CN114797700B - Continuous flow field synthesis equipment - Google Patents
Continuous flow field synthesis equipment Download PDFInfo
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- CN114797700B CN114797700B CN202210291125.9A CN202210291125A CN114797700B CN 114797700 B CN114797700 B CN 114797700B CN 202210291125 A CN202210291125 A CN 202210291125A CN 114797700 B CN114797700 B CN 114797700B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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Abstract
The invention belongs to the technical field of pipeline reactors, and particularly relates to continuous flow field synthesis equipment. The equipment comprises a reaction pipeline, a first storage tank, a second storage tank and a power device; the reaction pipeline is vertically arranged and has a constant inner diameter; the lower part of the reaction pipeline is provided with a feed inlet, and the upper part of the reaction pipeline is provided with a discharge outlet; a reaction section for feeding liquid to react is arranged in the reaction pipeline, and a rectification section for enabling the feed liquid to form a stable flow state is arranged below the reaction section; the first storage tank is communicated with a feed inlet of the reaction pipeline; the second storage tank is communicated with a discharge hole of the reaction pipeline; the power device drives the feed liquid in the reaction pipeline to flow from bottom to top. The invention provides continuous flow field synthesis equipment, which can effectively eliminate interference factors which cause disturbance to a flow field and exist in the existing continuous flow field reactor, thereby being better applied to fine synthesis.
Description
Technical Field
The invention belongs to the technical field of pipeline reactors, and particularly relates to continuous flow field synthesis equipment.
Background
Continuous flow field synthesis is a synthesis that changes the traditional kettle reaction to a reaction in a continuous tube. The raw materials are uniformly heated in the synthesis mode, the flow state is more stable, and compared with the traditional kettle type reaction product, the reaction product generally has better consistency, is suitable for fine synthesis of pharmaceutical and chemical products, and particularly has remarkable advantages in synthesis of nano materials with lower entropy and regular micro morphology.
Although the flow state of the continuous flow field synthesis is more stable compared with that of a kettle type reaction synthesizer, and the continuous flow field synthesis is more beneficial to the growth of regular nano materials, a plurality of interference factors which are difficult to eliminate still exist in the existing continuous flow field reactor to disturb the flow field, so that local turbulence is caused, and the morphology of the nano materials is influenced. On the first hand, when the reaction liquid is heated by any existing heating mode, a temperature gradient is inevitably generated inside the reaction liquid, otherwise, heat cannot be transferred, but a density gradient is inevitably generated inside the reaction liquid due to the existence of the temperature gradient, so that convection motion is caused in the reaction liquid, and disturbance is caused to the growth of the nano material. In the second aspect, the reaction liquid is required to flow in the reaction pipeline, and a power device for pushing the reaction liquid to flow is necessarily required to overcome the flow resistance, but any existing power device for driving the reaction liquid to flow, such as a centrifugal pump, a peristaltic pump, etc., cannot continuously generate a stable laminar flow state for a long time. In the third aspect, synthesis reaction usually requires mixing two or more raw material liquids for reaction, but adding a certain volume of one raw material liquid to another raw material liquid can cause obvious interference to the flow state of the raw material liquid.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides continuous flow field synthesis equipment, aiming at eliminating at least part of interference factors which cause disturbance to a flow field in the prior continuous flow field reactor, so as to be better applied to fine synthesis.
In order to achieve the purpose, the invention is realized by the following technical scheme: a continuous flow field synthesis apparatus comprising:
the reaction pipeline is vertically arranged and has a constant inner diameter; the lower part of the reaction pipeline is provided with a feeding hole, and the upper part of the reaction pipeline is provided with a discharging hole; a reaction section for feeding liquid to react is arranged in the reaction pipeline, and a rectification section for enabling the feed liquid to form a stable flow state is arranged below the reaction section;
the first storage tank is communicated with the feeding hole of the reaction pipeline;
the second storage tank is communicated with the discharge hole of the reaction pipeline;
the power device drives the feed liquid in the reaction pipeline to flow from bottom to top.
Furthermore, a rectifying grid for dividing the cross section of the pipeline into a plurality of grid units is arranged in the rectifying section, a feed pipe is arranged on the rectifying grid, and the feed pipe extends from the lower end of the rectifying grid to the upper end of the rectifying grid along the central axis of the rectifying section.
Further, the rectification grid comprises a plurality of grid sections which are sequentially connected along the vertical direction, the grid units formed by dividing the grid sections which are lower are more dense, and the grid units formed by dividing the grid sections which are upper are more sparse.
Further, in any two adjacent grid sections, the cross-sectional area blocked by the lower grid section can completely cover the cross-sectional area blocked by the upper grid section.
Further, the upper end of the feed pipe exceeds the rectifying grid for a certain distance.
Furthermore, each grid section is composed of a plurality of grid plates which are connected in a cross mode, cross lines formed by crossing any two grid plates are parallel to the reaction pipeline, and the feeding pipes are arranged on the cross lines of the grid plates.
Furthermore, the lower end of the feeding pipe is connected with a feeding pipe, and the feeding pipe extends from the center of the reaction pipeline to the pipe wall along the grid plate and extends out of the pipe wall.
Furthermore, the continuous flow field synthesis equipment is provided with a plurality of reaction sections which are connected up and down, a heating device with controllable temperature is sleeved outside each reaction section, and the temperature of the heating device which is closer to the upper part is higher.
Further, the heating device is a heating jacket, and a constant-temperature liquid heat-conducting medium continuously flows through the heating jacket.
Further, the reaction pipeline is fixed on a structure by using a plurality of fixing seats to prevent the reaction pipeline from vibrating.
Advantageous effects
The continuous flow field synthesis equipment provided by the invention enables the feed liquid to form a stable laminar flow state through the design of the integral structure and the arrangement of the rectification grids with the specific structure, thereby providing a stable flow field environment for the reaction of the feed liquid.
Furthermore, the continuous flow field synthesis equipment is provided with a feed pipe for supplying the second feed liquid, so that the continuous flow field synthesis equipment is suitable for synthesis reaction of no more than two solutions, and simultaneously, the feed pipe and the rectification grid are skillfully fused, so that disturbance is avoided from being newly generated, and the second feed liquid is stably conveyed to the center of the first feed liquid.
Furthermore, the temperature of a plurality of reaction sections arranged on the continuous flow field synthesis equipment can be independently controlled, and the reaction sections are arranged in a high-temperature field distribution state and a low-temperature field distribution state, so that the controllable heating of the material liquid is realized, and the interference to the flow state caused by heating is avoided.
Drawings
FIG. 1 is a schematic structural view of a continuous flow field synthesis apparatus.
Fig. 2 is a schematic view of the structure of the rectifying grid in the rectifying section.
Fig. 3 is a bottom view of the rectifying grid.
Fig. 4 isbase:Sub>A cross-sectional view taken along the planebase:Sub>A-base:Sub>A in fig. 2.
Fig. 5 is a cross-sectional view taken along the plane B-B in fig. 2.
FIG. 6 is a schematic diagram of the flow regime distribution of perfect laminar flow in a round tube.
FIG. 7 is a schematic diagram of a single-stage reaction section.
Detailed Description
The invention is further illustrated by the following specific examples, which are illustrative and intended to illustrate the problem and explain the invention, but not limiting.
Example 1
A continuous flow field synthesis apparatus, as shown in fig. 1, comprising:
the reaction pipeline is vertically arranged, and the inner diameter of the reaction pipeline is constant so as to prevent liquid from generating vortex due to change of a flow section when the liquid flows inside; the lower part of the reaction pipeline is provided with a feed inlet, and the upper part of the reaction pipeline is provided with a discharge outlet; a reaction section 12 in which a feed solution is reacted is provided in the reaction conduit; a rectifying section 11 which enables the feed liquid to form a stable flow state is arranged below the reaction section, so that the feed liquid forms a stable flow state before entering the reaction section 12;
the first storage tank 2 is communicated with the feed inlet of the reaction pipeline, and is used for supplying feed liquid to the reaction pipeline;
the second storage tank 3 is communicated with a discharge hole of the reaction pipeline and is used for storing a product after reaction;
the power device 4, such as a centrifugal pump or other liquid conveying device capable of forming a stable flow rate, may be installed between the rectifying section 11 and the first storage tank 2, so as to pump the material liquid in the first storage tank 2 into the reaction pipeline, so that the material liquid in the reaction pipeline flows from bottom to top against the gravity.
The rectifying section 11 is internally provided with a rectifying grid which divides the cross section of the pipeline into a plurality of grid units, the rectifying grid is provided with a feed pipe 61, and the feed pipe 61 extends from the lower end of the rectifying grid to the upper end of the rectifying grid along the central axis of the rectifying section 11. The kinetic energy of the vortex in the feed liquid is consumed through the rectification grids, so that the feed liquid forms a stable flow state. The second feed liquid can be injected into the reaction tube through the feed tube 61 to perform a synthesis reaction with the feed liquid existing in the reaction tube.
The rectification grid comprises a plurality of sections of grid sections which are connected in sequence along the vertical direction, grid units formed by dividing the grid sections which are closer to the lower part are more dense, and grid units formed by dividing the grid sections which are closer to the upper part are more sparse. As shown in fig. 2 to 5, three grid sections are taken as an example for description, and the rectification grid comprises a first grid section 111, a second grid section 112 and a third grid section 113 from bottom to top; the grid form may be a square grid, a rectangular grid, a diamond grid, a hexagonal grid, a fan grid, with the square grid shown being preferred. The grid units of the lower grid section are dense, the ability of consuming eddy current and disturbing flow is stronger, but the interference of the grid units to the flow of the feed liquid is larger; the grid units of the upper grid section are sparse, the capability of consuming eddy current and disturbing flow is slightly weak, but the interference of the grid units to the flow of the feed liquid is obviously weakened. Based on the arrangement mode and principle, when the feed liquid flows through the rectification grids from bottom to top, the fast rectification is firstly obtained, the flow directions of all parts of the cross section of the pipeline are fast and tend to be consistent, the rectification function can be gradually weakened along with the upward flow of the feed liquid, the feed liquid continues to stably flow upwards under the action of inertia under the condition of no external disturbance, meanwhile, the grids are more and more sparse, the friction resistance applied to the feed liquid is gradually reduced, and the flow velocity distribution of the feed liquid at all parts of the cross section of the pipeline gradually forms a perfect laminar flow state with the distribution form of a rotating paraboloid as shown in figure 6.
In any two adjacent grid sections at the upper end and the lower end, the cross section area blocked by the lower grid section can completely cover the cross section area blocked by the upper grid section, so that the feed liquid can not encounter a new grid plate to be divided when advancing, and the deviation of the flow state of the feed liquid to the direction far away from the perfect laminar flow state caused by the new division is avoided.
The upper end of the feed tube 61 extends beyond the rectifying grid by a distance, preferably 1 to 3 times the inner diameter of the reaction tube, which is illustrated in the drawing as 1 time the inner diameter of the reaction tube. The upper end of the feed pipe 61 exceeds 1-3 times of the inner diameter of the reaction pipeline, so that the influence of residual rectification grids can be fully digested when the feed liquid flows upwards. Generally, the outer diameter of the feed pipe 61 is much smaller than the inner diameter of the reaction tube, i.e., usually not more than 1/10 of the inner diameter of the reaction tube, preferably not more than 1/20 of the inner diameter of the reaction tube, so that the feed pipe 61 has little influence on the flow state of the feed liquid, thereby further facilitating the feed liquid to form a perfect laminar flow state as shown in FIG. 6.
On the basis that the material liquid forms an approximate perfect laminar flow state, the ratio of the average flow velocity and the maximum flow velocity (namely the flow velocity at the center of the reaction pipeline) of the material liquid in the reaction pipeline can be determined according to the distribution of the revolution paraboloids, and the average flow velocity of the material liquid in the reaction pipeline can be accurately known according to the flow of the power device 4 and the inner diameter of the reaction pipeline, so that the flow velocity of the material liquid at the center of the reaction pipeline can be known. Thus, the flow of the feed tube 61 can be controlled, so that the flow velocity of the feed liquid output by the feed tube 61 is consistent with the flow velocity of the feed liquid in the center of the reaction pipeline. In addition, the proportion of materials required by synthesis can be realized by adjusting the concentrations of the two feed liquids. The operation can perfectly mix the two feed liquids, so that the two feed liquids do not have mutual disturbance on a macroscopic scale or a mesoscale, and only have molecular diffusion motion on a microscopic scale generated by the concentration gradient of the materials, thereby creating a very stable flow field environment for the synthesis reaction and being beneficial to forming the nano material with low entropy and regular morphology.
Each grid section is composed of a plurality of grid plates which are connected in a crossing way, the crossing line formed by crossing any two grid plates is parallel to the reaction pipeline, and the feed pipe 61 is arranged on the crossing line of the grid plates to reduce the interference to the flow state as much as possible.
The lower end of the feed pipe 61 is connected with a feed pipe 62, and the feed pipe 62 extends from the center of the reaction pipeline to the pipe wall along the grid plate and extends to the outside of the pipe wall. The feeding pipe 62 is used for conveniently injecting second feed liquid for reaction from the outside of the reaction pipeline to the inside, the feeding pipe 62 is positioned at the lower end of the rectification grid and arranged along the grid plate, the disturbance caused by the feeding pipe 62 can be reduced as much as possible, the rectification distance of the rectification grid to the formed disturbance is prolonged as much as possible, and the disturbance is eliminated to the greatest extent.
The continuous flow field synthesis equipment comprises a plurality of reaction sections 12 connected up and down, the single-section reaction section 12 is shown in fig. 7, a heating device with controllable temperature is sleeved outside each reaction section 12, and the temperature of the heating device above the reaction section is higher. The reaction sections 12 with gradually rising temperature from bottom to top are arranged, disturbance to the flow state of the feed liquid caused by the heating process can be eliminated, the higher the temperature is, the smaller the density is, the more the feed liquid tends to move upwards, the density of the feed liquid in different reaction sections 12 is gradually decreased from bottom to top, and therefore, spontaneous power for mixing the feed liquid up and down does not exist, and flow state disturbance caused by the heating process is avoided.
The heating device is a heating jacket, and a constant-temperature liquid heat-conducting medium continuously flows through the heating jacket. A liquid heat transfer medium such as heat transfer silicone oil, deionized water, etc., preferably flows through the heating jacket at a constant flow rate in a bottom-in-top-out manner.
The reaction pipeline is fixed on a structure such as a structural wall by using a plurality of fixing seats so as to prevent the reaction pipeline from vibrating.
The above embodiments are exemplary only, and are intended to illustrate the technical concept and features of the present invention so that those skilled in the art can understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (5)
1. A continuous flow field synthesis apparatus, characterized by: the method comprises the following steps:
the reaction pipeline is vertically arranged and has a constant inner diameter; the lower part of the reaction pipeline is provided with a feeding hole, and the upper part of the reaction pipeline is provided with a discharging hole; a reaction section (12) for feed liquid reaction is arranged in the reaction pipeline, and a rectification section (11) for enabling feed liquid to form a stable flow state is arranged below the reaction section (12);
the first storage tank (2), the first storage tank (2) is communicated with the feeding hole of the reaction pipeline;
the second storage tank (3), the said second storage tank (3) is communicated with discharge port of the said reaction pipeline;
the power device (4), the said power device (4) drives the feed liquid in the said reaction pipeline to flow from bottom to top;
the rectifying section (11) is internally provided with a rectifying grid for dividing the section of the pipeline into a plurality of grid units, the rectifying grid is provided with a feeding pipe (61), and the feeding pipe (61) extends from the lower end of the rectifying grid to the upper end of the rectifying grid along the central axis of the rectifying section (11);
the rectification grid comprises a plurality of sections of grid sections which are sequentially connected along the vertical direction, grid units formed by dividing grid sections which are closer to the lower part are more dense, and grid units formed by dividing grid sections which are closer to the upper part are more sparse;
the upper end of the feeding pipe (61) exceeds the rectifying grid for a certain distance;
each grid section is composed of a plurality of grid plates which are connected in a crossing manner, crossing lines formed by crossing any two grid plates are parallel to the reaction pipeline, and the feeding pipes (61) are arranged on the crossing lines of the grid plates;
the continuous flow field synthesis equipment is provided with a plurality of reaction sections (12) which are connected up and down, a heating device with controllable temperature is sleeved outside each reaction section (12), and the temperature of the heating device which is closer to the upper part is higher.
2. The continuous flow-field synthesis apparatus of claim 1, wherein: in any two adjacent grid sections, the cross section area blocked by the lower grid section can completely cover the cross section area blocked by the upper grid section.
3. The continuous flow-field synthesis apparatus of claim 1, wherein: the lower end of the feeding pipe (61) is connected with a feeding pipe (62), and the feeding pipe (62) extends from the center of the reaction pipeline to the pipe wall along the grid plate and extends to the outside of the pipe wall.
4. The continuous flow-field synthesis apparatus of claim 1, wherein: the heating device is a heating jacket, and a constant-temperature liquid heat-conducting medium continuously flows through the heating jacket.
5. The continuous flow-field synthesis apparatus of claim 1, wherein: fixing the reaction pipeline on a structure by using a plurality of fixing seats to prevent the reaction pipeline from vibrating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210291125.9A CN114797700B (en) | 2022-03-23 | 2022-03-23 | Continuous flow field synthesis equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210291125.9A CN114797700B (en) | 2022-03-23 | 2022-03-23 | Continuous flow field synthesis equipment |
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| CN114797700A CN114797700A (en) | 2022-07-29 |
| CN114797700B true CN114797700B (en) | 2023-02-17 |
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| CN202210291125.9A Active CN114797700B (en) | 2022-03-23 | 2022-03-23 | Continuous flow field synthesis equipment |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958143A (en) * | 2006-09-29 | 2007-05-09 | 浙江大学 | Oscillatory flow tubular reactor of balking ring baffle |
| WO2020126311A1 (en) * | 2018-12-19 | 2020-06-25 | IFP Energies Nouvelles | Tubular reactor having a conveyor screw |
| CN111706579A (en) * | 2020-07-09 | 2020-09-25 | 上海交通大学 | Flow regulator suitable for regulating fluid flow velocity distribution at rear end of bent pipe |
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2022
- 2022-03-23 CN CN202210291125.9A patent/CN114797700B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958143A (en) * | 2006-09-29 | 2007-05-09 | 浙江大学 | Oscillatory flow tubular reactor of balking ring baffle |
| WO2020126311A1 (en) * | 2018-12-19 | 2020-06-25 | IFP Energies Nouvelles | Tubular reactor having a conveyor screw |
| CN111706579A (en) * | 2020-07-09 | 2020-09-25 | 上海交通大学 | Flow regulator suitable for regulating fluid flow velocity distribution at rear end of bent pipe |
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| Publication number | Publication date |
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| CN114797700A (en) | 2022-07-29 |
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