CN112457155A - Intelligent enhanced production system and process of 1, 4-butanediol - Google Patents

Intelligent enhanced production system and process of 1, 4-butanediol Download PDF

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CN112457155A
CN112457155A CN201910839975.6A CN201910839975A CN112457155A CN 112457155 A CN112457155 A CN 112457155A CN 201910839975 A CN201910839975 A CN 201910839975A CN 112457155 A CN112457155 A CN 112457155A
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reaction
reaction device
butanediol
micro
production system
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张志炳
周政
孟为民
王宝荣
杨高东
罗华勋
张锋
李磊
杨国强
田洪舟
曹宇
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Nanjing Institute of Microinterface Technology Co Ltd
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Nanjing Institute of Microinterface Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/09Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
    • C07C29/095Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of organic acids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/04Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds
    • C07C67/05Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds with oxidation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/28Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group
    • C07C67/283Preparation of carboxylic acid esters by modifying the hydroxylic moiety of the ester, such modification not being an introduction of an ester group by hydrogenation of unsaturated carbon-to-carbon bonds

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention is suitable for the technical field of butanediol production, and provides an intelligent enhanced production system and process of 1, 4-butanediol, wherein the system comprises the following steps: the reaction device comprises a first reaction device, a second reaction device and a third reaction device; the micro-interface generator comprises a first micro-interface generator and a second micro-interface generator, and is respectively positioned at the bottom of the first reaction device and the bottom of the second reaction device; the mixing and stirring device comprises a guide rod, a fixed shell, a power shaft and a steering device, wherein the steering device comprises a fixed shaft, a rotating part and a guide wheel fixedly connected with the rotating part; the intelligent control device comprises a strategy setting unit, a parameter control unit and a model setting unit. Therefore, the invention can effectively improve the reaction efficiency and the working quality and can realize the intelligent regulation of the reaction parameters.

Description

Intelligent enhanced production system and process of 1, 4-butanediol
Technical Field
The invention relates to the technical field of butanediol production, in particular to an intelligent enhanced production system and process of 1,4 butanediol.
Background
1, 4-butanediol is one of methanol series product chains and is an important basic organic chemical and fine chemical raw material, a manufacturer generally does not use 1, 4-butanediol as a final product in the process of producing 1, 4-butanediol, but pays attention to the extension of a 1, 4-butanediol derivative, and the 1, 4-butanediol derivative is a fine chemical product with higher added value and is widely used as a solvent, a medicine, a cosmetic, a plasticizer, a curing agent, a pesticide, an herbicide, foamed artificial leather, fiber, engineering plastics and the like; because of the wide application and large consumption of 1, 4-butanediol, the production technology of 1, 4-butanediol needs to be improved continuously.
The production method of the 1, 4-butanediol mainly comprises the following steps: (1) a Reppe method (alkynal method) using formaldehyde and acetylene as raw materials; (2) butadiene acetoxylation with butadiene and acetic acid as raw materials; (3) a propylene oxide process using propylene oxide/propylene alcohol as a raw material; (4) davy method using n-butane/maleic anhydride as a raw material. Because butadiene and propylene oxide are in short supply in China, the 1, 4-butanediol produced by the two methods is not mature, the production method is selected according to resource advantages, and the Reppe method (acetylenic aldehyde method) is mainly used in China.
Butadiene acetoxylation with butadiene and acetic acid as raw materials is carried out by acetylating butadiene with acetic acid and oxygen to generate 1, 4-diacetyloxy butylene, catalytic hydrogenation to generate 1, 4-diene acetoxy butane, and hydrolyzing to obtain 1, 4-butanediol. However, the hydrogenation section of the prior art still has the following problems:
1. in order to promote the reaction in the hydrogenation section, manufacturers increase the amount of catalyst, and increase the production cost.
2. Because the amount of the catalyst in the hydrogenation section is increased, the incomplete reaction of the catalyst often occurs, the waste of the residual catalyst is caused, and the normal production of a subsequent system is influenced after the residual catalyst enters the subsequent system.
3. In the process of mixing hydrogen and slurry, a stirring dead angle still exists, and the problems of uneven stirring of hydrogen, catalyst and slurry still exist, so that the reaction in a hydrogenation working section is insufficient, and the yield of 1, 4-butanediol is influenced.
4. The agitation does not or does not completely break the bubbles of the hydrogen gas, and the hydrogen gas cannot be uniformly mixed with the slurry.
In view of the above, the prior art is obviously inconvenient and disadvantageous in practical use, and needs to be improved.
Disclosure of Invention
In view of the above-mentioned drawbacks, the present invention provides an intelligent enhanced production system and process for 1, 4-butanediol, which can effectively improve the working efficiency and the working quality.
In order to achieve the above object, the present invention provides an intelligent intensive production system of 1, 4-butanediol, comprising: the reaction device comprises a first reaction device, a second reaction device and a third reaction device, wherein the first reaction device is positioned above the second reaction device and is mutually connected through an output pipeline, the third reaction device is positioned on the side of the second reaction device, and a channel is arranged between the third reaction device and the second reaction device; the micro-interface generator comprises a first micro-interface generator and a second micro-interface generator which are respectively positioned at the bottoms of the first reaction device and the second reaction device, so that the gas is crushed to form micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm so as to improve the mass transfer area between the oxygen source solution and the gas, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the oxygen source solution and the micron-sized bubbles are mixed to form a gas-liquid emulsion after being crushed so as to enhance the mass transfer efficiency and the reaction efficiency between the oxygen source solution and the propylene gas within a preset operating condition range; mix agitating unit, mix agitating unit includes guide bar, set casing, power shaft and turns to the device, turn to the leading wheel that the device includes fixed axle, rotating member and fixed connection rotating member, the fixed axle passes through the elastic component and connects the rotating member tip, just be equipped with the stopper on the fixed axle, be equipped with the locating part on the set casing, be equipped with the auxiliary rod on the rotating member. The intelligent control device comprises a strategy setting unit, a learning strategy setting unit and a control unit, wherein the strategy setting unit is used for setting the range of reaction parameters and the learning strategy, and the reaction parameters at least comprise a first reaction parameter and a second reaction parameter; the parameter control unit is used for controlling the reaction parameters of the reaction device according to a preset strategy and the range of the reaction parameters; and the model setting unit is used for establishing a correlation model of the reaction parameters and the target object parameters. The learning strategy comprises: respectively acquiring a group of parameter data which accord with an arithmetic sequence from the first reaction parameter range and the second reaction parameter range, and recording the parameter data as a first reaction sequence and a second reaction sequence; each reaction, respectively acquiring data from the first reaction sequence and the second reaction sequence, and controlling reaction parameters according to the acquired data; traversing the first reaction sequence and the second reaction sequence; and intelligently selecting reaction parameters according to the established association model.
Further, install a plurality of inlet pipes and discharging pipe on reaction unit, the inlet pipe includes raw materials inlet pipe and additive inlet pipe, just first reaction unit is all connected to raw materials inlet pipe and additive inlet pipe, utilize raw materials inlet pipe and additive inlet pipe to carry out the water conservancy diversion to the raw materials and add the frame and add, make it effectively flow in first reaction unit, thereby can realize effective reaction in first reaction unit, improve reaction quality and reaction efficiency, in order to guarantee reaction quality, can set up the counter on raw materials inlet pipe and additive inlet pipe, this counter adopts the counter among the prior art, the counter that plays is for effectively measuring raw materials and additive dosage, thereby can effectively accurately add to the material of different volumes, and the quality of processing is improved.
Furthermore, a stirring device is arranged in the first reaction device, the stirring device comprises a driving shaft and a plurality of stirring rods positioned on the driving shaft, the stirring rods are provided with bending angles and are provided with three rows, the lengths of the three rows of stirring rods are sequentially shortened from top to bottom, so that the stirring periods from top to bottom are inconsistent in the stirring process, raw materials are further enabled to form vortex rotation, the raw materials can be conveyed into the second reaction device from an output pipeline of the second reaction device while being fully mixed, in order to ensure the conveying quality, the upper end of the output pipeline is arranged in an arc shape, the lower end of the whole second reaction device is arranged in a conical shape, the output pipeline is positioned at the conical tip end, the output efficiency and the output quality are improved, meanwhile, an electronic valve can be further arranged on the output pipeline, and the manual opening and closing time is reduced by, the working efficiency is improved, the electronic valve adopts the prior art, and the working principle and the connection structure are not described in detail.
Furthermore, the power shaft is connected with a driving part, the driving part is a motor, a thread structure is arranged on the power shaft, anti-skid lines are arranged on the guide wheel, the motor is used for driving the power shaft to rotate, and in the rotating process of the power shaft, the thread structure is arranged on the power shaft, so that the friction force between the power shaft and the guide wheel is enhanced, and the guide wheel can axially realize effective rotating movement along the power shaft. In order to ensure the effective movement of the guide wheel, the depth of the thread structure at the position is not too deep, namely about 1-3 cm, and the depth of the anti-skid thread is not too deep, namely about 0.5-1.5 cm.
Further, be equipped with on the set casing and hold the rotatory removal space of rotating member, just the guide bar is cup jointed to the set casing, when utilizing the set casing to inject the position of fixed axle and rotating member, can guarantee that the rotating member has sufficient removal space at rotatory in-process, utilizes the rotation of rotating member to drive the leading wheel and realizes rotatoryly, and then changes the direction of advance of leading wheel, improves work efficiency and operating mass with rated load.
Further, fixed axle upper end fixed connection set casing, the rotating member cup joints the fixed axle lower extreme, just the leading wheel passes through the rotation axis and connects the rotating member, utilizes the fixed axle to inject the position of rotating member, and the rotating member can be followed the radial realization of fixed axle and rotated simultaneously, and then guarantees that the rotating member can realize rotatoryly under the drive of elastic component, makes it drive the fixed connection leading wheel direction of rotation change with it, and then realizes that the leading wheel follows the cyclic shift of power shaft, improves work efficiency and operating mass with.
Further, the elastic component is a spring, the two ends of the spring are respectively connected with the fixed shaft and the rotating component through the fixed columns, reverse acting force is provided for rotation of the rotating component through the spring, the rotating component can rotate along with jacking of the limiting component when moving to the tail end, the elastic component can move reversely in the rotating process, when one of the two ends of the rotating component moves, the elastic component drives the rotating component to rotate under the elastic force of the elastic component, the direction of the rotating component is changed, and the direction of the guide wheel is changed.
Furthermore, two are symmetrically installed on the limiting part, the limiting part and the rotating part are both provided with buffering cushions, the buffering cushions are used for buffering the collision between the limiting part and the rotating part, the abrasion between the limiting part and the rotating part is reduced, the service life of the limiting part and the rotating part is further prolonged, and the manufacturing cost is reduced.
Furthermore, two are symmetrically installed on the limiting part, pulleys are arranged on the limiting part and the rotating part, the friction principle of the limiting part and the rotating part is changed by utilizing a wheel changing wheel, sliding friction of the wheel changing wheel is converted into rolling friction, the friction degree of the limiting part and the rotating part is further reduced, and the maintenance cost is reduced while the working efficiency and the working quality are improved.
A preparation process for preparing 1, 4-butanediol by using an intelligent enhanced production system of 1, 4-butanediol comprises the following steps:
A. adding butadiene into the first reaction device through the raw material feeding pipe, adding an additive into the first reaction device through the additive feeding pipe, wherein the additive is an iron-molybdenum catalyst, and the ratio of the butadiene to the iron-molybdenum catalyst is 1: 0.2;
B. step A, in the reaction process, adding oxygen into a first reaction device through a raw material feeding pipe, wherein the oxygen content of the oxygen is 18%;
C. b, generating 1, 4-diacetoxy and 2-butene in the reaction process, wherein in the reaction process, a Raney nickel catalyst needs to be added into a second reaction device, the content of the Raney nickel catalyst is 0.5, the reaction temperature in the process is 20-70 ℃, and the reaction pressure is 0.1-0.8 MPa;
D. step C, in the reaction process, adding hydrogen, wherein the content ratio of the hydrogen to the Raney nickel catalyst is 1.5:0.6, introducing the hydrogen and the 1, 4-diacetoxy group into a second micro-interface generator after adding the hydrogen, crushing the large hydrogen bubbles by the micro-interface generator to form micron-sized bubbles, wherein the diameter of the micron-sized bubbles is more than or equal to 1 mu m and less than 1mm, and fully mixing the micron-sized bubbles with the 1, 4-diacetoxy group to form a gas-liquid emulsion containing the 1, 4-diacetoxy group;
E. and D, introducing the gas-liquid emulsion formed in the step D into a third reaction device, and hydrolyzing the 1, 4-diacetoxy gas-liquid emulsion in the third reaction device to obtain 1, 4-butanediol.
Compared with the prior art, the invention has the beneficial effects that: the bubbles in the reaction process are crushed by the micro-interface generator to form micron-sized bubbles with micron scale, and the micron-sized bubbles are mixed with the raw material liquid to form gas-liquid emulsion, so that the phase interface area of gas-liquid two phases is increased, and the effect of strengthening mass transfer within a lower preset operation condition range is achieved; meanwhile, the reaction device is provided with the mixing and stirring device, the reaction device is circularly moved and stirred by the mixing and stirring device, and the gas-liquid phase mixing area is increased, so that the mixing quality and the mixing efficiency are improved, the materials can be effectively and fully mixed in the reaction process, and the reaction is fully and effectively carried out.
In addition, the range of the mixing and stirring device can be flexibly adjusted according to different product requirements or different catalysts, so that the full and effective reaction is further ensured, the reaction rate is further ensured, and the purpose of strengthening the reaction is achieved.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is an enlarged schematic view of FIG. 1 at 3;
FIG. 3 is a schematic view showing the construction of a rotating member and a fixed shaft according to the present invention;
FIG. 4 is a schematic view of the construction of the rotary member and guide wheel of the present invention;
FIG. 5 is a top view of a stationary shaft according to the present invention;
FIG. 6 is a schematic diagram of the process steps in the present invention;
in the figure, 11-the first reaction unit, 111-the raw material inlet, 112-the additive inlet, 12-the second reaction unit, 121-the conveying pipe, 122-the channel, 13-the third reaction unit, 131-the material pipe, 132-the outlet, 2-the output pipe, 3-the mixing and stirring device, 31-the guide rod, 32-the stationary housing, 33-the power shaft, 34-the limit piece, 41-the driving shaft, 42-the stirring rod, 51-the first micro-interface generator, 52-the second micro-interface generator, 61-the stationary shaft, 611-the limit piece, 62-the rotating member, 63-the guide wheel, 64-the auxiliary rod, 65-the elastic member.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and embodiments, it being understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; 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 by those skilled in the art according to specific situations.
Referring to fig. 1 to 5, the present invention provides an intelligent enhanced production system for 1, 4-butanediol, comprising: the reaction device comprises a first reaction device 11, a second reaction device 12 and a third reaction device 13, wherein the first reaction device 11 is positioned above the second reaction device 12 and is connected with the second reaction device 12 through an output pipeline 2, the third reaction device 13 is positioned at the side of the second reaction device 12, and a channel 122 is arranged between the third reaction device 13 and the second reaction device 12; a micro-interface generator, which comprises a first micro-interface generator 51 and a second micro-interface generator 52, and is respectively positioned at the bottom of the first reaction device 11 and the second reaction device 12; mix agitating unit 3, mix agitating unit 3 includes guide bar 31, set casing 32, power shaft 33 and turns to the device, turn to the device and include fixed axle 61, rotating member 62 and the leading wheel 63 of fixed connection rotating member 62, fixed axle 61 passes through elastic component 65 and connects the end of rotating member 62, just be equipped with stopper 611 on the fixed axle 61, be equipped with locating part 34 on the set casing 32, be equipped with auxiliary rod 64 on the rotating member 62.
When the device is operated, raw materials and additives enter the first reaction device 11 from the raw material inlet 111 and the additive inlet 112, wherein the raw materials are butadiene, and the additives are iron-molybdenum catalysts. The driving part drives the driving shaft 41 and the stirring rod 42 positioned on the driving shaft 41 to rotate, and in the rotating process, the stirring rod 42 is used for fully stirring the raw materials and the additives to realize mixing. Adding oxygen in the reaction process of butadiene and the iron-molybdenum catalyst, and reacting the butadiene, the iron-molybdenum catalyst and the oxygen to form 1, 4-diacetoxy and 2-butene. Since the stirring rod 42 has a curvature and the length thereof is sequentially shortened from top to bottom, in the stirring process, the stirring range is inconsistent, and the mixed material is swirled during stirring, and the output pipe 2 is located at the bottom of the swirled material, so that the 1, 4-diacetoxy group can be effectively discharged, and the 2-butene is discharged through the exhaust pipe, which adopts the prior art, i.e., a pipe having a reflux valve, which is not described in detail herein.
The stirred 1, 4-diacetyloxy is conveyed into a second reaction device 12 through an output pipeline 2, and in the output process, because a first micro-interface generator 51 is arranged at the bottom of a first reaction device 11, the micro-interface generator is a pneumatic micro-interface generator, bubbles formed by the 1, 4-diacetyloxy in the conveying process are crushed by the micro-interface generator, micron-scale bubbles are formed, the gas-liquid phase mixing efficiency of the micron-scale bubbles is improved, the full mixing of the micron-scale bubbles is realized, and the working quality is improved.
The reacted 1, 4-diacetoxy solution is conveyed into and out of the pipeline 2 to the second reaction device 12, the second reaction device 12 is connected with the conveying pipeline 121, the conveying pipeline 121 is used for effectively conveying the required reaction substances in the second reaction device 12, the substances are hydrogen and Raney nickel catalysts, the substances are subjected to mixing reaction with the 1, 4-diacetoxy solution formed by reaction in the first reaction device 11, in order to enhance the mixing degree of the substances and achieve full mixing, the mixing and stirring device 3 is arranged below the second reaction device 12, and the substances in the second reaction device 12 are effectively stirred by the mixing and stirring device 3, so that the substances are fully mixed. When the mixing and stirring device 3 is used for mixing and stirring, the power shaft 33 is driven by the motor to rotate, and in the rotating process, because the power shaft 33 and the guide wheel 63 are provided with gear structures or anti-skid lines which are matched and meshed with each other, when the power shaft 33 rotates, the guide wheel 63 can move along the axial direction of the power shaft 33, and the moving direction of the guide wheel is determined according to the inclined direction of the guide wheel 63. When the guide wheel 63 is in an initial state, an inclined included angle is formed between the guide wheel and the axial direction of the power shaft 33, the included angle is 15-30 degrees, and the optimal angle is 25 degrees. The power shaft 33 drives the guide wheel 63 to rotate in the rotating process, so that the guide wheel is moved along the axial direction of the power shaft 33, when the power shaft is moved to the tail end, the rotating part 62 connected with the guide wheel 63 abuts against the limiting part 43, and under the continuous rotation of the power shaft 33, the rotating part 62 is rotated under the action of the elastic part 65 and drives the guide wheel 63 to rotate, the rotating angle and the initial state form a central symmetry angle, so that the moving direction of the guide wheel 63 is enabled to move in the reverse direction, and further the auxiliary rod 64 is enabled to be driven to move in the second reaction device 12, materials in the second reaction device 12 are stirred, and the materials are enabled to be fully mixed. In the rotating process of the rotating member 62, in order to ensure the rotating range, a limiting block 611 needs to be installed on the fixed shaft 61, the limiting block 611 is installed in an arc shape, the arc shape of the limiting block 611 is semicircular, the rotating member 62 moves in an arc-shaped space formed by the limiting block 611 and the fixed shaft 61, the length of the rotating member 62 is blocked by the limiting block 611, and the influence of the too large rotating range on the moving direction of the guide wheel 63 is prevented.
In order to prevent the 1, 4-diacetoxy solution and hydrogen from generating bubbles during the reaction process and affecting the sufficient mixing, a second micro-interface generator 52 is arranged below the second reaction device 12, and the micro-interface generator is a hydrodynamic type or gas-liquid linkage type micro-interface generator, so that the bubbles generated during the stirring process are broken to form micron-sized bubbles, the contact area of the bubbles is enlarged, the reaction residence time of the bubbles in the second reaction device 12 is prolonged, and the bubbles are sufficiently mixed to form a 1, 4-diacetoxy gas-liquid emulsion.
The stirred 1, 4-diacetoxy gas-liquid emulsion flows into a third reaction device 13 through a channel, a material pipeline 131 and a discharge port 132 are installed on the third reaction device 13, the third reaction device 13 is used for hydrolyzing the 1, 4-diacetoxy gas-liquid emulsion to obtain 1, 4-butanediol, and the reacted 1, 4-butanediol flows into an aggregate device through the discharge port 132 to be collected. In order to improve the working efficiency and the working quality, the pipelines installed on each reaction device are controlled by electromagnetic valves, the flowability and the flow of materials are effectively and accurately controlled by the electromagnetic valves, and the working efficiency and the working quality are improved.
The intelligent control device comprises a strategy setting unit, a learning strategy setting unit and a control unit, wherein the strategy setting unit is used for setting the range of reaction parameters and the learning strategy, and the reaction parameters at least comprise a first reaction parameter and a second reaction parameter; the parameter control unit is used for controlling the reaction parameters of the reaction device according to a preset strategy and the range of the reaction parameters; and the model setting unit is used for establishing a correlation model of the reaction parameters and the target object parameters. The learning strategy comprises: respectively acquiring a group of parameter data which accord with an arithmetic sequence from the first reaction parameter range and the second reaction parameter range, and recording the parameter data as a first reaction sequence and a second reaction sequence; each reaction, respectively acquiring data from the first reaction sequence and the second reaction sequence, and controlling reaction parameters according to the acquired data; traversing the first reaction sequence and the second reaction sequence; and intelligently selecting reaction parameters according to the established association model.
Examples are: temperature 10-30 ℃, first sequence: … … 30 deg.C at 10 deg.C, 10.5 deg.C, 11 deg.C, 11.5 deg.C, and 11.5 deg.C;
pressure: 0.05-0.15 MPa, a first sequence: 0.05MPa, 0.06MPa, 0.07MPa, … … 0.15.15 MPa;
if the first reaction is carried out, the temperature-pressure is (10-0.05 MPa), and target object parameters are collected after the reaction is finished; and during the second reaction, the temperature-pressure is 10-0.06 MPa, the target object parameters are collected after the reaction is finished, and different data are selected from the sequence for each reaction until all data combinations are traversed.
The control and transmission of the temperature and the pressure are respectively realized by a control device and a sensor, the sensors are respectively a temperature sensor and a pressure sensor, the temperature and the pressure in the reaction device are sensed and transmitted by a control center, and then the temperature and the pressure are adjusted by the control device to be in accordance with the optimal reaction environment of reactants, so that the reaction efficiency is improved.
Example 1:
referring to fig. 6, a process for preparing 1, 4-butanediol using an intelligent enhanced production system of 1, 4-butanediol, comprising the steps of:
A. adding butadiene into the first reaction device 11 through a raw material feeding pipe 111, adding an additive into the first reaction device 11 through an additive feeding pipe 112, wherein the additive is an iron-molybdenum catalyst, and the ratio of the butadiene to the iron-molybdenum catalyst is 1: 0.2;
B. step A, in the reaction process, adding oxygen to a first reaction device 11 through a raw material feeding pipe 111, wherein the oxygen content of the oxygen is 18%;
C. b, generating 1, 4-diacetoxy and 2-butene in the reaction process, wherein in the reaction process, a Raney nickel catalyst needs to be added into the second reaction device 12, the content of the Raney nickel catalyst is 0.5, the reaction temperature in the process is 20-70 ℃, and the reaction pressure is 0.1-0.8 MPa;
D. step C, in the reaction process, hydrogen is required to be added, the ratio of the hydrogen content to the Raney nickel catalyst content is 1.5:0.6, after the hydrogen is added, the hydrogen and the 1, 4-diacetoxy group are introduced into a second micro-interface generator 52, the micro-interface generator breaks the large hydrogen bubbles to form micron-sized bubbles, and then the micron-sized bubbles and the 1, 4-diacetoxy group are fully mixed to form a gas-liquid emulsion containing the 1, 4-diacetoxy group;
E. and D, introducing the gas-liquid emulsion formed in the step D into a third reaction device 13, and hydrolyzing the gas-liquid emulsion of the 1, 4-diacetoxy in the third reaction device 13 to obtain the 1, 4-butanediol.
Wherein the reaction temperature in the reactor in the process is 20 ℃, the reaction pressure is 0.1MPa, and the molar ratio of the butadiene to the oxygen source solution is 1.2: 1, the space velocity of the catalyst is 1.20h-1(ii) a The gas-liquid ratio in the first micro-interfacial generator 51 is 1100: 1, a gas-liquid ratio in the second micro-interfacial generator 52 of 500: 1.
after the system and the process are used, the conversion rate of butadiene is 97.5 percent.
Example 2:
a preparation process for preparing 1, 4-butanediol by using an intelligent enhanced production system of 1, 4-butanediol comprises the following steps:
A. adding butadiene into the first reaction device 11 through a raw material feeding pipe 111, adding an additive into the first reaction device 11 through an additive feeding pipe 112, wherein the additive is an iron-molybdenum catalyst, and the ratio of the butadiene to the iron-molybdenum catalyst is 1: 0.2;
B. step A, in the reaction process, adding oxygen to a first reaction device 11 through a raw material feeding pipe 111, wherein the oxygen content of the oxygen is 18%;
C. b, generating 1, 4-diacetoxy and 2-butene in the reaction process, wherein in the reaction process, a Raney nickel catalyst needs to be added into the second reaction device 12, the content of the Raney nickel catalyst is 0.5, the reaction temperature in the process is 20-70 ℃, and the reaction pressure is 0.1-0.8 MPa;
D. step C, in the reaction process, hydrogen is required to be added, the ratio of the hydrogen content to the Raney nickel catalyst content is 1.5:0.6, after the hydrogen is added, the hydrogen and the 1, 4-diacetoxy group are introduced into a second micro-interface generator 52, the micro-interface generator breaks the large hydrogen bubbles to form micron-sized bubbles, and then the micron-sized bubbles and the 1, 4-diacetoxy group are fully mixed to form a gas-liquid emulsion containing the 1, 4-diacetoxy group;
E. and D, introducing the gas-liquid emulsion formed in the step D into a third reaction device, and hydrolyzing the gas-liquid emulsion of the 1, 4-diacetoxy in the third reaction device 13 to obtain the 1, 4-butanediol.
Wherein the reaction temperature in the reactor in the process is 20 ℃, the reaction pressure is 0.1MPa, and the molar ratio of the butadiene to the oxygen source solution is 1.5: 1, the space velocity of the catalyst is 1.05h-1(ii) a The gas-liquid ratio in the first micro-interfacial generator 51 was 1200: 1, a gas-to-liquid ratio in the second micro-interfacial generator 52 of 450: 1.
after the system and the process are used, the conversion rate of butadiene is 95.5 percent.
Example 3:
a preparation process for preparing 1, 4-butanediol by using an intelligent enhanced production system of 1, 4-butanediol comprises the following steps:
A. adding butadiene into the first reaction device 11 through a raw material feeding pipe 111, adding an additive into the first reaction device 12 through an additive feeding pipe 112, wherein the additive is an iron-molybdenum catalyst, and the ratio of the butadiene to the iron-molybdenum catalyst is 1: 0.2;
B. step A, in the reaction process, adding oxygen to a first reaction device 11 through a raw material feeding pipe 111, wherein the oxygen content of the oxygen is 18%;
C. b, generating 1, 4-diacetoxy and 2-butene in the reaction process, wherein in the reaction process, a Raney nickel catalyst needs to be added into the second reaction device 12, the content of the Raney nickel catalyst is 0.5, the reaction temperature in the process is 20-70 ℃, and the reaction pressure is 0.1-0.8 MPa;
D. step C, in the reaction process, adding hydrogen, wherein the content ratio of the hydrogen to the Raney nickel catalyst is 1.5:0.6, introducing the hydrogen and the 1, 4-diacetoxy into a second micro-interface generator after adding the hydrogen, crushing the large hydrogen bubbles by the micro-interface generator to form micron-sized bubbles, and fully mixing the micron-sized bubbles with the 1, 4-diacetoxy to form a gas-liquid emulsion containing the 1, 4-diacetoxy;
E. and D, introducing the gas-liquid emulsion formed in the step D into a third reaction device 13, and hydrolyzing the gas-liquid emulsion of the 1, 4-diacetoxy in the third reaction device 13 to obtain the 1, 4-butanediol.
Wherein the reaction temperature in the reactor in the process is 20 ℃, the reaction pressure is 0.1MPa, and the molar ratio of the butadiene to the oxygen source solution is 1.9: 1, the space velocity of the catalyst is 0.7h-1(ii) a The gas-liquid ratio in the first micro-interface generator 51 is 1230: 1, gas-to-liquid ratio in the second micro-interfacial generator 52 is 490: 1.
after the system and the process are used, the conversion rate of butadiene is 98.0 percent.
Example 4
A preparation process for preparing 1, 4-butanediol by using an intelligent enhanced production system of 1, 4-butanediol comprises the following steps:
A. adding butadiene into the first reaction device 11 through a raw material feeding pipe 111, adding an additive into the first reaction device 12 through an additive feeding pipe 112, wherein the additive is an iron-molybdenum catalyst, and the ratio of the butadiene to the iron-molybdenum catalyst is 1: 0.2;
B. step A, in the reaction process, adding oxygen to a first reaction device 11 through a raw material feeding pipe 111, wherein the oxygen content of the oxygen is 18%;
C. b, generating 1, 4-diacetoxy and 2-butene in the reaction process, wherein in the reaction process, a Raney nickel catalyst needs to be added into the second reaction device 12, the content of the Raney nickel catalyst is 0.5, the reaction temperature in the process is 20-70 ℃, and the reaction pressure is 0.1-0.8 MPa;
D. step C, in the reaction process, adding hydrogen, wherein the content ratio of the hydrogen to the Raney nickel catalyst is 1.5:0.6, introducing the hydrogen and the 1, 4-diacetoxy into a second micro-interface generator after adding the hydrogen, crushing the large hydrogen bubbles by the micro-interface generator to form micron-sized bubbles, and fully mixing the micron-sized bubbles with the 1, 4-diacetoxy to form a gas-liquid emulsion containing the 1, 4-diacetoxy;
E. and D, introducing the gas-liquid emulsion formed in the step D into a third reaction device 13, and hydrolyzing the gas-liquid emulsion of the 1, 4-diacetoxy in the third reaction device 13 to obtain the 1, 4-butanediol.
Wherein the reaction temperature in the reactor in the process is 20 ℃, the reaction pressure is 0.1MPa, and the molar ratio of the butadiene to the oxygen source solution is 1.3: 1, the space velocity of the catalyst is 0.4h-1(ii) a The gas-liquid ratio in the first micro-interface generator 51 is 1010: 1, a gas-to-liquid ratio within the second micro-interfacial generator 52 of 410: 1.
after the system and the process are used, the conversion rate of butadiene is 96.3 percent.
Comparative example
The prior art is used for preparing 1,4 butanediol from butadiene, wherein the process parameters selected in the embodiment are the same as those in the embodiment 2.
After the system and the process are used, the conversion rate of butadiene is 93.0 percent.
Figure BDA0002193379460000131
Figure BDA0002193379460000141
In summary, an intelligent enhanced production system using 1, 4-butanediol comprises: the reaction device comprises a first reaction device, a second reaction device and a third reaction device, wherein the first reaction device is positioned above the second reaction device and is mutually connected through an output pipeline, the third reaction device is positioned on the side of the second reaction device, and a channel is arranged between the third reaction device and the second reaction device; the micro-interface generator comprises a first micro-interface generator and a second micro-interface generator, and is respectively positioned at the bottoms of the first reaction device and the second reaction device; mix agitating unit, mix agitating unit includes guide bar, set casing, power shaft and turns to the device, turn to the leading wheel that the device includes fixed axle, rotating member and fixed connection rotating member, the fixed axle passes through the elastic component and connects the rotating member tip, just be equipped with the stopper on the fixed axle, be equipped with the locating part on the set casing, be equipped with the auxiliary rod on the rotating member.
The invention has the beneficial effects that: the bubbles in the reaction process are crushed by the micro-interface generator to form micron-sized bubbles with micron scale, and the micron-sized bubbles are mixed with the raw material liquid to form gas-liquid emulsion, so that the phase interface area of gas-liquid two phases is increased, and the effect of strengthening mass transfer within a lower preset operation condition range is achieved; meanwhile, the reaction device is provided with the mixing and stirring device, the reaction device is circularly moved and stirred by the mixing and stirring device, and the gas-liquid phase mixing area is increased, so that the mixing quality and the mixing efficiency are improved, the materials can be effectively and fully mixed in the reaction process, and the reaction is fully and effectively carried out. In addition, the range of the mixing and stirring device can be flexibly adjusted according to different product requirements or different catalysts, so that the full and effective reaction is further ensured, the reaction rate is further ensured, and the purpose of enhancing the reaction is achieved
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. An intelligent enhanced production system of 1,4 butanediol, comprising:
the reaction device comprises a first reaction device, a second reaction device and a third reaction device, wherein the first reaction device is positioned above the second reaction device and is mutually connected through an output pipeline, the third reaction device is positioned on the side of the second reaction device, and a channel is arranged between the third reaction device and the second reaction device;
the micro-interface generator comprises a first micro-interface generator and a second micro-interface generator which are respectively positioned at the bottoms of the first reaction device and the second reaction device, so that the gas is crushed to form micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm so as to improve the mass transfer area between the oxygen source solution and the gas, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the oxygen source solution and the micron-sized bubbles are mixed to form a gas-liquid emulsion after being crushed so as to enhance the mass transfer efficiency and the reaction efficiency between the oxygen source solution and the propylene gas within a preset operating condition range;
the mixing and stirring device comprises a guide rod, a fixed shell, a power shaft and a steering device, wherein the steering device comprises a fixed shaft, a rotating part and a guide wheel fixedly connected with the rotating part, the fixed shaft is connected with the end part of the rotating part through an elastic part, a limiting block is arranged on the fixed shaft, a limiting part is arranged on the fixed shell, and an auxiliary rod is arranged on the rotating part;
the intelligent control device comprises a strategy setting unit, a learning strategy setting unit and a control unit, wherein the strategy setting unit is used for setting the range of reaction parameters and the learning strategy, and the reaction parameters at least comprise a first reaction parameter and a second reaction parameter; the parameter control unit is used for controlling the reaction parameters of the reaction device according to a preset strategy and the range of the reaction parameters; the model setting unit is used for establishing a correlation model of the reaction parameters and the target object parameters;
the learning strategy comprises: respectively acquiring a group of parameter data which accord with an arithmetic sequence from the first reaction parameter range and the second reaction parameter range, and recording the parameter data as a first reaction sequence and a second reaction sequence; each reaction, respectively acquiring data from the first reaction sequence and the second reaction sequence, and controlling reaction parameters according to the acquired data; traversing the first reaction sequence and the second reaction sequence; and intelligently selecting reaction parameters according to the established association model.
2. The intelligent enhanced production system of 1, 4-butanediol of claim 1, wherein the reaction device is provided with a plurality of feeding pipes and discharging pipes, the feeding pipes comprise a raw material feeding pipe and an additive feeding pipe, and the raw material feeding pipe and the additive feeding pipe are both connected with the first reaction device.
3. The intelligent enhanced production system of 1, 4-butanediol according to claim 1, wherein a stirring device is arranged in the first reaction device, the stirring device comprises a driving shaft and a plurality of stirring rods positioned on the driving shaft, the stirring rods have bending angles and are provided with three rows, and the lengths of the three rows of stirring rods are sequentially shortened from top to bottom.
4. The intelligent enhanced production system of 1, 4-butanediol of claim 1, wherein the power shaft is connected with a driving part, the driving part is a motor, the power shaft is provided with a thread structure, and the guide wheel is provided with anti-skid threads.
5. The intelligent enhanced production system of 1, 4-butanediol of claim 1, wherein the fixed shell is provided with a moving space for accommodating the rotation of the rotating member, and the fixed shell is sleeved with the guide rod.
6. The intelligent enhanced production system of 1, 4-butanediol of claim 1, wherein the upper end of the fixed shaft is fixedly connected with a fixed shell, the rotating member is sleeved on the lower end of the fixed shaft, and the guide wheel is connected with the rotating member through a rotating shaft.
7. The intelligent enhanced production system of 1, 4-butanediol of claim 1, wherein the elastic member is a spring, and two ends of the spring are respectively connected with the fixed shaft and the rotating member through fixed columns.
8. The system for intelligent and intensive production of 1, 4-butanediol as defined in claim 1, wherein there are two stoppers symmetrically mounted thereon, and the stoppers and the rotary member are provided with cushions.
9. The intelligent enhanced production system of 1, 4-butanediol of claim 1, wherein two limiting members are symmetrically arranged, and pulleys are arranged on the limiting members and the rotating members.
10. A process for preparing 1, 4-butanediol by using the intelligent enhanced production system of 1, 4-butanediol as claimed in any one of claims 1 to 9, comprising the steps of:
A. adding butadiene into the first reaction device through the raw material feeding pipe, adding an additive into the first reaction device through the additive feeding pipe, wherein the additive is an iron-molybdenum catalyst, and the ratio of the butadiene to the iron-molybdenum catalyst is 1: 0.2;
B. step A, in the reaction process, adding oxygen into a first reaction device through a raw material feeding pipe, wherein the oxygen content of the oxygen is 18%;
C. b, generating 1, 4-diacetoxy and 2-butene in the reaction process, wherein in the reaction process, a Raney nickel catalyst needs to be added into a second reaction device, the content of the Raney nickel catalyst is 0.5, the reaction temperature in the process is 20-70 ℃, and the reaction pressure is 0.1-0.8 MPa;
D. step C, in the reaction process, adding hydrogen, wherein the content ratio of the hydrogen to the Raney nickel catalyst is 1.5:0.6, introducing the hydrogen and the 1, 4-diacetoxy into a second micro-interface generator after adding the hydrogen, crushing the large hydrogen bubbles by the micro-interface generator to form micron-sized bubbles, and fully mixing the micron-sized bubbles with the 1, 4-diacetoxy to form a gas-liquid emulsion containing the 1, 4-diacetoxy;
E. and D, introducing the gas-liquid emulsion formed in the step D into a third reaction device, and hydrolyzing the 1, 4-diacetoxy gas-liquid emulsion in the third reaction device to obtain 1, 4-butanediol.
CN201910839975.6A 2019-09-06 2019-09-06 Intelligent enhanced production system and process of 1, 4-butanediol Pending CN112457155A (en)

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