CN210145530U - Equipment for producing acetyl n-propanol by continuous hydrogenation of 2-methylfuran - Google Patents
Equipment for producing acetyl n-propanol by continuous hydrogenation of 2-methylfuran Download PDFInfo
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- CN210145530U CN210145530U CN201920755574.8U CN201920755574U CN210145530U CN 210145530 U CN210145530 U CN 210145530U CN 201920755574 U CN201920755574 U CN 201920755574U CN 210145530 U CN210145530 U CN 210145530U
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Abstract
The utility model relates to the field of chemical industry, in particular to a device for producing acetyl n-propanol by continuous hydrogenation of a 2-methylfuran fixed bed. The mixed mixture of water, solvent and 2-methylfuran enters a reactor through a metering pump and metered hydrogen, the mixture passes through an atomizer, certain temperature and pressure are kept, hydrogenation reaction is carried out in a fixed bed under an atomization state, reaction liquid is directly discharged into a gas-liquid separator, the discharged material liquid is in a gas-liquid mixing form, after the material liquid enters the gas-liquid separator, the liquid part is discharged from the bottom of the gas-liquid separator, and after the material liquid is neutralized by a secondary reactor, subsequent distillation and rectification treatment are carried out; the hydrogen gas on the upper part of the gas-liquid separator passes through a condenser, the residual liquid in the reaction liquid is further cooled and remained in a liquid phase, and the non-condensable hydrogen gas enters a hydrogen compressor through a hydrogen return pipe for recycling; the feeding amount is controlled by a metering pump, and the discharging amount is controlled by the liquid level in the gas-liquid separator to keep a balanced state.
Description
Technical Field
The utility model relates to the field of chemical industry, in particular to equipment for producing acetyl-n-propanol by continuous hydrogenation of 2-methylfuran.
Background
Acetyl n-propanol is an important medical intermediate, is a main intermediate of anti-AIDS drugs efavirenz and irinotecan, is used for antimalarial drugs chloroquine phosphate, can also be used for producing vitamin B1 and the like, and is also an intermediate of bactericide cyprodinil and cyproconazole
At present, the production process of the acetyl-n-propanol mainly comprises 3 types: the fine organic chemical raw materials and the intermediate handbook (Xuke-master edition) relate to two types: the method has the advantages that the method is a 2-methyl furan palladium chloride catalytic hydrogenation method, the reaction period is long (about 120 hours per batch), and the industrial efficiency is low; the gamma-butyrolactone method has high requirements on reaction temperature (350-;
thirdly, the method for producing the acetyl-n-propanol by intermittently catalyzing and hydrogenating the 2-methylfuran in the Chinese patent CN102140058A by using a palladium-carbon catalyst has the advantages of simple operation, convenient control and mild reaction conditions, and is suitable for industrial production.
SUMMERY OF THE UTILITY MODEL
The purpose of the utility model is that: in order to provide a better device and a better method for producing acetyl-n-propanol by continuously hydrogenating 2-methylfuran, the specific aim is seen in a plurality of substantial technical effects of the concrete implementation part.
In order to achieve the purpose, the utility model adopts the following technical proposal:
2-methyl furan continuous hydrogenation production acetyl n-propanol production equipment, characterized in that, the production equipment comprises a water metering tank 1, a 2-methyl furan metering tank 2, a solvent metering tank 3, the pipeline below the water metering tank 1, the 2-methyl furan metering tank 2, the solvent metering tank 3 is connected with a stirring part, the stirring part comprises a first stirring and mixing device 10 and a second stirring and mixing device 11, the stirred material can come out from the first stirring and mixing device 10 and the second stirring and mixing device 11 and then enter a first-stage reactor 9 through a pipeline and a water phase flowmeter 12, the pipeline below the first-stage reactor extends out and is connected with a gas-liquid separator 8, the upper part of the first-stage reactor comprises a hydrogen gas return port 4, the pipeline extending out of the hydrogen gas return port 4 is connected with a hydrogen compressor and then is connected with a condenser 5, the gas-liquid separator 8 is connected below the condenser, the pipeline extending out of the gas-liquid separator 8 is connected with a secondary reactor 6, and the secondary reactor is connected with a crude propanol metering tank 7.
The utility model discloses a further technical scheme lies in, the condenser be water cooling plant, contain cold water inlet and cold water outlet on it, contain the gas outlet above it, the hydrogen press is being connected to this gas outlet.
The utility model discloses a further technical scheme lies in, first order reactor 9 contain first order reactor casing, this first order reactor casing top contains atomizer 901, and atomizer 901 below is wire mesh distributor 903, wire mesh distributor below be fixed bed 905, placed catalyst 906 on the fixed bed, the fixed bed below is accepted by stainless wire net 907, the stainless wire net below is stainless steel sieve plate 908.
The utility model discloses a further technical scheme lies in, the fixed bed in the first order reactor on include the teletransmission thermometer, can wireless communication's temperature sensor.
The utility model discloses a further technical scheme lies in, secondary reactor 6 contain the casing, the casing top contains built-in stainless steel water cap 601, the inside ion exchange resin 604 that contains of casing contains top stainless steel net 602 and top stainless steel sieve plate 603 on the casing, top stainless steel net 602 is in top stainless steel sieve plate 603 top, ion exchange resin 604 below contains below stainless steel net 605 and below stainless steel sieve plate 606, below stainless steel net 605 is on below stainless steel sieve plate 606.
The production method for producing the acetyl-n-propanol by continuously hydrogenating the 2-methylfuran is characterized in that a mixture of uniformly mixed water, a solvent and the 2-methylfuran enters a reactor through a metering pump and a metered hydrogen block, passes through an atomizer, keeps a certain temperature and pressure, performs hydrogenation reaction in a fixed bed in an atomization state, directly discharges reaction liquid into a gas-liquid separator, discharges discharged feed liquid in a gas-liquid mixing form, discharges a liquid part from the bottom of the gas-liquid separator after the feed liquid enters the gas-liquid separator, neutralizes the liquid part through a secondary reactor, and performs subsequent distillation and rectification treatment; the hydrogen gas on the upper part of the gas-liquid separator passes through a condenser, the residual liquid in the reaction liquid is further cooled and remained in a liquid phase, and the non-condensable hydrogen gas enters a hydrogen compressor through a hydrogen return pipe for recycling; wherein the feeding amount is controlled by a metering pump, and the discharging amount is controlled by the liquid level in the gas-liquid separator, so that the feeding amount and the discharging amount are kept in a balanced state.
The further technical proposal of the utility model is that the first stirring and mixing device 10 and the second stirring and mixing device 11 are used as material mixing devices, the material mixing kettle is composed of two reaction kettles with completely the same function, when one kettle feeds materials into the reaction kettle, the other kettle can carry out material mixing operation, the two kettles are switched back and forth, and the continuous material of continuous reaction is kept;
the reaction device is not provided with a fixed bed, an atomization device is arranged at the inlet of the fixed bed, when hydrogen and liquid raw materials enter the atomization device, reaction liquid is atomized under the injection action of the hydrogen, and then uniformly enters the fixed bed to carry out hydrogenation reaction after passing through a distributor, and the reaction liquid directly enters a gas-liquid separator behind the reaction liquid; the hydrogen returning device is controlled by a pressure transmitter arranged on the gas-liquid separator and an automatic regulating valve connected with the gas-liquid separator and the condenser to judge whether hydrogen is required to be returned or not, when the pressure in the gas-liquid separator reaches a certain pressure, the automatic regulating valve is automatically opened, and the hydrogen returning gas enters the hydrogen compressor through the condenser for recycling; a gas-liquid separation device: gas in the gas-liquid separator is recycled through the hydrogen back-off device, liquid is discharged from the bottom of the gas-liquid separator, and the discharging speed is controlled through the linkage of the liquid level height and the discharging self-regulating valve, so that the balance of feeding and discharging in the reaction is ensured.
The further technical proposal of the utility model is that the solvent is one or more of methanol, ethanol, isopropanol, acetone and 2-methyl tetrahydrofuran, and the main function is to ensure that the water phase and the organic phase are uniformly mixed into a uniform phase before the reactor is removed.
The utility model discloses a further technical scheme lies in, the catalyst is palladium metal catalyst, and the essential element is palladium nitrate and resin carrier.
Adopt above technical scheme the utility model discloses, for prior art have following beneficial effect: the process has the advantages that the novel catalyst is used, so that the reaction can be carried out in a fixed bed for continuous hydrogenation reaction, the treatment links before and after the operation of a single kettle are omitted, hydrochloric acid is removed, the subsequent neutralization and filtration processes are omitted, the time is greatly saved, the efficiency is improved, hydrogen in the reaction can be recycled, the hydrogen loss is greatly reduced, and the pollution to the atmosphere caused by the discharge of hydrogen waste gas into the air is reduced.
Drawings
For further explanation of the present invention, reference is made to the following description taken in conjunction with the accompanying drawings:
FIG. 1 is a schematic structural view of the utility model;
FIG. 2 is a schematic diagram of a first-stage reactor of the utility model;
FIG. 3 is a top view of the structure of the first-stage reactor of the utility model;
FIG. 4 is a schematic diagram of the structure of a two-stage reactor;
FIG. 5 is a flow diagram of a fixed bed hydrogenation process line;
wherein: 1. a water metering tank; 2.2-methylfuran metering tank; 3. a solvent metering tank; 4. a hydrogen return port; 5. a condenser; 6. a secondary reactor; 7. a metering tank for a crude propanol product; 8. a gas-liquid separator; 9. a first stage reactor; 10. a first stirring and mixing device; 11. a second stirring and mixing device; 12. a water phase flow meter; 13. a hydrogen press. 901. An atomizer; 902. an atomizer buffer space; 903. a wire mesh distributor; 904. a remote thermometer; 905. a fixed bed; 906. a catalyst; 907. a stainless steel wire mesh; 908. a stainless steel sieve plate; 601. a stainless steel water cap is arranged inside; 602. an upper stainless steel wire mesh; 603. a stainless steel sieve plate is arranged above the screen; 604. an ion exchange resin; 605. a lower stainless steel wire mesh; lower stainless steel screen deck 606.
Detailed Description
The present invention will be further explained with reference to the accompanying drawings and embodiments, which are to be understood as illustrative only and not limiting the scope of the invention. In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "top", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, as they may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The patent provides a plurality of parallel schemes, and different expressions belong to an improved scheme based on a basic scheme or a parallel scheme. Each solution has its own unique features.
2-methyl furan continuous hydrogenation production acetyl n-propanol production equipment, characterized in that, the production equipment comprises a water metering tank 1, a 2-methyl furan metering tank 2, a solvent metering tank 3, the pipeline below the water metering tank 1, the 2-methyl furan metering tank 2, the solvent metering tank 3 is connected with a stirring part, the stirring part comprises a first stirring and mixing device 10 and a second stirring and mixing device 11, the stirred material can come out from the first stirring and mixing device 10 and the second stirring and mixing device 11 and then enter a first-stage reactor 9 through a pipeline and a water phase flowmeter 12, the pipeline below the first-stage reactor extends out and is connected with a gas-liquid separator 8, the upper part of the first-stage reactor comprises a hydrogen gas return port 4, the pipeline extending out of the hydrogen gas return port 4 is connected with a hydrogen compressor and then is connected with a condenser 5, the gas-liquid separator 8 is connected below the condenser, the pipeline extending out of the gas-liquid separator 8 is connected with a secondary reactor 6, and the secondary reactor is connected with a crude propanol metering tank 7. The technical scheme of the invention has the following substantial technical effects and the realization process thereof;
the utility model discloses a further technical scheme lies in, the condenser be water cooling plant, contain cold water inlet and cold water outlet on it, contain the gas outlet above it, the hydrogen press is being connected to this gas outlet.
The utility model discloses a further technical scheme lies in, first order reactor 9 contain first order reactor casing, this first order reactor casing top contains atomizer 901, and atomizer 901 below is wire mesh distributor 903, wire mesh distributor below be fixed bed 905, placed catalyst 906 on the fixed bed, the fixed bed below is accepted by stainless wire net 907, the stainless wire net below is stainless steel sieve plate 908.
The utility model discloses a further technical scheme lies in, the fixed bed in the first order reactor on include the teletransmission thermometer, can wireless communication's temperature sensor.
The utility model discloses a further technical scheme lies in, secondary reactor 6 contain the casing, the casing top contains built-in stainless steel water cap 601, the inside ion exchange resin 604 that contains of casing contains top stainless steel net 602 and top stainless steel sieve plate 603 on the casing, top stainless steel net 602 is in top stainless steel sieve plate 603 top, ion exchange resin 604 below contains below stainless steel net 605 and below stainless steel sieve plate 606, below stainless steel net 605 is on below stainless steel sieve plate 606.
Key production device introduction:
1. the material mixing device comprises: the mixing kettle consists of two reaction kettles with completely identical functions, when one kettle feeds materials into the reaction kettle, the other kettle can carry out mixing operation, and the two kettles are switched back and forth to keep continuous reaction.
2. A reaction device: the device mainly comprises a fixed bed, wherein an atomization device is arranged at the inlet of the fixed bed, when hydrogen and liquid raw materials enter the atomization device, reaction liquid is atomized under the injection action of the hydrogen, and then evenly enters the fixed bed to perform hydrogenation reaction after passing through a distributor, and the reaction liquid directly enters a gas-liquid separator behind the fixed bed.
3. A hydrogen returning device: the pressure transmitter arranged on the gas-liquid separator and the automatic regulating valve linked with the gas-liquid separator and the condenser control whether hydrogen return is needed, when the pressure in the gas-liquid separator reaches a certain pressure, the automatic regulating valve automatically opens, and the hydrogen return gas enters the hydrogen compressor through the condenser for recycling;
4. a gas-liquid separation device: gas in the gas-liquid separator is recycled through the hydrogen back-off device, liquid is discharged from the bottom of the gas-liquid separator, and the discharging speed is controlled through the linkage of the liquid level height and the discharging self-regulating valve, so that the balance of feeding and discharging in the reaction is ensured.
The brief introduction of the process:
the method comprises the following steps of (1) enabling a mixture of water, a solvent and 2-methylfuran which are uniformly mixed according to a certain proportion to enter a reactor through a metering pump and metered hydrogen, keeping a certain temperature and pressure through an atomizer, carrying out hydrogenation reaction in a fixed bed under an atomization state, directly discharging reaction liquid into a gas-liquid separator, enabling discharged material liquid to be in a gas-liquid mixing form, enabling the material liquid to enter the gas-liquid separator, enabling a liquid part to be discharged from the bottom of the gas-liquid separator, neutralizing through a secondary reactor, and carrying out subsequent distillation, rectification and other treatments; the hydrogen gas on the upper part of the gas-liquid separator passes through a condenser, the residual liquid in the reaction liquid is further cooled and remained in a liquid phase, and the non-condensable hydrogen gas enters a hydrogen compressor through a hydrogen return pipe for recycling. Wherein the feeding amount is controlled by a metering pump, and the discharging amount is controlled by the liquid level in the gas-liquid separator, so that the feeding amount and the discharging amount are kept in a balanced state.
The advantages are that:
1. one set of mixing kettle is formed by combining two kettles, and the two kettles are switched back and forth, so that the continuous material feeding can be ensured, the daily productivity of a single reactor is 1t, and the productivity efficiency is greatly improved;
2. all material transferring processes use pumps to transfer materials, so that a barreled material transferring mode of intermittent feeding is avoided, the safety is improved, the operation flow is simplified, and the operation difficulty is reduced;
3. the continuous feeding and discharging operation saves the processes of manual material transfer in the middle and material transfer to the kettle, nitrogen and hydrogen replacement in each batch and the like, simplifies the operation flow, greatly saves the operation time,
4. the hydrogen return device is added, so that the use amount of hydrogen is greatly saved, and the pollution to the atmosphere caused by the exhaust of hydrogen waste gas into the air is reduced.
5. The novel catalyst is replaced, so that the reaction is carried out in a fixed bed, and the condition that the catalyst is not good in activity or reaction effect due to uneven stirring and the like is avoided;
example (b):
respectively replacing a fixed bed reactor and related pipelines with nitrogen and hydrogen for three times in sequence, controlling the reaction temperature of the reactor to be 25-30 ℃, starting to feed hydrogen into the reactor, keeping the hydrogen feeding pressure to be 0.30MPa, pumping 2-methylfuran from a mixing kettle at 280kg/h by a metering pump, opening a discharge valve after a feed pump of a mixture of a solvent and water (the ratio of the three is 4: 2: 1), pressing reaction liquid into a gas-liquid separator by a filter in the kettle, automatically opening a bottom valve after filtrate in the gas-liquid separator reaches a certain liquid level, feeding the reaction liquid into a secondary reactor for neutralization, collecting the neutralization liquid into a receiving tank, carrying out subsequent distillation and other operations to obtain a qualified product, wherein the yield is 85.3%, and distilling a small amount of unreacted 2-methylfuran, the solvent and a byproduct 2-methyltetrahydrofuran, 2-methylfuran and solvent are recycled, and 2-methyltetrahydrofuran is sold as a byproduct;
and hydrogen on the upper part of the gas-liquid separator passes through a condenser and enters a hydrogen compressor through a hydrogen return pipe for recycling. The feeding amount is controlled by a metering pump, the discharging amount is controlled by the combination of liquid level change in a gas-liquid separator and the opening degree of a discharging valve, the hydrogen-returning gas is automatically controlled by the linkage of the pressure in the gas-liquid separator and an exhaust valve, the exhaust pressure range is kept between 0.15 and 0.25MPa, and the feeding amount and the discharging amount are kept in a balanced state.
Comparative example: 720kg of 2-methylfuran, 200kg of water, 5kg of 31% hydrochloric acid and 5kg of palladium carbon catalyst are counted in a reaction kettle, nitrogen and hydrogen are used for replacing for three times respectively, the reaction temperature in the kettle is controlled to be 25-30 ℃, the pressure in the kettle is slowly increased to 0.28MPa until hydrogen is not absorbed, the temperature is reduced after the reaction is finished, the nitrogen is used for replacing the hydrogen in the kettle for three times, the materials are subjected to pressure filtration to a neutralization kettle, the pH value is adjusted to be 6-7 by using sodium carbonate solution, the neutralized materials are subjected to pressure filtration and desalting and then transferred to a distillation kettle, a small amount of unreacted 2-methylfuran and a byproduct 2-methyltetrahydrofuran are distilled out at normal pressure, then the reduced pressure distillation is carried out, a small amount of water is evaporated, the temperature is reduced to normal temperature, and a small amount of residual salt is filtered out to obtain the acetyl-n. The method is a batch method, has long time, low efficiency, more byproducts, easy inactivation of the catalyst, large environmental pollution because hydrogen and air need to be replaced by nitrogen, troublesome slow pressure raising control and the like.
Creatively, the above effects exist independently, and the combination of the above results can be completed by a set of structure.
It should be noted that the plurality of schemes provided in this patent include their own basic schemes, which are independent of each other and are not restricted to each other, but they may be combined with each other without conflict, so as to achieve a plurality of effects.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are intended to illustrate the principles of the invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention, all of which are intended to be covered by the appended claims.
Claims (5)
- The equipment for producing the acetyl-n-propanol by continuously hydrogenating the 2-methylfuran is characterized in that the production equipment comprises a water metering tank (1), a 2-methylfuran metering tank (2) and a solvent metering tank (3), pipelines below the water metering tank (1), the 2-methylfuran metering tank (2) and the solvent metering tank (3) are connected with a stirring part, the stirring part comprises a first stirring and mixing device (10) and a second stirring and mixing device (11), stirred materials can flow out of the first stirring and mixing device (10) and the second stirring and mixing device (11) and then enter a primary reactor (9) through a pipeline and a water phase flowmeter (12), a pipeline extending out of the lower part of the primary reactor is connected with a gas-liquid separator (8), a hydrogen gas return port (4) is arranged above the primary reactor, a pipeline extending out of the hydrogen gas return port (4) is connected with a hydrogen compressor and then connected with a condenser (5), the lower part of the condenser is connected with a gas-liquid separator (8), a pipeline extending out of the gas-liquid separator (8) is connected with a secondary reactor (6), and the secondary reactor is connected with a propanol crude product metering tank (7).
- 2. The apparatus for continuously hydrogenating 2-methylfuran to produce n-propanol including acetyl acetate according to claim 1, wherein the condenser is a water cooling device having a cold water inlet and a cold water outlet, and a gas outlet connected to a hydrogen press.
- 3. The apparatus for producing n-propyl acetyl alcohol by continuous hydrogenation of 2-methylfuran according to claim 1, wherein the primary reactor (9) comprises a primary reactor shell, an atomizer (901) is arranged above the primary reactor shell, a wire mesh distributor (903) is arranged below the atomizer (901), a fixed bed (905) is arranged below the wire mesh distributor, a catalyst (906) is arranged on the fixed bed, the stainless steel wire mesh (907) is arranged below the fixed bed, and a stainless steel screen plate (908) is arranged below the stainless steel wire mesh.
- 4. The apparatus for producing N-propyl acetoacetate by continuously hydrogenating 2-methylfuran according to claim 3, wherein the fixed bed in the first-stage reactor contains a remote thermometer, i.e. a temperature sensor capable of wireless communication.
- 5. The apparatus for continuously hydrogenating 2-methylfuran to produce n-propanol including acetyl acetate according to claim 1, wherein the secondary reactor (6) comprises a housing, a stainless steel water cap (601) is arranged above the housing, the housing contains an ion exchange resin (604), an upper stainless steel wire mesh (602) and an upper stainless steel sieve plate (603) are arranged above the housing, the upper stainless steel wire mesh (602) is arranged above the upper stainless steel sieve plate (603), a lower stainless steel wire mesh (605) and a lower stainless steel sieve plate (606) are arranged below the ion exchange resin (604), and the lower stainless steel wire mesh (605) is arranged above the lower stainless steel sieve plate (606).
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| CN201920755574.8U CN210145530U (en) | 2019-05-24 | 2019-05-24 | Equipment for producing acetyl n-propanol by continuous hydrogenation of 2-methylfuran |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110052049A (en) * | 2019-05-24 | 2019-07-26 | 山东一诺生物质材料有限公司 | The device and method of 2- methylfuran continuously hydrogen adding production acetyl normal propyl alcohol |
| CN115121191A (en) * | 2022-07-13 | 2022-09-30 | 重庆大学 | Preparation of PEDOT by gas-liquid two-phase reaction: PSS device and method |
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2019
- 2019-05-24 CN CN201920755574.8U patent/CN210145530U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110052049A (en) * | 2019-05-24 | 2019-07-26 | 山东一诺生物质材料有限公司 | The device and method of 2- methylfuran continuously hydrogen adding production acetyl normal propyl alcohol |
| CN110052049B (en) * | 2019-05-24 | 2024-02-09 | 山东一诺生物质材料有限公司 | Equipment and method for producing acetyl n-propanol by continuous hydrogenation of 2-methyl furan |
| CN115121191A (en) * | 2022-07-13 | 2022-09-30 | 重庆大学 | Preparation of PEDOT by gas-liquid two-phase reaction: PSS device and method |
| CN115121191B (en) * | 2022-07-13 | 2023-08-04 | 重庆大学 | And (3) preparing PEDOT by gas-liquid two-phase reaction: PSS device and method |
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