CN213286769U - Reaction device - Google Patents
Reaction device Download PDFInfo
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- CN213286769U CN213286769U CN202020845168.3U CN202020845168U CN213286769U CN 213286769 U CN213286769 U CN 213286769U CN 202020845168 U CN202020845168 U CN 202020845168U CN 213286769 U CN213286769 U CN 213286769U
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Abstract
The utility model provides a reaction device, include: the system comprises a raw material preparation kettle, a reaction kettle, a first heat exchange loop, a second heat exchange loop, a flow regulating valve, a flow limiting orifice plate and a distributor; a material outlet of the raw material preparation kettle is connected with a material inlet of the reaction kettle sequentially through the flow regulating valve and the flow limiting orifice plate; the tail end of a material inlet pipeline of the reaction kettle is provided with a distributor, the outer surface of the raw material preparation kettle is provided with a first jacket, and a first heat exchange loop is a loop formed by an outlet of the first jacket and inlets of a first heat exchanger, a first medium transfer pump and the first jacket; the outer surface of the reaction kettle is provided with a second jacket, and the second heat exchange loop is a loop formed by an outlet of the second jacket and inlets of the second heat exchanger, the second medium transfer pump and the second jacket. The utility model provides a reaction unit, simple structure is applicable to raw materials poor stability, the reaction exotherm is big, the low industrialization Suzuki coupling reaction production demand of catalyst load, overhauls and easy maintenance.
Description
Technical Field
The utility model relates to a chemical industry reaction equipment technical field, in particular to reaction unit.
Background
The Suzuki coupling reaction is also called Suzuki-Miyaura reaction (Suzuki-Miyaura reaction), and the reaction is a cross coupling reaction which takes palladium complex as a catalyst, inorganic/organic base as an additive and boric acid/boric acid ester and arene/olefin containing various leaving groups under the heating condition. Because aryl/alkenyl boric acid and boric acid ester can react with arene/olefin containing leaving groups such as chlorine, bromine, iodine, trifluoromethanesulfonyl, diazonium salt, iodonium salt, aryl sulfonium salt and the like in the Suzuki coupling reaction, and functional groups such as aldehyde, ketone, ester, ether, cyano, nitro, fluorine and the like are not influenced, the Suzuki-Miyaura coupling reaction has very good tolerance to various functional groups and very strong substrate universality, is commonly used for synthesizing derivatives of polyene, styrene and biphenyl, is applied to synthesis of various natural products and organic materials, and is widely applied to industrial production.
However, the Suzuki coupling reaction is usually carried out by adding reactants, catalysts, other additives and the like into a reaction kettle to carry out a one-pot reaction, and has a plurality of disadvantages, such as: (1) when the reaction is carried out in an alkaline system at a higher reaction temperature, boric acid/boric acid ester is easy to decompose, so that the reaction yield is reduced; (2) palladium catalysts, including palladium salts and ligands, are generally expensive, and if the amount of catalyst is not at a low level, the production cost will be lost from market competitiveness; (3) the reaction is usually batch-wise, which not only affects conversion, yield and cost, but also risks the safety of uncontrollable reaction exotherms.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to overcome prior art Suzuki coupling reaction raw materials easy degradation, reaction conversion rate is low, exothermic uncontrollable, defect that manufacturing cost is high, provide a reaction unit who is applicable to the industrialization that can effective control raw materials decomposition rate and reaction heat release rate to improve catalyst utilization rate, the device simple structure, convenient operation, equipment investment are low.
The utility model discloses an above-mentioned technical problem is solved through following technical scheme:
a reaction apparatus, characterized in that it comprises: the system comprises a raw material preparation kettle, a reaction kettle, a first heat exchange loop, a second heat exchange loop, a flow regulating valve, a flow limiting orifice plate and a distributor; a material outlet of the raw material preparation kettle is in closed connection with a material inlet of the reaction kettle through a pipeline sequentially through the flow regulating valve and the flow limiting orifice plate; the material inlet pipeline of the reaction kettle extends to the inner space of the reaction kettle, and the distributor is arranged at the tail end of the material inlet pipeline of the reaction kettle and is used for uniformly dripping the raw materials from the raw material preparation kettle into the reaction kettle;
the outer surface of the raw material preparation kettle is provided with a first jacket, and the first heat exchange loop is a loop formed by an outlet of the first jacket and inlets of a first heat exchanger, a first medium transfer pump and the first jacket;
the outer surface of the reaction kettle is provided with a second jacket, and the second heat exchange loop is a loop formed by an outlet of the second jacket and inlets of a second heat exchanger, a second medium transfer pump and the second jacket;
the outer diameter of the distributor is 0.6-0.7 times of the inner diameter of the reaction kettle, the inner diameter of the distributor is 0.5-0.55 times of the inner diameter of the reaction kettle, raw material dripping holes or jet holes are formed in the distributor, and the diameters of the raw material dripping holes and the jet holes are 1-5 mm.
Preferably, the outer layer of the connecting pipeline between the raw material preparation kettle and the reaction kettle is provided with a heat insulation layer.
Preferably, the heat insulation layer is a polyurethane heat insulation layer or an electric tracing band.
Preferably, the volume of the raw material preparation kettle is less than or equal to the volume of the reaction kettle, and more preferably, the volume of the raw material preparation kettle and the volume of the reaction kettle both range from 50L to 20000L; more preferably 500 to 6300L.
Preferably, the material of the raw material preparation kettle and the reaction kettle is selected from glass lining or stainless steel, more preferably 304/304L/316/316L stainless steel, and further more preferably 304 or 316 stainless steel.
Preferably, the distributor is made of any one of teflon, glass-lined or stainless steel, and more preferably 304 or 316 stainless steel.
Preferably, the material of the connecting pipeline between the raw material preparation kettle and the reaction kettle is selected from glass lining or 304/304L/316/316L stainless steel; more preferably 304 or 316 stainless steel.
Preferably, the materials of the first heat exchanger and the second heat exchanger are selected from glass lining or 304/304L/316/316L stainless steel; more preferably 304 or 316 stainless steel.
Preferably, the vehicle is selected from ethylene glycol or hydrogenated terphenyl; more preferably ethylene glycol.
Preferably, the working temperature of the flow regulating valve is-100 to 250 ℃; more preferably 20 to 120 ℃.
Preferably, the adjustable flow rate of the flow regulating valve is 1-200 mL/s; more preferably 1 to 100 mL/s.
Preferably, the working temperature of the flow limiting orifice plate is-100 to 250 ℃; more preferably 20 to 120 ℃.
Preferably, the adjustable flow rate of the flow limiting orifice plate is 1-200 mL/s; more preferably 1 to 100 mL/s.
Preferably, the working temperature of the first medium transfer pump and the working temperature of the second medium transfer pump are both-100 ℃ to 250 ℃; more preferably 20 to 120 ℃.
Preferably, the working temperature of the first heat exchanger and the working temperature of the second heat exchanger are both-100 ℃ to 250 ℃; more preferably 20 to 120 ℃.
Preferably, the working temperature of the distributor is-100 to 250 ℃; more preferably 20 to 120 ℃.
Preferably, the adjustable flow rate of the distributor is 1-200 mL/s; more preferably 1 to 100 mL/s.
Preferably, the working temperature of a connecting pipeline between the raw material preparation kettle and the reaction kettle is-100-250 ℃; more preferably 20 to 120 ℃.
The utility model discloses an actively advance the effect and lie in:
1) the utility model provides an industrial reaction device which has simple structure, convenient operation and low equipment investment, can effectively control the decomposition rate of raw materials and the reaction heat release rate and ensure that the catalyst loading capacity is at a lower level;
2) the utility model discloses a set up flow control valve, current-limiting orifice plate when the raw materials adds, the raw materials input speed and the flow that the two-stage control comes from in the raw materials cauldron to combine to set up the distributor in reation kettle's feed inlet, make the raw materials add into reation kettle fast uniformly more, accelerate the combination of raw materials and catalyst in the reation kettle, thereby effective control reaction rate, the utility model discloses a reaction unit is particularly useful for as the device of Suzuki coupling reaction, can greatly reduce the hydrolysis of boric acid/boric acid ester raw materials under alkaline high temperature condition in the Suzuki coupling reaction;
3) by controlling the continuous constant-temperature dropping of the reaction materials and controlling the adding rate and the adding amount of the raw materials, the loading capacity of the catalyst is kept at a lower level compared with the quantitative raw materials, and the utilization rate of the catalyst can be improved;
4) the respective temperatures of the raw material preparation kettle and the reaction kettle are effectively controlled by independently arranging the heat exchange loops for the raw material preparation kettle and the reaction kettle.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for Suzuki coupling reaction according to an embodiment of the present invention.
Fig. 2 is a schematic top view of the distributor 7 of fig. 1.
Reference numerals:
1. a raw material preparation kettle; 2. a first medium transfer pump; 3. a first heat exchanger; 4. a flow regulating valve; 5. a restriction orifice plate; 6. a reaction kettle; 7. a distributor; 8. a second medium transfer pump; 9. a second heat exchanger.
Detailed Description
The present invention will be more clearly and completely described below with reference to the accompanying drawings.
Example 1
As shown in fig. 1 and 2, the reaction apparatus of the present embodiment includes: the system comprises a raw material preparation kettle 1, a reaction kettle 6, a first heat exchange loop, a second heat exchange loop, a flow regulating valve 4, a flow limiting orifice plate 5 and a distributor 7; a material outlet of the raw material preparation kettle 1 is in closed connection with a material inlet of the reaction kettle 6 through a pipeline sequentially through a flow regulating valve 4 and a flow limiting orifice plate 5; a material inlet pipeline of the reaction kettle 6 extends to the inner space of the reaction kettle 6, and the tail end of the material inlet pipeline of the reaction kettle 6 is provided with a distributor 7 for uniformly dripping the raw material from the raw material preparation kettle 1 into the reaction kettle 6;
a first jacket is arranged on the outer surface of the raw material preparation kettle 1, and a loop formed by an outlet of the first jacket and inlets of the first heat exchanger 3, the first medium transfer pump 2 and the first jacket forms a first heat exchange loop;
a second jacket is arranged on the outer surface of the reaction kettle 6, and a loop formed by an outlet of the second jacket and inlets of a second heat exchanger 9, a second medium transfer pump 8 and the second jacket forms a second heat exchange loop;
the outer diameter of the distributor 7 is 0.6 times of the inner diameter of the reaction kettle 6, the inner diameter of the distributor 7 is 0.5 times of the inner diameter of the reaction kettle 6, raw material dripping holes or spraying holes are arranged on the distributor 7, and the aperture is 3 mm. The material of the distributor 7 is 304 stainless steel, and the raw material solution is uniformly dripped into the reaction solution through all the pore diameters of the distributor 7.
The volume of the raw material preparation kettle 1 is 5000L, the kettle is made of glass lining, and the first heat exchanger 3 matched with the kettle is made of glass lining.
The reactor volume of the reaction kettle 6 is 6300L, the kettle is made of 316 stainless steel, and the second heat exchanger 9 matched with the kettle is made of glass lining.
The connecting pipeline between the raw material preparation kettle 1 and the reaction kettle 6 is insulated by a polyurethane insulating layer on the outer layer.
Test example 1
Comparison of the reaction yield of the reaction apparatus of example 1 with that of a one-pot method for Suzuki coupling reaction:
the following Suzuki coupling reaction was performed using a one-pot method: 860Kg of 2-fluoro-3-chloro-phenylboronic acid, 1035Kg of ethyl 2-methyl-3-amino-4-chlorobenzoate, 1.72Kg of 2-triphenylphosphine-2-palladium chloride and 516Kg of potassium carbonate are reacted in an acetonitrile-water (3440 Kg:860Kg) system at a reaction temperature of 65-75 ℃ by a one-pot method to obtain a yield of 76%.
Using the reaction apparatus in example 1, 860Kg of 2-fluoro-3-chloro-phenylboronic acid and 1720Kg of acetonitrile are added into 5000L of raw material preparation kettle 1 to prepare a solution, and the working temperature of the raw material preparation kettle 1 is 65-75 ℃; 1035Kg of ethyl 2-methyl-3-amino-4-chlorobenzoate, 1.72Kg of 2-triphenylphosphine-2-palladium chloride, and 516Kg of potassium carbonate were dissolved in acetonitrile-water (weight: 1720Kg:860Kg) and then charged into 6300L reactor 6. The adjustable flow rate of the flow regulating valve 4 is 60-65 mL/s, the working temperature is 65-75 ℃, the adjustable flow rate of the flow limiting orifice plate 5 is 50-55 mL/s, and the working temperature is as follows: 65-75 ℃, and the average value of the raw material feeding speed is about 53 mL/s; the working temperature of the first medium transfer pump 2 and the second medium transfer pump 8 is 65-75 ℃, the circulating media (namely the media) outside the raw material preparation kettle 1 and the reaction kettle 6 are both ethylene glycol, and the working temperature of the first heat exchanger 4 and the second heat exchanger 9 is 65-75 ℃. The amount of the reaction mass added and other conditions were the same as in the one-pot method. The obtained reaction yield is 86 percent and can be increased by about 10 percent compared with the yield obtained by a one-pot method.
Although specific embodiments of the present invention have been described above, it will be understood by those skilled in the art that this is by way of example only and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and the principles of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (8)
1. A reaction apparatus, characterized in that it comprises: the system comprises a raw material preparation kettle, a reaction kettle, a first heat exchange loop, a second heat exchange loop, a flow regulating valve, a flow limiting orifice plate and a distributor; a material outlet of the raw material preparation kettle is in closed connection with a material inlet of the reaction kettle through a pipeline sequentially through the flow regulating valve and the flow limiting orifice plate; the material inlet pipeline of the reaction kettle extends to the inner space of the reaction kettle, and the distributor is arranged at the tail end of the material inlet pipeline of the reaction kettle and is used for uniformly dripping the raw materials from the raw material preparation kettle into the reaction kettle;
the outer surface of the raw material preparation kettle is provided with a first jacket, and the first heat exchange loop is a loop formed by an outlet of the first jacket and inlets of a first heat exchanger, a first medium transfer pump and the first jacket;
the outer surface of the reaction kettle is provided with a second jacket, and the second heat exchange loop is a loop formed by an outlet of the second jacket and inlets of a second heat exchanger, a second medium transfer pump and the second jacket;
the outer diameter of the distributor is 0.6-0.7 times of the inner diameter of the reaction kettle, the inner diameter of the distributor is 0.5-0.55 times of the inner diameter of the reaction kettle, raw material dripping holes or jet holes are formed in the distributor, and the aperture sizes of the raw material dripping holes and the jet holes are 1-5 mm.
2. The reaction device of claim 1, wherein the outer layer of the connecting pipeline between the raw material preparation kettle and the reaction kettle is provided with an insulating layer.
3. The reaction apparatus of claim 2, wherein the insulation layer is a polyurethane insulation layer or an electric tracing band.
4. The reaction apparatus of claim 1, wherein the volume of the raw material preparation tank is equal to or less than the volume of the reaction tank.
5. The reaction apparatus of claim 1, wherein the raw material preparation vessel and the reaction vessel are made of a material selected from glass lining and stainless steel.
6. The reaction device of claim 1, wherein the material of the connecting pipeline between the raw material preparation kettle and the reaction kettle is glass lining or stainless steel.
7. The reactor according to claim 1, wherein the distributor is made of any one of polytetrafluoroethylene, glass-lined material and stainless steel.
8. The reactor according to claim 1, wherein the first heat exchanger and the second heat exchanger are made of glass-lined or stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020845168.3U CN213286769U (en) | 2020-05-19 | 2020-05-19 | Reaction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020845168.3U CN213286769U (en) | 2020-05-19 | 2020-05-19 | Reaction device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN213286769U true CN213286769U (en) | 2021-05-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202020845168.3U Expired - Fee Related CN213286769U (en) | 2020-05-19 | 2020-05-19 | Reaction device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN213286769U (en) |
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2020
- 2020-05-19 CN CN202020845168.3U patent/CN213286769U/en not_active Expired - Fee Related
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210528 |
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| CF01 | Termination of patent right due to non-payment of annual fee |