CN116078316A - Blade reactor with ultrasonic assistance and suitable for high polymer polymerization - Google Patents
Blade reactor with ultrasonic assistance and suitable for high polymer polymerization Download PDFInfo
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- CN116078316A CN116078316A CN202211691049.7A CN202211691049A CN116078316A CN 116078316 A CN116078316 A CN 116078316A CN 202211691049 A CN202211691049 A CN 202211691049A CN 116078316 A CN116078316 A CN 116078316A
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- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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Abstract
The invention relates to a blade reactor with ultrasonic assistance suitable for high polymer polymerization, which comprises a reactor body and a premixing device (2), wherein the reactor body comprises a reactor shell (1) and a plurality of groups of blade reaction units with ultrasonic assistance, and two sides of the reactor shell (1) are in a plurality of groups of folding arc shapes to form a plurality of arc-shaped channels; the blade type reaction unit with ultrasonic assistance comprises a temperature control element (8) consisting of heat exchange plate bundles and a unit type ultrasonic assistance device (9). Compared with the prior art, the invention integrates the advantages that the traditional reactor can realize industrial production and the micro-reactor can precisely control the reaction temperature, is applicable to polymerization reactions with large quantity of heat release and high conversion rate requirements, is a polymerization reactor in mesoscale, and has good application prospect.
Description
Technical Field
The invention relates to a reactor, in particular to a blade reactor for polymerization reaction, which is assisted by ultrasonic waves and is in critical dimension.
Background
The reaction process of forming a high polymer from a low molecular monomer is called a polymerization reaction, and can be classified into two major types, namely, addition polymerization and polycondensation, according to the change of the elemental composition and structure. Regardless of the type of reaction, a large amount of heat is evolved during the polymerization of the monomers, and how to remove the heat of reaction in time is a key factor in ensuring production and quality.
The polymerization reaction is usually carried out using a tank reactor. In the traditional reactor, a jacket is arranged on the wall of the reactor or a heat exchange surface is arranged in the reactor for heat exchange, so that when the reactor is applied to industrialized mass production, along with the progress of the reaction, the viscosity of a system in the reactor is increased, and adverse effects such as uneven reaction, overlong reaction time or difficult post-treatment caused by the increase of byproducts due to the adhesion of high-viscosity materials on the inner wall of the reactor can occur; meanwhile, the reaction heat of the reactor is limited by the structure, the reaction conversion rate is increased along with the progress of the reaction, the viscosity of the system is increased, and heat dissipation becomes difficult. Particularly, after the gel phenomenon is generated, the heat release rate is accelerated, the heat dissipation is more difficult, the local overheating can be caused, the relative molecular weight distribution is widened, the mechanical stirring can be influenced, and even the explosion aggregation can be generated in severe cases. Meanwhile, continuous production is difficult to realize by the stirring type reaction kettle, and the production efficiency is seriously affected by an intermittent operation mode.
Compared with the traditional reactor, the micro-reactor technology can overcome some defects when carrying out reaction at a microscopic angle, and has the advantages of high mass and heat transfer efficiency, short reaction time, no amplification effect, safety, reliability, high integration level, green production flow and the like in the reaction process. The main application fields of the microreactor comprise the fields of fine chemical engineering, pharmaceutical industry, genetic engineering and the like. However, the microreactor itself has some disadvantages, in that when solid substances are involved in the reaction materials, precipitation, growth or bridging phenomena in the channels limit the flow rate of the liquid in the microreactor, affect the mixing of the liquid, increase the pressure, and finally lead to reaction failure. Meanwhile, when the microreactor is applied to large-scale production, the expensive price, the complex structure and the redundant system of the microreactor bring a plurality of uncertain factors to industrial production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the blade reactor with ultrasonic assistance suitable for high-molecular polymerization, which can meet the requirements of large-scale production of the traditional stirring reaction kettle and high selectivity of products produced by the micro-reactor, can use polymerization reaction with large heat release in industrial production and reaction process and high requirement on conversion rate of the reaction products, and can be used for high-molecular polymerization reaction in a high-viscosity fluid state.
The aim of the invention can be achieved by the following technical scheme: the blade reactor with the ultrasonic assistance suitable for the high polymer polymerization comprises a reactor body and a premixing device, wherein the reactor body comprises a reactor shell and a plurality of groups of blade reaction units with the ultrasonic assistance, and two sides of the reactor shell are in a plurality of groups of folding arc shapes to form a plurality of arc-shaped channels;
the blade type reaction unit with ultrasonic assistance comprises a temperature control element consisting of heat exchange plate bundles and a unit type ultrasonic assistance device; the temperature control elements are arranged in parallel in the reactor shell, and each group of temperature control elements and the corresponding shell form an arc-shaped reaction cavity; each arc-shaped reaction cavity is internally provided with a unit type ultrasonic auxiliary device;
the reaction materials firstly enter a first arc-shaped reaction cavity and a first arc-shaped channel after being mixed by a premixing device, a polymerization reaction occurs under an ultrasonic auxiliary device, then enter a plurality of groups of arc-shaped reaction cavities and arc-shaped channels which are connected in series, and finally a product is obtained at the bottom of a reactor body.
The reactor shell accords with the folding characteristic of a plurality of groups of blade units, the side walls on two sides are arc-shaped with different sizes, the junction of the adjacent arc-shaped wall surfaces of the side walls on one side is connected with a temperature control element, and the other side wall surface opposite to the temperature control element is near the central line of an arc-shaped channel to form a folding structure.
Specifically, the temperature control element consists of a heat exchange plate bundle, wherein the heat exchange plate bundle consists of a plurality of heat exchange plate pairs, and two sides of each heat exchange plate pair are connected with the inner wall of the reactor shell. An arc-shaped reaction cavity is formed between the adjacent temperature control elements and the arc-shaped side walls (namely arc-shaped channels) of the reactor shells at the two sides, a first arc-shaped reaction cavity is formed between the first temperature control elements and the upper cover plate of the reactor shell, and a tail end arc-shaped reaction cavity is formed between the last temperature control element at the bottom of the reactor shell and the lower cover plate.
The reaction area is divided into blade units (each blade unit is in mesoscale and larger than the corresponding microscopic scale of the molecule and smaller than the corresponding macroscopic scale of the equipment) through the structure. Each group of reaction cavity is provided with an independent temperature control element, and a plurality of groups of blade units are connected in a folding way, so that the requirements of industrialized mass production are met on the premise of meeting continuous production, and the pain point of a conventional stirred tank reactor in the later stage of polymerization reaction is also solved.
Further, each group of heat exchange plate pair-to-pair heat exchange cavities corresponds to a group of distribution branch pipes and collection branch pipes of heat exchange media. The distribution branch pipe and the collection branch pipe of the heat exchange medium are relatively independent, and the conditions of the types, the flow, the temperature and the like of the heat exchange medium in the heat exchange cavities of the temperature control elements in different groups can be set according to specific reactions, so that the average temperature and the temperature difference of the corresponding reaction cavities of each group of temperature control elements can be accurately controlled, and the occurrence of local overheating phenomenon in the reaction process is avoided.
The heat exchange plates are respectively arranged in multiple sections in the axial direction of the reactor, the intervals between the heat exchange plates are mutually independent and adjustable, the intervals between the heat exchange plates in the reaction cavity can be determined according to the heat exchange amount required by the specific polymerization reaction process, and the stable control of the temperature in the reaction process is facilitated. The spacing between the heat exchange plate pairs arranged in the vertical direction of the components in the reaction cavity can be the same or different according to the reaction progress. The reaction materials enter from a reaction medium feed inlet above the reactor, the reaction conversion rate is smaller at the beginning, and the required heat exchange amount is lower; with the progress of the reaction, the conversion rate increases, the viscosity of the system increases, and heat dissipation becomes difficult, and at this time, a high heat exchange amount is required to reduce the temperature so as to prevent the occurrence of a gel phenomenon and ensure the smooth progress of the reaction. Therefore, the requirement on the initial heat exchange amount of the reaction is small, and the plate pair spacing close to the inlet of the reactor is large; as the reaction medium circulates along the reactor channel, the heat exchange requirement gradually increases, the distance between the heat exchange plates is reduced to increase the turbulence degree of the fluid, and the heat transfer effect is enhanced.
The average distance between the heat exchange plates is 10-15mm.
The unit type ultrasonic auxiliary device is an ultrasonic vibration rod inserted into each arc-shaped reaction cavity, and the front end of the transmitting head of the ultrasonic vibration rod penetrates into the arc-shaped reaction cavity and is placed in parallel with the temperature control element.
The unit type ultrasonic auxiliary device is an ultrasonic patch vibrator, and the ultrasonic patch vibrators are uniformly arranged on the wall surface of the reaction cavity in the reactor shell at intervals.
The ultrasonic vibration rod and the ultrasonic patch vibrator assist in efficient polymerization reaction under the action of the ultrasonic generator.
The number of the arc-shaped channels and the arc-shaped reaction chambers is regulated according to specific polymerization characteristics.
The premixing device comprises a reaction medium feeding pipe and a mixing nozzle connected with the reaction medium feeding pipe, wherein the mixing nozzle penetrates through the wall of the reactor shell and extends into a first arc-shaped reaction cavity of the reactor body, so that reactants enter the reactor after being fully mixed to perform polymerization reaction.
The reactor shell also comprises a reaction medium inlet, a reaction medium outlet, an upper cover plate, a lower cover plate and an exhaust hole.
The blade reactor shell accords with the folding characteristic of a plurality of groups of blade units, provides a reaction space for high-viscosity polymerization reaction, and a plurality of groups of temperature control elements are arranged in parallel in the shell, and each group of temperature control elements corresponds to an arc-shaped reaction cavity provided by the shell. The arc reaction cavity in the reactor is in a blade unit series structure, and the reaction materials enter the reactor and then undergo polymerization reaction in the shell side. After being mixed by the premixing device, the reaction materials firstly enter a first reaction cavity and a first arc-shaped channel corresponding to the first blade unit, and polymerization reaction is carried out under the assistance of ultrasonic waves. And then the reaction chamber and the arc-shaped channel corresponding to the series blade units enter, and finally the reaction medium outlet pipe at the bottom of the reactor is obtained. The reaction fluid flows through the blade type unit reaction channel formed by the temperature control element and the arc-shaped shell, the periodicity of fluid flow is destroyed in the flow process from top to bottom, and the compression, stretching, deformation and stacking of the fluid-fluid boundary increase the interface area where diffusion occurs, so that the mixing efficiency is improved. The fluid flows through the arc-shaped shell side channel, so that a flow dead zone possibly generated when a reaction medium passes through the corner of the reactor can be effectively avoided, the heat transfer efficiency is enhanced, the scaling phenomenon is reduced, and the service life of the reactor can be effectively prolonged.
In order to overcome the disadvantages of the existing polymerization reactors both from a macroscopic and from a microscopic point of view, the polymerization can be carried out on a mesoscale. Mesoscale refers to the transition scale between macroscopic and microscopic, and the reactor is studied on the mesoscale, i.e. has macroscopic fluid dimensions, which can expand the reactor scale and also has flexible control advantages on the microscopic scale. Meanwhile, the invention also refers to the concept of a blade unit module, and the reaction areas can be flexibly overlapped according to the characteristics of different polymerization reactions, and for the reactor, the ultrasonic waves can make reactants do intense motion in the reaction cavity so as to fully mix, strengthen the transmission and diffusion of substances, and enable the reaction to be carried out with high efficiency. The introduction of ultrasonic assistance into the reactor may enhance the polymerization process.
Compared with the prior art, the invention has the following beneficial effects:
(1) In the polymerization reaction accompanied by a large amount of heat release, the reaction medium is fully mixed in a premixing device according to a certain proportion and then is added into a reactor. The reaction medium passes through the shell side in the polymerization reaction process, and the heat exchange medium is introduced between the plate pairs through the plate pair corresponding heat exchange medium inlets in the reaction cavity, namely, introduced into the plate side, so that the occurrence of the condition that the reaction materials are heated unevenly can be effectively avoided, and the continuous proceeding of the reaction is facilitated.
(2) The size and the number of the temperature control elements in the reactor can be flexibly adjusted, the temperature control elements can respectively correspond to cooling media with different types and temperatures, so that the reactor can meet the heat exchange requirements of different polymerization reactions and different heat exchange requirements before and after the same polymerization reaction, can accurately control the temperatures of different reaction stages in the polymerization reaction, further can ensure the efficient performance of the polymerization reaction, and greatly improves the production efficiency.
(3) The reactor disclosed by the invention divides the reaction area into a plurality of blade unit reaction cavities (each unit is in a mesoscale, larger than a microscopic scale corresponding to molecules and smaller than a macroscopic scale corresponding to equipment), the size of a unit channel in a critical scale is small, the specific surface area is large, the reaction materials have an efficient mixing effect, the temperature can be accurately controlled, and the occurrence of a local overheating phenomenon can be effectively reduced. Compression and folding of the fluid within the channel may increase the mixing effect of the fluid. The quantity of the blade units is increased, the quantity of the temperature control elements is correspondingly and flexibly adjusted according to different reaction characteristics, the yield of the polymerization reactor can be increased, and the scale of industrial production can be achieved on the premise of reducing the amplification effect as much as possible.
(4) The reactor of the invention is assisted by ultrasonic waves, and can accelerate the intermolecular mutual penetration by applying the high-frequency vibration and cavitation pressure and the high-temperature effect of the ultrasonic waves, so that reactants do intense motion in the reaction cavity to be fully mixed, the transfer and diffusion of substances are enhanced, and the efficient performance of the polymerization reaction is facilitated.
(5) The polymerization reactor integrates the advantages of industrial production of the traditional reactor and accurate control of the reaction temperature of the microreactor, can be suitable for polymerization reactions with large quantity of heat release and high conversion rate requirements, is a polymerization reactor in mesoscale, and has good application prospect.
Drawings
FIG. 1 is a schematic view of a blade reactor configuration for polymerization at critical dimensions with ultrasonic assistance in an example.
The figure indicates:
1-reactor shell, 2-premixing device, 3-reaction medium inlet, 4-reaction medium outlet, 5-upper cover plate, 6-lower cover plate, 7-exhaust hole, 8-temperature control element, 9-ultrasonic auxiliary device, 10-distribution branch pipe, 11-collection branch pipe, 12-first arc reaction cavity, 13-first arc channel and 14-heat exchange cavity.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
Examples:
as shown in fig. 1, a blade reactor with ultrasonic assistance suitable for high molecular polymerization comprises a reactor body and a premixing device 2, wherein the reactor body comprises a reactor shell 1 and a plurality of groups of blade reaction units with ultrasonic assistance, the reactor shell 1 comprises a reaction medium inlet 3, a reaction medium outlet 4, an upper cover plate 5, a lower cover plate 6 and an exhaust hole 7 arranged at the upper end of the shell, and side walls which are connected with the side surfaces of the upper cover plate 5 and the lower cover plate 6 and form a reaction cavity of the reactor, the side walls at two sides are arc-shaped with different sizes, a temperature control element 8 for exchanging heat of polymerization reaction is connected at the joint of adjacent arc-shaped wall surfaces of one side wall, and the other side wall surface opposite to the temperature control element 8 is near the central line of an arc-shaped channel to form a folding structure.
The temperature control elements 8 are arranged in the reactor shell 1, a reaction cavity for polymerization reaction is formed by shell passes between the reactor shell 1 and the temperature control elements 8, a plurality of groups of temperature control elements 8 are arranged in parallel in the reactor shell 1, and each group of temperature control elements 8 and the corresponding shell form an arc reaction cavity; each arc-shaped reaction cavity is internally provided with a unit type ultrasonic auxiliary device 9, the cavity in each group of temperature control elements 8 is a heat exchange cavity 14, the reaction medium inlet 3 and the reaction medium outlet 4 are connected with the reaction cavity of the reactor, and each group of heat exchange cavities is connected with a distribution branch pipe 10 and a collection branch pipe 11 of the heat exchange medium.
The temperature control element 8 consists of a heat exchange plate bundle, wherein the heat exchange plate bundle consists of a plurality of heat exchange plate pairs, and two sides of each heat exchange plate pair are connected with the inner wall of the reactor shell 1. An arc-shaped reaction cavity is formed between the adjacent temperature control elements 8 and the arc-shaped side walls (namely arc-shaped channels) of the reactor shells at two sides, a first arc-shaped reaction cavity 12 is formed between the first temperature control elements 8 and the upper cover plate of the reactor shell, the side walls of the first arc-shaped reaction cavity are first arc-shaped channels 13, and a tail end arc-shaped reaction cavity is formed between the last temperature control element at the bottom of the reactor shell and the lower cover plate. The average spacing of the pairs of heat exchanger plates is 10-15mm, in this embodiment 10mm. The premixing device 2 comprises a reaction medium feeding pipe and a mixing nozzle connected with the reaction medium feeding pipe, wherein the mixing nozzle extends into a first arc-shaped reaction cavity 12 of the reactor body through the wall of the reactor shell 1 so as to enable reactants to enter the reactor for polymerization reaction after being fully mixed.
In this embodiment, an ultrasonic vibration rod is selected as the reactor ultrasonic auxiliary device 9, and penetrates through the reactor shell 1 to the reaction cavity of the blade unit of the reactor, and the ultrasonic vibration rod is connected with an ultrasonic generator outside the reactor to assist the polymerization reaction. The high-frequency vibration of the ultrasonic wave, the pressure of cavitation and the high-temperature effect can accelerate the interpenetration among molecules, promote the violent movement of the reaction materials in the blade-type reaction cavity so as to fully mix, strengthen the transmission and diffusion of the materials and facilitate the efficient implementation of the polymerization reaction. In other embodiments, the polymerization reaction may also occur using an ultrasonic patch vibrator as an auxiliary device.
The reactor is used for polymerization reaction, and the method is as follows:
the reaction materials enter through a reaction medium inlet 3, are premixed through a premixing device 2, and enter into the reaction cavity of the blade reactor through a pipe orifice extending into the reactor shell 1 after being mixed. Firstly, the reaction materials enter the first blade unit, are filled on the first blade unit, namely the first arc-shaped channel 13 of the first arc-shaped reaction cavity 12, and heat generated by polymerization reaction is timely removed through the temperature control element 8 corresponding to the first arc-shaped channel 13 under the assistance of the ultrasonic vibration rod. Because the average distance between the reaction channel and the temperature control element is set at 10mm, the size of the mesoscopic channel is met, under the size, the material can fill the first arc-shaped channel 13, and the reaction material enters the second blade unit after passing through the first arc-shaped channel 13. When the reactant passes through the first arc-shaped channel 13, the reactant is cut by the control Wen Banpian of the first blade unit, and the arc-shaped channel can compress and fold the reactant repeatedly, so that the mixing efficiency of the reactant is improved. Cooling water is introduced between the temperature control plates corresponding to the first blade units through the distribution branch pipe 10 of the heat exchange medium, namely the heat exchange cavity 14 of the control Wen Banpian is filled with the cooling water, and the cooling water can timely remove heat released by polymerization reaction in the reaction cavity. The reaction mass passes through the first arcuate channel 13 and then enters the second blade unit in series, then five blade units in series, and the polymerization reaction product is output from the reaction medium outlet 4.
The invention is not limited to the above embodiments, but can be modified in various ways within the scope of the invention as claimed. The scope of the invention is to be determined strictly in accordance with the scope of the claims.
Claims (10)
1. The blade reactor with the ultrasonic assistance for high polymer polymerization is characterized by comprising a reactor body and a premixing device (2), wherein the reactor body comprises a reactor shell (1) and a plurality of groups of blade reaction units with the ultrasonic assistance, and two sides of the reactor shell (1) are in a plurality of groups of folding arc shapes to form a plurality of arc-shaped channels;
the blade type reaction unit with ultrasonic assistance comprises a temperature control element (8) consisting of heat exchange plate bundles and a unit type ultrasonic assistance device (9); the temperature control elements (8) are arranged in parallel in the reactor shell (1), and each group of temperature control elements (8) and the corresponding shell form an arc-shaped reaction cavity; each arc-shaped reaction cavity is internally provided with a unit type ultrasonic auxiliary device (9);
the reaction materials firstly enter a first arc-shaped reaction cavity and a first arc-shaped channel after being mixed by a premixing device (2), the polymerization reaction is carried out under an ultrasonic auxiliary device (9), then a plurality of groups of arc-shaped reaction cavities and arc-shaped channels which are connected in series after entering the reaction materials, and finally, the product is obtained at the bottom of the reactor body.
2. The blade reactor with ultrasonic assistance suitable for high molecular polymerization according to claim 1, characterized in that the temperature control element (8) consists of a heat exchange plate bundle consisting of several heat exchange plate pairs, two sides of each heat exchange plate pair being connected to the inner wall of the reactor shell (1).
3. A blade reactor with ultrasound assistance suitable for high molecular polymerization according to claim 2, characterized in that each group of heat exchange plate inter-pair heat exchange chambers corresponds to a group of distribution branch pipes (10) and collection branch pipes (11) for heat exchange medium.
4. A blade reactor with ultrasonic assistance suitable for high molecular polymerization according to claim 2 or 3, wherein the heat exchange plate pairs are respectively arranged in a plurality of sections in the axial direction of the reactor, and the distance between the heat exchange plate pairs is mutually independent and adjustable.
5. A blade reactor with ultrasound assistance suitable for high molecular polymerization according to claim 4, characterized in that the average spacing of the heat exchange plate pairs is 10-15mm.
6. The blade reactor with ultrasonic assistance suitable for high molecular polymerization according to claim 1, wherein the unit type ultrasonic assistance device (9) is an ultrasonic vibration rod inserted into each arc reaction cavity, and the front end of the emission head of the ultrasonic vibration rod extends into the arc reaction cavity and is placed in parallel with the temperature control element (8).
7. The blade reactor with ultrasonic assistance suitable for high molecular polymerization according to claim 1, wherein the unit type ultrasonic assistance device (9) is an ultrasonic patch vibrator, and the ultrasonic patch vibrators are uniformly arranged on the wall surface of the reaction cavity in the reactor shell at intervals.
8. The blade reactor with ultrasonic assistance for polymer polymerization according to claim 1, wherein the number of the arc-shaped channels and the arc-shaped reaction chambers is adjusted according to specific polymerization characteristics.
9. A blade reactor with ultrasound assistance suitable for high molecular polymerization according to claim 1, characterized in that the premixing device (2) comprises a reaction medium feed pipe and a mixing nozzle connected thereto, which extends through the wall of the reactor housing (1) into the first arc-shaped reaction chamber (12) of the reactor body, so that the reactants after thorough mixing enter the reactor for polymerization.
10. A blade reactor with ultrasound assistance suitable for high molecular polymerization according to claim 1, characterized in that the reactor housing (1) further comprises a reaction medium inlet (3) and a reaction medium outlet (4), an upper cover plate (5), a lower cover plate (6) and an exhaust vent (7).
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| CN202211691049.7A CN116078316A (en) | 2022-12-28 | 2022-12-28 | Blade reactor with ultrasonic assistance and suitable for high polymer polymerization |
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| CN202211691049.7A CN116078316A (en) | 2022-12-28 | 2022-12-28 | Blade reactor with ultrasonic assistance and suitable for high polymer polymerization |
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