CN106378021B - Parallel micro-impact flow mixing device and using method thereof - Google Patents
Parallel micro-impact flow mixing device and using method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
- B01F25/23—Mixing by intersecting jets
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
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Abstract
The invention discloses a parallel micro impinging stream mixing device, which comprises a micro impinging stream module, a front feeding module, a rear sealing module and a connecting device, wherein the front feeding module is arranged on the front feeding module; the micro impinging stream module is internally provided with mutually parallel sample feeding channels, an impinging channel is arranged perpendicular to the sample feeding channels, the impinging channel is of a T-shaped structure, and the bottom of the impinging channel is provided with a gradually expanding discharge hole; the outlet end of the front feeding module is connected with the inlet end of the micro impinging stream module, and the tail end of the micro impinging stream module is sealed by a rear sealing module; the front feeding module, the micro impinging stream module and the rear sealing module are connected and fastened through a connecting device. The device mainly aims at a liquid-liquid rapid reaction system, can be used as a premixing and distributing device of a rotating packed bed, and can also be independently used as a reactor for liquid-liquid rapid reaction to prepare superfine/nano functional materials; through the parallel impinging stream mixing, the problem of amplification of a micro impinging stream mixer is solved, and the further improvement of the RPB micro mixing performance is realized.
Description
Technical Field
The invention relates to a parallel micro impinging stream mixing device and a using method thereof, belonging to the technical field of chemical process reinforcement.
Background
The molecular-scale micromixing is a precondition for the reaction, and the reaction condition can be greatly improved by enhancing the micromixing, so that a high-quality product is obtained. Common process intensification techniques include impinging stream, hypergravity, microchannel techniques, and the like.
Impinging Stream (impacting Stream) is an important fluid mixing and strengthening technology, and is particularly effective for chemical processes of diffusion control. Over the years, the continuous phase of the impinging stream has expanded from the gas phase to the liquid phase, thereby further highlighting the advantages of the impinging stream in enhancing the micromixing of the liquid phase. For micromixing research on liquid-phase impinging stream devices, both free-Flow (FIS) and restricted impinging stream (CIS) configurations have been mainly focused abroad, while submerged configurations proposed by Wuyuan (CN1463789A, CN2455353Y) have been mainly focused domestically. The residence time of the free and restricted impinging stream devices is extremely short, and both devices can be operated continuously, wherein the micromixing effect of the restricted impinging stream is obviously superior to that of the free impinging stream; the submerged impinging stream device is mainly characterized by long residence time, but is mainly suitable for intermittent operation, and the micromixing effect is weaker than that of the FIS and CIS devices. Compared with the traditional kettle type reactor, the impinging stream device has simple structure and high mixing efficiency, so the impinging stream technology plays an important role in the fields of powder drying, superfine/nano functional material preparation, emulsification and the like.
Supergravity is another important process intensification technique, and its core equipment is a rotating packed bed. In the rotating packed bed, the fluid is torn into liquid drops, liquid filaments and liquid films under the action of centrifugal force, so that the reaction process controlled by mass transfer diffusion is greatly enhanced. The supergravity device is disclosed in chinese patent ZL95215430.7, etc. The supergravity technology has been successfully applied to the fields of separation, analysis, organic synthesis, ultrafine powder preparation and the like. The micro-mixing performance of the super-gravity Rotating Packed Bed (RPB) is obviously superior to that of other process strengthening equipment, and the micro-mixing time is 0.01-0.1 ms. However, the conventional supergravity rotating packed bed has the following problems: (1) the materials are directly injected into the rotary filler without premixing, so that part of reactants are discharged without contacting, and the utilization rate of the materials is reduced; (2) the axial distribution of the fluid in the rotating packed bed is poor, so that the utilization rate of the packing is generally low.
In order to solve the above problems, chinese patent (CN1425493A) discloses an impinging stream-rotating packed bed (IS-RPB), in which a free impinging stream device IS installed at the center of a drum cavity, so that the materials are first premixed, and simultaneously fluid impingement generates a large amount of dispersed droplets, which are captured by the rotating packing for further mixing and reaction. The utility model discloses a break through the technical problem of rotatory packed bed, improved the microcosmic mixing performance of rotatory packed bed. However, the product mixing effect is affected by the trapping rate of the droplets; most importantly, the micro-mixing performance of the free impinging stream is obviously weaker than that of the limited impinging stream, the impinging surface is easily affected by the disturbance of the fluid, and the running stability of the equipment is poor. Meanwhile, when the method is applied to an industrial amplifying device, mutual interference can be generated among the multi-stage parallel free impact flows, and the product quality is not favorably improved. In addition, liquid drops generated by free impact splash, so that the pipe fitting and the shell are easily seriously polluted, and the cleaning and maintenance difficulty of the device is increased.
Disclosure of Invention
The invention aims to provide a parallel micro impinging stream device, which adopts a plurality of groups of limited impinging stream modules to be connected front and back to form a multistage parallel mixing device, thereby solving the problem of IS-RPB amplification application; the device can further promote the micro-mixing performance of the RPB, improve the stability of equipment operation, and reduce the difficulty of equipment cleaning and maintenance. The invention also provides a using method of the device.
The invention provides a parallel micro impinging stream mixing device which comprises a micro impinging stream module, a front feeding module, a rear sealing module and a connecting device, wherein the front feeding module is arranged on the front feeding module;
the micro impinging stream module is of a cuboid structure, sample feeding channels which are parallel to each other are arranged in the micro impinging stream module, an impinging channel is arranged at the center of the cuboid and is vertical to the sample feeding channels, the impinging channel is of a T-shaped structure, and the bottom of the impinging channel is connected with a discharge hole;
the inlet of the front feeding module is of a tower or thread structure, the interior of the front feeding module is a through hole, the outlet end of the front feeding module is provided with the inlet end of a micro impinging stream module, and the tail end of the micro impinging stream module is sealed by a rear sealing module; the rear sealing module is a rectangular plate;
the connecting device comprises a connecting rod and a nut; the front feeding module, the micro-impinging stream module and the rear sealing module are sequentially connected and fastened through connecting devices, and joints of the modules are sealed by gaskets.
In the device, the micro impinging stream module is a core component of the device, sample injection channels of the module are parallel to each other, the inner diameter D of each channel is 8.0-10.0 mm, the length of each channel is 10.0-20.0 mm, and the distance I of each channel is 6.0-10.0 mm; the T-shaped impact channel is a place for mixing/reacting fluid, the plane of the T-shaped impact channel is perpendicular to the plane of the sample feeding channel, the impact channel is an equal-diameter tee joint, the drift diameter d is 1.0-2.0 mm, the small channel scale promotes the formation of a micro-area effect, the micro-mixing of the fluid is greatly enhanced, and the length of the impact channel is 6.0-10.0 mm; the fluid discharge port is located below the impact channel structure and is in a gradually-expanding cone shape, the upper end of the discharge port is connected with the bottom of the impact channel, the inner diameter of the discharge port is 1.0-2.0 mm, the inner diameter of the discharge port is 3.3-5.3 mm, the cone angle alpha is 30-45 degrees, and the fluid discharge port is mainly used for uniformly distributing liquid.
In the device, the inlet section of the front feeding module is designed to be of a tower type or a threaded structure, so that the front feeding module is convenient for pipeline connection, the inner diameter of the front feeding module is 8.0-10.0 mm, the thickness of the front feeding module is 2.0mm, and the length of the front feeding module is 50-100 mm. The long inlet section tube can be used for feeding materials and also can be used for adjusting the spatial position of the device in the reaction system (such as a rotating packed bed). The rear sealing module is matched with the front sealing module and used for sealing the whole device, and high sealing is realized through the bolts, the connecting rods and the grooves, so that fluid leakage is prevented.
The inlet section of the pre-feeding module is required to be connected with a pipeline, the tower structure is mainly used for connecting a hose, and other common connecting modes such as threads or flanges can be adopted, so that the inlet section of the pre-feeding module is designed into a tower or thread structure.
In the device, holes are respectively formed in four corners of the front end face and the rear end face of the micro impinging stream module, the same holes are respectively formed in four corners of the front feeding module and the rear sealing module corresponding to the micro impinging stream module, and the connecting rod penetrates through the holes and is fixed through the nuts.
In the device, the joint of the front feeding module and the micro impinging stream module, or the joint of the rear sealing module and the micro impinging stream module, or the joint of the two micro impinging stream modules is sealed by a gasket; the end part of the feed channel of each module is provided with an annular groove, the outlet end is provided with a bulge structure, the bulge and the groove are sequentially matched and connected, and the gasket is arranged in the groove.
In the invention, the modules are made of stainless steel, polytetrafluoroethylene or polymethyl methacrylate and other materials, and the modules are connected and sealed by bolts.
The invention provides a using method of a parallel micro-impinging stream mixing device, which comprises any one of the following steps:
(1) using one or more sets of micro-impinging-flow modules to form a single-stage or multi-stage structure for use as a mixer or reactor;
(2) one group or a plurality of groups of micro impinging stream modules are connected in parallel to form a single-stage or multi-stage impinging stream structure, and the single-stage or multi-stage impinging stream structure is coupled with a rotating packed bed and is used for industrial production.
The discharging direction of the multistage impinging stream structure is vertical to the rotating shaft; the modules of each group are mutually connected through an annular groove and a protruding structure, the groove is positioned at the feed end of each module, the width of the groove is 1.0mm, and the number of the modules is adjusted according to actual conditions.
In the multistage impinging stream structure, when multiple groups of micro impinging stream modules are coupled with the rotating packed bed, the distance K between the outlet and the inner edge of the packing and the thickness delta of the packing satisfy the following relations:
δ＝N·W(N＝1,2,3……) (2)
in the formula, H is the height of the micro impinging stream module body; l micro impinging stream module body length; w is the width of the micro impinging stream module body; d is the drift diameter of the impact channel; i is the feed channel spacing; alpha is the angle of the discharge hole of the micro impinging stream module; k is the distance between the tail end of the discharge port and the inner edge of the filler; delta is the filler thickness; and N is the number of the micro impinging stream module groups.
The device composed of a plurality of groups of micro impinging stream modules mainly adopts a continuous operation mode.
The invention provides a chemical mixing/reaction device, which is mainly used for a liquid-liquid rapid reaction system, can be coupled with a rotating packed bed to be used as a premixing and distributing device, and can also be independently used as a reactor for preparing functional materials on a large scale. The invention has the following beneficial effects:
(1) micro impact flow is formed in a limited space of the impact channel, the micro mixing effect is obviously improved, and the micro mixing performance of equipment can be further improved after the micro impact flow is combined with the rotary packed bed;
(2) the micro fluctuation of the fluid does not influence the running condition of the equipment, the stability of the equipment is improved, meanwhile, the splashing corrosion degree of the liquid drops is reduced, and the equipment is convenient to clean and maintain;
(3) the device has simple structure, is easy to realize parallel amplification, and can prepare superfine/nanometer functional materials when being independently used as mixing and reaction equipment.
Drawings
FIG. 1 is a perspective view of a side-by-side micro-impingement flow mixing device configuration of the present invention;
FIG. 2 is a perspective view of the micro impinging stream module of the present invention;
FIG. 3 is a schematic structural diagram of a micro impinging stream module of the present invention;
FIG. 4 is a cross-sectional view taken along line A-A of FIG. 3;
FIG. 5 is a schematic representation of the side-by-side micro-impingement flow mixing apparatus used in combination with a rotating packed bed in example 1;
FIG. 6 is a flow chart of a micromixing performance experiment of example 1 with a parallel micro-impingement flow-rotating packed bed (PMIS-RPB);
FIG. 7 is a three-dimensional block diagram of a single stage micro-impingement flow (MIS) device;
FIG. 8 IS a three-dimensional block diagram of a free impingement flow (IS) apparatus;
FIG. 9 IS a graph comparing micro-hybrid performance of a single stage MIS-RPB device with an IS-RPB device;
FIG. 10 is a flow chart of the parallel micro-impact flow reactor (PMISR) for preparing ultrafine powder in example 3.
In the figure: 1 is a front feeding module; 2 is a first-stage micro impinging stream module; 3 is a secondary micro impinging stream module; 4 is a rear sealing module; 5 is a connecting rod, 6 is a nut, 7 is a groove, 8 is a sample introduction channel, 9 is an impact channel, 10 is a discharge port, 11 is a first liquid storage tank, 12 is a pump I, 13 is a first flow regulating valve, 14 is a first flow meter, 15 is a product collector, 16 is a parallel micro impact flow-rotating packed bed, 17 is a second liquid storage tank, 18 is a pump II, 19 is a second flow regulating valve, 20 is a second flow meter, and 21 is a parallel micro impact flow reactor.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Firstly, explaining the structure of the invention, as shown in fig. 1-4, a parallel micro impinging stream mixing device comprises micro impinging stream modules 2 and 3, a front feeding module 1, a rear sealing module 4 and a connecting device;
fig. 1 includes two stages of micro impinging stream modules, including a first stage micro impinging stream module 2 and a second stage micro impinging stream module 3; the micro impinging stream module is of a cuboid structure, a sample feeding channel 8 which is parallel to each other is arranged in the micro impinging stream module, an impinging channel 9 is arranged at the center of the cuboid and is vertical to the sample feeding channel 8, the impinging channel 9 is of a T-shaped structure, and the bottom of the impinging channel is connected with a discharge hole 10;
the inlet of the front feeding module 1 is of a tower type or threaded structure, a straight-through hole is formed inside the front feeding module 1, the outlet end of the front feeding module 1 is connected with the inlet end of the micro impinging stream module, and the tail end of the micro impinging stream module is sealed by a rear sealing module 4; the rear sealing module 4 is a rectangular plate;
the connecting device comprises a connecting rod 5 and a nut 6; the front feeding module, the micro impinging stream module and the rear sealing module are connected and fastened through a connecting device.
The inner diameter of the sample feeding channel 8 is 8.0-10.0 mm; the length is 10.0-20.0 mm, and the channel interval is 6.0-10.0 mm; the drift diameter of the impact channel is 1.0-2.0 mm, and the length of the impact channel is 6.0-10.0 mm.
The inner diameter of the front feeding module 1 is 8.0-10.0 mm, the length of the front feeding module is 50-100 mm, and the inlet long pipe can adjust the spatial position of the device in the rotary packed bed.
The discharge port 10 is a gradually expanding cone, the upper end of the discharge port is connected with the bottom of the impact channel 9, the inner diameter of the discharge port is 1.0-2.0 mm, the inner diameter of the discharge port is 3.3-5.3 mm, and the cone angle is 30-45 degrees.
Holes are respectively formed in four corners of the front end face and the rear end face of the micro impact flow module, the same holes are respectively formed in four corners of the front feeding module 1 and the rear sealing module 4 corresponding to the micro impact flow module, and the connecting rod 5 penetrates through the holes and is fixed through the nut 6.
The module is made of one of stainless steel, polytetrafluoroethylene or polymethyl methacrylate.
The joint of the front feeding module and the micro impinging stream module or the joint of the two micro impinging stream modules is sealed by a gasket; the end part of the feed channel of each module is provided with an annular groove, the outlet end is provided with a convex structure, the convex structure is sequentially matched and connected with the groove, and the gasket is arranged in the groove.
The following description of the invention is given by way of specific examples:
example 1: the micro-mixing performance experimental study of the single-stage MIS-RPB device and the IS-RPB device.
FIG. 5 is a schematic diagram showing the use of the side-by-side micro-impingement flow mixing device of the present embodiment in combination with a rotating packed bed; fig. 5 shows that the discharge direction of the impinging stream module is perpendicular to the rotation axis.
FIG. 6 shows a flow chart of the micromixing performance experiment of the parallel micro-impingement flow-rotating packed bed (PMIS-RPB) of the present example; liquid A enters a parallel micro-impinging flow-rotating packed bed 16 from a first liquid storage tank 11 through a pump I12, a first flow regulating valve 13 and a first flow meter 14; the liquid B enters the parallel micro impinging flow-rotating packed bed 16 from the second liquid storage tank 17 through the pump II 18, the second flow regulating valve 19 and the second flow meter 20; the two materials are collided, mixed and reacted in a parallel micro-impinging stream-rotating packed bed 16. The parallel micro-impinging stream-rotating packed bed 16 is controlled by a motor and a frequency converter.
FIG. 7 is a three-dimensional block diagram of a single-stage MIS device;
FIG. 8 IS a three-dimensional structural view of an IS apparatus;
the single stage MIS used in this embodiment has the same characteristic dimensions as IS devices, except that the fluid impingement region of the latter IS not bounded by walls (see fig. 8).
The specific operation steps are as follows: preparing an iodide mixed solution A: taking 11.241g H 3 BO 3 And 3.636g NaOH to give H 3 BO 3 NaOH buffer solution. Then 0.6560g KI was added to the buffer, after mixing well, 0.7062g KIO was added 3 And obtaining a clear solution A after constant volume by using a 1L volumetric flask. Preparing a sulfuric acid solution B: accurately weighing 12.5g of 98% concentrated sulfuric acid, and diluting with deionized water respectively to obtain solution B with hydrogen ion concentration of 0.05 mol/L. The mixed solution A and the acid solution B are respectively conveyed into research equipment through pumps, the solutions are premixed and distributed under the action of strong impact, and then the reaction process is further strengthened through a rotating packed bed. After the equipment runs stably, collecting the product, measuring the absorbance of the product at the wavelength of 353nm by using a spectrophotometer, and converting according to Lambert-Beer law to obtain an ionization index X S The value is obtained.
As shown in FIG. 9, compared to IS-RPB device, single stage MIS-RPB device has the same Re condition, X S The value of (A) is smaller, which shows that the micro-mixing performance is obviously improved. Therefore, the present invention uses micro impinging streams for mixing process enhancement.
Example 2: preparing the superfine iron-doped manganese dioxide by using a single-stage micro impinging stream reactor.
This example uses a single-stage MIS device as an example to prepare ultra-fine functional materials.
Selecting FeCl 3 50mL of 0.1 mol.L is prepared as a doping source -1 Containing Fe 3+ Ionic KMnO 4 Solution A, manganese and iron in solution are proportioned to Mn 2+ :Fe 3+ 20: 1; 50mL of 0.15 mol. L was prepared -1 MnSO 4 And (4) solution B. The two solutions are introduced into an MIS reactor through a pump at a volume flow ratio of 1:1 for mixing and reaction, the experimental conditions are normal temperature (25 +/-1 ℃), and the inlet volume flow is 80L/h. Collecting the product with a beaker, stirring in a magnetic stirrer for 30min, vacuum filtering, washing, and drying in an oven at 80 deg.C for 12 h. Compared with the traditional stirring reactor, the sample prepared by adopting single-stage micro impinging stream has more uniform particle size distribution, the average particle size is about 120nm, the specific capacity of the product prepared by adopting the traditional stirring method is improved by 15 percent, and the specific capacity is attenuated by 10 percent after the product is circulated for 1000 times。
Example 3: the multistage micro impinging stream reactor is used for preparing the superfine iron-doped manganese dioxide in a large scale.
In this embodiment, a multi-stage MIS device is used as an example to prepare an ultra-fine functional material, and the flow is shown in fig. 10. Liquid A enters a parallel micro-impinging stream reactor 21 from a first liquid storage tank 11 through a pump I12, a first flow regulating valve 13 and a first flow meter 14; the liquid B enters a parallel micro-impinging stream reactor 21 from a second liquid storage tank 17 through a pump II 18, a second flow regulating valve 19 and a second flow meter 20; the two materials are collided, mixed and reacted in the parallel micro impinging stream reactor 21.
On the basis of the embodiment 2, the same reaction system and solution concentration are adopted, the multi-stage MIS device is used for replacing a single-stage MIS device, and the preparation scale of the superfine material is enlarged through a continuous operation mode on the premise of ensuring the performance of the original material, so that the industrial production of the functional material is realized.
Claims (7)
1. A parallel micro-impinging-stream mixing device, characterized by: the device comprises a micro impinging stream module, a front feeding module, a rear sealing module and a connecting device;
the micro impinging stream module is of a cuboid structure, mutually parallel sample feeding channels are arranged in the micro impinging stream module, an impinging channel is arranged at the center of the cuboid and is vertical to the sample feeding channels, the impinging channel is of a T-shaped structure, and the bottom of the impinging channel is connected with a discharge hole; the discharge hole is in a gradually expanding cone shape;
the inlet of the front feeding module is of a tower or thread structure, a straight-through hole is formed inside the front feeding module, the outlet end of the front feeding module is connected with the inlet end of the micro impinging stream module, and the tail end of the micro impinging stream module is sealed by a rear sealing module; the rear sealing module is a rectangular plate;
the connecting device comprises a connecting rod and a nut; the front feeding module, the micro impinging stream module and the rear sealing module are connected and fastened through a connecting device;
the use method of the parallel micro impinging stream mixing device comprises the steps of forming a single-stage or multi-stage impinging stream structure by using one group or a plurality of groups of micro impinging stream modules connected in parallel and coupling the single-stage or multi-stage impinging stream structure with a rotary packed bed; the discharging direction of the multistage impinging stream structure is vertical to the rotating shaft; the modules in each group are matched and connected with each other through an annular groove and a protruding structure, the groove is positioned at the feeding end of the modules, and the depth of the groove is 1.0 mm;
in a multistage impinging stream structure, when multiple groups of micro impinging stream modules are coupled with a rotating packed bed, the distance between an outlet and the inner edge of the packingKAnd filler thicknessδThe following relationship is satisfied:
in the formula (I), the compound is shown in the specification,His the micro impinging stream module body height;Lis the micro impinging stream module body length;Wis the width of the micro impinging stream module body;dthe drift diameter of the impact channel;Iis the feed channel spacing;αthe angle of the discharge hole of the micro impinging stream module;Kthe distance between the tail end of the discharge port and the inner edge of the filler;δis the filler thickness;Nthe number of the micro impinging stream module groups.
2. The side-by-side micro-impingement flow mixing device of claim 1, wherein: the inner diameter of the sample feeding channel is 8.0-10.0 mm; the length is 10.0-20.0 mm, and the channel interval is 6.0-10.0 mm; the drift diameter of the impact channel is 1.0-2.0 mm, and the length of the impact channel is 6.0-10.0 mm.
3. The side-by-side micro-impingement flow mixing device of claim 1, wherein: the internal diameter of leading feeding module is 8.0~10.0 mm, and length is 50~100 mm, and the spatial position of device in rotatory packed bed can be adjusted to the entry long tube.
4. The side-by-side micro-impingement flow mixing device of claim 1, wherein: the discharge gate upper end is connected with striking passageway bottom, and the discharge gate internal diameter is 1.0~2.0 mm, and the internal diameter in exit is 3.3~5.3 mm, and the cone angle is 30~ 45.
5. The side-by-side micro-impingement flow mixing device of claim 1, wherein: holes are respectively formed in four corners of the front end face and the rear end face of the micro impact flow module, holes with the same size are respectively formed in the four corners of the front feeding module and the rear sealing module and the positions corresponding to the micro impact flow module, and the connecting rod penetrates through the holes and is fixed through nuts.
6. The side-by-side micro-impingement flow mixing apparatus of claim 1, wherein: the module is made of one of stainless steel, polytetrafluoroethylene or polymethyl methacrylate.
7. The side-by-side micro-impingement flow mixing device of claim 1, wherein: the joint of the front feeding module or the rear sealing module and the micro impinging stream module or the joint of the two micro impinging stream modules is sealed by a gasket; the end part of the feed channel of each module is provided with an annular groove, the outlet end is provided with a bulge structure, the bulge and the groove are sequentially matched and connected, and the gasket is arranged in the groove.
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