CN1669631A - Liquid-liquid fast-mixing reactor - Google Patents
Liquid-liquid fast-mixing reactor Download PDFInfo
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Abstract
The invention relates to a liquid-liquid fast-mixing reactor, which comprises a housing, an inner casing, a liquid conducting tube, an injector, a demister, a backing sheet, a pad, an adjusting valve, a manometer, wherein the housing (1) has a liquid feed inlet (8), the necked-in parts, and a liquid outlet (3); the inner casing (2) has the liquid conducting tube (5), the injector (4), the air outlet (10), the adjusting valve (11) and the manometer (12) inside. The space between the inwall of the housing (1) and the inner casing (2) forms a channel cyclone or non-cyclone through which a fold of liquid inlets, and another liquid passes the liquid conducting tube and the injector and forms the droplet distributed circlewise, the droplet connects with the film formed when the first fold of liquid passing the chine, and the two folds of liquid mix in the meeting point rapidly, then the product will be discharged from the liquid outlet (3).
Description
Technical Field
The invention relates to an industrial high-efficiency liquid-liquid rapid mixing reactor, belonging to the technical field of high-efficiency mixing and reaction of industrial liquid and liquid.
Background
The rapid liquid-liquid reaction system is widely used in the industrial processes of fine chemical engineering, polymerization process, pharmaceutical industry, biochemical industry and the like. For example, in the process of preparing solid particles by using a liquid-liquid two-phase codeposition method, the mixing effect of the liquid phase and the liquid phase directly influences the particle size distribution of the particles; in the process of preparing the high polymer by using liquid-liquid reaction, the mixing effect of liquid and liquid phases also directly influences the molecular weight distribution of the high polymer; in other production processes, when complex liquid-liquid two-phase rapid parallel competitive reactions or parallel-serial competitive reactions occur in the liquid phase, reaction products or intermediate products and certain components of raw materials can further react, so that the initial mixing effect of the liquid-liquid two phases greatly influences the final product distribution, the product yield and quality, and simultaneously influences the design, energy consumption and other indexes of the whole production process. When the main reaction is a transient reaction, the initial mixing of liquid and liquid not only requires a uniform phase distribution on a molecular level on a spatial scale, but also requires a time scale generally on a millisecond (even microsecond) level. Therefore, the successful design of the rapid liquid-liquid mixing reactor has important significance for improving the quality of reaction products and reducing the yield of byproducts.
The liquid-liquid mixing mechanism mainly includes laminar mixing and turbulent mixing, and for the mixing process of high-viscosity liquid, the mixing process is generally laminar mixing. For mixing of low viscosity liquids, turbulent mixing is typical. In industrial production, turbulent flow can be generated by mechanical stirring, designing a tortuous flow passage, high-speed impact of liquid or spraying at higher pressure, and the like, so that the mixing efficiency of the low-viscosity liquid is increased.
Aiming at the mixing problem of low-viscosity liquid, the existing liquid-liquid mixing reactor mainly comprises a stirring kettle, a static mixer, an impinging stream mixer, a jet mixer and the like.
The common stirred tank mixer mainly comprises a stirred tank, a shaft seal device and a stirring device. Wherein the stirring device comprises a transmission device, a stirring shaft and an impeller. One impeller or a plurality of impellers can be arranged on the stirring shaft, and the main forms of the impellers include paddle type, turbine type, propelling type, Bruman type, toothed sheet type, anchor type, frame type and the like. About 85% of liquid-liquid mixing process in industrial production is completed in a stirring kettle. A stirring kettle is adopted to mix two streams of fluid, the liquid-liquid mixing process is completed in the whole stirring kettle, the mixing space scale is the whole stirring kettle, the time scale is within minutes or even hours, the method belongs to the macro mixing category, and the method is usually used for a reaction system with relatively slow reaction rate.
The static mixer is designed with different complex structures on the fluid pipeline, such as a combination of twisted blades or staggered flat plates, and the like, and the fluid continuously performs the processes of division, movement, recombination and subdivision after passing through the structural units, thereby achieving the aim of mixing the liquid. The main advantage of static mixers is that the fluids can be mixed over a wide range of reynolds numbers and that no mechanical parts need to be designed for mixing. However, the static mixer is used for liquid-liquid mixing, the mixing time scale is about several seconds or sub-second, the static mixer belongs to liquid-liquid mixing on the mesoscale, and the mixing process with solid generation is easy to cause blockage and is difficult to clean.
Impinging two streams at high velocity in some manner is also a common method of achieving rapid mixing of the streams. For example, in german patent GB901377, two streams of fluid are passed through a helical structure to increase the turbulence of the fluid, and the two highly turbulent streams are rapidly mixed in a mixing chamber. Another type of impinging stream mixer is disclosed in us patent GB1238669, in which two streams pass through two narrow flow passages, and two high-speed streams are mixed at a high speed in a collision manner at a slit, and this type of mixer also has the disadvantages of clogging and difficulty in cleaning. US4289732 describes mixing two reactants in a cylindrical mixing chamber by impacting each other in a fan-shaped jet. This method not only requires a high inlet pressure, but also tends to form dead zones in the cylindrical mixing chamber which are not prone to flow and to cause blockage of the reaction process where solids are produced. US33531 describes mixing two streams of fluid through two high pressure liquid jets, where the sheet-like liquid films formed by the jets impinge on each other, and reports a time scale of about 0.1 ms for the two streams to mix, but to achieve effective contact of the two streams, the process is critical and the inlet pressure is high.
Jet mixers are another type of equipment for realizing rapid mixing of two flows, and the design idea is to jet one flow of liquid into the other flow of liquid at a higher speed, and the mixing effect is enhanced by the strong turbulence generated by the high-speed liquid. The jet fluid can generate high-speed fluid jet to enter the main body fluid through a pipeline with a smaller inner diameter, a Venturi reducing hole or a small hole and the like so as to realize rapid mixing.
The pipeline with a smaller diameter is arranged in the middle of the pipeline where the main body flows or in the radial direction of the pipeline, the jet fluid generates higher speed after passing through the pipeline with the smaller diameter, and the main body fluid is jetted into the main body fluid at high speed along the axis of the main body fluid or in the direction vertical to the axis, so that the liquid and the liquid are quickly mixed, and the jet reactor is simpler. For example, US3226410 discloses a tubular reactor for a rapid competitive-series reaction process, one stream entering along the axis or tangential direction of the other stream. The jet reactor adopting the form has a simpler structure, but the mixing time scale is about a dozen of seconds to a few seconds, and other forms of liquid-liquid mixing equipment are often used for occasions with high requirements on the initial mixing degree of liquid-liquid.
The jet mixer is another form of realization by providing a venturi constriction on the conduit. The flow channel is designed into a Venturi form, and the flow speed of the two flows of fluid is increased by reducing the diameter, so that the turbulence degree of the fluid is increased, and the two flows of fluid can achieve a good mixing effect in a short time. For example, US3507626 discloses an industrial liquid-liquid jet mixing device with venturi structure, the mixer is composed of two coaxial venturi tubes, wherein a first fluid flows between the gap formed by the inner and outer venturi tubes, a second fluid flows from the inner venturi tube, the inner venturi tube isreduced in diameter, the second fluid flows out through a slit or uniformly distributed small holes and then collides with the first fluid to mix, thereby achieving fast mixing of the fluids.
Patent ZL88105194.3 reports another type of jet mixer in which one stream of fluid reaches a higher velocity through a reduced diameter and the other stream enters the first stream through uniformly distributed orifices in the reduced diameter to achieve rapid mixing of the two streams. ZL00124388.8 relates to a jet reactor with rotary atomizer, the mixing part of the jet reactor is designed to be similar to a double-flow nozzle, wherein one flow enters into a reaction zone through an outer ring, the other flow enters into the reaction zone after passing through the rotary atomizer, the reaction zone is in an inverted cone shape, and the two flows realize rapid mixing in the inverted cone-shaped reaction zone. These injection reactors are relatively complex in structure, and in the industrial production process, when solids are produced, there is a problem of clogging to a certain extent, and the mixing effect is greatly affected by the operating conditions, and the operating flexibility of the apparatus is small.
As described above, in order to achieve efficient mixing of liquid and liquid fluids and solve practical problems of blockage, cleaning, operational flexibility, pressure loss, etc. in industrial production, other more efficient liquid and liquid rapid mixing devices need to be designed to improve product quality, reduce byproduct yield and achieve higher economic benefits.
Disclosure of Invention
The invention aims to provide a liquid-liquid rapid mixing reactor which can ensure that two liquids are uniformly mixed in a short time through rapid contact of liquid films and liquid drops. The liquid film is formed mainly by the coexistence of slit limitation or rotational flow, the liquid film moves along the wall under the action of gravity and falls along the cone, the moving speed of the liquid film is accelerated, and the film thickness is further kept or reduced; the fog drops with the diameter of less than 200 mu m are formed through the atomizing nozzle, the specific surface area of the fog drops is large, the contact and mass transfer speed with a liquid film is high, and the mixing speed is greatly improved compared with the common liquid-liquid continuous contact; the time scale of mixing is on the order of milliseconds and the spatial scale of mixing is close to the molecular level. Meanwhile, the mixing process of the two flows is completed in a larger space, so that the problem that the generated solid matters block equipment is effectively prevented, and the generated gas can be discharged in time when gas is generated in the reaction process.
The purpose of the invention can be realized by the following scheme: a liquid-liquid rapid mixing reactor, comprising: the device comprises an outer shell (1), an inner shell (2), a liquid conveying pipe (5), a nozzle (4), a supporting sheet (6), a demister (7), a gasket (9), an adjusting valve (11) and a pressure gauge (12); the upper part of the shell (1) is provided with a liquid feeding hole (8), the lower part is a reducing part, and the taper a of the reducing part is 20-80 degrees, preferably 30-60 degrees; a liquid outlet (3) is arranged below the reducing hole; a liquid conveying pipe (5) is arranged in the middle of the inner shell (2), and the lower end of the liquid conveying pipe (5) is connected with a liquid nozzle (4); a swirl plate demister (7) made of metal or nonmetal or an irregular or regular porous filling layer demister (7) made of wire mesh is also arranged in the middle of the inner shell (2); the upper part of the inner shell (2) is provided with a gas outlet (10), an adjusting valve (11) and a pressure gauge (12); a gap of 0.5-5mm is formed between the diameter-reduced part of the lower part of the outer shell (1) and the lower part of the inner shell (2), and the optimal size of the gap is 0.5-2 mm; the size of the gap can be adjusted by the thickness or the thread rotation of the gasket (9) at the upper joint of the outer shell (1) and the inner shell (2), the position of the gap formed by the inner shell (2) and the outer shell (1) is 1/5-4/5 from the top of the reduced diameter of the outer shell (1), and the preferable position is 1/3-2/3 from the top of the reduced diameter of the outer shell (1); a channel is formed between the inner wall of the outer shell (1) and the inner shell (2), and the channel can also be a channel with a rotational flow structure; the channel is fixed with a certain number of supporting sheets (6) for fixing the position of the inner shell (2) so that the size of a gap formed between the diameter-reducing part of the lower part of the outer shell (1) and the lower part of the inner shell (2) is consistent. The support sheets (6) have the same size, and the thickness d of the support sheets is slightly smaller than the distance from the inner wall of the outer shell to the outer wall of the inner shell; the support sheets (6) are uniformly fixed at the positions of the inner wall of the shell (1) at the same distance from the bottom, and the number N of the support sheets (6) is more than or equal to 3. The number of the nozzles (4) connected with the lower part of the liquid conveying pipe (5) is one, the nozzles (4) are directly connected with the lower end of the liquid conveying pipe (5), the nozzles (4) form an annular fog drop belt, the annular fog drop belt is sprayed onto a liquid film formed by the outer shell (1) and the inner shell (2) at a certain angle b, and the size of b is 10-80 degrees, preferably 30-60 degrees.
The number of the nozzles (4) connected with the lower part of the liquid conveying pipe(5) can be more than one, when the number of the nozzles is more than one, the liquid conveying branch pipes (14) are uniformly distributed at the lower end of the liquid conveying pipe (5) along the circumferential direction, the nozzles are correspondingly connected with the liquid conveying branch pipes (14), each nozzle forms a fan-shaped fog drop belt, all the nozzles form an annular fog drop belt, the annular fog drop belt is sprayed onto a liquid film formed by the outer shell (1) and the inner shell (2) at a certain angle, and the size of b is 10-80 degrees, preferably 30-60 degrees.
The reactor consists of an outer shell, an inner shell, a liquid conveying pipe, a nozzle, a demister, a supporting sheet, a gasket, an adjusting valve and a pressure gauge; the size of the gap can be adjusted by the thickness of the gasket at the joint of the outer shell and the upper part of the inner shell or the rotation of the threads; the inner wall of the outer shell is fixed with a certain number of supporting sheets for fixing the position of the inner shell, so that the size of a gap formed between the diameter-reduced part of the lower part of the outer shell and the lower part of the inner shell is consistent; a liquid feed port is arranged at the upper part of the shell, and after a strand of liquid enters from the feed port at the upper part of the shell, the strand of liquid moves downwards in the shell in a rotational flow mode or a non-rotational flow mode and forms a liquid film with uniform thickness after passing through a gap at the lower part of the shell; be equipped with the liquid delivery pipe in the middle part of the inner shell, the lower extreme of liquid delivery pipe even has liquid nozzle, and another strand of liquid gets into the liquid nozzle of delivery pipe lower extreme through the liquid delivery pipe, forms ring distribution's fog drop through the nozzle, and the fog drop contacts with the liquid film that forms through the gap, reaches the flash mixedof two strands of liquid in the twinkling of an eye in the contact department, and the liquid after the mixture continues downstream along shell lower part undergauge department, further mixes on the conical surface. The inner shell is provided with a demister in the middle, a gas outlet, an adjusting valve and a pressure gauge in the upper part, when gas is generated after two flows of fluid react, the adjusting valve on the upper part of the inner shell is opened, the gas generated by the reaction is defoamed by the demister and then is discharged from a gas discharge port on the upper part of the inner shell, and a liquid mixture formed by reaction products generated after the reaction and part of unreacted raw materials is discharged from a liquid discharge port on the lower part of the outer shell. Has the following advantages:
(1) the liquid film is formed by the coexistence of slit limitation or rotational flow, the liquid film moves along the wall under the action of gravity, the liquid film falls along the cone, the moving speed of the liquid film is accelerated, and the film thickness is further kept or reduced; the atomizing nozzle is used for forming fog drops with the size of about 50-200 mu m, the specific surface area of the fog drops is large, the contact and mass transfer speed with a liquid film is high, and the mixing speed is greatly improved compared with the common liquid-liquid continuous contact; the spatial scale of mixing is close to the molecular level, and the time scale of mixing is even lower in the millisecond level;
(2) the contact mixing of the liquid film and the fog drop zone is carried out in a relatively large space, the liquid film flows at a high speed, when solid is generated in the mixing reaction process, the reactor can effectively prevent equipment blockage caused by accumulation of solid particles while realizing high-efficiency and quick mixing, ensure the normal operation of industrial operation andovercome the defect of easy blockage caused by the realization of mixing in a slit of the conventional quick mixing reactor;
(3) the upper part of the equipment is provided with a gas outlet, when gas which is not beneficial to improving the yield of the main product is generated in the reaction process, the gas can be removed in time, so that the yield of the main product is effectively increased;
(4) the size of the slit formed between the inner shell and the outer shell can be adjusted according to the size of the feeding quantity and the size of the mixing degree required to be achieved, so that the operation flexibility of the mixing reactor is improved;
(5) the nozzle used for generating the fog drop zone can be one or a plurality of nozzles, the selection and the arrangement of the nozzles can be determined according to the characteristics of the reaction process and the size of the mixing effect required to be achieved, and the selection elasticity is added to the selection of the liquid-liquid rapid mixing reactor.
The liquid-liquid rapid mixing reactor can be used for preparing solid particles with uniform particle size through liquid-liquid rapid reaction, and can also be used for preparing high polymer products with relatively narrow molecular weight distribution through liquid-liquid rapid reaction, thereby being beneficial to improving the quality of the products. In addition, when instant (or rapid) parallel competitive reaction or serial competitive reaction occurs in some liquid-liquid mixing processes, the higher mixing efficiency can effectively improve the yield and selectivity of the main product and reduce the energy consumption in the production process.
Drawings
FIG. 1 is a schematicdiagram of a liquid-liquid rapid mixing reactor according to the present invention;
FIG. 2 is a sectional view of a liquid-liquid rapid mixing reactor A-A' according to the present invention;
FIG. 3 is a schematic diagram of a cyclone structure of the liquid-liquid rapid mixing reactor of the present invention;
FIG. 4 shows another nozzle arrangement for a liquid-liquid rapid mixing reactor according to the present invention.
Detailed Description
FIG. 1 is a schematic diagram of a liquid-liquid rapid mixing reactor according to the present invention. A liquid-liquid rapid mixing reactor mainly comprises an outer shell 1, an inner shell 2, a liquid conveying pipe 5, a nozzle 4 and a demister 7; the size of the gap can be adjusted by the thickness of a gasket 9 at the joint of the outer shell 1 and the upper part of the inner shell 2 or the rotation of threads; a certain number of supporting sheets 6 are fixed on the inner wall of the outer shell 1 and used for fixing the position of the inner shell 2, so that the size of a gap formed between the diameter-reduced part of the lower part of the outer shell 1 and the lower part of the inner shell 2 is consistent; a liquid feed port 8 is arranged at the upper part of the shell 1, wherein a strand of liquid enters from the feed port 8 at the upper part of the shell 1 and then moves downwards in the shell 1 in a rotational flow mode or a non-rotational flow mode, and a liquid film with uniform thickness is formed after passing through a gap at the lower part of the shell 1; be equipped with liquid delivery pipe 5 in the middle part of inner shell 2, liquid delivery pipe 5's lower extreme even has liquid nozzle 4, and another strand of liquid gets into liquid nozzle 4 of delivery pipe 5 lower extreme through liquid delivery pipe 5, through nozzle 4 formation ring distribution's droplet, the droplet contacts with the liquid film that forms through the gap, reaches the flash mixed of two strands of liquid in the twinkling of an eye in the department of contact, and the liquid after the mixture continues downstream along 1 lower part undergauge department of shell, further mixes on the conical surface. A demister 7 is arranged in the middle of the inner shell 2, a gas outlet 10, a regulating valve 11 and a pressure gauge 12 are arranged at the upper part of the inner shell 2, when gas is generated after two flows of fluid react, the regulating valve 11 at the upper part of the inner shell 2 is opened, the gas generated by the reaction is defoamed by the demister 7 and then is discharged from a gas discharge port 10 at the upper part of the inner shell 2, and a liquid mixture formed by reaction products generated after the reaction and part of unreacted raw materials is discharged from a liquid discharge port 3 at the lower part of the outer shell 1.
The size of the gap can be designed according to the effect required by mixing and the flow rate of two flows of fluid by forming a gap with adjustable size between 0.5 mm and 5mm, preferably between 0.5 mm and 2mm at the reduced diameter part of the lower part of the outer shell 1 and the lower part of the inner shell 2 by a certain taper at the lower part of the outer shell 1, wherein the taper (indicated by a) is 20-80 degrees, preferably 30-60 degrees. Under the same operation adjustment, the smaller gap can easily reach larger fluid speed, the formed liquid film is thinner, and the flaky fog drops formed by the nozzle 4 can realize rapid mixing with the thinner liquid film.
A certain number of supporting sheets 6 are arranged inside the outer shell 1 and used for fixing the position of the inner shell 2, so that a gap with uniform size is formed between the outer shell 1 and the inner shell 2. The support pieces 6 are the same in size, and the thickness (indicated by d) of the support pieces is slightly smaller than the distance from the inner wall of the outer shell to the outer wall of the inner shell; the supporting sheets 6 can be uniformly fixed at the positions of the inner wall of the shell 1 at the same distance from the bottom, the number of the supporting sheets is about 3-10, and the number of the supporting sheets is at least three. FIG. 2 is a sectional view of a liquid-liquid rapid mixing reactor A-A' according to the present invention.
The inner part of the outer shell 1 can be designed into a rotational flow structure 13, so that liquid passing through the outer shell 1 is accelerated by the rotational flow structure 13 and then passes through a gap formed between the diameter-reduced part of the lower part of the outer shell 1 and the lower part of the inner shell 2 at a high speed, and the inner part of the outer shell 1 can also be designed into a common form without the rotational flow structure 13. FIG. 3 is a schematic diagram of the rotational flow structure of the liquid-liquid rapid mixing reactor of the present invention.
The position of the gap formed by inner shell 2 and outer shell 1 is determined by the diameter of inner shell 2, and the position of the gap is 1/5-4/5, preferably 1/3-2/3, from the reduced diameter top of outer shell 1. The closer the gap is to the reduced diameter tip, the longer the two streams are mixed and the better the mixing.
The number of the nozzles 4 can be one or more, and when only one nozzle is arranged, the nozzle 4 is directly connected with the lower end of the liquid conveying pipe 5; when a plurality of nozzles are adopted at the lower part, the liquid conveying branch pipes 14 are uniformly distributed at the lower end of the liquid conveying pipe 5 along the circumferential direction, and the nozzles 4 are correspondingly connected to the liquid conveying branch pipes 14; FIG. 4 shows another nozzle(s) arrangement for a liquid-liquid rapid mixing reactor according to the present invention. The type of the nozzle 4 can be an industrial nozzle or a self-made nozzle; when only one nozzle 4 is used, the nozzle 4 is required to form an annular mist droplet zone, when a plurality of liquid nozzles 4 are used, each nozzle 4 is required to form a fan-shaped mist droplet zone, and all the nozzles 4 form an annular mist droplet zone; the annular mist droplet band is sprayed onto the liquid film formed by the outer shell 1 and the inner shell 2 at an angle (denoted b) of 10-80 degrees, preferably 30-60 degrees. The demister 7 is provided inside the reactor inner shell 2, and when gas is generated in the process, a gas discharge port 10 must be provided above the reactor in order to timely take out the gas from the system, and the demister 7 must be provided to remove a part of liquid droplets entrained in the rising gas because the rising gas easily entrains a part of liquid droplets. The demister can be a swirl plate demister made of metal or nonmetal or an irregular or regular porous filling layer defoaming device made of wire mesh. The demister 7 must be positioned at a certain height from the mixed liquid surface to ensure a necessary liquid settling section so as to reduce the entrainment of the liquid.
The upper part of the inner shell (2) is also provided with an adjusting valve 11 and a pressure gauge 12, when gas is generated in the liquid-liquid mixing reaction process, the adjusting valve 11 on the upper part of the inner shell 2 is opened, the gas is discharged from a gas outlet 10 on the upper part of the inner shell 2, and the adjusting valve 11 and the pressure gauge 12 are used for controlling the pressure in the mixing chamber together. The lower part of the shell 1 is provided with a liquid outlet 3, and a liquid mixture formed by reaction products generated after reaction and part of unreacted raw materials is discharged from the liquid outlet 3.
The following are specific examples of the present invention. The specific embodiments are illustrative of the invention and do not limit the invention.
Example 1
The laser induced fluorescence technology is an advanced quantitative evaluation method for evaluating liquid-liquid mixing effect, and the main principle is that some fluorescent substances (such as rhodamine B or rhodamine 6G) are used for generating visible light waves with certain wavelength under the excitation of laser induction, and then a high-speed digital camera is used for continuously shooting pictures of a flow field. When the concentration of the rhodamine in the solution is below a certain value, the concentration of the rhodamine solution and the gray value of the corresponding picture pixel have a linear relation, so that the concentration distribution of the fluorescent substance in the flow field can be obtained by analyzing the shot picture of the flow field, and the mixing condition of two flows of liquid and liquid can be further analyzed. The evaluation method is used for evaluating the mixing effect of the liquid-liquid rapid mixing reactor, the laser adopts a PIV-100 solid laser manufactured by Danec company, and the generated laser intensity is 100 mJ; the model of the digital camera is Hisense PIV/PLIFC4742-53-12NRB digital camera, and the resolution is 1280 multiplied by 1024 pixels; the adopted fluorescent material is rhodamine B, and under the experimental conditions, when the concentration of the rhodamine B in the solution is 0-140 micrograms/liter, the concentration of the rhodamine B and the corresponding picture pixel gray value have a linear relation.
By adopting the liquid-liquid rapid mixing reactor, the inner diameter of the outer shell is 300mm, the outer diameter of the inner shell is 240mm, the tapera at the reducing part of the outer shell is 60 degrees, the size of a gap formed between the reducing part of the outer shell and the inner shell is 2mm, and the inner part of the outer shell adopts a non-rotational flow form. The nozzle adopts an industrial nozzle, and the model is as follows: spraying Systems Co. 4BFSJ-SILCRB 1201400 nozzle with 120 degree jet angle (30 degree corresponding to the jet angle b of the present invention) and flow rate of 66m at 3 bar jet pressure3And/h, adopting a single-nozzle spraying form. The tracer rhodamine B is continuously injected from the upper part of the liquid conveying pipe, and the concentration of the tracer rhodamine B is 100 micronsGram/liter, the feed inlet at the upper part of the shell feeds tap water at a constant speed, and the pressure of the water at the inlet is 3.5kg/cm2The water quantity is 60m3H, its velocity at the passage through the slit is about 11.5 m/s. The mixing effect between the water solution with the tracer rhodamine B and tap water is evaluated by a laser-induced fluorescence technology, the distance for the two streams to reach the 95% mixing effect (the 95% gray value of the mixing region on the image is consistent) is 22mm, and the mixing time scale is about 0.9 millisecond.
Example 2
In the chemical production process, the initial mixing effect of the liquid phase and the liquid phase greatly affects the final product distribution, the product yield and the product quality along with the complex liquid-liquid two-phase rapid parallel competition reaction or parallel-serial competition reaction. A common parallel competition reaction system is competition reaction between acid-base-ester, instant chemical reaction occurs between acid and base, ester is subjected to rapid hydrolysis reaction under alkaline conditions, when the initial mixing effect of liquid-liquid two phases is high, the contact between the two phases is basically at amolecular level, the time scale of the reaction between the acid and the base is smaller than that of liquid-liquid mixing, acid-base neutralization reaction mainly occurs in a liquid phase, and hydrolysis reaction of the ester under alkaline conditions does not occur basically. When the initial mixing effect of the liquid-liquid two phases is poor and the time scale of the ester hydrolysis reaction is close to that of the mixing of the liquid-liquid two phases, part of the alkali in the liquid phase and the ester are subjected to hydrolysis reaction. Parallel competing reactions can therefore evaluate the mixing effect of the mixing device. Selecting HCl-NaOH-CH2ClCOOC2H5The parallel competition reaction between the two liquid-liquid mixing devices evaluates the mixing effect of the designed liquid-liquid mixing device, and the reactions and corresponding reaction rates are as follows:
the liquid-liquid rapid mixing reaction of the inventionThe inner diameter of the outer shell of the reactor is 150mm, the outer diameter of the inner shell is 120mm, the taper a at the reducing position of the outer shell is 60 degrees, the size of a gap formed between the reducing position of the outer shell and the inner shell is 1mm, and a rotational flow structure is arranged in the outer shell. The nozzle adopts an industrial nozzle, and the model is as follows: 3/8A-SS 25-30W manufactured by Spraying Systems CoA spray angle of 88-144 degrees (18-46 degrees corresponding to the spray angle b of the present invention, and 45 degrees is selected), and a flow rate of 15m is set at a spray pressure of 4 bar3And/h, adopting a single-nozzle spraying form. 0.1mol/L NaOH solution continuously enters from a liquid feed inlet at the upper part of the shell, and the flow rate is 15m3H; containing 0.1mol/L HCl and 0.1mol/L CH2ClCOOC2H5The mixed solution continuously enters from the upper end of the liquid conveying pipe with the flow rate of 15m3H, after being sprayed by a liquid nozzle, the formed annular fog drops are contacted with a liquid film containing NaOH solution, a sample is taken at an outlet at the lower part of the shell, and CH in the mixed solution is analyzed by gas chromatography2ClCOOC2H5The concentration of the mixed solution is continuously analyzed by three times of sampling, and CH in the mixed solution2ClCOOC2H5The concentration of (A) is respectively 0.496mol/L, 0.492mol/L and 0.497mol/L, which indicates that 99 percent of NaOH and HCl have chemical reaction, and only trace amount of NaOH and CH2ClCOOC2H5Hydrolysis occurs and the contacting of the liquid-liquid phases is essentially a contacting mixing at the molecular level.
Claims (10)
1. A liquid-liquid rapid mixing reactor, comprising: the device comprises an outer shell (1), an inner shell (2), a liquid conveying pipe (5), a nozzle (4), a supporting sheet (6), a demister (7), a gasket (9), an adjusting valve (11) and a pressure gauge (12);
the upper part of the shell (1) is provided with a liquid feed inlet (8), the lower part is a reducing part, the taper α at the reducing part is 20-80 degrees, and a liquid discharge outlet (3) is arranged below the reducing part;
a liquid conveying pipe (5) is arranged in the middle of the inner shell (2), and the lower end of the liquid conveying pipe (5) is connected with a liquid nozzle (4); a swirl plate demister (7) made of metal or nonmetal or an irregular or regular porous filling layer demister (7) made of wire mesh is also arranged in the middle of the inner shell (2); the upper part of the inner shell (2) is provided with a gas outlet (10), an adjusting valve (11) and a pressure gauge (12);
a gap of 0.5-5mm is formed between the diameter-reduced part of the lower part of the outer shell (1) and the lower part of the inner shell (2), the size of the gap can be adjusted by the thickness or the thread rotation of a gasket (9) at the joint of the outer shell (1) and the upper part of the inner shell (2), and the position of the gap formed between the inner shell (2) and the outer shell (1) is 1/5-4/5 away from the diameter-reduced top part of the outer shell (1);
a channel is formed between the inner wall of the outer shell (1) and the inner shell (2), and a certain number of supporting sheets (6) are fixed in the channel and used for fixing the position of the inner shell (2) so that the size of a gap formed between the reducing position of the lower part of the outer shell (1) and the lower part of the inner shell (2) is consistent.
2. A liquid-liquid rapid mixing reactor according to claim 1, characterized in that a channel with a cyclone structure is formed between the inner wall of the outer shell (1) and the inner shell (2) of the reactor.
3. A liquid-liquid rapid mixing reactor according to claim 1 or 2, characterized in that the taper α at the reduced diameter of the lower part of the shell (1) is preferably 30-60 degrees.
4. A liquid-liquid rapid mixing reactor according to claim 1 or 2, characterized in that the size of the gap formed between the reduced diameter of the lower part of the outer shell (1) and the lower part of the inner shell (2) is 0.5-2 mm.
5. A liquid-liquid rapid mixing reactor according to claim 1 or 2, characterized in that a certain number of support plates (6) are fixed inside the outer shell (1), the support plates (6) have the same size, and the thickness d thereof is slightly smaller than the distance from the inner wall of the outer shell to the outer wall of the inner shell; the support sheets (6) are uniformly fixed at the positions of the inner wall of the shell (1) at the same distance from the bottom, and the number N of the support sheets (6) is more than or equal to 3.
6. A liquid-liquid rapid mixing reactor according to claim 1 or 2, characterized in that the gap formed by the inner shell (2) and the outer shell (1) is preferably located at 1/3-2/3 from the top of the reduced diameter of the outer shell (1).
7. The liquid-liquid rapid mixing reactor according to claim 1 or 2, wherein the number of the nozzles (4) connected to the lower portion of the liquid conveying pipe (5) is one, the nozzles (4) are directly connected to the lower end of the liquid conveying pipe (5), the nozzles (4) form an annular mist droplet band, the annular mist droplet band is sprayed onto the liquid film formed by the outer shell (1) and the inner shell (2) at a certain angle b, and the size of b is 10-80 degrees.
8. A liquid-liquid rapid mixing reactor according to claim 7, characterized in that the annular band of mist droplets is sprayed onto the liquid film formed by the outer shell (1) and the inner shell (2) at an angle b, the size of b being 30-60 degrees.
9. The liquid-liquid rapid mixing reactor according to claim 1 or 2, wherein the number of the nozzles (4) connected to the lower part of the liquid conveying pipe (5) is more than one, the liquid conveying branch pipes (14) are uniformly distributed along the circumferential direction at the lower end of the liquid conveying pipe (5), the nozzles are correspondingly connected to the liquid conveying branch pipes (14), each nozzle forms a fan-shaped mist droplet belt, all the nozzles form an annular mist droplet belt, the annular mist droplet belt is sprayed onto the liquid film formed by the outer shell (1) and the inner shell (2) at a certain angle, and the size of b is 10-80 degrees.
10. A liquid-liquid rapid mixing reactor according to claim 9, characterized in that the annular band of mist droplets is sprayed onto the liquid film formed by the outer shell (1) and the inner shell (2) at an angle b, the size of b being 30-60 degrees.
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