CN215480653U - System for preparing octenal by condensing n-butyraldehyde - Google Patents
System for preparing octenal by condensing n-butyraldehyde Download PDFInfo
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- CN215480653U CN215480653U CN202121593875.9U CN202121593875U CN215480653U CN 215480653 U CN215480653 U CN 215480653U CN 202121593875 U CN202121593875 U CN 202121593875U CN 215480653 U CN215480653 U CN 215480653U
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- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 title claims abstract description 182
- 238000006243 chemical reaction Methods 0.000 claims abstract description 99
- 239000003513 alkali Substances 0.000 claims abstract description 50
- 238000006482 condensation reaction Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims description 50
- 238000009833 condensation Methods 0.000 claims description 48
- 230000005494 condensation Effects 0.000 claims description 48
- 239000012071 phase Substances 0.000 claims description 27
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 26
- 239000007791 liquid phase Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 15
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 14
- 239000007789 gas Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000011552 falling film Substances 0.000 description 4
- PYLMCYQHBRSDND-SOFGYWHQSA-N (E)-2-ethyl-2-hexenal Chemical compound CCC\C=C(/CC)C=O PYLMCYQHBRSDND-SOFGYWHQSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000012043 crude product Substances 0.000 description 2
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000016507 interphase Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical compound O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
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Abstract
The utility model provides a system for preparing octenal by condensing n-butyraldehyde, which comprises the following components: the system comprises a reaction tower, a micro-interface unit, a n-butyl aldehyde pipeline and an alkali liquor pipeline, wherein the n-butyl aldehyde pipeline and the alkali liquor pipeline are both connected with the micro-interface unit, alkali liquor is dispersed and crushed in the micro-interface unit into micro-droplets at the micron level, and the micro-droplets enter the reaction tower to undergo condensation reaction; and a product outlet is arranged on the side wall of the reaction tower. The system has the advantages of low energy consumption, low cost, high safety, low required reaction temperature and high n-butyraldehyde conversion rate, and is worthy of wide popularization and application.
Description
Technical Field
The utility model relates to the technical field of n-butyraldehyde condensation, in particular to a system for preparing octenal by n-butyraldehyde condensation.
Background
Butanol and octanol are important raw materials for synthesizing fine chemical products, the yield of butanol and octanol in China is huge at present, which accounts for about 21 percent of the total amount of the world, and the butanol and octanol are mainly used for producing plasticizers, solvents, dehydrating agents, defoaming agents, dispersing agents, flotation agents, petroleum additives, synthetic spices and the like. Due to its wide use, the yield and the amount of butanol and octanol are also increased year by year.
The butanol and octanol can be prepared by n-butyl aldehyde condensation, and specifically comprises the following steps:
(1) condensation of n-butyraldehyde to produce 2-ethyl-3-propylacrolein (EPA):
2CH3CH2CH3CHO→CH3CH2CH2CH＝C(C2H5)CHO+H2O
(2) hydrogenation of 2-ethyl-3-propylacrolein to octanol:
CH3CH2CH2CH＝C(C2H5)CHO+2H2→CH3CH2CH2CH(CH2CH3)CH2OH
currently, the n-butyraldehyde condensation process has the following drawbacks:
(1) alkali liquor and n-butyraldehyde directly enter a stirred tank condensation reactor in a liquid-liquid two-phase manner, the two-phase distribution uniformity is limited, liquid drops are irregular in shape and large in diameter, the liquid-liquid phase interface area is small, and the interphase mass transfer and reaction efficiency are influenced;
(2) in order to ensure the expected butyraldehyde condensation reaction speed in the condensation reactor, the existing reaction kettle has high operation temperature, high concentration of alkali liquor NaOH and excessively long retention time of reaction products, so that heavy components are increased, and the yield of n-butyraldehyde is influenced;
(3) the whole-course yield of the condensation reaction needs to be improved, and the butyraldehyde content at the bottom of the tower is higher;
(4) the tower bottom reboiler of the condensation circulating tower has large liquid holdup and overlong product retention time, which brings local overtemperature and may cause the increase of heavy component content.
In view of the above, the present invention is particularly proposed.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a system for preparing octenal by condensing n-butyraldehyde, which disperses and breaks alkali liquor into micron-level micro-droplets by using a micro interface unit and then mixes the micro-droplets with the n-butyraldehyde, thereby increasing the mass transfer area between the alkali liquor and the n-butyraldehyde, improving the distribution uniformity of two phases, ensuring the droplets to have uniform shapes and small diameters, greatly improving the mass transfer rate and reducing the temperature and pressure required by the reaction.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the utility model provides a system for preparing octenal by condensing n-butyraldehyde, which comprises the following components: the system comprises a reaction tower, a micro-interface unit, a n-butyl aldehyde pipeline and an alkali liquor pipeline, wherein the n-butyl aldehyde pipeline and the alkali liquor pipeline are both connected with the micro-interface unit, alkali liquor is dispersed and crushed in the micro-interface unit into micro-droplets in the micron level, and the micro-droplets enter the reaction tower to catalyze n-butyl aldehyde to carry out condensation reaction;
a product outlet is formed in the side wall of the reaction tower; the product outlet is connected with a condensation circulating tower; a gas phase outlet is formed in the top of the condensation circulating tower, and a liquid phase outlet is formed in the bottom of the condensation circulating tower; the gas phase outlet is sequentially connected with a condenser and a liquid separator, the liquid separator is provided with a water outlet and an organic outlet, and the organic outlet is connected with the n-butyl aldehyde pipeline;
and the liquid phase outlet is connected with a reboiler, part of the product discharged from the liquid phase outlet is heated by the reboiler and then flows back to the condensation circulating tower, and part of the product is extracted through an extraction pipeline. In fact, the liquid phase outlet is also connected to the top of the condensation recycling column to recycle the bottom liquid to the top of the column as condensate.
In the prior art, the preparation of octenal by condensing n-butyl aldehyde is an important link in the preparation process of butanol and octanol. However, in the existing n-butyraldehyde condensation process, alkali liquor and n-butyraldehyde directly enter a stirred tank condensation reactor in a liquid-liquid two-phase mode, the two-phase distribution uniformity is limited, liquid drops are irregular in shape and large in diameter, the liquid-liquid phase interface area is small, and the interphase mass transfer and reaction efficiency are influenced; and because the operation temperature in the reaction kettle is higher, the concentration of the alkali liquor NaOH is higher, and the retention time of the reaction product is too long, heavy components are increased, and the yield of the n-butyraldehyde is influenced.
In order to solve the technical problems, the utility model provides a system for preparing octenal by condensing n-butyraldehyde, which disperses and breaks alkali liquor and n-butyraldehyde into micron-level micro-droplets by using a micro-interface unit, increases the mass transfer area between the alkali liquor and the n-butyraldehyde, improves the two distribution uniformity, has uniform droplet shape and small diameter, greatly improves the mass transfer rate, and reduces the temperature and pressure required by reaction.
Preferably, the micro interface unit is arranged outside the reaction tower, and the micro interface unit is connected with the reaction tower. The setting is convenient for to the control of little interface unit like this, can improve the operational safety nature.
Preferably, a distribution disc is arranged at an inlet of the micro interface unit connected with the reaction tower. By arranging the distribution disc, the raw material micro-droplets can be uniformly distributed in the reaction tower, and the liquid-liquid phase boundary mass transfer is enhanced.
Preferably, the micro interface unit is arranged inside the reaction tower; the micro-interface unit comprises a first micro-interface generator and a second micro-interface generator, and the first micro-interface generator is positioned above the second micro-interface generator; the first micro-interface generator and the second micro-interface generator are both connected with the n-butyraldehyde pipeline and the alkali liquor pipeline; the first micro-interface generator is opposite to the outlet of the second micro-interface generator. At the moment, the micro-interface unit is arranged in the reaction tower, so that the equipment integration degree is high, and the occupied area is small. The alkali liquor and the n-butyraldehyde are dispersed and crushed simultaneously by the two micro-interface generators, so that the alkali liquor and the n-butyraldehyde can be dispersed and crushed into micro-droplets, the distribution uniformity of two phases is improved, the mass transfer area of a liquid-liquid phase boundary is improved, the temperature and pressure required by the reaction are reduced, and the mass transfer and heat transfer efficiency of the n-butyraldehyde into the alkali liquor is improved; the gas phase outlets of the two micro-interface generators are opposite to each other so as to enable micro-droplets to be uniformly distributed, and the mass transfer efficiency is improved.
Preferably, the micro-interface unit comprises a third micro-interface generator and a mixed micro-interface generator; the third micro-interface generator is arranged outside the reaction tower, and the mixed micro-interface generator is arranged inside the reaction tower.
Preferably, the mixed micro-interface generator comprises a fourth micro-interface generator arranged above the liquid level in the reaction tower and a fifth micro-interface generator positioned below the liquid level in the reaction tower, and the fourth micro-interface generator is connected with the fifth micro-interface generator through a micro-droplet pipeline; and the top of the fifth micro interface generator is tightly attached with a micro-droplet outlet, and the outlet of the micro-droplet pipeline is communicated with the micro-droplet outlet.
Preferably, the direction of the micro-droplet outlet is horizontally or vertically arranged upwards.
Furthermore, the product outlet is connected with a dehydration system, and a crude product generated in the reaction tower is dehydrated by the dehydration system and then is extracted.
The fourth micro-interface generator and the fifth micro-interface generator are combined to form the hybrid micro-interface generator SBBS, so that the application effect of the single micro-interface generator is improved; on one hand, collision flow can be formed between the fourth micro-interface generator and the fifth micro-interface generator, and micro liquid drops are further dispersed and crushed; on the other hand, when the fifth micro interface generator is blocked, the interior of the fifth micro interface generator can be flushed by the liquid flow of the fourth micro interface generator, so that the blockage is prevented. And set up like this and can also improve fixed effect, play the supporting effect to fourth micro-interface generator through the pipeline that is connected between fourth micro-interface generator and the fifth micro-interface generator. The space in the reactor of own is narrower, if the normal work of reactor also can be influenced to too dispersion that micro-interface generator set up, the design also shortens each micro-interface generator's distance for holistic structure in addition, strengthens the cooperation ability each other between each part, through the broken bubble collision impact back each other of micro-interface to improve dispersion crushing effect.
In addition, in the scheme of the utility model, the fourth micro interface generator and the fifth micro interface generator are connected into a whole through a micro liquid drop pipeline, the micro liquid drop pipeline is directly communicated with a micro liquid drop outlet arranged at the upper part of the fifth micro interface generator, the micro liquid drop outlet is an outlet of micro liquid drops formed after the fifth micro interface generator is dispersed and crushed, and power is provided for materials discharged from the micro liquid drop outlet through the guiding effect of the micro liquid drop channel. In addition, this micro-droplet export can set up to along horizontal direction or perpendicular direction up, and the horizontal direction is the direct injection just away, and perpendicular ascending direction is equivalent to set up 180 the inflection in the exit to promote the circulation energy of micro-droplet mixing flow more, also can drive the material that is located the mixing effect difference on upper portion and carry out the backmixing and break again. And a third micro-interface generator is arranged in front of the reaction tower, so that the feeding can be fully broken into micro-droplets in the micron level from the source, and the crushing effect after the feeding into the reactor is more sufficient.
Preferably, the outlets of the first micro-interface generator and the second micro-interface generator are both provided with a distribution disc. By arranging the distribution disc, the raw material micro-droplets can be uniformly distributed in the reaction tower, and the liquid-liquid phase boundary mass transfer is enhanced.
Preferably, a plurality of through holes are arranged on the distribution disc. During reaction, the micro-droplets are sprayed in different directions along the through holes, so that the distribution uniformity of the two phases of the alkali liquor and the n-butyl aldehyde is promoted.
Preferably, a circulating pipeline is arranged on one side of the reaction tower, an inlet of the circulating pipeline is located below the liquid level in the reaction tower along the vertical direction, and an outlet of the circulating pipeline is connected with the first micro-interface generator. The device can make the feed liquid in the reactor circularly enter the micro-interface generator, thereby improving the dispersion effect and the reaction rate.
Preferably, the reboiler is a falling film reboiler. The falling film reboiler is arranged, so that the liquid holdup at the bottom of the condensation circulating tower can be reduced, the retention time of the product octenal is reduced, the temperature of a heating medium is properly reduced, and the local overtemperature is reduced, so that the content of heavy components is further reduced.
The utility model disperses and crushes the alkali liquor and the n-butyraldehyde by arranging the micro interface unit, so that the alkali liquor is dispersed into micro-droplets in the micron level. During reaction, alkali liquor is dispersed and crushed into micron-level micro-droplets by a micro-interface unit and then mixed into n-butyraldehyde, and the n-butyraldehyde is subjected to condensation reaction under the catalytic action of the alkali liquor, so that the distribution uniformity of two phases is improved, the catalytic effect is improved, the mass transfer area of a phase boundary is increased, and the temperature of required reaction is reduced.
It should be noted that, in the present invention, the two dispersed and broken phases of the micro interface unit are both liquid phases, because the alkali solution and the n-butyl aldehyde are both liquid phases, but the two liquid phases are not mixed with each other, the alkali solution is a water phase, the n-butyl aldehyde is an oil phase, and the alkali solution plays a role of a catalyst in the condensation reaction of the n-butyl aldehyde, and in the present invention, the alkali solution is a dispersed phase, and the n-butyl aldehyde is a continuous phase, in order to increase the contact area between the two liquid phases and to mix them uniformly, thereby achieving the optimal catalytic effect, the micro interface unit is used for micro interface breaking of the dispersed phase alkali solution, so that the alkali solution is dispersed into micro droplets of micron level, and the introduction of the n-butyl aldehyde is used for providing power, and also for uniformly distributing the alkali solution micro droplets in the n-butyl aldehyde, thereby improving the mixing uniformity of the two phases and improving the catalytic effect and reaction rate of the alkali solution on the condensation reaction.
In the present invention, the micro interface unit may be disposed outside the reaction tower or may be disposed inside the reaction tower. When the device is arranged outside the reaction tower, the n-butyraldehyde pipeline and the alkali liquor pipeline are simultaneously introduced into the micro-interface unit, and the two-phase hydraulic power is utilized for dispersing and crushing. The advantage that sets up like this can externally control and overhaul the little interface unit, and control is convenient.
When the micro interface unit is arranged inside, the n-butyraldehyde pipeline and the alkali liquor pipeline penetrate through the side wall of the reaction tower to be connected with the micro interface unit. At this time, the micro interface unit is composed of two micro interface generators, and the outlets of the two micro interface generators are opposite, so that the micro droplets are further crushed by utilizing the opposite impact action of two micro droplet streams, and the micro droplets can be uniformly dispersed in the reaction tower. In the utility model, no matter the micro interface unit is arranged outside the reaction tower or inside the reaction tower, the distribution disc is arranged at the outlet of the micro interface unit communicated with the reaction tower, so that the arrangement is to change the flow direction of micro liquid drops and promote the micro liquid drops to be distributed more uniformly.
The utility model also arranges a falling film reboiler at the bottom of the condensation circulating tower, thus reducing the liquid holdup at the bottom of the condensation circulating tower, reducing the retention time of the product octenal, properly reducing the temperature of a heating medium, and reducing local overtemperature so as to further reduce the content of heavy components. Therefore, the distributor and the micro-interface unit are combined with n-butyl aldehyde condensation reaction, and the rectification process of the condensation circulating tower is optimized, so that the reaction rate is improved, and the energy consumption is reduced.
It will be appreciated by those skilled in the art that the micro-interface generator used in the present invention is described in the prior patents of the present inventor, such as the patents of application numbers CN201610641119.6, CN201610641251.7, CN201710766435.0, CN106187660, CN105903425A, CN109437390A, CN205833127U and CN 207581700U. The detailed structure and operation principle of the micro bubble generator (i.e. micro interface generator) is described in detail in the prior patent CN201610641119.6, which describes that "the micro bubble generator comprises a body and a secondary crushing member, wherein the body is provided with a cavity, the body is provided with an inlet communicated with the cavity, the opposite first end and second end of the cavity are both open, and the cross-sectional area of the cavity decreases from the middle of the cavity to the first end and second end of the cavity; the secondary crushing member is disposed at least one of the first end and the second end of the cavity, a portion of the secondary crushing member is disposed within the cavity, and an annular passage is formed between the secondary crushing member and the through holes open at both ends of the cavity. The micron bubble generator also comprises an air inlet pipe and a liquid inlet pipe. "the specific working principle of the structure disclosed in the application document is as follows: liquid enters the micro-bubble generator tangentially through the liquid inlet pipe, and gas is rotated at a super high speed and cut to break gas bubbles into micro-bubbles at a micron level, so that the mass transfer area between a liquid phase and a gas phase is increased, and the micro-bubble generator in the patent belongs to a pneumatic micro-interface generator.
In addition, the first patent 201610641251.7 describes that the primary bubble breaker has a circulation liquid inlet, a circulation gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed inlet with the gas-liquid mixture outlet, which indicates that the bubble breakers all need to be mixed with gas and liquid, and in addition, as can be seen from the following drawings, the primary bubble breaker mainly uses the circulation liquid as power, so that the primary bubble breaker belongs to a hydraulic micro-interface generator, and the secondary bubble breaker simultaneously introduces the gas-liquid mixture into an elliptical rotating ball for rotation, thereby realizing bubble breaking in the rotating process, so that the secondary bubble breaker actually belongs to a gas-liquid linkage micro-interface generator. In fact, the micro-interface generator is a specific form of the micro-interface generator, whether it is a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator, however, the micro-interface generator adopted in the present invention is not limited to the above forms, and the specific structure of the bubble breaker described in the prior patent is only one of the forms that the micro-interface generator of the present invention can adopt.
Furthermore, the prior patent 201710766435.0 states that the principle of the bubble breaker is that high-speed jet flows are used to achieve mutual collision of gases, and also states that the bubble breaker can be used in a micro-interface strengthening reactor to verify the correlation between the bubble breaker and the micro-interface generator; moreover, in the prior patent CN106187660, there is a related description on the specific structure of the bubble breaker, see paragraphs [0031] to [0041] in the specification, and the accompanying drawings, which illustrate the specific working principle of the bubble breaker S-2 in detail, the top of the bubble breaker is a liquid phase inlet, and the side of the bubble breaker is a gas phase inlet, and the liquid phase coming from the top provides the entrainment power, so as to achieve the effect of breaking into ultra-fine bubbles, and in the accompanying drawings, the bubble breaker is also seen to be of a tapered structure, and the diameter of the upper part is larger than that of the lower part, and also for better providing the entrainment power for the liquid phase.
Since the micro-interface generator was just developed in the early stage of the prior patent application, the micro-interface generator was named as a micro-bubble generator (CN201610641119.6), a bubble breaker (201710766435.0) and the like in the early stage, and is named as a micro-interface generator in the later stage along with the continuous technical improvement, and the micro-interface generator in the present invention is equivalent to the micro-bubble generator, the bubble breaker and the like in the prior art, and has different names. In summary, the micro-interface generator of the present invention belongs to the prior art.
Preferably, a feed cooler is arranged on the n-butyraldehyde pipeline.
The utility model also provides a preparation method of the system for preparing octenal by adopting the condensation of n-butyraldehyde, which comprises the following steps:
after the alkali liquor is broken into micron-level micro-droplets through a micro interface, n-butyl aldehyde is catalyzed to carry out condensation reaction, and the generated product is purified and separated to obtain the product octenal.
Preferably, the condensation reaction temperature is 114-.
The octenal product obtained by the reaction method of the utility model has good quality and high yield. And the preparation method has low reaction energy consumption and obviously reduced cost.
Compared with the prior art, the utility model has the beneficial effects that:
the system for preparing octenal by condensing n-butyraldehyde disperses and breaks alkali liquor into micron-level micro-droplets by using the micro-interface unit, increases the mass transfer area between the alkali liquor and the n-butyraldehyde, improves the two-phase distribution uniformity, has uniform droplet shape and small diameter, greatly improves the mass transfer rate, and improves the reaction space-time yield, the octenal yield and the energy efficiency and physical efficiency under the conditions of reducing the operation temperature and reaction space-time.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the utility model. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a system for producing octenal by condensation of n-butanol according to example 1 of the present invention;
FIG. 2 is a schematic structural diagram of a system for producing octenal by condensation of n-butanol according to example 2 of the present invention;
FIG. 3 is a schematic structural diagram of a system for preparing octenal by condensation of n-butanol according to embodiment 3 of the present invention.
Description of the drawings:
10-a feed cooler; a 20-n-butyraldehyde line;
30-an alkaline liquor line; 40-micro interface unit;
50-a reaction tower; 60-a distribution disk;
70-a condensation recycle column; 80-a condenser;
90-liquid separator; 100-a reboiler;
110-a second micro-interface generator; 120-a first micro-interface generator;
130-a circulation line; 140-a circulation pump;
150-a fifth micro-interface generator; 160-a fourth micro-interface generator;
170-a third micro-interface generator; 180-dehydration system.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; 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 meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to more clearly illustrate the technical solution of the present invention, the following description is made in the form of specific embodiments.
Example 1
Referring to fig. 1, this embodiment provides a system for preparing octenal by condensation of n-butanol, comprising: the reaction tower 50, the micro-interface unit 40, the n-butyraldehyde pipeline 20 and the alkali liquor pipeline 30 are connected with the micro-interface unit 40, the alkali liquor is dispersed and crushed into micron-level micro-droplets in the micro-interface unit 40, and the micro-droplets enter the reaction tower 50 to catalyze the n-butyraldehyde to carry out condensation reaction.
Wherein, a product outlet is arranged on the side wall of the reaction tower 50; the product outlet is connected with a condensation circulating tower 70; the top of the condensation circulating tower 70 is provided with a gas phase outlet, and the bottom is provided with a liquid phase outlet; the gas phase outlet is connected with a condenser 80 and a knockout 90 in sequence, the knockout 90 is provided with a water outlet and an organic outlet, the organic outlet is connected with the n-butyraldehyde pipeline 20, and a circulating pump 140 is arranged between the organic outlet and the n-butyraldehyde pipeline 20.
Specifically, the micro interface unit 40 is disposed outside the reaction tower 50, and the micro interface unit 40 is connected to the reaction tower 50. A distribution plate 60 is provided at an inlet of the micro interface unit 40 connected to the reaction tower 50.
The liquid phase outlet is connected to a reboiler 100, and a part of the product discharged through the liquid phase outlet is heated by the reboiler 100 and refluxed to the condensation circulating tower 70, and a part of the product is withdrawn through a withdrawal line. In fact, the liquid phase outlet is also connected to the top of the condensation recycling column to recycle the bottom liquid to the top of the column as condensate.
In this embodiment, the reboiler 100 is a falling film reboiler 100. The n-butyraldehyde line 20 is provided with a feed cooler 10.
During reaction, n-butyraldehyde is cooled to a certain temperature by the feeding cooler 10 and then enters the micro interface unit 40, alkali liquor is metered and then also enters the micro interface unit 40, the alkali liquor is crushed into micro-droplets by a micro interface and then enters the reaction tower 50 to be mixed with the n-butyraldehyde to catalyze the n-butyraldehyde to carry out condensation reaction, the condensation reaction product enters the condensation circulating tower 70, unreacted n-butyraldehyde is condensed by the condenser 80 at the top of the condensation circulating tower 70 and is separated at the liquid separator 90, and the separated organic component returns to the micro interface unit 40. The reaction liquid from the bottom of the condensation circulating tower 70 enters a reboiler 100, and a part of the reaction liquid is heated by the reboiler 100 and then flows back to the condensation circulating tower 70 to provide a heat source for the condensation circulating tower; the other path is the reaction product octenal.
Example 2
The system in this example differs from the system in example 1 only in that the micro interface unit of this example is located inside the reaction column 50.
As shown in fig. 2, the micro interface unit is disposed inside the reaction tower 50, and includes: a first micro-interface generator 120 and a second micro-interface generator 110, the first micro-interface generator 120 being located above the second micro-interface generator 110; the first micro-interface generator 120 and the second micro-interface generator 110 are connected with the n-butyraldehyde pipeline 20 and the alkali liquid pipeline 30; the first micro-interface generator 120 is opposite the outlet of the second micro-interface generator 110.
In this embodiment, the distribution plate 60 is disposed at the outlet of each of the first micro-interface generator 120 and the second micro-interface generator 110. The distribution plate 60 is provided with a plurality of through holes.
In this embodiment, a circulation pipeline 130 is disposed at one side of the reaction tower 50, an inlet of the circulation pipeline 130 is located below the liquid level in the reaction tower 50 along the vertical direction, and an outlet of the circulation pipeline 130 is connected to the first micro-interface generator 120. The device can make the feed liquid in the reactor circularly enter the micro-interface generator, thereby improving the dispersion effect and the reaction rate.
During reaction, n-butyl aldehyde is cooled to a certain temperature by the feeding cooler 10 and then enters the reaction tower 50, alkali liquor is metered and then also enters the reaction tower 50, the alkali liquor is dispersed and crushed into micro-droplets by the first micro-interface generator 120 and the second micro-interface generator 110 in the reaction tower 50 and then enters the reaction tower 50 to be mixed with n-butyl aldehyde to catalyze the n-butyl aldehyde for condensation reaction, and the feed liquid in the reaction tower 50 is circulated by the circulating pipeline 130 and enters the first micro-interface generator 120 to be dispersed and crushed. The condensation reaction product enters a condensation circulating tower 70, unreacted n-butyl aldehyde is condensed by a condenser 80 at the top of the condensation circulating tower 70 and is separated at a liquid separator 90, and the separated organic component returns to the micro interface unit 40. The reaction liquid from the bottom of the condensation circulating tower 70 enters a reboiler 100, and a part of the reaction liquid is heated by the reboiler 100 and then flows back to the condensation circulating tower 70 to provide a heat source for the condensation circulating tower; the other path is the reaction product octenal.
Example 3
Referring to FIG. 3, the present embodiment provides a system for preparing octenal by condensing n-butyraldehyde, comprising: the reaction tower 50, the micro-interface unit 40, the n-butyraldehyde pipeline 20 and the alkali liquor pipeline 30 are connected with the micro-interface unit 40, the alkali liquor is dispersed and crushed into micron-level micro-droplets in the micro-interface unit 40, and the micro-droplets enter the reaction tower 50 to catalyze the n-butyraldehyde to carry out condensation reaction.
Wherein, a product outlet is arranged on the side wall of the reaction tower 50; the product outlet is connected with a dehydration system 180, and the crude product generated in the reaction tower is dehydrated by the dehydration system 180 and then is extracted.
Specifically, the micro-interface unit includes a third micro-interface generator 170 and a hybrid micro-interface generator; the third micro-interface generator 170 is disposed outside the reaction tower, and the hybrid micro-interface generator is disposed inside the reaction tower. The alkali liquor is dispersed and crushed by the third micro-interface generator 170 and the mixed micro-interface generator in sequence, and enters the reaction tower to catalyze n-butyraldehyde for condensation reaction. The mixed micro-interface generator comprises a fourth micro-interface generator 160 arranged above the liquid level in the reaction tower and a fifth micro-interface generator 150 positioned below the liquid level in the reaction tower, wherein the fourth micro-interface generator 160 is connected with the fifth micro-interface generator 150 through a micro-droplet pipeline; the top of the fifth micro interface generator 150 is closely provided with a micro-droplet outlet, and the outlet of the micro-droplet pipeline is communicated with the micro-droplet outlet. The direction of the micro-droplet outlet is horizontally or vertically arranged upwards. Although not explicitly shown in the figures, the specific structure of the droplet outlet is clear from the text of the present invention.
The preparation of octenal was carried out by the systems of example 1, example 2 and example 3 at various temperatures and pressures, and it is known that the reaction temperature of the existing industrial apparatus was 118-120 ℃ and the reaction pressure was 0.3-0.5 MPa. The space time of the reaction was 8.13min, and the space time yield of the reactor was 2.227t/m3H, the once-through conversion rate of n-butyraldehyde is 91.65%, the content of n-butyraldehyde at the bottom of the condensation circulating tower is 1.2%, and n-butyraldehyde generates octylThe selectivity of the olefine aldehyde is 96.87 percent, and the effective utilization rate of the n-butyl aldehyde is 96.90 percent.
Wherein the temperature of the experimental example 1 is 114 ℃, and the pressure is 0.3 MPa; the temperature of experimental example 2 was 115 ℃ and the pressure was 0.4 MPa; the temperature in Experimental example 3 was 117 ℃ and the pressure was 0.5 MPa. The specific process parameters are as follows:
experimental example 1 parameter Table
Experimental example 2 parameter Table
Experimental example 3 parameter Table
Comparative example
In this example, no micro interface unit was used, and the remaining conditions were the same as in example 1.
The reaction space time in this example was 8.23min, the reactor space time yield 2.117t/m3H, the once-through conversion rate of n-butyraldehyde is 90.88%, the content of n-butyraldehyde at the bottom of the condensation cycle tower is 1.3%, the selectivity of n-butyraldehyde for generating octenal is 96.13%, and the effective utilization rate of n-butyraldehyde is 96.56%.
Therefore, the system for preparing the octenal by condensing the n-butyl aldehyde can improve the space-time yield of the reaction, the yield of the octenal and the energy efficiency and physical efficiency under the condition of reducing the operation temperature and the space time of the reaction.
In a word, compared with the reaction system for preparing octenal by condensing n-butyraldehyde in the prior art, the system has the advantages of low energy consumption, low cost, high safety, low required reaction temperature and high n-butyraldehyde conversion rate, and is worthy of wide popularization and application.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the utility model has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A system for preparing octenal by condensing n-butyraldehyde, comprising: the system comprises a reaction tower, a micro-interface unit, a n-butyl aldehyde pipeline and an alkali liquor pipeline, wherein the n-butyl aldehyde pipeline and the alkali liquor pipeline are both connected with the micro-interface unit, alkali liquor is dispersed and crushed in the micro-interface unit into micro-droplets in the micron level, and the micro-droplets enter the reaction tower to catalyze n-butyl aldehyde to carry out condensation reaction; and a product outlet is arranged on the side wall of the reaction tower.
2. The system for the condensation of n-butyraldehyde to octenal according to claim 1, wherein the product outlet is connected to a condensation cycle column; a gas phase outlet is formed in the top of the condensation circulating tower, and a liquid phase outlet is formed in the bottom of the condensation circulating tower; the gas phase outlet is sequentially connected with a condenser and a liquid separator, the liquid separator is provided with a water outlet and an organic outlet, and the organic outlet is connected with the n-butyl aldehyde pipeline;
and the liquid phase outlet is connected with a reboiler, part of the product discharged from the liquid phase outlet is heated by the reboiler and then flows back to the condensation circulating tower, and part of the product is extracted through an extraction pipeline.
3. The system for preparing octenal by condensation of n-butanol according to claim 2, wherein the micro interface unit is disposed outside the reaction column, and the micro interface unit is connected to the reaction column.
4. The system for preparing octenal by condensing n-butyraldehyde according to claim 3, wherein a distribution tray is provided at an inlet of the micro interface unit connected to the reaction column.
5. The system for condensing n-butyraldehyde to octenal according to claim 2, wherein the micro interface unit is disposed inside the reaction column; the micro-interface unit comprises a first micro-interface generator and a second micro-interface generator, and the first micro-interface generator is positioned above the second micro-interface generator; the first micro-interface generator and the second micro-interface generator are both connected with the n-butyraldehyde pipeline and the alkali liquor pipeline; the first micro-interface generator is opposite to the outlet of the second micro-interface generator.
6. The system for preparing octenal by condensation of n-butanol according to claim 5, wherein the outlets of the first micro-interface generator and the second micro-interface generator are provided with distribution plates.
7. The system for condensing n-butyraldehyde to octenal according to claim 1, wherein the micro-interface unit comprises a third micro-interface generator and a hybrid micro-interface generator; the third micro-interface generator is arranged outside the reaction tower, and the mixed micro-interface generator is arranged inside the reaction tower.
8. The system for preparing octenal by condensing n-butanol according to claim 7, wherein the mixed micro-interface generator comprises a fourth micro-interface generator disposed above the liquid level in the reaction column and a fifth micro-interface generator disposed below the liquid level in the reaction column, and the fourth micro-interface generator is connected to the fifth micro-interface generator through a micro-droplet pipeline; and the top of the fifth micro interface generator is tightly attached with a micro-droplet outlet, and the outlet of the micro-droplet pipeline is communicated with the micro-droplet outlet.
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