanger, when water flows through the fin regions, the heat exchange efficiency will be greatly improved due to the increase of the heat exchange area, and at this time, for the regions with large temperature change, the heat transfer speed will be greatly improved, and for the regions with slow heat transfer, the heat transfer efficiency will be improved due to the increase of the contact area, the detection will be more accurate, and the system will control the reaction temperature more accurately, so that the decomposition efficiency of the initiator and the production load of the reactor can be effectively controlled, and the molecular weight distribution of LDPE can be improved.
As shown in fig. 5, in a preferred embodiment of the present invention, under certain polymerization pressure and temperature conditions, threads are added at the front and rear ends of each heat exchanger, after circulating water is injected into the heat exchanger, when water flows through the threaded area, the heat exchange efficiency will be greatly improved due to the increase of the heat exchange area, and the change of the water flow mode will cause the advance occurrence of water flow turbulence in the heat exchanger, at this time, the heat transfer speed will be greatly improved for the area with large temperature change, and the heat transfer efficiency will be improved due to the increase of the contact area for the area with slow heat transfer, the detection will be more accurate, and the control of the reaction temperature by the system will be more accurate, so that the decomposition efficiency of the initiator and the production load of the reactor can be effectively controlled, and the molecular weight distribution of LDPE can be improved.
Example 1
A high-pressure tubular process reactor and its operation as shown in fig. 2 were used. The heat exchange area is increased by 25 percent by adding fins at a plurality of positions at the tail end of each subarea of the high-pressure tubular reactor. During normal production, the polymerization pressure at the inlet of the first zone of the high-pressure tubular reactor is 250MPa, the initiation temperature is 175 ℃, the peak temperature of the reactor is 296 ℃, the cooling medium water and the reaction materials in the heat exchange jacket perform countercurrent heat exchange, the initial temperature of the cooling water is 150 ℃, and the average flow velocity of the water is 1 m/s. After circulating water is injected into the heat exchanger, when water flows through the fin area, the temperature change sensitivity is obviously increased due to the increase of the heat exchange area, and the control on the temperature is more accurate during polymerization. Therefore, the production amount of LDPE was increased by 2.7% and the width of the molecular weight distribution of LDPE was increased from 6.63 to 6.81 as compared with comparative example 1.
Example 2
A high-pressure tubular process reactor and its operation as shown in fig. 3 were used. The fins are added at a plurality of positions at the front end of each subarea of the high-pressure tubular reactor, and the heat exchange area is increased by 25 percent. During normal production, the polymerization pressure at the inlet of the first zone of the high-pressure tubular reactor is 250MPa, the initiation temperature is 175 ℃, the peak temperature of the reactor is 296 ℃, the cooling medium water and the reaction materials in the heat exchange jacket perform countercurrent heat exchange, the initial temperature of the cooling water is 130 ℃, and the average flow velocity of the water is 0.98 m/s. After the circulating water is injected into the heat exchanger, when water flows through the fin area, the sensitivity to temperature change is obviously increased due to the increase of the heat exchange area. The temperature control during polymerization is more accurate, the problem of too high temperature during temperature runaway is effectively solved, and the effective reaction area is increased. Therefore, the production of LDPE was increased by 2.2% and the breadth of the molecular weight distribution of LDPE was increased from 6.63 to 6.78 compared to comparative example 1.
Example 3
A high pressure tubular process reactor and method of operating the same as shown in figure 4. The fins are added at a plurality of positions at the front end and the tail end of each subarea of the high-pressure tubular reactor, and the heat exchange area is increased by 50 percent. During normal production, the polymerization pressure at the inlet of the first zone of the high-pressure tubular reactor is 250MPa, the initiation temperature is 175 ℃, the peak temperature of the reactor is 296 ℃, the cooling medium water and the reaction materials in the heat exchange jacket perform countercurrent heat exchange, the initial temperature of the cooling water is 140 ℃, and the average flow velocity of the water is 1.12 m/s. To the great region of temperature variation, heat transfer rate will improve greatly, has reduced the proportion that initiator decomposition efficiency reduces when the flying temperature phenomenon appears, to the slower region of heat transfer, because area of contact's increase, the sensitivity of heat transfer is higher, detects more accurately, effectively alleviates because of the slow problem of heat transfer that the wall sticking phenomenon leads to, and the control of system to reaction temperature will be more accurate. Therefore, the production amount of LDPE was increased by 5.4% and the width of the molecular weight distribution of LDPE was increased from 6.63 to 6.98 as compared with comparative example 1.
Example 4
A high pressure tubular process reactor and method of operating the same as shown in figure 5. The front end and the tail end of each section of heat exchanger are provided with threads, and the heat exchange area is increased by 64 percent. During normal production, the polymerization pressure at the inlet of the first zone of the high-pressure tubular reactor is 250MPa, the initiation temperature is 175 ℃, the peak temperature of the reactor is 296 ℃, the cooling medium water and the reaction materials in the heat exchange jacket perform countercurrent heat exchange, the initial temperature of the cooling water is 135 ℃, and the average flow rate of the water is 1.24 m/s. After circulating water is injected into the heat exchanger, when water flows through the fin area, the heat exchange efficiency is improved within the range of 43-68%. At the moment, the heat transfer speed is improved more obviously for the area with larger temperature change, so that the highest temperature during temperature runaway is reduced, the proportion of reduction of the decomposition efficiency of the initiator when the temperature runaway phenomenon occurs is reduced, and in the area with slower heat transfer, the sensitivity of heat transfer is higher due to the increase of the contact area, the detection is more accurate, the problem of slow heat transfer caused by the wall sticking phenomenon is effectively relieved, and the control of the system on the reaction temperature is more accurate. Therefore, the production amount of LDPE was increased by 7.3% and the width of the molecular weight distribution of LDPE was increased from 6.63 to 7.22 as compared with comparative example 1.
Comparative example 1
Comparative example 1 differs from example 1 in that no steric structure is added to the wall of the tubular reactor, the LDPE production is 26t/h and the breadth of the molecular weight distribution of the LDPE is 6.63.
Comparative example 2
The difference between the comparative example 2 and the example 2 is that the wall of the tubular reactor is not added with a three-dimensional structure, the output of LDPE is 24.3t/h, and the molecular weight distribution width of LDPE is increased from 6.63 to 6.81.
Comparative example 3
The difference between the comparative example 3 and the example 3 is that the wall of the tubular reactor is not added with a three-dimensional structure, the output of LDPE is 27t/h, and the molecular weight distribution width of LDPE is increased from 6.63 to 7.01.
Comparative example 4
Comparative example 4 differs from example 4 in that the wall of the tubular reactor is not sterically increased, the yield of LDPE is 27.6t/h and the breadth of the molecular weight distribution of LDPE increases from 6.63 to 7.29.
As can be seen from the above four examples and four comparative examples, the productivity was greatly improved by the high-pressure tubular process reactor and the operation method thereof according to the present invention. In addition, through the effective control to the temperature, can adjust the reactor internal initiator decomposition efficiency, reach the purpose of adjusting product molecular weight distribution and improving product quality, effectively reduce the energy consumption simultaneously, the energy cost is saved accomplishes green production better.
Claims (10)
1. A high-pressure tubular reactor is characterized by comprising at least two partitions, wherein the outer wall surface of each partition is wrapped by at least one heat exchange jacket; at least one space structure for strengthening heat exchange is arranged in the outer wall surface area of at least one reactor for exchanging heat with the heat exchange jacket of at least one partition, and the space structure for strengthening heat exchange is a fin or spiral space structure for strengthening heat exchange.
2. A high pressure tubular reactor according to claim 1 wherein the zones are contained in a zone in the reaction tube where wall sticking is likely to occur leading to inefficient heat transfer or a zone in the reaction tube where temperature runaway is likely to occur at the initiator feed inlet, or both.
3. The high pressure tubular reactor of claim 1, wherein the three-dimensional structure is a protrusion having a certain height on the outer wall surface of the reactor.
4. A high pressure tubular reactor according to claim 1 wherein each of said zones has a separate initiator feed at its inlet.
5. The high pressure tubular reactor of claim 1, wherein when the three-dimensional structure is selected as fins, the fins are arranged in circles around the tube wall at the position where temperature control is required, wherein each circle is in a scattered point type distribution, and the number of the fins arranged in each circle ranges from 3 to 10.
6. A high pressure tubular reactor according to claim 1 wherein when the three-dimensional structure is selected as a helix, the helix is arranged helically around the wall of the tube where temperature control is required, the number of turns of the helix being in the range of 5-20 turns.
7. A high pressure tubular reactor according to claim 1, wherein the height of the three-dimensional structure is in the range of 2-15 cm.
8. A high pressure pipe reactor according to any of claims 1 to 7 wherein the high pressure pipe reactor is a pipe reactor for LDPE in a tubular process.
9. A method for improving the yield and regulating and controlling the molecular weight distribution of a product in the production process of tubular LDPE is characterized in that,
selecting at least two partitions on a high-pressure tubular reactor, wherein the outer wall surface of each partition is wrapped by at least one heat exchange jacket;
at least one three-dimensional structure for strengthening heat exchange is arranged on the outer wall surface of at least one high-pressure tubular reactor wrapped by a heat exchange jacket;
the cooling medium in the heat exchange jacket exchanges heat with the reaction materials in the tubular reactor, the flow rate of the cooling medium in the heat exchange jacket is controlled to be 0.2-2m/s, and the temperature of the cooling medium is controlled to be 30-180 ℃.
10. The method of claim 9, wherein the cooling medium is liquid water.
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| CN202110299663.8A CN112973575A (en) | 2021-03-22 | 2021-03-22 | High-pressure tubular reactor and operation method thereof |
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| CN202110299663.8A CN112973575A (en) | 2021-03-22 | 2021-03-22 | High-pressure tubular reactor and operation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114602392A (en) * | 2022-03-17 | 2022-06-10 | 浙江大学宁波“五位一体”校区教育发展中心 | Operation method of tubular high-pressure polyethylene reactor with ultrasonic descaling device |
| EP4389775A1 (en) | 2022-12-20 | 2024-06-26 | ExxonMobil Chemical Patents Inc. | Initiator injection line for high pressure polymerization |
| EP4389273A1 (en) | 2022-12-20 | 2024-06-26 | ExxonMobil Chemical Patents Inc. | A tubular reactor comprising a thermocouple device for measuring a temperature within the tubular reactor |
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| CN1440427A (en) * | 2000-05-05 | 2003-09-03 | 巴塞尔聚烯烃股份有限公司 | Method for the continuous production of ethylene homo-and ethylene co-polymers |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114602392A (en) * | 2022-03-17 | 2022-06-10 | 浙江大学宁波“五位一体”校区教育发展中心 | Operation method of tubular high-pressure polyethylene reactor with ultrasonic descaling device |
| EP4389775A1 (en) | 2022-12-20 | 2024-06-26 | ExxonMobil Chemical Patents Inc. | Initiator injection line for high pressure polymerization |
| EP4389273A1 (en) | 2022-12-20 | 2024-06-26 | ExxonMobil Chemical Patents Inc. | A tubular reactor comprising a thermocouple device for measuring a temperature within the tubular reactor |
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