CN114602393A - Device and method for removing cineole in p-cymene through continuous reaction - Google Patents
Device and method for removing cineole in p-cymene through continuous reaction Download PDFInfo
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- CN114602393A CN114602393A CN202210277676.XA CN202210277676A CN114602393A CN 114602393 A CN114602393 A CN 114602393A CN 202210277676 A CN202210277676 A CN 202210277676A CN 114602393 A CN114602393 A CN 114602393A
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Abstract
The invention discloses a device and a method for removing cineole in p-cymene by continuous reaction, and the device comprises a reaction tower, wherein the top of the reaction tower is provided with a feed pipe, the feed pipe is connected with a feed liquid input piece, and the bottom of the reaction tower is provided with a discharge pipe; the discharge pipe is connected with a second pump through a pipeline, and the liquid outlet end of the second pump is connected with the rectifying tower through a pipeline; the reaction tower comprises a fixed bed reactor and a tower top connected to the top of the fixed bed reactor; according to the invention, cineole in p-cymene is removed through continuous reaction, 1, 8-cineole is hydrolyzed and converted into alcohol with high boiling point by a crude p-cymene containing cineole through a fixed bed reactor by an acid catalytic isomerization method, so that the alcohol is easy to separate from p-cymene through rectification, the content of cineole in the obtained p-cymene meets the standard, and the production quality and efficiency are improved.
Description
Technical Field
The invention relates to the technical field of p-cymene cineole removal, in particular to a device and a method for removing cineole in p-cymene through continuous reaction.
Background
P-cymene, also known as p-cymene, known by the chemical name 1-methyl-4-isopropylbenzene, is a colorless, transparent, aromatic liquid that is present in a variety of essential oils. The p-cymene is also a derivative of turpentine oil which is a bulk product of forestation in China, is an important organic synthesis intermediate, and has wide application. It can be directly used in soft drink, ice food, candy, chewing gum, flavoring agent, and used for preparing essence for cosmetic, soap and detergent; can be made into soft capsule, and can be used for relieving cough, eliminating phlegm, and treating chronic tracheitis; can be used for synthesizing various polycyclic musk perfumes and other perfumes containing aromatic rings, medicines, herbicides, bactericides and the like.
In general, p-cymene is industrially prepared from dipentene through disproportionation reaction and rectification. Because the industrial dipentene carries a small amount of cineole (about 1.5 percent, mainly 1, 8-cineole) and is carried into finished product p-cymene in the reaction and rectification processes, the fragrance of the product on the p-cymene is easily influenced, and part of enterprises with high requirements on the fragrance have high requirements on the content of the cineole, the content of the cineole needs to be controlled below 0.1 percent, and because the boiling point of the 1, 8-cineole is 176-177 ℃ which is the same as the boiling point of the p-cymene (the boiling point is 177.1 ℃), the removal of the cineole through the reaction has great significance.
Aiming at the problems, a device and a method for continuously reacting and removing cineole in p-cymene are provided.
Disclosure of Invention
The invention aims to provide a device and a method for continuously reacting and removing cineole in p-cymene, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a device for removing cineole in p-cymene by continuous reaction comprises a reaction tower, wherein a feed pipe is arranged at the top of the reaction tower and connected with a feed liquid input piece, and a discharge pipe is arranged at the bottom of the reaction tower;
the crude product containing eucalyptol can input p-cymene from a feeding pipe, and then the 1, 8-eucalyptol is subjected to hydrolysis reaction to be converted into alcohol with high boiling point after the treatment of isomerization reaction in a reaction tower;
the discharge pipe is connected with a second pump through a pipeline, and the liquid outlet end of the second pump is connected with the rectifying tower through a pipeline;
the rectifying tower can carry out rectification separation on the feed liquid after reaction in the reaction tower, so that cineole contained in p-cymene can be separated from p-cymene, and p-cymene with the cineole content lower than 0.1% is obtained;
the reaction tower comprises a fixed bed reactor and a tower top connected to the top of the fixed bed reactor, two groups of catalyst layers are arranged in the fixed bed reactor, and a shunt ring arranged on the inner wall of the fixed bed reactor is arranged in a cavity between the two groups of catalyst layers;
a flow distribution disc is arranged in the tower top, the top of the flow distribution disc is connected with an input pipe, the top of the input pipe is connected with a feeding pipe through a rotary joint, and the bottom of the flow distribution disc is connected with a flow distribution pipe communicated with the inner cavity of the input pipe;
a driving piece for driving the shunting plate to rotate is arranged on the fixed bed reactor;
the top of the catalytic layer arranged at one side close to the top of the tower is provided with a cover plate, and the bottom of the diverter disc is connected with a rolling pressing piece for pressing the cover plate.
Preferably, the driving piece includes the gear, diverter plate inner wall top be connected with gear engagement's ring gear, the actuating lever is connected to gear top axle head, the top of the tower inner wall is equipped with and is used for the stable pivoted fixed plate of actuating lever, the top of the tower top is installed and is used for driving actuating lever pivoted drive device.
Preferably, the inner wall of the tower top is provided with an annular groove for stable rotation of the diverter tray.
Preferably, the rolling pressing piece comprises a pressing roller, the two ends of the pressing roller are rotatably connected with mounting blocks, the mounting blocks are close to one side of the splitter plate and fixedly connected with a sliding column, the sliding column is slidably arranged in a fixed cylinder, a spring for connecting the sliding column is arranged in the fixed cylinder, and one end of the fixed cylinder, far away from the splitter plate, is fixedly connected with the splitter plate.
Preferably, the compression roller contacts with the apron top, the apron top is equipped with the spacing ring of connection at the fixed bed reactor inner wall, the spacing ring bottom evenly is provided with a plurality of circular slot, install the spring in the circular slot, the circular slot one end connection apron is kept away from to the spring.
Preferably, a set of catalysis layer that sets up in the bottom includes two sets of fixed nets, be equipped with the catalyst between the fixed net, a set of catalysis layer that sets up at the top includes a set of fixed net, be equipped with the catalyst between fixed net and the apron, be equipped with on the fixed bed reactor and be arranged in with two sets of catalysis layer catalyst exhaust discharge pipe, still be equipped with a plurality of temperature measurement mouths to the fixed bed reactor inner chamber temperature measurement on the fixed bed reactor, the catalyst includes strong acid ion exchange resin.
Preferably, two groups of flow dividing rings are arranged between the two groups of catalyst layers, and the inner wall of each flow dividing ring is connected with a plurality of groups of flow dividing plates which are uniformly arranged.
Preferably, be equipped with the heating chamber between fixed bed reactor outer wall and the inner wall, the intracavity is equipped with the coil pipe, fixed bed reactor bottom one side is equipped with the heat source input port of being connected with coil pipe feed liquor end, the fixed bed reactor top is equipped with the heat source delivery outlet of being connected with coil pipe play liquid end.
Preferably, the feed liquid input piece includes the head tank, head tank play liquid end passes through the first pump machine of pipe connection, first pump machine play liquid end passes through the pipe connection inlet pipe.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, cineole in p-cymene is removed through continuous reaction, a catalyst (which can be selected from strong acid ion exchange resin) in a fixed bed reactor can react with cineole to convert the cineole into alcohol with high boiling point, so that the cineole is easy to separate from p-cymene through rectification, the cineole content in the p-cymene obtained after rectification meets the standard, and the production quality and efficiency are improved;
according to the invention, the distribution plate can uniformly feed the material liquid into the catalyst layer at the top, so that the material liquid can uniformly react with the catalyst, and in the rotating process of the distribution plate, the pressing roller repeatedly extrudes the cover plate to uniformly compress the catalyst;
according to the invention, the splitter plate is arranged between the two catalytic layers, so that the feed liquid flowing out of the top catalytic layer can be dispersed and then fall onto the bottom catalytic layer for secondary reaction after passing through the splitter plate, the reaction is sufficient, and the subsequent rectification of the feed liquid is facilitated.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a schematic view of the structure inside a fixed-bed reactor in the present invention.
Fig. 3 is a schematic structural view of a flow distribution plate according to the present invention.
FIG. 4 is a schematic view of the structure inside the column top in the present invention.
Fig. 5 is a schematic structural view of the bottom of the diverter tray in the present invention.
FIG. 6 is a diagram showing the equations of the chemical reaction in the present invention.
In the figure: 11-raw material tank, 12-first pump, 13-reaction tower, 14-feed pipe, 15-discharge pipe, 16-second pump, 17-rectification tower, 18-fixed bed reactor, 19-catalyst, 20-discharge pipe, 21-heat source input port, 22-fixed net, 23-splitter ring, 24-temperature measuring port, 25-cover plate, 26-limit ring, 27-splitter plate, 28-tower top, 29-splitter plate, 30-toothed ring, 31-gear, 32-drive rod, 33-fixed plate, 34-drive equipment, 35-input pipe, 36-rotary joint, etc, 37-shunt tubes, 38-fixed cylinders, 39-sliding columns, 40-mounting blocks, 41-press rollers.
Detailed Description
Referring to fig. 1-5, in an embodiment of the present invention, an apparatus for continuously reacting and removing cineole from p-cymene includes a reaction tower 13, a feed pipe 14 is disposed at the top of the reaction tower 13, the feed pipe 14 is connected to a feed liquid input member, and a discharge pipe 15 is disposed at the bottom of the reaction tower 13; the crude product containing eucalyptol can input p-cymene from a feeding pipe 14, and then after isomerization reaction treatment is carried out in a reaction tower 13, 1, 8-eucalyptol is subjected to hydrolysis reaction and converted into alcohol with high boiling point;
the discharge pipe 15 is connected with a second pump 16 through a pipeline, and the liquid outlet end of the second pump 16 is connected with a rectifying tower 17 through a pipeline; the rectifying tower 17 can carry out rectification separation on the feed liquid after reaction in the reaction tower 13, so that cineole contained in p-cymene can be separated from p-cymene, and p-cymene with the cineole content lower than 0.1% is obtained; the obtained p-cymene has eucalyptol content meeting the standard, and has improved production quality and efficiency.
The reaction tower 13 comprises a fixed bed reactor 18 and a tower top 28 connected to the top of the fixed bed reactor 18, two groups of catalyst layers are arranged in the fixed bed reactor 18, and a shunt ring 23 arranged on the inner wall of the fixed bed reactor 18 is arranged in a cavity between the two groups of catalyst layers;
the synthesis of p-cymene by catalytic dehydrogenation of dipentene usually comprises a gas phase method and a liquid phase method, the gas phase method has been industrialized abroad, the used dehydrogenation catalyst is mainly a catalyst loaded with noble metals such as Pd and R, the yield is over 80 percent, but the catalyst used in the process is very expensive and the production cost is high; the catalysts used in domestic gas phase dehydrogenation mainly comprise CrO3-Al203, Cu-Cr-Al203, 0.5 percent Pd-C and the like; catalysts used in liquid phase reactions have also been reported in the literature, such as 5% Pd impregnated activated carbon, Raney-Ni, nickel formate, copper formate-nickel formate, and the like. The catalyst for dehydrogenating dipentene to prepare p-cymene includes mainly Ni-series catalyst and noble metal catalyst. However, the nickel-based catalyst has the disadvantages of high reaction temperature, long reaction time, high requirement on reaction equipment, harsh operation conditions and poor selectivity in the process of catalyzing the dehydrogenation reaction of dipentene.
In the application, strong acid ion exchange resin (such as NKC-9, CD500 and the like) can be filled in the catalytic layer, crude p-cymene containing cineole is pumped into the fixed bed reactor 18 by a pump, isomerization reaction is carried out in the catalytic layer in the fixed bed reactor 18 at the speed of 0.1-1h < -1 > of airspeed, the reaction temperature is controlled at 30-80 ℃ and the normal pressure is realized; a plurality of catalytic layers are arranged to continuously react the cymene;
a distribution tray 29 is arranged in the tower top 28, the top of the distribution tray 29 is connected with an input pipe 35, the top of the input pipe 35 is connected with the feeding pipe 14 through a rotary joint 36, and the bottom of the distribution tray 29 is connected with a distribution pipe 37 communicated with the inner cavity of the input pipe 35;
a driving piece for driving the diverter disc 29 to rotate is arranged on the fixed bed reactor 18;
a cover plate 25 is arranged at the top of the catalytic layer close to one side of the tower top 28, and a rolling pressing piece for pressing the cover plate 25 is connected to the bottom of the diversion plate 29.
The driving part comprises a gear 31, the top of the inner wall of the diverter tray 29 is connected with a toothed ring 30 meshed with the gear 31, the shaft end of the top of the gear 31 is connected with a driving rod 32, the inner wall of the tower top 28 is provided with a fixing plate 33 used for the driving rod 32 to stably rotate, and the top of the tower top 28 is provided with a driving device 34 used for driving the driving rod 32 to rotate; an annular groove for stable rotation of the diverter disc 29 is formed in the inner wall of the tower top 28; in practical use, the driving device drives the driving rod 32 to rotate, so that the gear 31 rotates, the gear 31 can drive the toothed ring 30 to rotate, so that the diverter plate 29 stably rotates in the annular groove, and the diverter pipe 37 rotates along with the diverter plate 29, so that the feed liquid input in the input pipe 35 can be uniformly output to the catalyst layer.
The rolling pressing piece comprises a pressing roller 41, two ends of the pressing roller 41 are rotatably connected with mounting blocks 40, one side, close to the diverter tray 29, of each mounting block 40 is fixedly connected with a sliding column 39, each sliding column 39 is arranged in a fixed cylinder 38 in a sliding mode, a spring for connecting the sliding columns 39 is arranged in the fixed cylinder 38, and one end, far away from the sliding columns 39, of the fixed cylinder 38 is fixedly connected with the diverter tray 29; the diverter disc 29 rotates and simultaneously drives the pressing roller 41 to rotate, and the pressing roller 41 rolls on the surface of the cover plate 25.
The compression roller 41 is in contact with the top of the cover plate 25, the top of the cover plate 25 is provided with a limiting ring 26 connected to the inner wall of the fixed bed reactor 18, the bottom of the limiting ring 26 is uniformly provided with a plurality of circular grooves, springs are arranged in the circular grooves, and one ends, far away from the circular grooves, of the springs are connected with the cover plate 25; when catalyst in the catalysis layer is filled more fully, apron 25 contact spacing ring 26, slip post 39 shrink in solid fixed cylinder 38, the catalyst is after reacting with the feed liquid, the content appears reducing, or make the catalyst of filling everywhere the reaction degree is not in the interim sunken appears, diverter plate 29 can drive compression roller 41 extrusion apron 25 in the pivoted, apron 25 extrusion catalyst, extrude apron 25 repeatedly and can be even and compress tightly the catalyst, the feed liquid of being convenient for can effectively react through the catalysis layer.
A set of catalysis layer that sets up in the bottom includes two sets of fixed nets 22, be equipped with catalyst 19 between the fixed net 22, a set of catalysis layer that sets up at the top includes a set of fixed net 22, be equipped with catalyst 19 between fixed net 22 and the apron 25, be equipped with on the fixed bed reactor 18 and be arranged in with two sets of catalysis layer catalyst 19 exhaust discharge pipe 20, still be equipped with a plurality of temperature measurement mouths 24 to the temperature measurement of fixed bed reactor 18 inner chamber on the fixed bed reactor 18, catalyst 19 includes strong acid ion exchange resin.
Two groups of flow distribution rings 23 are arranged between the two groups of catalyst layers, and the inner wall of the flow distribution ring 23 is connected with a plurality of groups of flow distribution plates 27 which are uniformly arranged; as shown in fig. 3, a gap is left between the splitter plates 27 for the passage of the feed liquid, and the feed liquid flowing out from the top catalytic layer is dispersed, so that the feed liquid uniformly enters the bottom catalytic layer.
A heating cavity is arranged between the outer wall and the inner wall of the fixed bed reactor 18, a coil is arranged in the heating cavity, a heat source input port 21 connected with the liquid inlet end of the coil is arranged on one side of the bottom of the fixed bed reactor 18, and a heat source output port connected with the liquid outlet end of the coil is arranged at the top of the fixed bed reactor 18; the heat source may be heat conducting oil or hot water.
The feed liquid input part comprises a feed liquid tank 11, the liquid outlet end of the feed liquid tank 11 is connected with a first pump 12 through a pipeline, and the liquid outlet end of the first pump 12 is connected with a feeding pipe 14 through a pipeline; crude p-cymene can be stored in feed tank 11.
Referring to fig. 1-6, when the catalytic layer is used, the catalytic layer can be filled with strong acid ion exchange resin (such as NKC-9, CD500, etc.), crude p-cymene containing cineole is loaded in the raw material tank 11, the coil pipe in the heating cavity of the fixed bed reactor 18 is led into the heat source, the temperature of the inner cavity of the reaction tower 13 is kept at 30-80 ℃, the temperature is kept at normal pressure, the first pump 12 works to pump the material liquid in the raw material tank 11 into the reaction tower 13, and the material liquid enters the input pipe 35 through the material inlet pipe 14;
the driving device 34 works to drive the driving rod 32 to rotate, so that the gear 31 drives the diverter disc 29 to rotate in the annular groove, the diverter pipes 37 evenly distribute the feed liquid into the catalytic layer at the top, and the feed liquid performs isomerization reaction in the catalytic layer;
the diverter disc 29 drives the press roller 41 to press the cover plate 25 while rotating, and when the catalyst in the top catalytic layer is reduced or is unevenly distributed, the press roller 41 repeatedly presses the cover plate 25 to evenly compress the catalyst;
after reacting in the catalyst layer at the top, the feed liquid enters the catalyst layer at the bottom for secondary reaction through the dispersion of the flow distribution plate 27;
the cineole reacts in the catalyst layer to be converted into alcohol with high boiling point, then the feed liquid is input into the rectifying tower 17, and the cineole after reaction is easy to separate from p-cymene through rectification.
Claims (10)
1. A device for removing cineole in p-cymene by continuous reaction comprises a reaction tower (13), wherein a feed pipe (14) is arranged at the top of the reaction tower (13), the feed pipe (14) is connected with a feed liquid input piece, and a discharge pipe (15) is arranged at the bottom of the reaction tower (13);
the method is characterized in that: the discharge pipe (15) is connected with a second pump (16) through a pipeline, and the liquid outlet end of the second pump (16) is connected with a rectifying tower (17) through a pipeline;
the reaction tower (13) comprises a fixed bed reactor (18) and a tower top (28) connected to the top of the fixed bed reactor (18), two groups of catalyst layers are arranged in the fixed bed reactor (18), and a shunt ring (23) arranged on the inner wall of the fixed bed reactor (18) is arranged in a cavity between the two groups of catalyst layers;
a shunting disc (29) is arranged in the tower top (28), the top of the shunting disc (29) is connected with an input pipe (35), the top of the input pipe (35) is connected with a feeding pipe (14) through a rotary joint (36), and the bottom of the shunting disc (29) is connected with a shunting pipe (37) communicated with the inner cavity of the input pipe (35);
a driving piece for driving the diverter disc (29) to rotate is arranged on the fixed bed reactor (18);
a cover plate (25) is arranged at the top of the catalytic layer close to one side of the tower top (28), and a rolling pressing piece for pressing the cover plate (25) is connected to the bottom of the diverter disc (29).
2. The device for continuously removing cineole from p-cymene according to claim 1, wherein: the driving piece includes gear (31), diverter plate (29) inner wall top is connected with ring gear (30) with gear (31) meshing, actuating lever (32) is connected to gear (31) top axle head, top of the tower (28) inner wall is equipped with and is used for actuating lever (32) to stabilize pivoted fixed plate (33), top of the tower (28) top is installed and is used for driving actuating lever (32) pivoted drive arrangement (34).
3. The device for continuously removing cineole from p-cymene according to claim 1, wherein: and an annular groove for stable rotation of the diverter disc (29) is formed in the inner wall of the tower top (28).
4. The device for continuously removing cineole from p-cymene according to claim 1, wherein: the rolling pressing piece comprises a pressing roller (41), two ends of the pressing roller (41) are rotatably connected with an installation block (40), the installation block (40) is close to one side of the diverter disc (29) and is fixedly connected with a sliding column (39), the sliding column (39) is slidably arranged in a fixed cylinder (38), a spring used for connecting the sliding column (39) is arranged in the fixed cylinder (38), and the fixed cylinder (38) is far away from one end of the sliding column (39) and is fixedly connected with the diverter disc (29).
5. The device for continuously removing cineole from p-cymene according to claim 4, wherein: compression roller (41) and apron (25) top contact, apron (25) top is equipped with spacing ring (26) of connection at fixed bed reactor (18) inner wall, spacing ring (26) bottom evenly is provided with a plurality of circular slot, install the spring in the circular slot, circular slot one end connection apron (25) are kept away from to the spring.
6. The device for continuously removing cineole from p-cymene according to claim 1, wherein: a set of catalysis layer that sets up in the bottom includes two sets of fixed networks (22), be equipped with catalyst (19) between fixed network (22), a set of catalysis layer that sets up at the top includes a set of fixed network (22), be equipped with catalyst (19) between fixed network (22) and apron (25), be equipped with on fixed bed reactor (18) and be arranged in catalyst (19) exhaust discharge pipe (20) in two sets of catalysis layers, still be equipped with temperature measurement mouth (24) of a plurality of temperature measurements to fixed bed reactor (18) inner chamber on fixed bed reactor (18), catalyst (19) include strong acid ion exchange resin.
7. The device for continuously removing cineole from p-cymene according to claim 6, wherein: two groups of flow distribution rings (23) are arranged between the two groups of catalyst layers, and the inner wall of each flow distribution ring (23) is connected with a plurality of groups of flow distribution plates (27) which are uniformly arranged.
8. The device for continuously removing cineole from p-cymene according to claim 1, wherein: be equipped with the heating chamber between fixed bed reactor (18) outer wall and the inner wall, the intracavity is equipped with the coil pipe, fixed bed reactor (18) bottom one side is equipped with heat source input port (21) of being connected with coil pipe feed liquor end, fixed bed reactor (18) top is equipped with the heat source delivery outlet of being connected with coil pipe liquid outlet end.
9. The device for continuously removing cineole from p-cymene according to claim 1, wherein: the feed liquid input piece comprises a feed tank (11), the liquid outlet end of the feed tank (11) is connected with a first pump (12) through a pipeline, and the liquid outlet end of the first pump (12) is connected with a feeding pipe (14) through a pipeline.
10. A method of using the apparatus for continuously reacting and removing cineole from p-cymene according to any one of claims 1 to 9, comprising the steps of:
step one, crude p-cymene containing cineole is filled in a raw material tank (11), a coil pipe in a heating cavity on a fixed bed reactor (18) is introduced with a heat source, the temperature of the inner cavity of a reaction tower (13) is kept at 30-80 ℃, a first pump (12) works to pump the material liquid in the raw material tank (11) into the reaction tower (13), and the material liquid enters an input pipe (35) through a material inlet pipe (14);
step two, the driving device (34) works to drive the driving rod (32) to rotate, so that the gear (31) drives the flow distribution disc (29) to rotate in the annular groove, the flow distribution pipe (37) uniformly distributes the material liquid into the catalyst layer at the top, and the material liquid performs an isomerization reaction in the catalyst layer;
step three, the diverter disc (29) can drive the press roller (41) to extrude the cover plate (25) while rotating, and when the catalyst in the catalytic layer at the top is reduced or is unevenly distributed, the press roller (41) repeatedly extrudes the cover plate (25) to evenly press the catalyst;
step four, after the reaction of the feed liquid in the catalytic layer at the top, the feed liquid enters the catalytic layer at the bottom through the dispersion of the flow distribution plate (27) to carry out the secondary reaction;
step five, reacting the cineole in the catalytic zone to convert into alcohol with high boiling point, inputting the feed liquid into a rectifying tower (17), and rectifying and separating the cineole after reaction from p-cymene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210277676.XA CN114602393B (en) | 2022-03-21 | 2022-03-21 | Device and method for removing eucalyptol in p-cymene through continuous reaction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210277676.XA CN114602393B (en) | 2022-03-21 | 2022-03-21 | Device and method for removing eucalyptol in p-cymene through continuous reaction |
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| CN114602393B CN114602393B (en) | 2023-05-26 |
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