CN113548951A - Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde and preparation method - Google Patents
Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde and preparation method Download PDFInfo
- Publication number
- CN113548951A CN113548951A CN202110793921.8A CN202110793921A CN113548951A CN 113548951 A CN113548951 A CN 113548951A CN 202110793921 A CN202110793921 A CN 202110793921A CN 113548951 A CN113548951 A CN 113548951A
- Authority
- CN
- China
- Prior art keywords
- micro
- butyraldehyde
- interface
- reaction zone
- interface generator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/67—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton
- C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
- C07C45/74—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups combined with dehydration
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde, which comprises the following components: a reactor; a partition plate is arranged in the reactor, and the internal space of the reactor is divided into two mutually independent spaces along the partition plate; the space below the partition plate is a first reaction zone; the side wall of the first reaction zone is provided with a n-butyraldehyde inlet and an alkali liquor inlet, a first micro-interface generator is arranged in the first reaction zone, the first micro-interface generator is connected with the n-butyraldehyde inlet and the alkali liquor inlet, and alkali liquor enters the first reaction zone to catalyze the n-butyraldehyde to carry out condensation reaction after being dispersed and crushed into micron-level micro-droplets by the first micro-interface generator. The micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde 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 invention relates to the technical field of n-butyraldehyde condensation, in particular to a micro-interface strengthening system for preparing octenal by n-butyraldehyde condensation and a preparation method thereof.
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.
Disclosure of Invention
The first purpose of the invention is to provide a micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde, wherein the reaction system divides a reactor into an upper reaction zone and a lower reaction zone, so that raw materials are subjected to two reactions, the raw materials are subjected to more complete reactions, and the conversion rate of the raw materials is improved; the first micro-interface generator is arranged in the first reaction zone, and the alkali liquor is dispersed and crushed into micro-droplets of micron level by the first micro-interface generator and then dispersed into the n-butyraldehyde solution, so that the uniformity of two-phase distribution is improved, the droplets are uniform in shape and small in diameter, the mass transfer rate is greatly improved, the temperature required by the reaction is reduced, and the product yield is improved.
The second purpose of the invention is to provide a preparation method for preparing octenal by adopting the system, the preparation method is simple and convenient to operate, the butyraldehyde conversion rate is high, the product quality is high, the energy consumption is reduced, and the reaction effect better than that of the existing process is achieved.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde, which comprises the following components: a reactor; a partition plate is arranged in the reactor, and the internal space of the reactor is divided into two mutually independent spaces along the partition plate; the space below the partition plate is a first reaction zone;
the side wall of the first reaction zone is provided with a n-butyraldehyde inlet and an alkali liquor inlet, a first micro-interface generator is arranged in the first reaction zone, the first micro-interface generator is connected with the n-butyraldehyde inlet and the alkali liquor inlet, and alkali liquor enters the first reaction zone to catalyze the n-butyraldehyde to carry out condensation reaction after being dispersed and crushed into micron-level micro-droplets by the first micro-interface generator.
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 invention provides a micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde, which divides a reactor into an upper reaction zone and a lower reaction zone, so that raw materials are subjected to two reactions, the raw materials are subjected to more complete reactions, and the conversion rate of the raw materials is improved; through set up first micro-interface generator in first reaction zone, utilize first micro-interface generator to disperse the alkali lye and break into micron level micro-droplet and disperse to n-butyraldehyde solution after, improved the degree of consistency of two-phase distribution, the droplet shape is even, and the diameter is little, increases substantially mass transfer rate, has reduced the temperature that the reaction needs, has improved the product yield, and this system need not to use rectifying column, and area is little.
Preferably, a second reaction zone is positioned above the separation plate; the second reaction zone is internally provided with a second micro-interface generator, the first reaction zone is connected with a first circulating pipeline, the inlet of the first circulating pipeline is connected with the first reaction zone, and the outlet of the first circulating pipeline is respectively connected with the first micro-interface generator and the second micro-interface generator.
Preferably, the system also comprises a second condenser and a decanter; a product outlet is formed in the side wall of the second reaction zone, the product outlet is connected with a second circulating pipeline, and a first condenser is arranged on the second circulating pipeline; and one part of the material circulated by the second circulation pipeline flows back to the second micro-interface generator after being condensed by the first condenser, and the other part of the material flows into the decanter after being condensed by the second condenser.
Preferably, the outlets of the first micro-interface generator and the second micro-interface generator are both provided with a distribution disc.
Preferably, the distribution disc is conical, and a plurality of through holes are vertically formed in the distribution disc.
According to the invention, the reactor is divided into the first reaction zone and the second reaction zone, so that the reaction materials are subjected to two reactions, the material reaction is more sufficient, and the raw material reaction is more sufficient; all be provided with little interfacial generator in first reaction zone and the second reaction zone, can disperse alkali lye and become behind the micron level's microbubble, evenly disperse to the n-butyraldehyde in, improved the mixing degree of consistency between them, improved catalytic effect. During reaction, alkali liquor is dispersed and crushed into micron-level micro-droplets by the first micro-interface generator, then is dispersed into n-butyraldehyde, the n-butyraldehyde is catalyzed to carry out condensation reaction, a reactant flow flows back to the first reaction area along with one part of the first circulating pipeline and continues to react under the dispersion and crushing of the first micro-interface generator, and the other part of the reactant flow flows into the second reaction area; and introducing the material flow flowing into the second reaction zone into a second micro-interface generator, wherein the alkali liquor is dispersed into micro-droplets by the second micro-interface generator and then dispersed into the second reaction zone to catalyze the unreacted n-butyraldehyde to continue to react. The n-butyraldehyde and the alkali liquor have high mixing uniformity, the catalytic effect is improved, the mass transfer area of a phase boundary is increased, and the temperature required by the reaction is reduced.
It should be noted that, in the present invention, the two phases dispersed and broken by the micro-interface generator 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 breaking is performed on the dispersed phase alkali solution by the micro-interface generator, so that the alkali solution is dispersed into micro-droplets in the micron level, and the introduction of the n-butyl aldehyde is not only for providing power, but 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 the reaction rate of the alkali solution on the condensation reaction.
In the invention, the number of the first micro-interface generator and the second micro-interface generator can be only one, or can be a plurality of micro-interface generators which are mutually connected in series or in parallel, and when the number of the micro-interface generators is a plurality of micro-interface generators which are mutually connected in parallel, the outlets of two adjacent micro-interface generators are opposite, so that two opposite micro-droplet flows can be utilized to form a hedging flow, the dispersion uniformity of alkali liquor micro-droplets in n-butyraldehyde is improved, and the catalytic effect is improved.
In the invention, the outlets of the first micro-interface generator and the second micro-interface generator are respectively provided with the distribution disc, so that the micro-droplets are promoted to be uniformly distributed in the n-butyraldehyde through the distribution discs, and the uniformity of two-phase mixing is improved. During reaction, one part of micro liquid drops flow and disperse around the surface of the distribution plate, and the other part of micro liquid drops are distributed in different directions through the through holes in the distribution plate.
When the micro-interface strengthening system for preparing the octenal by condensing the n-butyraldehyde is used, a rectifying tower is not needed, because the material conversion rate basically meets the requirement after two reactions in the reactor and rectification is not needed again. Therefore, the system of the invention has small integral occupied area and convenient use.
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, the n-butyraldehyde inlet is connected with a n-butyraldehyde pipeline, and the alkali liquor inlet is connected with an alkali liquor pipeline.
Preferably, the bottom of the chromatographic device is provided with an alkali liquor outlet, and the alkali liquor outlet is connected with the alkali liquor pipeline.
Preferably, a production outlet is arranged at the bottom of the decanter, and the production outlet is connected with the second condenser; and a product separated by the chromatograph is extracted through an extraction port, and is extracted after exchanging heat with a material flow flowing out of the second circulating pipeline in the second condenser.
Preferably, the top of the chromatographic device is provided with a non-condensable gas outlet.
The invention also provides a preparation method of the micro-interface strengthening system for preparing octenal by adopting the condensation of n-butyraldehyde, which comprises the following steps:
after the alkali liquor is broken into micro-droplets in the micron level through a micro interface, n-butyl aldehyde is catalyzed to carry out condensation reaction, and the product octenal is obtained.
Preferably, the condensation reaction temperature is 110-120 ℃, and the pressure is 0.1-0.8 MPa. Further, the condensation reaction temperature is 114-.
The octenal product obtained by the reaction method of the invention 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 invention has the beneficial effects that:
according to the micro-interface strengthening system for preparing the octenal by condensing the n-butyraldehyde, the reactor is divided into the upper reaction zone and the lower reaction zone, so that the raw materials are subjected to two reactions, the raw material reaction is more sufficient, and the conversion rate of the raw materials is improved; the first micro-interface generator and the second micro-interface generator are respectively arranged in the first reaction area and the second reaction area, and the micro-interface generator is used for dispersing and crushing the alkali liquor into micro-droplets of micron level and then dispersing the micro-droplets into the n-butyl aldehyde solution, so that the uniformity of two-phase distribution is improved, the droplets are uniform in shape and small in diameter, the mass transfer rate is greatly improved, the temperature required by the reaction is reduced, and the product yield is improved.
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 invention. 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 micro-interface enhancement system for preparing octenal by condensation of n-butyraldehyde according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a reactor provided in an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a distribution plate according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a reaction system for producing octenal by condensation of n-butanol according to comparative example 2 of the present invention.
Description of the drawings:
10-a reactor; 20-a first reaction zone;
201-alkali liquor inlet; 202-n-butyraldehyde inlet;
203-a first micro-interface generator; 204-a distribution disk;
205-a via hole;
30-a second reaction zone; 301-a second micro-interface generator;
302-product outlet; 40-an alkaline liquor line;
a 50-n-butyraldehyde line; 60-a first recycle line;
70-a second circulation line; 80-a first condenser;
90-a second condenser; 100-a chromatography device;
1001-alkali liquor outlet; 1002-extraction outlet;
1003-noncondensable gas outlet; 110-a partition plate.
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.
Examples
Referring to fig. 1-3, the present embodiment provides a system for enhancing micro-interface of n-butyraldehyde condensation to produce octenal, comprising: a reactor 10; a partition plate 110 is arranged in the reactor 10, and the internal space of the reactor 10 is divided into two mutually independent spaces along the partition plate 110; below the partition plate 110 is a first reaction zone 20, above the partition plate is a second reaction zone 30; the reactor 10 may be a reaction kettle, a reaction tower or a reaction tank.
As shown in FIG. 2, the sidewall of the first reaction zone 20 is provided with a n-butyraldehyde inlet 202 and an alkali liquor inlet 201, the n-butyraldehyde inlet 202 is connected with a n-butyraldehyde pipeline 50, and the alkali liquor inlet 201 is connected with an alkali liquor pipeline 40. A first micro-interface generator 203 is arranged in the first reaction zone 20, the first micro-interface generator 203 is connected with the n-butyraldehyde inlet 202 and the alkali liquor inlet 201, and the alkali liquor is dispersed and crushed into micron-level micro-droplets by the first micro-interface generator 203 and then enters the first reaction zone 20 to catalyze the n-butyraldehyde to carry out condensation reaction.
With continued reference to fig. 2, a second micro-interface generator 301 is disposed in the second reaction zone 30, the first reaction zone 20 is connected to a first circulation line 60, an inlet of the first circulation line 60 is connected to the first reaction zone 20, and an outlet of the first circulation line 60 is connected to the first micro-interface generator 203 and the second micro-interface generator 301, respectively.
The micro-interface enhancement system of the present embodiment further comprises a second condenser 90 and a chromatograph 100; a product outlet 302 is arranged on the side wall of the second reaction zone 30, the product outlet 302 is connected with a second circulating pipeline 70, and a first condenser 80 is arranged on the second circulating pipeline 70; one part of the material circulated in the second circulation line 70 is condensed by the first condenser 80 and then flows back to the second micro-interface generator 301, and the other part is condensed by the second condenser 90 and then flows into the decanter 100.
As shown in fig. 3, a distribution plate 204 is disposed at the outlet of each of the first micro-interface generator 203 and the second micro-interface generator 301. The distribution plate 204 is conical, and a plurality of through holes 205 are vertically arranged on the distribution plate 204.
In this embodiment, the bottom of the chromatography device 100 is provided with an alkaline solution outlet 1001, and the alkaline solution outlet 1001 is connected to the alkaline solution pipeline 40. The bottom of the decanter 100 is provided with a production outlet 1002, and the production outlet 1002 is connected with the second condenser 90; the product separated by the decanter 100 is extracted through an extraction port 1002, and is extracted after heat exchange with the stream flowing out from the second circulating line 70 in the second condenser 90. The top of the decanter 100 is provided with a noncondensable gas outlet 1003 for discharging noncondensable gas.
During reaction, n-butyraldehyde and alkali liquor respectively enter the first micro-interface generator 203, the alkali liquor is dispersed and crushed into micron-level micro-droplets in the first micro-interface generator 203 and then is mixed with the n-butyraldehyde to catalyze the condensation of the n-butyraldehyde to generate octenal; the reacted materials flow into the second reaction zone 30 through the first circulation pipeline 60 and are further dispersed and crushed in the second micro-interface generator 301, n-butyraldehyde which is not reacted continues to react, the generated products enter the chromatograph 100 after being condensed by the second condenser 90, octenal which is separated by chromatography is extracted from the extraction port 1002, one part of mixed alkali liquor is directly discharged, and the other part flows back to the alkali liquor pipeline 40 to continuously participate in the reaction.
Comparative example 1
The present example differs from the embodiment only in that the first and second micro-interface generators are not provided in the present example.
Comparative example 2
As shown in FIG. 4, the difference between this example and the embodiment is that in this example, there is no partition board inside the reactor 10, there is an integral reaction space inside the reactor 10, the first micro-interface generator 203 and the second micro-interface generator 301 are both disposed therein, and the first micro-interface generator 203 and the second micro-interface generator 301 are both connected to the n-butyraldehyde pipeline and the alkali liquid pipeline, and the reaction product is condensed by the second condenser and then enters the layer analyzer for purification and separation to obtain DMC.
The preparation of octenal was carried out at different temperatures and pressures in the systems of examples and comparative examples, wherein the temperature of experimental example 1 was 110 ℃ and the pressure was 0.1 MPa;
the temperature of experimental example 2 was 114 ℃ and the pressure was 0.2 MPa;
the temperature of Experimental example 3 was 115 ℃ and the pressure was 0.3 MPa;
the temperature of Experimental example 4 was 117 ℃ and the pressure was 0.4 MPa;
the temperature in Experimental example 5 was 120 ℃ and the pressure was 0.8 MPa.
The specific process parameters are as follows:
experimental example 1 parameter Table
Experimental example 2 parameter Table
Experimental example 3 parameter Table
Experimental example 4 parameter Table
Experimental example 5 parameter Table
Therefore, the micro-interface strengthening system for preparing the octenal by condensing the n-butyraldehyde can improve the space-time yield of the reaction, the yield of the octenal and the energy efficiency and physical efficiency under the conditions of reducing the operation temperature and the space time of the reaction.
In a word, compared with the reaction system for preparing the octenal by condensing the n-butyraldehyde in the prior art, the micro-interface strengthening system for preparing the octenal by condensing the n-butyraldehyde 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 invention 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 (10)
1. A micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde, comprising: a reactor; a partition plate is arranged in the reactor, and the internal space of the reactor is divided into two mutually independent spaces along the partition plate; the space below the partition plate is a first reaction zone;
the side wall of the first reaction zone is provided with a n-butyraldehyde inlet and an alkali liquor inlet, a first micro-interface generator is arranged in the first reaction zone, the first micro-interface generator is connected with the n-butyraldehyde inlet and the alkali liquor inlet, and alkali liquor enters the first reaction zone to catalyze the n-butyraldehyde to carry out condensation reaction after being dispersed and crushed into micron-level micro-droplets by the first micro-interface generator.
2. The system of claim 1, wherein a second reaction zone is located above the separation plate; the second reaction zone is internally provided with a second micro-interface generator, the first reaction zone is connected with a first circulating pipeline, the inlet of the first circulating pipeline is connected with the first reaction zone, and the outlet of the first circulating pipeline is respectively connected with the first micro-interface generator and the second micro-interface generator.
3. The system of claim 2, further comprising a second condenser and a decanter; a product outlet is formed in the side wall of the second reaction zone, the product outlet is connected with a second circulating pipeline, and a first condenser is arranged on the second circulating pipeline; and one part of the material circulated by the second circulation pipeline flows back to the second micro-interface generator after being condensed by the first condenser, and the other part of the material flows into the decanter after being condensed by the second condenser.
4. The system of claim 2, wherein the outlets of the first micro-interface generator and the second micro-interface generator are both provided with a distribution plate.
5. The system of claim 4, wherein the distribution plate is tapered and has a plurality of through holes formed therein.
6. The micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde according to claim 3, wherein the n-butyraldehyde inlet is connected to a n-butyraldehyde pipeline, and the lye inlet is connected to a lye pipeline.
7. The micro-interface enhancement system for preparing octenal by condensing n-butyraldehyde according to claim 6, wherein the bottom of the chromatograph is provided with a lye outlet, and the lye outlet is connected with the lye pipeline.
8. The micro-interface enhancement system for preparing octenal by condensing n-butyraldehyde according to claim 7, wherein a withdrawal port is provided at the bottom of the decanter, and the withdrawal port is connected to the second condenser; and a product separated by the chromatograph is extracted through an extraction port, and is extracted after exchanging heat with a material flow flowing out of the second circulating pipeline in the second condenser.
9. The method for preparing the micro-interface strengthening system for preparing the octenal by condensing the n-butyraldehyde according to any one of claims 1 to 8, comprising the steps of:
after the alkali liquor is broken into micro-droplets in the micron level through a micro interface, n-butyl aldehyde is catalyzed to carry out condensation reaction, and the product octenal is obtained.
10. The reaction process as claimed in claim 9, wherein the condensation reaction temperature is 110-120 ℃ and the pressure is 0.1-0.8 MPa; preferably, the condensation reaction temperature is 114-.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110793921.8A CN113548951A (en) | 2021-07-14 | 2021-07-14 | Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde and preparation method |
| PCT/CN2021/109754 WO2023284024A1 (en) | 2021-07-14 | 2021-07-30 | Micro-interface strengthening system for preparing octenal by n-butyraldehyde condensation, and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110793921.8A CN113548951A (en) | 2021-07-14 | 2021-07-14 | Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113548951A true CN113548951A (en) | 2021-10-26 |
Family
ID=78131707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110793921.8A Pending CN113548951A (en) | 2021-07-14 | 2021-07-14 | Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde and preparation method |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN113548951A (en) |
| WO (1) | WO2023284024A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117229133A (en) * | 2023-11-16 | 2023-12-15 | 天津渤化工程有限公司 | Octenal preparation process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260149A (en) * | 2010-05-25 | 2011-11-30 | 上海焦化有限公司 | Preparation process of 2-ethyl hexenal and 2-ethyl hexanol |
| CN112933630A (en) * | 2021-01-29 | 2021-06-11 | 南京华基塔业有限公司 | Intelligent micro-interface reaction system and method for preparing lactide from lactic acid |
| CN112934139A (en) * | 2021-01-29 | 2021-06-11 | 南京华基塔业有限公司 | Reinforced micro-interface reaction system and method for preparing lactide from lactic acid |
| CN113019291A (en) * | 2021-03-23 | 2021-06-25 | 南京延长反应技术研究院有限公司 | Octanol production system and method |
| CN113045387A (en) * | 2021-03-23 | 2021-06-29 | 南京延长反应技术研究院有限公司 | Reaction system and method for preparing butanol and octanol through propylene carbonylation |
| CN113058517A (en) * | 2021-03-23 | 2021-07-02 | 南京延长反应技术研究院有限公司 | Micro-interface preparation device and method for butanol and octanol |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201785324U (en) * | 2010-05-25 | 2011-04-06 | 上海焦化有限公司 | Reactive system for producing 2-ethyl hexenoicaldehyde from butyric aldehyde |
| EP2925714B1 (en) * | 2012-11-30 | 2016-11-16 | Basf Se | Method for the catalytic aldol condensation of aldehydes |
| US10377690B1 (en) * | 2018-08-22 | 2019-08-13 | Eastman Chemical Company | Method for catalytic production of refined enal products from an aldehyde feed stream using a single enclosed unit |
| CN112479815A (en) * | 2019-09-12 | 2021-03-12 | 南京延长反应技术研究院有限公司 | Reaction system and process for preparing butanol and octanol through propylene carbonylation based on micro-interface reinforcement |
| KR102675020B1 (en) * | 2019-10-08 | 2024-06-14 | 한화솔루션 주식회사 | Apparatus for aldol condensation |
| CN113061081A (en) * | 2021-04-01 | 2021-07-02 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced reaction system and method for preparing butyraldehyde by propylene carbonylation |
-
2021
- 2021-07-14 CN CN202110793921.8A patent/CN113548951A/en active Pending
- 2021-07-30 WO PCT/CN2021/109754 patent/WO2023284024A1/en active Application Filing
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260149A (en) * | 2010-05-25 | 2011-11-30 | 上海焦化有限公司 | Preparation process of 2-ethyl hexenal and 2-ethyl hexanol |
| CN112933630A (en) * | 2021-01-29 | 2021-06-11 | 南京华基塔业有限公司 | Intelligent micro-interface reaction system and method for preparing lactide from lactic acid |
| CN112934139A (en) * | 2021-01-29 | 2021-06-11 | 南京华基塔业有限公司 | Reinforced micro-interface reaction system and method for preparing lactide from lactic acid |
| CN113019291A (en) * | 2021-03-23 | 2021-06-25 | 南京延长反应技术研究院有限公司 | Octanol production system and method |
| CN113045387A (en) * | 2021-03-23 | 2021-06-29 | 南京延长反应技术研究院有限公司 | Reaction system and method for preparing butanol and octanol through propylene carbonylation |
| CN113058517A (en) * | 2021-03-23 | 2021-07-02 | 南京延长反应技术研究院有限公司 | Micro-interface preparation device and method for butanol and octanol |
Non-Patent Citations (1)
| Title |
|---|
| 高常春等: "正丁醛缩合制辛烯醛生产工艺优化", 《能源化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117229133A (en) * | 2023-11-16 | 2023-12-15 | 天津渤化工程有限公司 | Octenal preparation process |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2023284024A1 (en) | 2023-01-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2022198873A1 (en) | Octanol production system and method | |
| CN113045387A (en) | Reaction system and method for preparing butanol and octanol through propylene carbonylation | |
| CN113058517B (en) | Micro-interface preparation device and method for butanol and octanol | |
| CN113061081A (en) | Micro-interface enhanced reaction system and method for preparing butyraldehyde by propylene carbonylation | |
| US11919845B2 (en) | Reaction system and method for preparing butyraldehyde by propylene carbonylation | |
| WO2023284030A1 (en) | Instant dewatering dmc preparation system and preparation method | |
| CN112321409A (en) | Reaction system and method for preparing formic acid by carbon dioxide hydrogenation | |
| WO2023284031A1 (en) | Built-in instant dehydration micro-interface enhanced dmc preparation system and method | |
| CN113546583A (en) | Micro-interface preparation system and preparation method of DMC | |
| CN112010746A (en) | External micro-interface strengthening system and method for preparing acetic acid through methanol carbonylation | |
| CN216024790U (en) | Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde | |
| CN112479852A (en) | Preparation system and method of formic acid | |
| CN113548951A (en) | Micro-interface strengthening system for preparing octenal by condensing n-butyraldehyde and preparation method | |
| CN216024781U (en) | N-butyraldehyde condensation reaction system based on micro-interface | |
| CN113479851B (en) | Micro-interface enhanced oxidation system and oxidation method for preparing hydrogen peroxide | |
| CN113546589A (en) | System and method for preparing DMC (dimethyl formamide) through micro-interface reinforcement | |
| CN112657430A (en) | Micro-interface reaction system and method for preparing formic acid by carbon dioxide hydrogenation | |
| CN215480653U (en) | System for preparing octenal by condensing n-butyraldehyde | |
| CN112403006A (en) | Enhanced micro-interface reaction system and method for preparing formic acid by carbon dioxide hydrogenation | |
| CN216778779U (en) | A micro-interface preparation system of trimellitic acid | |
| CN215540715U (en) | Built-in instant dehydration micro-interface strengthening DMC preparation system | |
| CN216024809U (en) | 2-methyl tetrahydrofuran's micro-interface preparation system | |
| CN214598924U (en) | Micro-interface preparation device of butanol and octanol | |
| CN215540720U (en) | System for preparing DMC (dimethyl formamide) through micro-interface strengthening | |
| CN113680286B (en) | Propylene carbonylation reaction system and method with recyclable catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211026 |