CN214937128U - Liquid-liquid heterogeneous continuous reaction system - Google Patents
Liquid-liquid heterogeneous continuous reaction system Download PDFInfo
- Publication number
- CN214937128U CN214937128U CN202122495282.5U CN202122495282U CN214937128U CN 214937128 U CN214937128 U CN 214937128U CN 202122495282 U CN202122495282 U CN 202122495282U CN 214937128 U CN214937128 U CN 214937128U
- Authority
- CN
- China
- Prior art keywords
- liquid
- unit
- continuous
- continuous reaction
- inlet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a heterogeneous continuous reaction system of liquid. The liquid-liquid heterogeneous continuous reaction system comprises a continuous feeding unit, a pipeline type mixing unit, a plug flow continuous reaction unit and a continuous post-treatment unit. The pipeline type mixing unit is provided with a reaction raw material inlet and a mixed material outlet, and the reaction raw material inlet is connected with the continuous feeding unit; the plug flow continuous reaction unit is provided with a mixed material inlet and a product system outlet, and the mixed material inlet is connected with the mixed material outlet; the continuous post-treatment unit is connected with a product system outlet of the plug flow continuous reaction unit. The above-mentioned heterogeneous continuous reaction system of whole liquid-liquid of this application collects continuous feeding unit, pipeline formula mixing unit, plug flow continuous reaction unit, continuous aftertreatment unit in an organic whole, greatly increased the security in the device uses, show the security that promotes the reaction and the stability of product quality, easily realize serialization large-scale production to improve the synthetic efficiency of methylsulfonyl azide.
Description
Technical Field
The utility model relates to a preparation technical field of methyl sulfonyl azide particularly, relates to a heterogeneous continuous reaction system of liquid-liquid.
Background
The methylsulfonyl azide is mainly used as a basic raw material for synthesizing penem drug intermediates, the social demand is large, and the product price is always high. The research on the synthesis process of the product reduces the product cost and has obvious economic and social benefits. For a long time, because the toluene sulfonyl azide is used as the starting material in China, the cost is high, the amount of the synthesized material is large by adopting the traditional batch reaction kettle method, and the sulfonyl azide is easy to decompose and the industrial production safety accidents of explosion are easy to occur during production. Therefore, how to realize safe and efficient continuous production in the process of preparing the methylsulfonyl azide is an important research direction of technicians.
The most critical reaction equipment has the phenomenon of unreasonable structural style or unit combination, so that the reaction efficiency is low, the comprehensive utilization of energy is unreasonable, the number of byproducts is large, the yield is low, and the normal operation of the reaction is possibly influenced by the generation and accumulation of the byproducts. Generally, the synthesis of methylsulfonyl azide uses a solution of methylsulfonyl chlorotoluene and an aqueous solution of sodium azide for the reaction. The reaction mainly occurs at a two-phase interface, and the effect of mixing the two phases has direct influence on the reaction conversion rate and the reaction rate, so that the problem of mixing raw materials related to a liquid-liquid two-phase immiscible system is the most critical technical difficulty, and the large enough contact area between the two phases must be fully considered in the development of the reactor of the reaction. Chinese patent application with patent application publication No. CN 109824556A discloses a microchannel synthesis method of aryl sulfonyl azide, wherein two raw materials are rapidly input into a microchannel reactor in a continuous feeding mode to prepare the aryl sulfonyl azide. The microreactors can be in parallel number but have weak processing capacity. The method can be used for production in the field with relatively small treatment capacity, the application needing mass production is less, the processing cost of some micro chemical equipment is high, and the economic applicability is weak. Therefore, the prior art for industrially preparing the methylsulfonyl azide still has many potential safety hazards, high preparation cost, incapability of continuous production and the like, and cannot meet the requirement of industrial production for preparing high-purity products at low cost and high safety.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a main aim at provides a heterogeneous continuous reaction system of liquid to adopt traditional intermittent type formula reation kettle method synthetic methyl sulfonyl azide to have the problem that the synthesis efficiency is low and product quality is unstable among the solution prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a liquid-liquid heterogeneous continuous reaction system including a continuous feeding unit, a pipe-type mixing unit, a plug-flow continuous reaction unit, and a continuous post-treatment unit. The pipeline type mixing unit is provided with a reaction raw material inlet and a mixed material outlet, and the reaction raw material inlet is connected with the continuous feeding unit; the plug flow continuous reaction unit is provided with a mixed material inlet and a product system outlet, and the mixed material inlet is connected with the mixed material outlet; the continuous post-treatment unit is connected with a product system outlet of the plug flow continuous reaction unit.
Further, the plug flow continuous reaction unit comprises any one of a horizontal tubular reactor, a vertical tubular reactor, a coil tubular reactor and a U-shaped tubular reactor.
Further, the aspect ratio of the plug flow continuous reaction unit is 0.5X 103~1×103:1。
Furthermore, a back pressure valve is arranged at the outlet of the plug flow continuous reaction unit.
Further, the above-mentioned pipeline type mixing unit adopts any one or more of an SV mixer, an SK mixer, an SX mixer, an SH mixer and an SL mixer.
Further, the above continuous feeding unit comprises: the device comprises a first raw material solution storage tank and a second raw material solution storage tank, wherein the first raw material solution storage tank is connected with a pipeline type mixing unit through a first pipeline, and a first feeding pump and a first flowmeter are arranged on the first pipeline; the second raw material solution storage tank is connected with the pipeline type mixing unit through a second pipeline, and a second feeding pump and a second flowmeter are arranged on the second pipeline.
Further, the first raw material solution storage tank is a sodium azide aqueous solution storage tank, and the second raw material solution storage tank is a methanesulfonyl chloride toluene solution storage tank.
Further, the continuous post-treatment unit comprises an alkali washing device, a first liquid dividing device, a salt washing device, a second liquid dividing device and a product storage tank, wherein the alkali washing device is provided with an alkali liquor inlet, a product system inlet and an alkali washed system outlet, and the product system inlet is connected with the product system outlet of the plug flow continuous reaction unit; the first liquid dividing device is provided with an alkali washing system inlet, a first water phase outlet and a first organic phase outlet, the alkali washing system inlet is connected with the alkali washing system outlet, the salt washing device is provided with a salt liquid inlet, a first organic phase inlet and a salt washing system outlet, and the first organic phase inlet is connected with the first organic phase outlet; the second liquid separation device is provided with a system inlet after salt washing, a second water phase outlet and a second organic phase outlet, the system inlet after salt washing is connected with the system outlet after salt washing, and the product storage tank is connected with the second organic phase outlet of the second liquid separation device.
Further, the alkali cleaning device has a pH detector.
Furthermore, the continuous post-treatment unit also comprises an alkali liquor storage tank and a salt liquor storage tank, wherein the alkali liquor storage tank is connected with the alkali liquor inlet through a third pipeline, and a third feeding pump is arranged on the third pipeline; the salt solution storage tank is connected with the salt solution inlet through a fourth pipeline, a fourth feeding pump is arranged on the fourth pipeline, the liquid-liquid heterogeneous continuous reaction system further comprises a PLC control unit, the PLC control unit is electrically connected with the first feeding pump, the first flowmeter, the second feeding pump, the second flowmeter, the third feeding pump, the fourth feeding pump and the pH value detector, and the PLC control unit receives the detection result of the pH value detector and adjusts the pump speed of the third feeding pump according to the detection result.
Use the technical scheme of the utility model, whole heterogeneous continuous reaction system of liquid collects continuous feed unit, pipeline formula mixing unit, plug flow continuous reaction unit, continuous aftertreatment unit in an organic whole, is a high-efficient, low serialization reaction unit who drops into. Particularly, through the combination of the pipeline type mixing unit and the plug flow continuous reaction unit, the flowing mixing direction of the liquid-liquid heterogeneous materials is continuously changed after the liquid-liquid heterogeneous materials pass through the internal components of the pipeline type mixing unit, so that not only is the central fluid pushed to the periphery, but also the peripheral fluid is pushed to the center, and the good radial mixing effect of the liquid-liquid two-phase heterogeneous raw materials is caused. The material enters the plug flow reactor to continuously flow forcibly under the rotation action of the pipeline type mixing unit, so that a large enough contact area and a sufficient reaction retention time are ensured between the two phases, the reaction system is uniformly heated because the material stably flows in the tubular reactor with higher heat exchange efficiency for heat exchange, the thermal efficiency of the unit is high, unstable reaction conditions and influence on the reaction process caused by the generation of by-products of methanesulfonic acid or hydrazoic acid due to the accumulation of the material in the reaction process in the traditional kettle type reaction process can be avoided, the safety of the device in use is greatly improved, the safety of the reaction and the stability of the product quality are obviously improved, the continuous large-scale production is easily realized, and the synthesis efficiency of the methylsulfonyl azide is improved.
Drawings
The accompanying drawings, which form a part of the present application, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic diagram of a liquid-liquid heterogeneous continuous reaction system provided according to embodiment 1 of the present invention.
Wherein the figures include the following reference numerals:
1. a continuous feed unit; 2. a pipe-type mixing unit; 3. a plug flow continuous reaction unit; 4. a continuous post-processing unit; 5. a PLC control unit; 101. a first raw material solution storage tank; 102. a first feed pump; 103. a first flow meter; 104. a second raw material solution storage tank; 105. a second feed pump; 106. a second flow meter; 401. an alkaline washing device; 402. a first liquid separation device; 403. a salt washing device; 404. a second liquid separation device; 405. a product storage tank; 406. an alkali liquor storage tank; 407. a salt solution storage tank; 408. a third feed pump; 409. a fourth feed pump.
Detailed Description
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
If the utility model discloses the background art is analyzed, adopt the synthetic methyl sulfonyl azide of traditional batch type reation kettle method to have the problem that the synthesis efficiency is low and product quality is unstable among the prior art, in order to solve this problem, the utility model provides a heterogeneous continuous reaction system of liquid.
In an exemplary embodiment of the present application, a liquid-liquid heterogeneous continuous reaction system is provided, as shown in fig. 1, which includes a continuous feeding unit 1, a pipe-type mixing unit 2, a plug-flow continuous reaction unit, and a continuous post-treatment unit 4. The pipeline type mixing unit 2 is provided with a reaction raw material inlet and a mixed material outlet, and the reaction raw material inlet is connected with the continuous feeding unit 1; the plug flow continuous reaction unit 3 is provided with a mixed material inlet and a product system outlet, and the mixed material inlet is connected with the mixed material outlet; the continuous post-treatment unit 4 is connected with the product system outlet of the plug flow continuous reaction unit 3.
The whole liquid-liquid heterogeneous continuous reaction system integrates a continuous feeding unit 1, a pipeline type mixing unit 2, a plug flow continuous reaction unit 3 and a continuous post-treatment unit 4, and is a high-efficiency and low-investment continuous reaction unit. Particularly, through the combination of the pipeline type mixing unit 2 and the plug flow continuous reaction unit 3, the flowing mixing direction of the liquid-liquid heterogeneous materials is continuously changed after the liquid-liquid heterogeneous materials pass through the internal components of the pipeline type mixing unit, so that not only is the central fluid pushed to the periphery, but also the peripheral fluid is pushed to the center, and the good radial mixing effect of the liquid-liquid two-phase heterogeneous raw materials is caused. The material enters the plug flow reactor to continuously flow forcibly under the rotation action of the pipeline type mixing unit, so that a large enough contact area and a sufficient reaction retention time are ensured between the two phases, the reaction system is uniformly heated because the material stably flows in the tubular reactor with higher heat exchange efficiency for heat exchange, the thermal efficiency of the unit is high, unstable reaction conditions and influence on the reaction process caused by the generation of by-products of methanesulfonic acid or hydrazoic acid due to the accumulation of the material in the reaction process in the traditional kettle type reaction process can be avoided, the safety of the device in use is greatly improved, the safety of the reaction and the stability of the product quality are obviously improved, the continuous large-scale production is easily realized, and the synthesis efficiency of the methylsulfonyl azide is improved.
Preferably, the plug flow continuous reaction unit 3 comprises any one of a horizontal tubular reactor, a vertical tubular reactor, a coil tubular reactor and a U-shaped tubular reactor, so that the reaction system can better meet the plug flow conditions when flowing in the reactor. Namely, the reaction system continuously enters from one end of the reactor at a more stable flow rate, reacts while flowing, and discharges from the other end of the tube to reach a predetermined conversion rate. In addition, the coil tube type reactor uses the advantage that the static mixer improves the fluid turbulence for reference, utilizes self structural advantage to produce the secondary vortex, and the existence of this kind of secondary flow has improved the radial mixture of reactant to it is favorable to improving the secondary flow effect to have increased the reynolds number, has avoided the drawback that the interpolation part is not convenient for to clear up and maintain simultaneously.
It is preferable that the inner wall material constituting the plug flow continuous reaction unit 3 is selected from any one or more of 316L stainless steel, glass, polytetrafluoroethylene, thereby contributing to the improvement of the corrosion resistance of the plug flow continuous reaction unit 3 to the mixed system.
Long diameter comparisonThe large tubular reactor is a typical representative of the plug flow reactor, and its structure is very simple, and it is preferable that the above-mentioned straight tubular reactor has a length-to-diameter ratio of 0.5X 103~1×1031, the residence time of the reaction raw materials in the plug flow continuous reaction unit 3 can be better controlled, thereby controlling the conversion rate and the efficiency of the reaction.
In one embodiment of the present application, a back pressure valve is provided at the outlet of the plug flow continuous reaction unit 3.
The back pressure valve can control the pressure in the plug flow continuous reaction unit 3, so that the liquid-liquid heterogeneous continuous reaction system can meet the high-pressure reaction.
In an embodiment of the present application, the above pipeline mixing unit 2 employs any one or more of an SV mixer, an SK mixer, an SX mixer, an SH mixer, and an SL mixer.
The ducted mixing unit 2 is made up of a series of mixing units of different specifications mounted in hollow ducts. The fluid flows in the pipeline and impacts various plate elements, the fluid rotates leftwards and rightwards due to the action of the mixing unit, the flowing mixing direction is changed continuously, the central fluid is pushed to the periphery, the peripheral fluid is pushed to the center, and therefore good radial mixing effect of heterogeneous raw materials is achieved. The static mixer is a high-efficiency mixing device without movement, and two or more strands of fluids are cut, sheared, rotated and re-mixed through the mixing unit internals fixed in the pipe, so that the purposes of good dispersion and full mixing among the fluids are achieved, the residence time of reaction raw materials is shortened, the relatively stable reaction can be effectively promoted, and the reaction efficiency is further improved.
Compared with traditional mixing equipment such as a stirrer, a colloid mill, a homogenizer, a venturi tube and the like, the SV mixer, the SK mixer, the SX mixer, the SH mixer and the SL mixer which are optimized in the application have the advantages of compact structure, low energy consumption, low investment, high operation flexibility, no need of maintenance, good mixing performance and the like, and are particularly suitable for the processes of mixing, emulsifying, neutralizing, absorbing, extracting, reacting, strengthening heat transfer and the like of a liquid-liquid system. The SV mixer, the SK mixer, the SX mixer, the SH mixer and the SL mixer are mainly characterized in that the mixing units with different specifications which are arranged in the hollow pipeline have different structures, for example, the SV type unit is a cylinder which is assembled by corrugated plates with certain specifications; the SK type static mixer is also called single-spiral static mixer, its unit is a spiral plate twisted by 180 deg. or 270 deg., when it is installed in the pipe shell, the adjacent spiral plates are respectively left-handed and right-handed. The SH units are composed of double channels, spiral sheets are arranged in the channels, the positions of the double channels of the adjacent units are staggered by 90 degrees, and fluid redistribution chambers are arranged between the units. The system is mixed more uniformly.
The inner wall material of the pipeline type mixing unit 2 is preferably selected from one or more of glass, titanium steel and Hastelloy steel, so that the corrosion resistance of the pipeline type mixing unit 2 to a mixing system is improved.
In one embodiment of the present application, as shown in fig. 1, the continuous feed unit 1 includes a first raw material solution tank 101 and a second raw material solution tank 104, the first raw material solution tank 101 is connected to the pipeline mixing unit 2 through a first pipeline, and a first feed pump 102 and a first flow meter 103 are disposed on the first pipeline; the second raw material solution tank 104 is connected to the inline mixing unit 2 through a second line on which a second feed pump 105 and a second flow meter 106 are provided.
The flow of the two reaction raw material fluids can be controlled by the continuous feeding unit 1 with the above structure, thereby controlling the mixing effect of the reaction system and the final efficiency of the reaction.
In an embodiment of the present application, the first raw material solution storage tank 101 is a sodium azide aqueous solution storage tank, and the second raw material solution storage tank 104 is a methanesulfonyl chloride toluene solution storage tank.
The liquid-liquid heterogeneous continuous reaction system is suitable for liquid-liquid heterogeneous mixed reaction and post-treatment reaction, and is particularly suitable for the preparation reaction of methylsulfonyl azide solution.
In one embodiment of the present application, as shown in fig. 1, the continuous post-treatment unit 4 includes an alkaline washing device 401, a first liquid dividing device 402, a salt washing device 403, a second liquid dividing device 404, and a product storage tank 405. The alkali washing device 401 is provided with an alkali liquor inlet, a product system inlet and an alkali washed system outlet, wherein the product system inlet is connected with the product system outlet of the plug flow continuous reaction unit 3; the first liquid dividing device 402 is provided with an alkali washing system inlet, a first water phase outlet and a first organic phase outlet, the alkali washing system inlet is connected with the alkali washing system outlet, the salt washing device 403 is provided with a salt liquid inlet, a first organic phase inlet and a salt washing system outlet, and the first organic phase inlet is connected with the first organic phase outlet; the second liquid separation device 404 is provided with a system inlet after salt washing, a second water phase outlet and a second organic phase outlet, the system inlet after salt washing is connected with the system outlet after salt washing, and the product storage tank 405 is connected with the second organic phase outlet of the second liquid separation device 404.
But through above-mentioned continuous aftertreatment unit 4 accurate control accessory substance hydrazoic acid or methanesulfonic acid remain, and carry out the serialization of impurity to the product system and get rid of, the continuous product that obtains, and choose for use the combination of pipeline formula mixing unit 2 and plug flow continuous reaction unit 3 to carry out the heterogeneous type of liquid-liquid reaction module and including alkaline cleaning device 401, first liquid separation device 402, salt washing device 403, second liquid separation device 404 and the aftertreatment module of product storage tank 405 combine together, can effectively save equipment area and equipment cost, guarantee equipment availability factor and equipment security and operational safety simultaneously.
The change of the pH value of the system can be detected on line through a pH value detector, as shown in figure 1, the alkaline cleaning device 401 is preferably provided with the pH value detector, the residue of the by-product, namely the azido acid or the methanesulfonic acid can be accurately controlled, the safety is good compared with the safety of accumulation of the azido acid in a kettle caused by centralized feeding of raw materials in the batch preparation process, the control precision is high, and the quality of the final product is stable.
In an embodiment of the present application, as shown in fig. 1, the continuous post-treatment unit 4 further comprises a lye storage tank 406 and a salt solution storage tank 407, wherein the lye storage tank 406 is connected to the lye inlet via a third pipeline, and a third feed pump 408 is disposed on the third pipeline; the salt solution storage tank 407 is connected with a salt solution inlet through a fourth pipeline, a fourth feeding pump 409 is arranged on the fourth pipeline, the liquid-liquid heterogeneous continuous reaction system further comprises a PLC control unit 5, the PLC control unit 5 is electrically connected with the first feeding pump 102, the first flowmeter 103, the second feeding pump 105, the second flowmeter 106, the third feeding pump 408, the fourth feeding pump 409 and the pH value detector, and the PLC control unit 5 receives a detection result of the pH value detector and adjusts the pump speed of the third feeding pump 408 according to the detection result.
The system enters the post-treatment module after the reaction to carry out continuous alkali washing, liquid separation, salt washing and other operations, wherein the alkali washing module can monitor the change of the pH value of the system on line, and compared with the traditional kettle type reactor, the automatic control of the liquid-liquid heterogeneous continuous reaction system can be realized by adopting the PLC control unit 5, if the automatic control of the alkali liquor feeding amount can ensure that no dangerous byproducts such as methanesulfonic acid, hydrazoic acid and the like are accumulated, and the system has the advantages of high control precision, short operation time, stable product quality and good safety.
The feeding amount of the salt solution can be calculated in advance according to the volume of the salt washing device 403 and the retention time of the first organic phase in the salt washing device 403 (generally, the retention time of the first organic phase in the salt washing device 403 is controlled to be 20-30 min), so that the feeding speed of the salt solution is preset, the feeding speed of the fourth feeding pump 409 is monitored in real time through the PLC control unit 5, the feeding amount of the salt solution is adjusted in real time, it is ensured that the water contained in the first organic phase ester layer can be removed in the salt washing process, and meanwhile, the solubility of the product in the water is reduced.
According to the target product amount and the target of the preset reaction time, the feeding amounts of the first raw material solution and the second raw material solution are calculated, so that the feeding speeds of the first raw material solution and the second raw material solution are preset, the feeding speeds of the first feeding pump 102 and the second feeding pump 105 are monitored in real time through the PLC control unit 5, the feeding amounts of the first raw material solution and the second raw material solution are adjusted in real time, and efficient and smooth reaction is ensured. Therefore, the PLC control unit 5 can be used for monitoring the continuous feeding unit 1, the pipeline type mixing unit 2, the plug flow continuous reaction unit 3 and the continuous post-treatment unit 4 on line in real time, so that the integral automatic control of the liquid-liquid heterogeneous continuous reaction system is realized.
The advantageous effects of the present application will be described below with reference to specific examples and comparative examples.
Example 1
As shown in figure 1, the liquid-liquid heterogeneous continuous reaction system is adopted to prepare methylsulfonyl azide, a toluene solution of methylsulfonyl chloride and an aqueous solution of sodium azide are quantitatively pumped into a reaction device through a PLC (programmable logic controller) control pump, 6.48g/min of methylsulfonyl chloride/toluene solution and 1.74g/min of aqueous solution of sodium azide are set, the mixture is mixed in the reaction system through a pipeline mixer and then enters a coil-type reactor to carry out continuous reaction step by step, the system retention time in the reactor is controlled to be 25min, a crude product is obtained and enters a post-treatment alkaline washing device, the sodium bicarbonate solution and the sodium chloride solution are quantitatively pumped into the alkaline washing and salt washing device through the PLC control pump at a rate of 3.3g/min, a qualified final product is produced through a light phase outlet of a continuous liquid-liquid separation device after salt washing, the production preparation is completed, the concentration of the detected product is 10.4%, and the yield is 95%.
Example 2
Example 2 differs from example 1 in that the reaction volume and the volume of the coil reactor were enlarged to 50 times, wherein 16.16kg/h of methanesulfonyl chloride/toluene solution and 4.37kg/h of sodium azide aqueous solution were set, the reaction time was 30min, and the product concentration was 10.8% and the product yield was 98% by performing the post-treatment of alkali washing and salt washing.
Comparative example 1
13g of sodium azide is added into 41g of purified water, and sodium azide aqueous solution is obtained after stirring and dissolving for later use. To 180g of toluene was added 20g of methanesulfonyl chloride, and stirring was started to obtain a methanesulfonyl chloride toluene solution for use. Controlling the temperature to be 10-20 ℃, slowly dripping the toluene solution of the methylsulfonyl chloride into the sodium azide aqueous solution in the reaction kettle, and reacting for 2-3 hours under the condition of heat preservation. After the reaction is finished, controlling the temperature to be 10-20 ℃, slowly and dropwise adding 100g of 7% sodium bicarbonate solution into the reaction system for alkali washing, and separating liquid after stirring. Controlling the temperature to be 10-20 ℃, adding 100g of 20% sodium chloride solution into the organic phase after liquid separation, performing salt washing, and stirring and separating the liquid. The content of the organic phase detected is 10.1 percent, and the yield is 92 percent.
From the above description, it can be seen that the above-mentioned embodiments of the present invention achieve the following technical effects:
the whole liquid-liquid heterogeneous continuous reaction system integrates a continuous feeding unit, a pipeline type mixing unit, a plug flow continuous reaction unit and a continuous post-treatment unit, and is a high-efficiency and low-investment continuous reaction unit. Particularly, through the combination of the pipeline type mixing unit and the plug flow continuous reaction unit, the flowing mixing direction of the liquid-liquid heterogeneous materials is continuously changed after the liquid-liquid heterogeneous materials pass through the internal components of the pipeline type mixing unit, so that not only is the central fluid pushed to the periphery, but also the peripheral fluid is pushed to the center, and the good radial mixing effect of the liquid-liquid two-phase heterogeneous raw materials is caused. The material enters the plug flow reactor to continuously flow forcibly under the rotation action of the pipeline type mixing unit, so that a large enough contact area and a sufficient reaction retention time are ensured between the two phases, the reaction system is uniformly heated because the material stably flows in the tubular reactor with higher heat exchange efficiency for heat exchange, the thermal efficiency of the unit is high, unstable reaction conditions and influence on the reaction process caused by the generation of by-products of methanesulfonic acid or hydrazoic acid due to the accumulation of the material in the reaction process in the traditional kettle type reaction process can be avoided, the safety of the device in use is greatly improved, the safety of the reaction and the stability of the product quality are obviously improved, the continuous large-scale production is easily realized, and the synthesis efficiency of the methylsulfonyl azide is improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A liquid-liquid heterogeneous continuous reaction system, comprising:
a continuous feed unit (1);
the pipeline type mixing unit (2) is provided with a reaction raw material inlet and a mixed material outlet, and the reaction raw material inlet is connected with the continuous feeding unit (1);
the plug flow continuous reaction unit (3) is provided with a mixed material inlet and a product system outlet, and the mixed material inlet is connected with the mixed material outlet;
and the continuous post-treatment unit (4) is connected with the product system outlet of the plug flow continuous reaction unit (3).
2. The liquid-liquid heterogeneous continuous reaction system according to claim 1, wherein the plug flow continuous reaction unit (3) comprises any one of a horizontal tubular reactor, a vertical tubular reactor, a coil tubular reactor and a U-shaped tubular reactor.
3. The liquid-liquid heterogeneous continuous reaction system according to claim 2, wherein the length-to-diameter ratio of the plug flow continuous reaction unit (3) is 0.5 x 103~1×103:1。
4. The liquid-liquid heterogeneous continuous reaction system according to any one of claims 1 to 3, wherein a back pressure valve is provided at the outlet of the plug flow continuous reaction unit (3).
5. The liquid-liquid heterogeneous continuous reaction system according to any one of claims 1 to 3, wherein the tubular mixing unit (2) employs any one or more of SV mixer, SK mixer, SX mixer, SH mixer, SL mixer.
6. The liquid-liquid heterogeneous continuous reaction system according to any one of claims 1 to 3, wherein the continuous feeding unit (1) comprises:
a first raw material solution storage tank (101) connected with the pipeline type mixing unit (2) through a first pipeline, wherein a first feeding pump (102) and a first flow meter (103) are arranged on the first pipeline;
and the second raw material solution storage tank (104) is connected with the pipeline type mixing unit (2) through a second pipeline, and a second feeding pump (105) and a second flow meter (106) are arranged on the second pipeline.
7. The liquid-liquid heterogeneous continuous reaction system according to claim 6, wherein the first raw material solution storage tank (101) is a sodium azide aqueous solution storage tank, and the second raw material solution storage tank (104) is a methylsulfonyl chlorotoluene solution storage tank.
8. The liquid-liquid heterogeneous continuous reaction system according to claim 6, wherein the continuous post-treatment unit (4) comprises:
the alkali washing device (401) is provided with an alkali liquor inlet, a product system inlet and an alkali washed system outlet, and the product system inlet is connected with the product system outlet of the plug flow continuous reaction unit (3);
a first liquid diversion device (402) having a post-caustic wash system inlet, a first aqueous phase outlet, and a first organic phase outlet, the post-caustic wash system inlet being connected to the post-caustic wash system outlet,
a salt washing device (403) having a salt solution inlet, a first organic phase inlet and a system outlet after salt washing, the first organic phase inlet being connected to the first organic phase outlet;
a second liquid separation device (404) having a post-salt-wash system inlet, a second aqueous phase outlet, and a second organic phase outlet, the post-salt-wash system inlet being connected to the post-salt-wash system outlet,
and the product storage tank (405) is connected with the second organic phase outlet of the second liquid separation device (404).
9. The liquid-liquid heterogeneous continuous reaction system according to claim 8, wherein the alkaline washing device (401) is provided with a pH value detector.
10. The liquid-liquid heterogeneous continuous reaction system according to claim 9, wherein the continuous post-treatment unit (4) further comprises a lye storage tank (406) and a salt solution storage tank (407), the lye storage tank (406) is connected with the lye inlet through a third pipeline, and a third feed pump (408) is arranged on the third pipeline; the salt solution storage tank (407) is connected with the salt solution inlet through a fourth pipeline, a fourth feeding pump (409) is arranged on the fourth pipeline,
the liquid-liquid heterogeneous continuous reaction system further comprises a PLC control unit (5), the PLC control unit (5) is electrically connected with the first feeding pump (102), the first flow meter (103), the second feeding pump (105), the second flow meter (106), the third feeding pump (408), the fourth feeding pump (409) and the pH value detector, and the PLC control unit (5) receives a detection result of the pH value detector and adjusts the pump speed of the third feeding pump (408) according to the detection result.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122495282.5U CN214937128U (en) | 2021-10-18 | 2021-10-18 | Liquid-liquid heterogeneous continuous reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122495282.5U CN214937128U (en) | 2021-10-18 | 2021-10-18 | Liquid-liquid heterogeneous continuous reaction system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN214937128U true CN214937128U (en) | 2021-11-30 |
Family
ID=79069480
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202122495282.5U Active CN214937128U (en) | 2021-10-18 | 2021-10-18 | Liquid-liquid heterogeneous continuous reaction system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN214937128U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805162A (en) * | 2022-04-26 | 2022-07-29 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
| CN114805162B (en) * | 2022-04-26 | 2024-05-31 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
-
2021
- 2021-10-18 CN CN202122495282.5U patent/CN214937128U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805162A (en) * | 2022-04-26 | 2022-07-29 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
| CN114805162B (en) * | 2022-04-26 | 2024-05-31 | 湖北华洲药业有限公司 | Continuous production method and device for meropenem side chain key intermediate O powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103936559B (en) | The method of continuous prodution Resorcinol | |
| CN102241558B (en) | Reaction device and process for preparing cyclohexene by selectively hydrogenating benzene | |
| CN109134231A (en) | A kind of chloroacetic device and process of differential circulation continuous production | |
| CN108892600B (en) | Method for continuously preparing 1-bromobutane | |
| GB2593792A (en) | Built-in micro interfacial enhanced reaction system and process for PTA production with PX | |
| CN104744295A (en) | Method and device for preparing ethylphenylhydrazine hydrochloride by pipelines | |
| CN103708426B (en) | Anthraquinone oxydol production apparatus | |
| CN111569454A (en) | Built-in micro-interface oxidation system and method for preparing terephthalic acid from p-xylene | |
| CN214937128U (en) | Liquid-liquid heterogeneous continuous reaction system | |
| CN102372684A (en) | Method for preparing epoxy chloropropane by micro-channel reactor | |
| CN101735019B (en) | Process for producing resorcinol by continuously hydrolyzing m-phenylenediamine | |
| CN109364868A (en) | A kind of continous way chloro thing process units | |
| CN109806816A (en) | A kind of chlorination reaction device of continuous round-robin method production | |
| CN111569788B (en) | External micro-interface oxidation system and method for preparing terephthalic acid from p-xylene | |
| CN102502566A (en) | Technology for synthesizing lithium hexafluorophosphate | |
| CN115124539B (en) | Preparation method of 7-iodopyrrolo [2,1-F ] [1,2,4] triazine-4-amine | |
| CN202860529U (en) | Reaction device for producing cyclohexene by partial hydrogenation of benzene | |
| CN1321990C (en) | Apparatus and method for monotubular multi-spiral static mixed tube style chlorohydrination of propene for production of epoxypropane | |
| CN113845405B (en) | Method for continuously synthesizing diflufenican intermediate m-trifluoromethylphenol | |
| CN109876746A (en) | A kind of system and method for the micro- reaction synthetic rubber anti-scorching agent CTP of continuous flow | |
| CN110841585A (en) | Benzyl cyanide production device and use method thereof | |
| CN104387258B (en) | A kind of production of chloroacetic acid method and chlorination reactor | |
| CN106146441A (en) | A kind of preparation technology of furfural | |
| CN106146434A (en) | A kind of preparation technology of 5 hydroxymethyl furfural | |
| CN109081772B (en) | Process and device capable of effectively improving chlorination reaction production efficiency of 4-chloro-3, 5-dimethylphenol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230412 Address after: 133700 No. 99, Hongda Road, Dunhua Economic Development Zone, Yanbian Korean Autonomous Prefecture, Jilin Province Patentee after: Kailaiying Pharmaceutical Chemistry (Jilin) Technology Co.,Ltd. Address before: No.71, 7th Street, Binhai New Area Economic and Technological Development Zone, Tianjin 300457 Patentee before: ASYMCHEM LIFE SCIENCE (TIANJIN) Co.,Ltd. |
|
| TR01 | Transfer of patent right |