CN210058205U

CN210058205U - Liquid phase reaction device

Info

Publication number: CN210058205U
Application number: CN201920423006.8U
Authority: CN
Inventors: 李雄; 徐正良
Original assignee: Wuhan Strong Feng Xinte Science And Technology Ltd
Current assignee: Wuhan Strong Feng Xinte Science And Technology Ltd
Priority date: 2019-03-29
Filing date: 2019-03-29
Publication date: 2020-02-14
Anticipated expiration: 2029-03-29

Abstract

The utility model discloses a liquid phase reaction unit, include: the raw material supply assembly comprises at least two sets, each set of raw material supply assembly comprises a raw material tank, a proportioning pump, a metering tank and a feeding pump which are sequentially connected through pipelines, wherein at least two metering tanks are connected between the proportioning pump and the feeding pump in parallel, and a feed inlet and a discharge outlet of each metering tank are respectively provided with a control valve; a microchannel reactor connecting the feed pump and a product tank; and the monitoring system comprises a control machine and a finished product sensor arranged at the downstream of the microchannel reactor, the finished product sensor is in signal connection with the control machine, and the control machine controls the opening and closing of all the control valves, all the proportioning pumps and all the feeding pumps. The utility model has the advantages that: the microchannel reactor is used as a reaction site, so that continuous production is realized, the magnitude of each reaction is small, and the safety is high; the liquid phase raw materials react quickly and fully, the reaction accuracy is high, and the production automation is realized.

Description

Liquid phase reaction device

Technical Field

The utility model relates to a liquid phase reaction unit.

Background

The existing liquid phase reaction is generally to pour liquid phase raw materials into a reaction kettle in proportion, react for a certain time under certain conditions (such as temperature adjustment, pressure adjustment and the like), assist the mixing of the raw materials in stirring and other ways during the reaction, and finally obtain the whole final product in the reaction kettle. There are disadvantages in that: 1. the reaction process is intermittent, the reaction of the next batch can be carried out only after the reaction of the current batch in the reaction kettle is finished, and continuous production cannot be realized; 2. the magnitude of each reaction is large, once an operation accident occurs, the danger coefficient is large, and the raw material waste is large; 3. the proportioning precision of the reaction materials is low, the homogenizing speed of the reaction materials is low, so that the reaction raw materials are insufficient or excessive, side reactants are locally generated, and the local reaction is insufficient; 4. in order to adapt to the reaction amount of different batch changes, corresponding process parameters need to be adjusted in a targeted manner in each reaction, playing in the process can be adjusted only according to the experience of an operator, and automatic production is difficult to realize.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to overcome above-mentioned technique not enough, provide a liquid phase reaction unit, solve among the prior art unable realization continuous production, the magnitude of reaction at every turn is big, the reaction precision is low and be difficult to realize automated production's technical problem.

In order to achieve the above technical object, the present invention provides a liquid phase reaction apparatus, comprising:

the raw material supply assembly comprises at least two sets, each set of raw material supply assembly comprises a raw material tank, a proportioning pump, a metering tank and a feeding pump which are sequentially connected through pipelines, wherein at least two metering tanks are connected between the proportioning pump and the feeding pump in parallel, and a feed inlet and a discharge outlet of each metering tank are respectively provided with a control valve;

a microchannel reactor connecting the feed pump and a product tank; and the monitoring system comprises a control machine and a finished product sensor arranged at the downstream of the microchannel reactor, the finished product sensor is in signal connection with the control machine, and the control machine controls the opening and closing of all the control valves, all the proportioning pumps and all the feeding pumps.

Compared with the prior art, the beneficial effects of the utility model include: the microchannel reactor is used as a reaction site, so that continuous production is realized, the production efficiency is greatly improved, and because of the microchannel reaction, the magnitude of each reaction is small, and the safety is high; the liquid phase raw materials are fully mixed in the microchannel reactor, the reaction is rapid and full, and the generation of side reactants is greatly reduced; each set of raw material supply assembly is provided with at least two metering tanks, a continuous feeding system for alternately metering and discharging is formed under the help of each control valve, and the control machine adjusts the raw material supply quantity at the upstream of the microchannel reactor in real time by combining the real-time monitoring feedback of a finished product sensor at the downstream of the microchannel reactor on the finished product, so that the reaction accuracy is ensured, and the production automation is realized.

Drawings

FIG. 1 is a schematic view of a liquid phase reaction apparatus according to the present invention;

FIG. 2 is a schematic diagram of the microchannel reactor of the present invention;

FIG. 3 is a schematic structural diagram of an embodiment of a microchannel reactor cutoff of the present invention;

FIG. 4 is a cross-sectional view A-A of FIG. 3;

FIG. 5 is a schematic structural diagram of a second embodiment of the microchannel reactor cutoff of the present invention;

FIG. 6 is a cross-sectional view B-B of FIG. 5;

FIG. 7 is a schematic diagram of a third embodiment of a microchannel reactor cutoff of the present invention;

FIG. 8 is a cross-sectional view C-C of FIG. 7;

fig. 9 is a schematic view of another state of fig. 7.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

As shown in fig. 1, the present invention provides a liquid phase reaction apparatus comprising: a feedstock supply assembly 100, a microchannel reactor 200, and a monitoring system 300.

The raw material supply assembly 100 comprises at least two sets, each set of raw material supply assembly 100 comprises a raw material tank 110, a dosing pump 120, a metering tank 130 and a feeding pump 140 which are sequentially connected through pipelines, wherein at least two metering tanks 130 are connected between the dosing pump 120 and the feeding pump 140 in parallel, and a feeding hole and a discharging hole of each metering tank 130 are respectively provided with a control valve 150.

Microchannel reactor 200 connects feed pump 140 and product tank 400.

The monitoring system 300 comprises a controller 310 and a product sensor 320 arranged at the downstream of the microchannel reactor 200, wherein the product sensor 320 is in signal connection with the controller 310, and the controller 310 controls the opening and closing of all the control valves 150, all the proportioning pumps 120 and all the feeding pumps 140.

The synthesis of sodium dimethyldithiocarbamate will be described below as an example. The production of sodium dimethyldithiocarbamate is carried out by putting three liquid phase raw materials of liquid alkali, dimethylamine and carbon disulfide into reactor, agitating and mixing for certain time.

The reaction place of the existing production process is a reaction kettle, the production process is in an interval operation mode, and the unorganized discharge cannot be avoided when the dimethylamine and carbon disulfide are fed into a volatile raw material metering tank and when the reaction kettle is loaded and unloaded. In addition, when raw materials are fed, a metering tank is used for metering feeding, and because the metering mode is visual metering, a large metering error is caused, so that the quality of a finished product is influenced, and even a refining and purifying process is required, so that the increase of waste water discharge is inevitable. In addition, in order to improve the production capacity, domestic production enterprises use over 2000L of high-pressure kettles for production, but dimethylamine and carbon disulfide raw materials are low-boiling-point, volatile, flammable and explosive chemicals, so that great potential safety hazards exist, and once a safety accident occurs, a great deal of raw material storage in a production workshop brings severe examination to safe production. In addition, the kettle type operation is adopted, a large number of operators are needed, and the labor cost is high.

When the liquid phase reaction device is used, each set of raw material supply assembly 100 is used for one reaction raw material, the raw material is respectively conveyed into the metering tank 130 from the raw material tank 110 through the proportioning pump 120, the metering tank 130 and the feeding pump 140 for metering, then the raw material is conveyed into the microchannel reactor 200 for fully mixing reaction, finally, a finished product is conveyed out, no matter the raw material or the finished product, the whole process is in a sealed environment, no dischargeable leakage point exists, and the unorganized discharge is greatly reduced. As the above pumps, a JYS series pump such as JYSZZ-100/4.0, JYSZZ-58/7.2, JYSZZ-110/9, etc. can be used. The metering tank may employ a Mettler weighing module, such as MT1041-20 KG.

In the process of metering the liquid-phase raw material, at least two metering tanks 130, such as double metering tanks, are arranged in parallel, so that the raw material can be metered precisely and finely, and meanwhile, the raw material can be metered and discharged alternately with the help of each control valve 150, so that continuous production without stopping the machine can be realized. Each control valve may be a pneumatic ball valve. And, the real-time monitoring feedback of the finished product sensor at the downstream of the microchannel reactor 200 is combined, and the controller adjusts the raw material supply amount at the upstream of the microchannel reactor 200 in real time, so that the reaction accuracy is ensured, and the production automation is realized. The finished product sensor can be a gas chromatograph or a liquid chromatograph, etc., and the proportioning precision of the reaction raw materials is deduced by detecting the residual quantity of a certain raw material in the finished product, and particularly, a 7890A type gas chromatograph of Agilent can be selected to measure the content of dimethylamine in the raw materials. For example, when a single material is measured with deviation, the controller automatically adjusts the proportioning pump to ensure that the deviation value is not more than 100 g (the precision cannot be realized in the existing interval type industrial production), when the deviation value is more than 100 g or other controllers cannot correct, the controller can automatically stop and alarm, the system can recover after manually searching and analyzing reasons and eliminating faults, and the product quality and raw materials are ensured not to be wasted. The liquid phase reaction device is adopted to synthesize the product once without refining treatment, thereby reducing the process links and greatly reducing the production cost.

As the reaction site of the liquid phase reaction device is the microchannel reactor 200, the total amount of process materials in the reactor is usually not more than 5kg, the total amount of materials in the raw material supply assembly 100 is usually not more than 80kg, the drift diameter of the reactor can be 20nm, the pressure bearing is more than 20MPa, and the safety production is greatly guaranteed. In addition, the monitoring system 300 and the raw material storage tank are subjected to linkage control, and then dimethylamine and a carbon disulfide concentration monitoring device are further matched, so that leakage of a system is detected, the system can be closed at the first time after the online detection concentration of the monitoring system 300 exceeds the standard, and once the accident linkage cut-off is carried out, the accident prevention is guaranteed; the automatic deviation rectifying adjustment is automatically controlled by the control machine, so that the misoperation factor of people is avoided.

The liquid phase reaction device realizes automatic control, only two inspection personnel are needed in each shift during production, no process operation is needed, and the cost of labor wages is greatly reduced. If the complex networking technology is further improved, the real-time production information of the liquid phase reaction device is uploaded to the cloud, and the fact that an administrator checks and controls the liquid phase reaction device through the portable handheld terminal can be achieved.

In order to optimize the structure of the microchannel reactor 200, the following specific schemes are proposed: the microchannel reactor 200 comprises a housing having a raw material inlet and a finished product outlet, and microchannels disposed in the housing and connecting the raw material inlet and the finished product outlet, wherein the number of the raw material inlet is adapted to the number of the raw material supply assembly 100. So that various liquid phase raw materials can smoothly enter the microchannel reactor 200 for reaction.

As shown in FIG. 2, as a specific embodiment, the microchannel comprises a series of heart-shaped structural units 221 connected end to end in series, a flow baffle 222 is arranged in each heart-shaped structural unit, and a plurality of through holes 223 are arranged on the flow baffle 222. The direction of the arrow in the figure is the flowing direction of the liquid phase raw material, and it can be seen that after the liquid phase raw material is pumped into the microchannel reactor and mixed in the microchannel, the heart-shaped structural unit 221 of the microchannel disturbs the mixed liquid material to stimulate the mutual mixing of the liquid materials, and the flow baffle 222 changes the flowing direction of the mixed liquid material to fully disturb the liquid material. The baffle plate 222 may be in an arc shape corresponding to the heart-shaped structural unit 221, so as to fully utilize the internal space of the heart-shaped structural unit 221 and plan a disturbance flow channel. The through holes 223 distributed on the flow baffle 222 increase the passage blocked by the flow baffle 222 for the mixed liquid, and the liquid passing through the passage forms lateral impact on the liquid bypassing the flow baffle 222, so that the disturbance of the liquid is further improved, and the mixing sufficiency is further improved. Further optimizing the material mixing scheme, the following scheme is proposed: the through holes are arranged along the direction of rays radiated to the periphery by taking the inlet of the heart-shaped structure unit as a starting point. Such an arrangement can reduce the loss of kinetic energy when the liquid material passes through the through holes 223, ensure that sufficient impact force is formed on the liquid material bypassing the baffle plate 222, and the through holes 223 can make the turbulent flow uniform in a radial arrangement manner.

Considering that many chemical reactions have certain requirements on the mixing sequence, the following scheme is proposed: the microchannel reactor 200 further includes a material guiding pipe 240 connecting the raw material inlet 230 and the microchannel, and a plurality of flow dividers 250 disposed in the material guiding pipe 240, wherein the flow dividers 250 divide the material guiding pipe 240 into a plurality of flow channels corresponding to the raw material inlet 230 in number, and the flow dividers 250 can slide along the axial direction of the material guiding pipe 240, as shown in fig. 2 to 9. The control of the feeding sequence during the mixing of the liquid-phase raw materials is realized by sliding the flow isolating plate 250 to change the length of the flow isolating plate in the guide pipe 240, thereby changing the time when the adjacent liquid materials separated by the flow isolating plate meet. Or taking the synthesis of sodium dimethyldithiocarbamate as an example, the raw materials include three kinds of liquid alkali, dimethylamine and carbon disulfide, 3 raw material inlets 230 are correspondingly provided (230 a, 230b and 230c respectively), and the following three specific examples are provided for the flow partitioner 250.

Example 1: as shown in fig. 3 and 4, both side edges of the flow partitioner 250 are slidably connected to the inner wall of the material guide tube 240, respectively. Specifically, the inner wall of the material guiding tube 240 may be provided with a guide rail 260 along the axial direction thereof, and the two flow partition plates 250 (250a, 250b) divide the material guiding tube 240 into 3 flow channels (240a, 240b, 240c) for corresponding to the three liquid-phase raw materials of the liquid caustic soda, the dimethylamine and the carbon disulfide. At this time, by adjusting the lengths of the

flow dividing plates

250a and 250b, the liquid in one

side flow channel

240a or 240b is purposefully contacted with the liquid in the middle flow channel 240b, and then mixed with the liquid in the other

side flow channel

240b or 240a, so as to achieve the process goal of feeding the liquids in the designated sequence.

Example 2: as shown in fig. 5 and 6, one side of each of the flow partitioners 250 is slidably connected to each other, and the other side is slidably connected to the inner wall of the guide tube 240. One side of one of the flow partitionings 250 is provided with a guide rail, and the corresponding side of any other flow partitionings 250 is slidably connected with the guide rail. The difference from embodiment 1 is that any two of the three flow channels separated by the flow partition plate 250 in this embodiment are adjacent, that is, in the case that there are three kinds of liquid materials, the two liquid materials adjacent to the flow partition plate 250 can be preferentially mixed by adjusting any one flow partition plate 250, that is, any two liquid materials can be mixed first and then mixed with the third liquid material.

Example 3: as shown in fig. 7 to 9, the flow partitioners 250 are cylindrical plates sleeved with each other, the outer wall of each flow partitioner 250 is slidably connected to the inner wall of the flow partitioner 250 sleeved outside the flow partitioner 250, and the outer wall of the flow partitioner 250 at the outermost layer is slidably connected to the inner wall of the material guiding pipe 240; the flow passage is formed by a gap between each flow partitioner 250 and its adjacent flow partitioner 250, a gap between the outermost flow partitioner 250 and the guide tube 240, and an inner cavity of the innermost flow partitioner 250. The difference with embodiment 2 lies in, not only can realize the liquid material and mix earlier of arbitrary two kinds of liquid materials under three circumstances, and this embodiment can realize the arbitrary order of arbitrary liquid material number of types and mix, and application scope is wider. In the state of fig. 7, the liquid in the flow channel 240a is mixed with the liquid in the flow channel 240b first, and then mixed with the liquid in the flow channel 240 c; in the state of fig. 9, the liquid in the flow channel 240b is mixed with the liquid in the flow channel 240c first, and then mixed with the liquid in the flow channel 240 a.

In order to ensure the sufficiency of the reaction, the following schemes are further proposed on the basis of all the schemes: referring again to fig. 1, the microchannel reactor 200 further includes a circulation pump 210 connected to the product outlet and the raw material inlet 230, and the circulation pump 210 is also controlled by the controller 310 to open and close. Some of the reactions that do not require longer reaction paths are returned to the microchannel reactor 200 to undergo mixing again, lengthening the reaction tube side.

The above description of the present invention does not limit the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the scope of the claims of the present invention.

Claims

1. A liquid phase reaction apparatus characterized by comprising:

2. The liquid-phase reaction apparatus according to claim 1, characterized in that: the microchannel reactor comprises a shell provided with a raw material inlet and a finished product outlet, and microchannels arranged in the shell and connected with the raw material inlet and the finished product outlet, wherein the number of the raw material inlets is adapted to the number of the raw material supply assemblies.

3. The liquid-phase reaction apparatus according to claim 2, characterized in that: the microchannel comprises a series of heart-shaped structural units which are connected in series end to end, wherein a flow baffle is arranged in each heart-shaped structural unit, and a plurality of through holes are arranged on the flow baffle.

4. A liquid phase reaction apparatus as claimed in claim 3, wherein: the through holes are arranged along the direction of rays radiated to the periphery by taking the inlet of the heart-shaped structure unit as a starting point.

5. The liquid-phase reaction apparatus according to claim 2, characterized in that: the microchannel reactor also comprises a material guide pipe connected with the raw material inlet and the microchannel, and a plurality of flow isolating plates arranged in the material guide pipe, wherein the flow isolating plates divide the material guide pipe into a plurality of flow channels corresponding to the raw material inlet in number, and the flow isolating plates can slide along the axial direction of the material guide pipe.

6. The liquid-phase reaction apparatus according to claim 5, characterized in that: two side edges of the flow partition plate are respectively connected with the inner wall of the material guide pipe in a sliding manner.

7. The liquid-phase reaction apparatus according to claim 5, characterized in that: one side edges of all the flow separation plates are mutually connected in a sliding manner, and the other side edge is connected with the inner wall of the material guide pipe in a sliding manner.

8. The liquid-phase reaction apparatus according to claim 7, characterized in that: one side of one of the flow separation plates is provided with a guide rail, and the corresponding side of any other flow separation plate is connected with the guide rail in a sliding manner.

9. The liquid-phase reaction apparatus according to claim 5, characterized in that: the flow partition plates are cylindrical plates which are sleeved with each other, the outer wall of each flow partition plate is connected with the inner wall of the flow partition plate sleeved outside the flow partition plate in a sliding mode, and the outer wall of the flow partition plate on the outermost layer is connected with the inner wall of the material guide pipe in a sliding mode; the flow channel is formed by a gap between each flow partition plate and the adjacent flow partition plate, a gap between the outermost flow partition plate and the material guide pipe and an inner cavity of the innermost flow partition plate.

10. The liquid-phase reaction apparatus according to any one of claims 2 to 9, characterized in that: the microchannel reactor also comprises a circulating pump connected with a finished product outlet and a raw material inlet of the microchannel reactor, and the opening and closing of the circulating pump are controlled by the control machine.