CN214915921U - Rearrangement reaction system - Google Patents
Rearrangement reaction system Download PDFInfo
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- CN214915921U CN214915921U CN202120300946.5U CN202120300946U CN214915921U CN 214915921 U CN214915921 U CN 214915921U CN 202120300946 U CN202120300946 U CN 202120300946U CN 214915921 U CN214915921 U CN 214915921U
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Abstract
The utility model relates to a caprolactam field discloses a rearrangement reaction system, and this rearrangement reaction system includes: the device comprises a vertical reactor, a first mixer, a second mixer and a pipeline communicated with the vertical reactor, the first mixer and the second mixer, wherein the vertical reactor is used for providing a reaction site for performing Beckmann rearrangement reaction on a mixed liquid of cyclohexane and cyclohexanone oxime and oleum to obtain heavy liquid; the first mixer is connected with the vertical reactor, a fuming sulfuric acid inlet is arranged on the first mixer, and the first mixer is used for premixing part of the heavy discharged liquid and fuming sulfuric acid to obtain a first premixed liquid; the second mixer is connected with the vertical reactor and the first mixer, a mixed solution inlet of the first cyclohexane and the cyclohexanone oxime is arranged on the second mixer, the second mixer is used for premixing the first premixed solution and the mixed solution of the cyclohexane and the cyclohexanone oxime to obtain a second premixed solution, and the second premixed solution is input into the vertical reactor.
Description
Technical Field
The utility model relates to a caprolactam field, concretely relates to rearrangement reaction system suitable for production caprolactam.
Background
In the production process of caprolactam, cyclohexanone oxime is generated through cyclohexanone ammoximation reaction, and the cyclohexanone oxime generates Beckmann molecular rearrangement reaction in the presence of 20% oleum to form caprolactam sulfuric acid solution and release a large amount of heat.
CN110511185A discloses a caprolactam rearrangement apparatus and method, wherein the caprolactam rearrangement apparatus includes a first reaction section, a second reaction section, a third reaction section and a buffer tank, wherein the first reaction kettle of the first reaction section is connected to the input end of the second circulation pump of the second reaction section, the input end of the third circulation pump of the third reaction section and the buffer tank, the rearrangement liquid of the first reaction kettle can overflow to the input end of the second circulation pump, the input end of the third circulation pump and the buffer tank, the second reaction kettle of the second reaction section is connected to the input end of the third circulation pump and the buffer tank, the rearrangement liquid of the second reaction kettle can overflow to the input end of the third circulation pump and the buffer tank, and the third reaction kettle of the third reaction section is connected to the buffer tank. In the patent document, the caprolactam rearrangement capacity is improved and the production yield is improved through multi-stage reaction, but the used equipment is complex, the occupied area is large, the cost is high, and the energy consumption of the process is high. In addition, the heat generated by the reaction can not be well utilized, which causes energy waste and difficult engineering amplification.
Further, the catalyst used in the rearrangement reaction is fuming sulfuric acid, and generates a caprolactam sulfuric acid solution accompanied by the generation of ammonium sulfate as a by-product. Because the value of ammonium sulfate is lower at present, and the price of ammonia is higher, the more ammonium sulfate is produced as a byproduct, and the more the caprolactam is processed.
Therefore, further improvements are needed in the existing caprolactam production processes.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a new rearrangement reaction system for overcoming the technical problems of complex caprolactam production equipment, large occupied area, high cost, more byproduct ammonium sulfate, energy waste and difficult engineering amplification in the prior art.
The inventor of the utility model has surprisingly found through a large number of experiments that the reaction raw materials (cyclohexane, cyclohexanone oxime and oleum) are premixed before entering the vertical reactor by arranging a mixer outside the vertical reactor, specifically, a first mixer is connected with the vertical reactor through control and is provided with an oleum inlet, the first mixer is used for premixing partial heavy liquor and oleum to obtain a first premixed liquid; the second mixer is connected with the vertical reactor and the first mixer, a mixed solution inlet of the first cyclohexane and the cyclohexanone oxime is arranged on the second mixer, the second mixer is used for premixing the first premixed solution and the mixed solution of the cyclohexane and the cyclohexanone oxime to obtain a second premixed solution, the second premixed solution is input into the vertical reactor, and the cyclohexanone oxime and the oleum are respectively fed through different mixers, so that the engineering amplification difficulty of the Beckmann rearrangement reaction in a solvent (cyclohexane) vaporization heat transfer mode in the material mixing process is solved, the micro mass transfer of the rapid reaction is strengthened, the multistage rearrangement is realized only by using a single tank and the mixer in the whole process, the retention time of raw materials is prolonged, the occurrence of side reactions is reduced, the yield of caprolactam is improved, and the equipment is simplified, reduces the equipment investment and has wide industrial application prospect.
In order to achieve the above object, an aspect of the present invention provides a rearrangement reaction system, including: a vertical reactor, a first mixer and a second mixer, and a line communicating the vertical reactor, the first mixer and the second mixer, wherein,
the vertical reactor is used for providing a reaction site for the Beckmann rearrangement reaction of the mixed solution of the cyclohexane and the cyclohexanone oxime and oleum to obtain heavy liquor;
the first mixer is connected with the vertical reactor and is provided with an oleum inlet, and the first mixer is used for premixing part of the heavy discharged liquid and oleum to obtain a first premixed liquid;
the second mixer is connected with the vertical reactor and the first mixer, a mixed solution inlet of the first cyclohexane and the cyclohexanone oxime is arranged on the second mixer, the second mixer is used for premixing the first premixed solution and the mixed solution of the cyclohexane and the cyclohexanone oxime to obtain a second premixed solution, and the second premixed solution is input into the vertical reactor.
Further, the rearrangement reaction system further comprises a plurality of third mixers, the third mixers are arranged in parallel, the third mixers are connected with the vertical reactor and the first mixer, a mixed solution inlet of second cyclohexane and cyclohexanone oxime is arranged on each third mixer, and the third mixers are used for premixing part of the heavy discharge liquid and the mixed solution of cyclohexane and cyclohexanone oxime to obtain a third premixed solution and inputting the third premixed solution into the vertical reactor.
Further, the rearrangement reaction system comprises 2 to 5 of the third mixers.
Further, the first mixer, the second mixer, and the third mixer are all static mixers.
Further, a cyclohexane steam outlet is arranged at the top end of the vertical reactor and used for discharging cyclohexane steam discharged from the vertical reactor.
Further, a demister is arranged inside the vertical reactor and used for refluxing caprolactam entrained in cyclohexane steam to the vertical reactor.
Further, the rearrangement reaction system further comprises an overflow tank, and the overflow tank is connected with the vertical reactor and is used for storing the rearrangement liquid overflowed from the vertical reactor.
Further, the third mixer and the overflow tank are arranged on two sides of the vertical reactor.
Further, the rearrangement reaction system further comprises a heat exchanger connected with the first mixer and the second mixer, wherein the heat exchanger is used for heating or cooling the first premixed liquid passing through the heat exchanger.
According to the utility model provides a rearrangement reaction system, this rearrangement reaction system has not only strengthened the microcosmic mass transfer of reaction, has only used single jar and blender to just realize the multistage rearrangement at whole in-process moreover, has not only prolonged the dwell time of raw materials, reduces the emergence of side reaction, improves the yield of caprolactam, has still simplified equipment, has reduced the equipment investment, has industrial application prospect.
Drawings
FIG. 1 is a schematic structural view of a rearrangement reaction system according to a preferred embodiment of the present invention.
Description of the reference numerals
100 vertical reactors, 200 first mixers, 300 second mixers, 400 third mixers, 500 overflow tanks, 600 heat exchangers, 11 cyclohexane steam outlets, 12 defoamers, 21 oleum inlets, 31 mixed liquid inlets of first cyclohexane and cyclohexanone oxime and 41 mixed liquid inlets of second cyclohexane and cyclohexanone oxime.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The utility model provides a rearrangement reaction system, as shown in figure 1, this rearrangement reaction system includes: a vertical reactor 100, a first mixer 200 and a second mixer 300, and a line communicating the vertical reactor 100, the first mixer 200 and the second mixer 300, wherein,
the vertical reactor 100 is used for providing a reaction site for performing Beckmann rearrangement reaction on the mixed solution of cyclohexane and cyclohexanone oxime and oleum to obtain heavy liquor;
the first mixer 200 is connected with the vertical reactor 100, a fuming sulfuric acid inlet 21 is arranged on the first mixer 200, and the first mixer 200 is used for premixing a part of heavy discharged liquid and fuming sulfuric acid to obtain a first premixed liquid;
the second mixer 300 is connected to the vertical reactor 100 and the first mixer 200, a mixed solution inlet 31 for the first cyclohexane and the cyclohexanone oxime is arranged on the second mixer 300, and the second mixer 300 is configured to pre-mix the first pre-mixed solution and the mixed solution for cyclohexane and cyclohexanone oxime to obtain a second pre-mixed solution, and input the second pre-mixed solution to the vertical reactor 100.
The utility model discloses in, through setting up first blender and second blender, can conveniently control and let in the volume ratio of cyclohexanone oxime and oleum in the vertical reactor to can reduce the emergence of side reaction.
The utility model discloses in, it is right the material of vertical reactor does not do the restriction, as long as can provide the reaction site for the reaction to do not take place chemical reaction with reaction raw materials and reaction product can, for example, can be stainless steel equipment, the material is 316L. In addition, the operating conditions of the vertical reactor are not limited, but the operating pressure in the vertical reactor is usually 0.05 to 0.06MPa and the operating temperature is usually 85 to 120 ℃ in order to increase the yield of caprolactam.
The utility model discloses in, will react the raw materials and carry to next reaction unit through the pump between equipment, wherein, do not restrict the model and the operating condition of pump, preferably, the material of pump is 316L, and flow controls at 500 sand-doped 800m generally3The head is usually 80 to 100 m.
In some embodiments of the present invention, in order to increase the number of rearrangement stages to reduce the acid oxime ratio, the rearrangement reaction system further includes a plurality of third mixers 400, the third mixers 400 are arranged in parallel, and the third mixers 400 are connected to the vertical reactor 100 and the first mixer 200, and a mixed liquid inlet 41 of the second cyclohexane and the cyclohexanone oxime is provided on the third mixers 400, and the third mixers 400 are used for premixing the part of the heavy discharged liquid and the mixed liquid of cyclohexane and cyclohexanone oxime to obtain a third premixed liquid, and inputting the third premixed liquid to the vertical reactor 100.
In some embodiments of the present invention, preferably, the rearrangement reaction system comprises 2 to 5 of the third mixers 400.
In some embodiments of the present invention, the first mixer 200, the second mixer 300, and the third mixer 400 are static mixers. The material of the static mixer is not limited, for example, the material can be 316L, the static mixer solves the difficulty of engineering amplification of the Beckmann rearrangement reaction in a solvent vaporization heat transfer mode in the material mixing process, and enhances the microscopic mass transfer of the rearrangement reaction.
In some embodiments of the present invention, the top end of the vertical reactor 100 is provided with a cyclohexane vapor outlet 11 for discharging cyclohexane vapor discharged from the vertical reactor 100. The heat of the solvent rearrangement reaction is removed without a cooling medium, and the heat is taken in a cyclohexane vaporization mode, so that the cyclohexane is recycled. In addition, the cyclohexane steam has high energy grade and can be used as a heat source of other heat utilization devices, thereby achieving the purpose of energy conservation.
In some embodiments of the present invention, a demister 12 is further disposed inside the vertical reactor 100, and the demister 12 is used for refluxing caprolactam entrained in cyclohexane vapor to the vertical reactor 100.
In some embodiments of the present invention, the rearrangement reaction system further comprises an overflow tank 500, and the overflow tank 500 is connected to the vertical reactor 100, and the overflow tank 500 is used for storing the heavy liquid overflowing from the vertical reactor 100. Specifically, the overflow tank can continuously slake and heat up the discharged liquid, so that unreacted cyclohexanone oxime continuously reacts to generate caprolactam sulfate, and some low-boiling-point impurities and residual cyclohexane are distilled away from the top.
In some embodiments of the present invention, in order to match the special structure of the vertical reactor 100 for left-in and right-out, the third mixer 400 and the overflow tank 500 are disposed at both sides of the vertical reactor 100.
In some embodiments of the present invention, the rearrangement reaction system further comprises a heat exchanger 600, the heat exchanger 600 is connected to the first mixer 200 and the second mixer 300, and the heat exchanger 600 is used for heating or cooling the first premixed liquid introduced into the heat exchanger 600. Specifically, the cooling medium of the heat exchanger 600 may be circulating water, and the heating medium may be steam.
The utility model discloses a use method of system in a preferred embodiment includes: as shown in fig. 1, two third mixers 400 are arranged in parallel, and the cyclohexane and cyclohexanone oxime mixed liquor is mixed with the heavy effluent and the first premixed liquor from the third mixer 400 and the second mixer 300 and then enters the vertical reactor 100, wherein the volume ratio (usually 3-5:7) of the cyclohexane and cyclohexanone oxime mixed liquor input into the third mixer 400 (the total amount of the cyclohexane and cyclohexanone oxime mixed liquor) and the second mixer 300 is controlled by a flow meter, wherein the volume ratio of the cyclohexane and cyclohexanone oxime mixed liquor in the third mixer 400 is usually 2-4:1 (it is not necessary to control the volume ratio of the cyclohexane and cyclohexanone oxime mixed liquor in the two third mixers 400 to be 2-4: 1), and the rearrangement liquor overflows from the vertical reactor to the overflow tank as the reaction proceeds. The solvent (cyclohexane) absorbs the heavy heat and is distilled out from the top of the vertical reactor 100. In the whole process, the single tank and the mixer are matched for use, so that multistage rearrangement is realized, the equipment investment is saved, the acid-oxime ratio is reduced, the side reaction is reduced, the yield of caprolactam is improved, the equipment is simplified, the equipment investment is reduced, and the method is suitable for industrial application.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. In the technical idea scope of the present invention, it can be right to the technical solution of the present invention perform multiple simple modifications, including each technical feature combined in any other suitable manner, these simple modifications and combinations should be regarded as the disclosed content of the present invention, and all belong to the protection scope of the present invention.
Claims (9)
1. A rearrangement reaction system, comprising: a vertical reactor (100), a first mixer (200) and a second mixer (300), and a line communicating the vertical reactor (100), the first mixer (200) and the second mixer (300), wherein,
the vertical reactor (100) is used for providing a reaction site for the Beckmann rearrangement reaction of the mixed liquid of the cyclohexane and the cyclohexanone oxime and oleum to obtain heavy liquid;
the first mixer (200) is connected with the vertical reactor (100), a fuming sulfuric acid inlet (21) is arranged on the first mixer (200), and the first mixer (200) is used for premixing a part of heavy discharged liquid and fuming sulfuric acid to obtain a first premixed liquid;
the second mixer (300) is connected with the vertical reactor (100) and the first mixer (200), a mixed solution inlet (31) of the first cyclohexane and the cyclohexanone oxime is arranged on the second mixer (300), the second mixer (300) is used for premixing the first premixed solution and the mixed solution of the cyclohexane and the cyclohexanone oxime to obtain a second premixed solution, and the second premixed solution is input into the vertical reactor (100).
2. The rearrangement reaction system according to claim 1, further comprising a plurality of third mixers (400), wherein the third mixers (400) are arranged in parallel, the third mixers (400) are connected with the vertical reactor (100) and the first mixer (200), a mixed solution inlet (41) of second cyclohexane and cyclohexanone oxime is arranged on the third mixers (400), and the third mixers (400) are used for premixing a part of the rearrangement liquid and the mixed solution of cyclohexane and cyclohexanone oxime to obtain a third premixed solution, and the third premixed solution is input to the vertical reactor (100).
3. The rearrangement reaction system according to claim 2, characterized in that the rearrangement reaction system comprises 2-5 of the third mixers (400).
4. The rearrangement reaction system according to claim 2, wherein the first mixer (200), the second mixer (300), and the third mixer (400) are all static mixers.
5. The rearrangement reaction system according to claim 1, wherein the vertical reactor (100) is provided at a top end thereof with a cyclohexane vapor outlet (11) for discharging cyclohexane vapor discharged from the vertical reactor (100).
6. The rearrangement reaction system according to claim 5, wherein a demister (12) is further disposed inside the vertical reactor (100), and the demister (12) is used for refluxing caprolactam entrained in cyclohexane vapor into the vertical reactor (100).
7. The rearrangement reaction system according to claim 2, characterized in that the rearrangement reaction system further comprises an overflow tank (500), and the overflow tank (500) is connected to the vertical reactor (100), and the overflow tank (500) is used for storing the rearrangement liquid overflowing from the vertical reactor (100).
8. The rearrangement reaction system according to claim 7, wherein the third mixer (400) and the overflow tank (500) are disposed on both sides of the vertical reactor (100).
9. The rearrangement reaction system according to claim 1, further comprising a heat exchanger (600), wherein the heat exchanger (600) is connected to the first mixer (200) and the second mixer (300), and the heat exchanger (600) is used for heating or cooling the first premixed liquid introduced into the heat exchanger (600).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120300946.5U CN214915921U (en) | 2021-02-02 | 2021-02-02 | Rearrangement reaction system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202120300946.5U CN214915921U (en) | 2021-02-02 | 2021-02-02 | Rearrangement reaction system |
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| CN214915921U true CN214915921U (en) | 2021-11-30 |
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