WO2021103462A1

WO2021103462A1 - Intelligent strengthening reaction system and process for preparing isoformaldehyde by using olefin carbonylation

Info

Publication number: WO2021103462A1
Application number: PCT/CN2020/092636
Authority: WO
Inventors: 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
Original assignee: 南京延长反应技术研究院有限公司
Priority date: 2019-11-25
Filing date: 2020-05-27
Publication date: 2021-06-03
Also published as: CN112827433A

Abstract

The present invention relates to an intelligent strengthening reaction system and process for preparing isoformaldehyde by using olefin carbonylation, comprising: a reactor, a micro-interface generator, an intelligent control module, and so on. The work of the entire system is controlled by means of the intelligent control module; the reactor and the micro-interface generator cooperating to work together is controlled by means of a PLC controller, such that the quantity of raw material supply and the reactant generation amount are recorded, and a corresponding optimal technical parameter can be found according to the record in order to be reused. The addition of the intelligent control module enables the stability and continuity of the operation of the entire system, effectively improving production efficiency, and production efficiency is stable. Hydrogen and carbon monoxide are crushed by means of the micro-interface generator such that same forms micron-scale micron-level bubbles, so as to increase the contact area between a gas phase and a liquid phase as well as achieve the effect of strengthening mass transfer, effectively improving the conversion rate and efficiency of preparing isoformaldehyde.

Description

Intelligent enhanced reaction system and process for preparing isoformaldehyde from olefin carbonylation

Technical field

The invention relates to the technical field of isoformaldehyde preparation, in particular to an intelligent enhanced reaction system and process for preparing isoformaldehyde by olefin carbonylation.

Background technique

At room temperature, in addition to formaldehyde as a gas, aliphatic aldehydes with less than 12 carbon atoms in the molecule are liquids, higher aldehydes are solids, and aromatic aldehydes are liquids or solids. Low-grade fatty aldehydes have a strong pungent odor. Aldehydes with 9 carbon atoms in the molecule and 10 carbon atoms in the molecule have a floral and fruity scent, and are often used in the perfume industry.

Due to the polarity of the carbonyl group, the boiling point of aldehydes is higher than that of hydrocarbons and ethers with similar relative molecular weights; because the carbonyl group cannot form hydrogen bonds between molecules, the boiling point is lower than that of the corresponding alcohols. Aldehydes are important chemical raw materials.

The synthetic method of isoformaldehyde includes olefin carbonylation method. The carbonylation reaction is the reaction of introducing carbonyl groups into olefin molecules. In the presence of carbon monoxide and hydrogen, the olefin has one end of the double bond through high temperature, high pressure and the action of a catalyst. A hydrogen atom is introduced and a formyl group is introduced at the other end to generate an isomeric aldehyde.

In the above-mentioned existing methods for producing isoformaldehyde, especially liquid olefins, that is, liquid olefins with carbon atoms between 5 and 18 have the following problems in the process of preparing aldehydes:

The poor stability and continuity of the existing industrial systems for the production of isomeric aldehydes result in low production efficiency and large errors in the statistics of raw material consumption and product generation.

Summary of the invention

To this end, the present invention provides an intelligent intensified reaction system and process for preparing isoformaldehyde from olefin carbonylation, so as to improve the conversion rate and efficiency of preparing isoformaldehyde in the prior art.

In one aspect, the present invention provides an intelligent enhanced reaction system for preparing isoformaldehyde from olefin carbonylation, including:

The reactor is used to provide a reaction place for liquid olefins, hydrogen and carbon monoxide to prepare isoformaldehyde, the reactor is provided with a catalyst, and the reactor is composed of a fully mixed flow reaction zone and a reflux reaction zone; the fully mixed flow reaction zone, It is arranged below the reactor to load liquid olefins, hydrogen, carbon monoxide and catalysts and to provide a reaction space for the olefin carbonylation reaction; the reflux reaction zone is arranged above the reactor to remove The unreacted hydrogen and carbon monoxide are refluxed and the unreacted hydrogen and carbon monoxide are reacted with the olefin again;

A micro-interface generator, which converts the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transmits it to the gas reactant, and breaks the gas reactant into micron-sized bubbles with a diameter of ≥1μm and <1mm to improve the gas reaction The mass transfer area between the liquid reactant and the liquid reactant reduces the thickness of the liquid film and reduces the mass transfer resistance. After being broken, the liquid reactant and the micron-sized bubbles of the gas reactant are mixed to form a gas-liquid mixture to operate in a preset manner. Enhance the mass transfer efficiency and reaction efficiency between the liquid reactant and the gas reactant within the range of conditions;

An intelligent control module, which includes a PLC controller, a sensor, and a cloud processor. The sensor transmits the collected electrical signals to the cloud processor. The cloud processor performs screening and comparison in the cloud database according to the response parameters returned by the sensor. Send out the corresponding command to the PLC controller after the optimal control parameters are output;

A hydrogen purification unit, which is arranged on one side of the reactor and is used to purify the hydrogen entering the reactor;

The gas recovery unit is arranged on one side of the reactor to recover unreacted hydrogen and carbon monoxide.

Further, the micro-interface generator includes:

The first micro-interface generator is a pneumatic micro-interface generator, the first micro-interface generator is located in the fully mixed flow reaction zone in the reactor, and the first micro-interface generator is used to break hydrogen gas into micron scale After the crushing is completed, the micron-level bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture;

The second micro-interface generator is a pneumatic micro-interface generator, the second micro-interface generator is located in the fully mixed flow reaction zone in the reactor, and the second micro-interface generator is used to break carbon monoxide into micron scale After the crushing is completed, the micron-level bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture;

The third micro-interface generator is a hydraulic micro-interface generator, the third micro-interface generator is located in the reflux reaction zone in the reactor, and the third micro-interface generator is in contact with the external heat exchanger and the liquid The pump is used in conjunction to crush and entrain the unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor to form micron-sized micro-sized bubbles, mix the micro-sized bubbles with liquid olefin to form a gas-liquid mixture and the gas-liquid mixture Output to the fully mixed flow reaction zone to oppose the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again, and at the same time adjust all The homogeneity of the mixture in the reactor and the reaction temperature are described.

Further, the fully mixed flow reaction zone includes:

The hydrogen inlet pipe is connected to the first micro-interface generator, the hydrogen inlet pipe is provided with a first pump body and a first flow meter, and the hydrogen inlet pipe is used to transmit hydrogen to the first Micro-interface generator;

The carbon monoxide inlet pipe is connected to the second micro-interface generator, the carbon monoxide inlet pipe is provided with a second pump body and a second flow meter, and the carbon monoxide inlet pipe is used to transfer carbon monoxide to the second Micro-interface generator;

A material discharge pipe communicates with the lower end of the reactor, the material discharge pipe is provided with a third flow meter and a first electronic control valve, and the material discharge pipe is used to discharge products.

Further, the reflux reaction zone includes:

A reflux tube, one end of which is connected to the third micro-interface generator, and the other end is located at the upper part of the reflux reaction zone, the reflux tube is used to transfer unreacted hydrogen and carbon monoxide to the third micro-interface generator;

A gas discharge pipe connected to the upper end of the reactor, a fourth flow meter is arranged on the gas discharge pipe, and the gas discharge pipe is used to discharge unreacted hydrogen and carbon monoxide;

The material inlet pipe communicates with the upper part of the side wall of the reactor. The material inlet pipe is provided with a fifth pump body and a fifth flow meter. The material inlet pipe is used to add liquid to the reactor. Olefins.

Further, the hydrogen purification unit includes:

A hydrogen purification tank, which is connected to the hydrogen inlet pipe, a molecular sieve is arranged in the hydrogen purification tank, and the molecular sieve is used for purifying hydrogen;

An electric heating jacket, which is located on the side wall of the hydrogen purification tank, an electric resistance wire is arranged in the electric heating jacket, and the electric heating jacket is used to heat the hydrogen purification tank to remove the molecular sieve. Moisture so that the molecular sieve can be reused.

Further, the gas recovery unit is composed of a gas storage tank, which is commonly connected with the gas discharge pipe to store the unreacted hydrogen and nitric oxide mixed gas entering the inside of the gas storage tank, and the gas storage tank is discharged from the gas. A one-way valve is provided at the connection point of the pipe.

Further, the catalyst is composed of an organic metal complex solvent Co ₂ (CO) ₈ solution impregnated with a porous carrier.

Further, the PLC controller includes:

The first PLC controller is used to control the operation of the fully mixed flow reaction zone;

The second PLC controller is used to control the operation of the reflux reaction zone;

The third PLC controller is used to control the operation of the micro-interface generator;

Further, the sensor includes:

A plurality of temperature sensors, which are respectively arranged in the reactor, the hydrogen purification unit and the gas recovery unit, to monitor the temperature of the system;

A plurality of pressure sensors are respectively arranged in the reactor, the hydrogen purification unit and the gas recovery unit to monitor the system pressure.

In another aspect, the present invention provides an intelligent enhanced reaction process for preparing isoformaldehyde from olefin carbonylation, including:

Step 1: Control the operation of the fully mixed flow reaction zone through the first PLC controller, and at the same time control the operation of the reflux reaction zone through the second PLC controller. The control process is through the second PLC controller The operation of the fifth pump body is controlled to suck liquid olefin into the reactor through the material inlet pipe, and at the same time, the fifth flow meter measures the incoming amount of liquid olefin, which is controlled by the first PLC The device controls the operation of the first pump body and the second pump body, and sucks hydrogen and carbon monoxide to the first micro-interface generator and the second micro-interface through the hydrogen inlet pipe and the carbon monoxide inlet pipe, respectively Inside the generator

Step 2: Hydrogen is purified by the hydrogen purification unit during the process of entering the first micro-interface generator in the hydrogen inlet pipe;

Step 3: Control the operation of the micro-interface generator through the third PLC controller, and the specific control process is to control the first micro-interface generator through the third PLC controller to break hydrogen gas into micron-sized micrometers After the crushing is completed, the micron-level bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture, and the third PLC controls The second micro-interface generator is controlled by the second micro-interface generator to crush carbon monoxide to form micro-scale micro-scale bubbles, and after the crushing is completed, the micro-scale bubbles are output to the fully mixed flow reaction zone in the reactor and the fully mixed flow in the reactor Liquid olefins in the reaction zone are mixed to form a gas-liquid mixture, and olefins, hydrogen and carbon monoxide undergo carbonylation reaction to form isoformaldehydes;

Step 4: In step 3, the unreacted hydrogen and carbon monoxide rise to the top of the reactor, and the third micro-interface generator, heat exchanger and liquid pump are controlled by the third PLC controller. The unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor will form the unreacted hydrogen and carbon monoxide into micron-sized micro-sized bubbles, mix the micro-sized bubbles with liquid olefins to form a gas-liquid mixture, and output the gas-liquid mixture to the The fully mixed flow reaction zone is opposed to the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again;

Step 5: A small amount of hydrogen and carbon monoxide that are not entrained on the top of the reactor are discharged into the gas storage tank along the gas discharge pipe, and the fourth flowmeter measures the total amount of gas discharged;

Step 6: After the reaction is completed, the first PLC controller is used to control the first electronic control valve to open, the generated material is discharged along the material discharge pipe, and the third flow meter measures the amount of discharged material .

Compared with the prior art, the beneficial effect of the present invention is that the present invention controls the work of the entire system through an intelligent control module, in which the PLC controller controls the reactor and the micro-interface generator to work together, so that the raw material supply and the reactant generation The quantity is recorded, and the corresponding optimal technical parameters can be found according to the record for repeated use. The addition of the intelligent control module makes the entire system stable and continuous, effectively improving production efficiency and stable production efficiency.

The invention uses the micro-interface generator to break hydrogen and carbon monoxide to form micro-scale micro-sized bubbles. The micro-scale bubbles have physical and chemical properties that conventional bubbles do not have. The calculation formula for the volume and surface area of the sphere shows that the total volume does not change. In this case, the total surface area of bubbles is inversely proportional to the diameter of a single bubble. It can be seen that the total surface area of micron-sized bubbles is huge. The micron-sized bubbles are mixed with liquid olefin to form a gas-liquid mixture to increase the contact area of the gas-liquid two-phase and achieve Enhance the effect of mass transfer within the lower preset operating conditions, effectively improve the conversion rate and efficiency of preparing isoformaldehyde;

Further, a reactor is used to provide a reaction place for liquid olefins, hydrogen and carbon monoxide to prepare isoformaldehyde, the reactor is provided with a catalyst, and the reactor is composed of a fully mixed flow reaction zone and a reflux reaction zone; the fully mixed flow The reaction zone is arranged below the reactor to load liquid olefins, hydrogen, carbon monoxide and catalysts and to provide reaction space for the olefin carbonylation reaction; the reflux reaction zone is arranged above the reactor, Used to reflux unreacted hydrogen and carbon monoxide and make unreacted hydrogen and carbon monoxide react with olefins again;

Further, the micro-interface generator includes:

The third micro-interface generator is a hydraulic micro-interface generator, the third micro-interface generator is located in the reflux reaction zone in the reactor, and the third micro-interface generator is connected to an external heat exchanger and liquid The pump is used in conjunction to crush and entrain the unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor to form micron-sized micro-sized bubbles, mix the micro-sized bubbles with liquid olefin to form a gas-liquid mixture and the gas-liquid mixture Output to the fully mixed flow reaction zone to oppose the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again, and at the same time adjust all The homogeneity of the mixture in the reactor and the reaction temperature are described.

Further, the fully mixed flow reaction zone includes:

Further, the reflux reaction zone includes:

Further, the hydrogen purification unit includes:

Further, the PLC controller includes:

The first PLC controller controls the operation of the fully mixed flow reaction zone, while the second PLC controller controls the operation of the reflux reaction zone. The control process is that the second PLC controller controls the The fifth pump body works to suck liquid olefin into the reactor through the material inlet pipe, and at the same time, the fifth flow meter measures the incoming amount of liquid olefin, and the first PLC controller controls all the liquid olefins. The first pump body and the second pump body work to suck hydrogen and carbon monoxide into the first micro-interface generator and the second micro-interface generator through the hydrogen inlet pipe and the carbon monoxide inlet pipe, respectively ；

The operation of the micro-interface generator is controlled by the third PLC controller, and the specific control process is that the third PLC controller controls the first micro-interface generator to break hydrogen gas into micro-scale micro-sized bubbles and After the crushing is completed, the micron-sized bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture, and the third PLC controller controls the The second micro-interface generator breaks carbon monoxide into micron-sized micro-sized bubbles and outputs the micro-sized bubbles to the fully mixed flow reaction zone in the reactor and the fully mixed flow reaction zone in the reactor after the crushing is completed The liquid olefins mixed to form a gas-liquid mixture, olefins, hydrogen and carbon monoxide undergo carbonylation reaction to produce isoformaldehydes;

The third micro-interface generator, heat exchanger and liquid pump are controlled by the third PLC controller to break and entrain the unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor. Carbon monoxide is broken to form micron-sized micro-sized bubbles, the micro-sized bubbles are mixed with liquid olefin to form a gas-liquid mixture, and the gas-liquid mixture is output to the fully mixed flow reaction zone and the first micro-interface generator and the second micro The gas-liquid mixture output by the interface generator is hedged, so that unreacted hydrogen and carbon monoxide participate in the reaction again;

Further, the sensor includes:

Description of the drawings

Fig. 1 is a schematic structural diagram of an intelligent enhanced reaction system for preparing isoformaldehyde from olefin carbonylation according to the present invention.

Detailed ways

The preferred embodiments of the present invention will be described below with reference to the drawings. Those skilled in the art should understand that these embodiments are only used to explain the technical principles of the present invention, and are not intended to limit the protection scope of the present invention.

It should be noted that in the description of the present invention, the terms "upper", "lower", "left", "right", "inner", "outer" and other terms indicating the direction or positional relationship are based on the attached drawings. The direction or position relationship shown is only for ease of description, and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention.

In addition, it should be noted that, in the description of the present invention, unless otherwise clearly defined and limited, the terms "installed", "connected", and "connected" should be interpreted in a broad sense, for example, it may be a fixed connection or It is a detachable connection or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication between two components. For those skilled in the art, the specific meaning of the above-mentioned terms in the present invention can be understood according to specific circumstances.

Please refer to Figure 1, which is a schematic structural diagram of an intelligent intensified reaction system based on the carbonylation of olefins to prepare isoformaldehyde according to the present invention, including:

The reactor 1 is used to provide a reaction place for liquid olefins, hydrogen and carbon monoxide to prepare isoformaldehyde, the reactor is provided with a catalyst, and the reactor is composed of a fully mixed flow reaction zone 11 and a reflux reaction zone 12; the fully mixed flow The reaction zone is arranged below the reactor to load liquid olefins, hydrogen, carbon monoxide and catalysts and to provide a reaction space for the olefin carbonylation reaction; the reflux reaction zone is arranged above the reactor, Used to reflux the unreacted hydrogen and carbon monoxide and make the unreacted hydrogen and carbon monoxide react with olefins again;

A micro-interface generator, which converts the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transmits it to the gas reactant, and breaks the gas reactant into micron-sized bubbles with a diameter of ≥1μm and <1mm to improve the gas reaction The mass transfer area between the reactant and the liquid reactant reduces the thickness of the liquid film and reduces the mass transfer resistance. After being broken, the liquid reactant and the micron-sized bubbles of the gas reactant are mixed to form a gas-liquid mixture to operate in a preset manner. Enhance the mass transfer efficiency and reaction efficiency between the liquid reactant and the gas reactant within the range of conditions;

It is understandable that the cloud processor can be, but is not limited to, a computer. The computer includes cloud receiving, cloud computing, cloud storage, and cloud control. The cloud processor is electrically or wirelessly connected to the PLC controller and the sensor, and the cloud is connected to the computer. Sensors return data to receive, store the received data through all storage, analyze, filter and compare cloud databases through cloud computing, optimize the best control parameters, and control the PLC controller through cloud control, thereby quickly Accurately adjust the process parameters;

It is understandable that PLC is the abbreviation of Programmable Logic Controller. A PLC controller is a digital electronic device with a microprocessor. It is a digital logic controller used for automatic control and can load control instructions into the memory for storage and execution at any time. The programmable controller is a modular combination of internal CPU, instruction and data memory, input and output units, power supply modules, digital analog and other units. The PLC controller has been widely used in the current industrial control field. Its principle of controlling electrical appliances I won’t repeat it here;

Please continue to refer to Figure 1. The micro-interface generator includes:

The first micro-interface generator 21 is a pneumatic micro-interface generator, the first micro-interface generator is located in the fully mixed flow reaction zone in the reactor, and the first micro-interface generator is used to break hydrogen into micrometers After the crushing is completed, the micron-sized bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture;

The second micro-interface generator 22 is a pneumatic micro-interface generator, the second micro-interface generator is located in the fully mixed flow reaction zone in the reactor, and the second micro-interface generator is used to break carbon monoxide into micrometers. After the crushing is completed, the micron-sized bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture;

The third micro-interface generator 23 is a hydraulic micro-interface generator, the third micro-interface generator is located in the reflux reaction zone in the reactor, and the third micro-interface generator is connected to an external heat exchanger and The liquid pump is used in conjunction to break and entrain the unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor to form micron-scale micron-scale bubbles, mix the micron-scale bubbles with liquid olefins to form a gas-liquid mixture and The mixture is output to the fully mixed flow reaction zone to oppose the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again and adjust at the same time The homogeneity of the mixture in the reactor and the reaction temperature.

Please continue to refer to Figure 1, the fully mixed flow reaction zone includes:

The hydrogen gas inlet pipe 111 is connected to the first micro-interface generator. The hydrogen gas inlet pipe is provided with a first pump body 31 and a first flow meter 41. The hydrogen gas inlet pipe is used to transmit hydrogen to all The first micro-interface generator;

The carbon monoxide inlet pipe 112 communicates with the second micro-interface generator. The carbon monoxide inlet pipe is provided with a second pump body 32 and a second flow meter 42. The carbon monoxide inlet pipe is used to transfer carbon monoxide to the The second micro-interface generator;

The material discharge pipe 113 communicates with the lower end of the reactor. The material discharge pipe is provided with a third flow meter 43 and a first electronic control valve 51, and the material discharge pipe is used to discharge products.

Please continue to refer to Figure 1, the reflux reaction zone includes:

One end of the reflux tube 121 is connected to the third micro-interface generator, and the other end is located at the upper part of the reflux reaction zone. The reflux tube is used to transfer unreacted hydrogen and carbon monoxide to the third micro-interface generator ；

A gas discharge pipe 122 communicates with the upper end of the reactor, a fourth flow meter 44 is provided on the gas discharge pipe, and the gas discharge pipe is used to discharge unreacted hydrogen and carbon monoxide;

The material inlet pipe 123 communicates with the upper part of the side wall of the reactor. The material inlet pipe is provided with a fifth pump body 35 and a fifth flow meter 45, and the material inlet pipe is used to feed the reactor to the reactor. Add liquid olefin inside.

Please continue to refer to Figure 1. The hydrogen purification unit includes:

A hydrogen purification tank 61 is connected to the hydrogen inlet pipe, and a molecular sieve is arranged in the hydrogen purification tank, and the molecular sieve is used for purifying hydrogen;

An electric heating jacket 62 is located on the side wall of the hydrogen purification tank, an electric resistance wire is arranged in the electric heating jacket, and the electric heating jacket is used to heat the hydrogen purification tank to remove the molecular sieve. The moisture to make the molecular sieve reused.

Please continue to refer to FIG. 1, the gas recovery unit is composed of a gas storage tank 71, which is connected to the gas discharge pipe to store unreacted hydrogen and nitric oxide mixed gas that enters the gas storage tank. A one-way valve 81 is provided at the connection of the gas discharge pipe.

Further, the PLC controller includes:

The first PLC controller is used to control the operation of the fully mixed flow reaction zone; that is, the first PLC controller is electrically connected to the fully mixed flow reaction zone;

The second PLC controller is used to control the work of the reflux reaction zone; that is, the second PLC controller is electrically connected to the reflux reaction zone;

The third PLC controller is used to control the operation of the micro interface generator; that is, the third PLC controller is electrically connected with the micro interface generator.

Further, the sensor includes:

Please continue to refer to Figure 1. The present invention provides an intelligent enhanced reaction process for preparing isoformaldehyde from olefin carbonylation, including:

Step 4: In step 3, the unreacted hydrogen and carbon monoxide rise to the top of the reactor, and the third micro-interface generator, heat exchanger and liquid pump are controlled by the third PLC controller. The unreacted hydrogen and carbon monoxide in the upper part of the reaction zone in the reactor are refluxed and the unreacted hydrogen and carbon monoxide are formed into micron-sized micro-sized bubbles, the micro-sized bubbles are mixed with liquid olefins to form a gas-liquid mixture and the gas-liquid mixture is output The fully mixed flow reaction zone is opposed to the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again;

Example 1

The above-mentioned system and process are used for the preparation of isoformaldehyde, among which:

The temperature of the reactor is 35°C, and the pressure inside the reactor is 0.2Mpa;

The gas-liquid ratio in the first micro-interface generator is 750:1.

The gas-liquid ratio in the second micro-interface generator is 750:1.

The gas-liquid ratio in the third micro-interface generator is 3:10000.

After testing, the conversion rate of olefins after using the system and process is 95.2%.

The reaction time is 3.5h.

Example 2

The temperature of the reactor is 38°C, and the pressure inside the reactor is 0.2Mpa;

The gas-liquid ratio in the first micro-interface generator is 750:1.

The gas-liquid ratio in the second micro-interface generator is 750:1.

The gas-liquid ratio in the third micro-interface generator is 3:10000.

After testing, the conversion rate of olefins after using the system and process is 95.9%.

The reaction time is 3.5h.

Example 3

The temperature of the reactor is 40°C, and the pressure inside the reactor is 0.3Mpa;

The gas-liquid ratio in the first micro-interface generator is 750:1.

The gas-liquid ratio in the second micro-interface generator is 750:1.

The gas-liquid ratio in the third micro-interface generator is 3:10000.

After testing, the conversion rate of olefins after using the system and process is 96.0%.

The reaction time is 3.5h.

Example 4

The temperature of the reactor is 42°C, and the pressure inside the reactor is 0.3Mpa;

The gas-liquid ratio in the first micro-interface generator is 750:1.

The gas-liquid ratio in the second micro-interface generator is 750:1.

The gas-liquid ratio in the third micro-interface generator is 3:10000.

The reaction time is 3.5h.

Example 5

The temperature of the reactor is 45°C, and the pressure inside the reactor is 0.4Mpa;

The gas-liquid ratio in the first micro-interface generator is 750:1.

The gas-liquid ratio in the second micro-interface generator is 750:1.

The gas-liquid ratio in the third micro-interface generator is 3:10000.

After testing, the conversion rate of olefins after using the system and process is 95.7%.

The reaction time is 3.5h.

Example 6

The temperature of the reactor is 45°C, and the pressure inside the reactor is 0.2Mpa;

The gas-liquid ratio in the first micro-interface generator is 750:1.

The gas-liquid ratio in the second micro-interface generator is 750:1.

The gas-liquid ratio in the third micro-interface generator is 3:10000.

After testing, the conversion rate of olefins after using the system and process is 96.1%.

The reaction time is 3.5h.

Comparison

The existing technology is used for the preparation of isoformaldehyde, wherein the process parameters selected in this comparative example are the same as the process parameters in Example 6.

After testing, the conversion rate of olefins was 89.0%.

The reaction time is 17h.

So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

The above are only the preferred embodiments of the present invention and are not used to limit the present invention; for those skilled in the art, the present invention can have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

An intelligent enhanced reaction system for preparing isoformaldehyde from olefin carbonylation, which is characterized in that it comprises:

The reactor is used to provide a reaction place for liquid olefins, hydrogen and carbon monoxide to prepare isoformaldehyde, the reactor is provided with a catalyst, and the reactor is composed of a fully mixed flow reaction zone and a reflux reaction zone; the fully mixed flow reaction zone, It is arranged below the reactor to load liquid olefins, hydrogen, carbon monoxide and catalysts and to provide a reaction space for the olefin carbonylation reaction; the reflux reaction zone is arranged above the reactor to remove The unreacted hydrogen and carbon monoxide are refluxed and the unreacted hydrogen and carbon monoxide are reacted with the olefin again;

A micro-interface generator, which converts the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubble and transmits it to the gas reactant, and breaks the gas reactant into micron-sized bubbles with a diameter of ≥1μm and <1mm to improve the gas reaction The mass transfer area between the liquid reactant and the liquid reactant reduces the thickness of the liquid film and reduces the mass transfer resistance. After being broken, the liquid reactant and the micron-sized bubbles of the gas reactant are mixed to form a gas-liquid mixture to operate in a preset manner. Enhance the mass transfer efficiency and reaction efficiency between the liquid reactant and the gas reactant within the range of conditions;

An intelligent control module, which includes a PLC controller, a sensor, and a cloud processor. The sensor transmits the collected electrical signals to the cloud processor. The cloud processor performs screening and comparison in the cloud database according to the response parameters returned by the sensor. Send out the corresponding command to the PLC controller after the optimal control parameters are output;

A hydrogen purification unit, which is arranged on one side of the reactor and is used to purify the hydrogen entering the reactor;

The gas recovery unit is arranged on one side of the reactor to recover unreacted hydrogen and carbon monoxide.
The intelligent intensified reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 1, wherein the micro-interface generator comprises:

The first micro-interface generator is a pneumatic micro-interface generator, the first micro-interface generator is located in the fully mixed flow reaction zone in the reactor, and the first micro-interface generator is used to break hydrogen gas into micron scale After the crushing is completed, the micron-level bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture;

The second micro-interface generator is a pneumatic micro-interface generator, the second micro-interface generator is located in the fully mixed flow reaction zone in the reactor, and the second micro-interface generator is used to break carbon monoxide into micron scale After the crushing is completed, the micron-level bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture;

The third micro-interface generator is a hydraulic micro-interface generator, the third micro-interface generator is located in the reflux reaction zone in the reactor, and the third micro-interface generator is connected to an external heat exchanger and liquid The pump is used in conjunction to crush and entrain the unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor to form micron-sized micro-sized bubbles, mix the micro-sized bubbles with liquid olefin to form a gas-liquid mixture and the gas-liquid mixture Output to the fully mixed flow reaction zone to oppose the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again, and at the same time adjust all The homogeneity of the mixture in the reactor and the reaction temperature are described.
The intelligent intensified reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 2, wherein the fully mixed flow reaction zone comprises:

The hydrogen inlet pipe is connected to the first micro-interface generator, the hydrogen inlet pipe is provided with a first pump body and a first flow meter, and the hydrogen inlet pipe is used to transmit hydrogen to the first Micro-interface generator;

The carbon monoxide inlet pipe is connected to the second micro-interface generator, the carbon monoxide inlet pipe is provided with a second pump body and a second flow meter, and the carbon monoxide inlet pipe is used to transfer carbon monoxide to the second Micro-interface generator;

A material discharge pipe communicates with the lower end of the reactor, the material discharge pipe is provided with a third flow meter and a first electronic control valve, and the material discharge pipe is used to discharge products.
The intelligent enhanced reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 2, wherein the reflux reaction zone comprises:

A reflux tube, one end of which is connected to the third micro-interface generator, and the other end is located at the upper part of the reflux reaction zone, the reflux tube is used to transfer unreacted hydrogen and carbon monoxide to the third micro-interface generator;

A gas discharge pipe connected to the upper end of the reactor, a fourth flow meter is arranged on the gas discharge pipe, and the gas discharge pipe is used to discharge unreacted hydrogen and carbon monoxide;

The material inlet pipe communicates with the upper part of the side wall of the reactor. The material inlet pipe is provided with a fifth pump body and a fifth flow meter. The material inlet pipe is used to add liquid to the reactor. Olefins.
The intelligent intensified reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 3, wherein the hydrogen purification unit comprises:

A hydrogen purification tank, which is connected to the hydrogen inlet pipe, a molecular sieve is arranged in the hydrogen purification tank, and the molecular sieve is used for purifying hydrogen;

An electric heating jacket, which is located on the side wall of the hydrogen purification tank, an electric resistance wire is arranged in the electric heating jacket, and the electric heating jacket is used to heat the hydrogen purification tank to remove the molecular sieve. Moisture so that the molecular sieve can be reused.
The intelligent intensified reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 4, wherein the gas recovery unit is composed of a gas storage tank, which is connected to the gas discharge pipe to store the incoming The unreacted hydrogen and nitric oxide mixed gas inside, the gas storage tank and the gas discharge pipe are connected with a one-way valve.
The intelligent intensified reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 1, wherein the catalyst is composed of a porous carrier impregnated with an organic metal complex solvent Co 2 (CO) 8 solution.
The intelligent intensified reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 1, wherein the PLC controller comprises:

The first PLC controller is used to control the operation of the fully mixed flow reaction zone;

The second PLC controller is used to control the operation of the reflux reaction zone;

The third PLC controller is used to control the operation of the micro-interface generator.
The intelligent enhanced reaction system for preparing isoformaldehyde from olefin carbonylation according to claim 1, wherein the sensor comprises:

A plurality of temperature sensors, which are respectively arranged in the reactor, the hydrogen purification unit and the gas recovery unit, to monitor the temperature of the system;

A plurality of pressure sensors are respectively arranged in the reactor, the hydrogen purification unit and the gas recovery unit to monitor the system pressure.
An intelligent enhanced reaction process for preparing isoformaldehyde from olefin carbonylation, which is characterized in that it comprises:

Step 1: Control the operation of the fully mixed flow reaction zone through the first PLC controller, and at the same time control the operation of the reflux reaction zone through the second PLC controller. The control process is through the second PLC controller Control the operation of the fifth pump body to suck liquid olefins into the reactor through the material inlet pipe, and at the same time, the fifth flow meter measures the incoming amount of liquid olefins, which is controlled by the first PLC The device controls the operation of the first pump body and the second pump body, and sucks hydrogen and carbon monoxide to the first micro-interface generator and the second micro-interface through the hydrogen inlet pipe and the carbon monoxide inlet pipe, respectively Inside the generator

Step 2: Hydrogen is purified by the hydrogen purification unit during the process of entering the first micro-interface generator in the hydrogen inlet pipe;

Step 3: Control the operation of the micro-interface generator through the third PLC controller, and the specific control process is to control the first micro-interface generator through the third PLC controller to break hydrogen gas into micron-sized micrometers After the crushing is completed, the micron-level bubbles are output to the fully mixed flow reaction zone in the reactor and the liquid olefin in the fully mixed flow reaction zone in the reactor is mixed to form a gas-liquid mixture, and the third PLC controls The second micro-interface generator is controlled by the second micro-interface generator to crush carbon monoxide to form micro-scale micro-scale bubbles, and after the crushing is completed, the micro-scale bubbles are output to the fully mixed flow reaction zone in the reactor and the fully mixed flow in the reactor Liquid olefins in the reaction zone are mixed to form a gas-liquid mixture, and olefins, hydrogen and carbon monoxide undergo carbonylation reaction to form isoformaldehydes;

Step 4: In step 3, the unreacted hydrogen and carbon monoxide rise to the top of the reactor, and the third micro-interface generator, heat exchanger and liquid pump are controlled by the third PLC controller. The unreacted hydrogen and carbon monoxide in the upper part of the reflux reaction zone in the reactor will form the unreacted hydrogen and carbon monoxide into micron-sized micro-sized bubbles, mix the micro-sized bubbles with liquid olefins to form a gas-liquid mixture, and output the gas-liquid mixture to the The fully mixed flow reaction zone is opposed to the gas-liquid mixture output by the first micro-interface generator and the second micro-interface generator, so that unreacted hydrogen and carbon monoxide participate in the reaction again;

Step 5: A small amount of hydrogen and carbon monoxide that are not entrained on the top of the reactor are discharged into the gas storage tank along the gas discharge pipe, and the fourth flowmeter measures the total amount of gas discharged;

Step 6: After the reaction is completed, the first PLC controller is used to control the first electronic control valve to open, the generated material is discharged along the material discharge pipe, and the third flow meter measures the amount of discharged material .