CN212942832U - Loop reactor for amination reaction of prochloraz product - Google Patents
Loop reactor for amination reaction of prochloraz product Download PDFInfo
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- CN212942832U CN212942832U CN202021452628.2U CN202021452628U CN212942832U CN 212942832 U CN212942832 U CN 212942832U CN 202021452628 U CN202021452628 U CN 202021452628U CN 212942832 U CN212942832 U CN 212942832U
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Abstract
The utility model belongs to the technical field of organic chemical industry, concretely relates to a loop reactor for amination of prochloraz product, include the reactor, be located venturi ejector, loop heat exchanger and the circulating pump of upper end in the reactor, the feed inlet of reactor passes through material pipeline, feeding valve and charge pump and is connected with the batching jar, the circulating pump with the bottom of reactor links to each other, loop heat exchanger's one end with the circulating pump links to each other, and the other end with venturi ejector's entry links to each other, constitutes circulation loop. The utility model can greatly shorten the time for synthesizing the amination of the prochloraz product and effectively inhibit the decomposition of materials and the occurrence of side reactions; meanwhile, the reaction temperature can be well controlled within a required temperature range through an external heat exchanger.
Description
Technical Field
The utility model belongs to the technical field of organic chemical industry, concretely relates to a loop reactor for prochloraz product amination.
Background
At present, a kettle type container with a stirring paddle is usually adopted for amination reaction of a prochloraz product, the reaction time is long, partial raw material etherate is decomposed, the product yield is low, more waste residues are generated, the energy consumption is high, meanwhile, the reaction temperature is not easy to control, and the reaction safety risk is high once the temperature is out of control.
Therefore, a new reactor-loop reactor which can shorten the reaction time and inhibit the decomposition of materials and the occurrence of side reactions is needed to be provided, and the reactor-loop reactor is applied to the synthesis of the amination reaction of the prochloraz product; in addition, the problem that the temperature cannot be well controlled in a required temperature range in the amination reaction process of the prochloraz product is solved.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects of the prior art and provide a loop reactor for amination reaction of prochloraz products.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a loop reactor for amination reaction of prochloraz product comprises a reactor, a venturi ejector, a loop heat exchanger and a circulating pump, wherein the venturi ejector is positioned at the upper end in the reactor, a feeding hole of the reactor is connected with a dosing tank through a material pipeline, a feeding valve and a feeding pump, the circulating pump is connected with the bottom end of the reactor, one end of the loop heat exchanger is connected with the circulating pump, and the other end of the loop heat exchanger is connected with an inlet of the venturi ejector to form a circulating loop.
Furthermore, the Venturi type ejector comprises an inlet section, a nozzle, a mixing section and a diffusion section which are communicated in sequence, the nozzle is of a reducing pipe type, the diffusion section is of a gradually expanding pipe type, annular gas chambers of a reducing type are arranged on the peripheries of the inlet section and the nozzle and communicated with the mixing section, and gas circulation pipes are arranged on the side surfaces of the gas chambers and connected with the top of the reactor.
Further, the ratio of the inner diameter of the opening of the inlet section to the inner diameter of the nozzle to the inner diameter of the closing opening of the air chamber to the length of the mixing section to the length of the diffusion section is 38:2.5:3.8:40:520, and the opening angle of the diffusion section is 21 degrees.
Furthermore, a coolant inlet, a coolant outlet, a steam inlet and a softened water outlet are arranged on the loop heat exchanger, air is replaced by inert gas in the reactor, and tail gas is discharged from the reactor through a condenser.
Furthermore, a connecting pipeline of the loop heat exchanger and the circulating pump is connected with a sampling port I through a sampling pipeline and a sampling valve; and a pipeline connecting the circulating pump and the bottom end of the reactor is connected with a sampling port II through a sampling pipeline and a sampling valve.
Furthermore, a pressure gauge I is arranged on a material pipeline between the feeding pump and the feeding hole of the reactor, a pressure gauge II, a thermometer and a liquid level meter are respectively arranged on the outer side of the reactor, and a pressure gauge III is arranged on a connecting pipeline of the loop heat exchanger and the circulating pump.
Further, the circulating heat exchanger is an external tubular heat exchanger or a plate heat exchanger.
Further, the lower end of the venturi eductor is located below the level of the material in the reactor.
Further, the reactor is made of steel lining glass lining.
The utility model discloses an advantage and positive effect:
the time for amination reaction synthesis of the prochloraz product can be greatly shortened, and material decomposition and side reaction are effectively inhibited; meanwhile, the reaction temperature can be well controlled within a required temperature range through an external heat exchanger.
The utility model discloses utilize the venturi ejector in circulating pump and the reactor to realize that the material mixes more fully, the mass transfer effect is more high-efficient, is favorable to the emergence of prochloraz product amination to can shorten reaction time, reduce the side reaction such as material decomposition and take place. Utilize return circuit heat exchanger to heat or cool off, can be more accurate, quick provide required heat for the reaction, also can be quick, accurate simultaneously move the reaction system outside with the waste heat that produces, be favorable to providing the stable condition that the reaction needs, guarantee the technology stability, realize the safety in production. The reactor is provided with the liquid level meter, so that the feeding condition can be monitored, the accurate feeding is facilitated, and the stable production is realized.
The utility model discloses a loop reactor, core component venturi sprayer, its structural design has critical effect to the liquid linear velocity of nozzle department and the control of the micron order bubble of production, and then influences the speed of heterogeneous reaction. Through optimizing the structural design of the Venturi ejector, the gas-liquid mass transfer process is promoted, and the product conversion rate is improved.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic diagram of a venturi eductor;
the notations in FIG. 1 have the following meanings: 1-reactor, 2-venturi ejector, 3-loop heat exchanger, 4-circulating pump, 5-feed inlet, 6-feed valve, 7-feed pump, 8-batching tank, 9-sample inlet I, 10-sample inlet II, 11-pressure gauge I, 12-pressure gauge II, 13-thermometer, 14-liquid level gauge, 15-pressure gauge III;
2-1-inlet section, 2-2-nozzle, 2-3-mixing section, 2-4-diffuser section;
3-1-refrigerant inlet, 3-2-refrigerant outlet, 3-3-steam inlet and 3-4-softened water outlet.
Detailed Description
In the description of the present invention, it is to be understood that the directions or positional relationships indicated by the terms "upper", "lower", "top", "bottom", "inner", "outer", etc. are all the directions or positional relationships shown on the drawings, and the objects are only for convenience of description of the present invention and simplification of description, and do not indicate or imply that the parts indicated must have a specific direction, be constructed and operated in a specific direction, and thus, are not to be construed as limiting the present invention.
The following detailed description of the embodiments of the present invention will be made with reference to the accompanying drawings.
A loop reactor for amination reaction of prochloraz product, as shown in figure 1-2, comprises a reactor 1, a venturi ejector 2 at the upper end in the reactor 1, a loop heat exchanger 3 and a circulating pump 4, wherein a feed inlet 5 of the reactor 1 is connected with a dosing tank 8 through a material pipeline, a feed valve 6 and a feed pump 7, the circulating pump 4 is connected with the bottom end of the reactor 1, one end of the loop heat exchanger 3 is connected with the circulating pump 4, and the other end is connected with an inlet of the venturi ejector 2, thus forming a circulating loop.
The material enters a loop heat exchanger 3 from the bottom end of the reactor 1 through a circulating pump 4, enters a Venturi ejector 2 from the top end of the reactor 1, and the loop heat exchanger 3 removes or provides heat released or absorbed in the reaction process.
The Venturi type ejector 2 (replacing a gas distributor or other gas distribution systems) is a high-performance gas-liquid mixing device; the Venturi type ejector 2 comprises an inlet section 2-1, a nozzle 2-2, a mixing section 2-3 and a diffusing section 2-4 which are sequentially communicated, the nozzle 2-2 is of a reducing pipe type, the diffusing section 2-4 is of a gradually expanding pipe type, a reducing annular gas chamber is arranged on the peripheries of the inlet section 2-1 and the nozzle 2-2 and communicated with the mixing section 2-3, and a gas circulation pipe is arranged on the side surface of the gas chamber and connected with the top of the reactor 1.
Pumping liquid through a nozzle 2-2 to form a rapid jet flow to carry gas in a gas chamber to jet out, wherein the liquid impacts a pipe wall to form energy consumption and a strong mixed vibration area, in each area, the strong turbulence enables foams to be well dispersed, the gas foams generated by impact are very small (30-70 microns), and meanwhile, the gas-liquid ratio reaches more than 0.5-2.0.
The ratio of the inner diameter of an opening of an inlet section 2-1 of the Venturi type ejector 2 to the inner diameter of a nozzle 2-2 to the inner diameter of a closing opening of an air chamber to the length of a mixing section 2-3 to the length of a diffusion section 2-4 is 38:2.5:3.8:40:520, and the opening angle of the diffusion section 2-4 is 21 degrees.
Aiming at a specific certain chemical reaction process under a certain pressure and temperature condition, the design structure size of the Venturi ejector 2 greatly influences the effect of mutual dispersion and contact among reaction substances, thereby finally influencing the chemical production efficiency.
The gas phase flow rate increases due to the pushing of the circulating liquid flowing through the venturi ejector 2, the reaction liquid is fully mixed in the ejector mixer to form a turbulent flow, and the gas-liquid phase contact area is increased.
The loop heat exchanger 3 is provided with a refrigerant inlet 3-1, a refrigerant outlet 3-2, a steam inlet 3-3 and a softened water outlet 3-4, air is replaced by inert gas in the reactor 1, and the reactor 1 discharges tail gas through a condenser.
The shell-side heat exchange fluid is cooling water and steam, and can be switched according to the temperature of the reactor.
A sampling port I9 is connected to a connecting pipeline of the loop heat exchanger 3 and the circulating pump 4 through a sampling pipeline and a sampling valve; and a pipeline connected with the circulating pump 4 and the bottom end of the reactor 1 is connected with a sampling port II 10 through a sampling pipeline and a sampling valve.
A pressure gauge I11 is arranged on a material pipeline between the feeding pump 7 and the feeding port 5 of the reactor 1, a pressure gauge II 12, a thermometer 13 and a liquid level meter 14 are respectively arranged on the outer side of the reactor 1, and a pressure gauge III 15 is arranged on a connecting pipeline between the loop heat exchanger 3 and the circulating pump 4.
The circulating heat exchanger 3 is an external tubular heat exchanger; the external heat exchanger (replacing coil pipe or built-in heat exchanger) can be made according to the heat exchange requirement of chemical reaction, compared with the prior built-in heat exchanger, the size of the external heat exchanger is not limited by the volume of the reaction vessel (reaction kettle). The external heat exchanger can work with the full heat exchange area even under the condition of reducing the working volume, such as semi-batch operation or semi-kettle material reaction.
The lower end of the venturi eductor 2 is located below the level of the feed in the reactor 1. It utilizes venturi ejector 2 to form the negative pressure through the major cycle of material, with reaction material intensive mixing and dispersion to spout into reactor 1, the material that jets strikes with the current material in the reactor 1, has the effect of secondary mixing.
The reactor 1 is made of steel lining glass lining.
Wherein, the material of the loop heat exchanger 3 runs through a tube pass, and a heating or cooling medium runs through a shell pass to provide a heat source for the reaction or take away a heat source; the reactor 1 provides a sufficient reaction place for reaction materials; the circulating pump 4 provides power for mixing the reaction materials, and simultaneously, the reaction materials pass through the heat exchanger to obtain energy required by the reaction or take away redundant energy generated by the reaction. The feeding pump conveys materials required by the reaction to the reactor. The temperature and pressure required by the reaction are monitored and controlled by the thermometer pressure gauge, and the temperature and pressure required by the reaction are timely adjusted by the heat exchanger according to the temperature and pressure system displayed in real time, so that the stable reaction is ensured.
N-propylamine and etherate which are required by amination reaction of prochloraz products are pumped into a reactor 1 through a feed pump 7 in proportion, the pumping degree of the materials can be observed through a liquid level meter 14, after the feeding is finished, a circulating pump 4 is started, the materials are circulated through a loop heat exchanger 3, the materials obtain required temperature and pressure through the loop heat exchanger 3 during circulation, the temperature and the pressure can be monitored through a thermometer 13/a pressure gauge II 12, and whether the feed pump 7 and the circulating pump 4 can provide the pressure required by corresponding pump operation can be observed through the conditions of a pressure gauge I11/a pressure gauge III 15. When the circulating pump 4 is circulated, the materials are fully mixed after being sprayed by the Venturi type sprayer 2 in the reactor 1, and then the reaction is accelerated. The reaction process can be sampled and detected through the sampling port I9 \ sampling port II 10 in the reaction process, and the reaction can be finished when the etherification of the main reaction raw materials is less than 0.3 percent. After the reaction is finished, the heat can be removed through the circulating heat exchanger 3, and the temperature is reduced to normal temperature and then the heat is transferred to other post-treatment lines for treatment.
The utility model discloses during the use, go on according to following step: the method comprises the steps of pumping n-propylamine and etherified substances required by an amination reaction of a prochloraz product into a reactor 1 through a feed pump 7 in proportion, closing a feed valve 6 after feeding is finished, replacing the interior of the reactor 1 with nitrogen for three times, replacing air in the reactor 1, closing related valves, starting a circulating pump 4, circulating the materials, opening a steam valve, starting a heating system of a loop heat exchanger 3, maintaining the temperature of the materials in the reactor 1 at about 90 ℃, sampling and detecting through a sampling port I9/sampling port II 10 after reacting for a period of time, finishing the reaction if the etherified substance is less than 0.3%, closing a steam heat source, opening a cooling water system, cooling to normal temperature through the loop heat exchanger 3, closing cooling water, and transferring the materials in the reactor 1 to other processes for treatment. In the operation process, the display numerical values of the pressure gauge I11, the pressure gauge II 12, the pressure gauge III 15, the thermometer 13, the liquid level meter 14 and other instruments are closely noticed, and if abnormity occurs, relevant measures are taken in time to ensure that the reaction is stably carried out.
The process principle of the reactor is as follows: utilize venturi ejector 2 in reactor 1, carry out high-efficient mass transfer heat transfer with the help of the high-speed jet that external circulating pump 4 produced and replace traditional stirring thick liquid, be favorable to accelerating the reaction and go on, shorten reaction time to reduce the side reaction and take place.
The utility model discloses replace traditional technology production with venturi circulation loop reactor, can realize continuous operation simultaneously. The Venturi type circulation loop reactor has the advantages of compact structure, low operation temperature, low energy consumption, good mass transfer effect, high production efficiency, and small equipment investment and occupied area. Because each subassembly of venturi type circulation loop reactor matches accurately to set up the accurate control reaction temperature of multi-functional heat exchanger, when reducing the side reaction, improve the degree of safety of technology, accord with green chemical industry and sustainable development's requirement.
The details of the present invention not described in detail in the specification are well known to those skilled in the art. The utility model discloses the standard part that uses all can purchase from the market, and dysmorphism piece all can be customized according to the record of description and attached drawing, and the concrete connection mode of each part all adopts conventional means such as ripe bolt, rivet, welding among the prior art, and machinery, part and equipment all adopt prior art, and conventional model is including the conventional connected mode of circuit connection adoption conventional among the prior art, and here detailed description is not again.
The above-mentioned embodiment is only the preferred embodiment of the present invention, all the basis the utility model discloses a technical entity all belongs to the utility model discloses any simple modification, modification and substitution change to what the above embodiment was done the within range of technical scheme.
Claims (7)
1. The loop reactor for amination reaction of prochloraz product is characterized by comprising a reactor (1), a Venturi ejector (2) positioned at the upper end in the reactor (1), a loop heat exchanger (3) and a circulating pump (4), wherein a feeding hole (5) of the reactor (1) is connected with a batching tank (8) through a material pipeline, a feeding valve (6) and a feeding pump (7), the circulating pump (4) is connected with the bottom end of the reactor (1), one end of the loop heat exchanger (3) is connected with the circulating pump (4), and the other end of the loop heat exchanger is connected with an inlet of the Venturi ejector (2) to form a circulating loop.
2. A loop reactor for amination reaction of prochloraz product according to claim 1, wherein said venturi injector (2) comprises an inlet section (2-1), a nozzle (2-2), a mixing section (2-3) and a diffusing section (2-4) which are sequentially communicated, said nozzle (2-2) is a tapered tube type, said diffusing section (2-4) is a tapered tube type, the periphery of said inlet section (2-1) and nozzle (2-2) is provided with a tapered annular gas chamber, the gas chamber is communicated with said mixing section (2-3), the side of the gas chamber is provided with a gas circulation tube and is connected with the top of the reactor (1).
3. The loop reactor for amination of prochloraz product according to claim 2, wherein the ratio of the inner diameter of the opening of the inlet section (2-1) of the venturi ejector (2) to the inner diameter of the nozzle (2-2) to the inner diameter of the closing-in of the gas chamber to the length of the mixing section (2-3) to the length of the diffuser section (2-4) is 38:2.5:3.8:40:520, and the opening angle of the diffuser section (2-4) is 21 °.
4. The loop reactor for amination of prochloraz product according to claim 1, wherein the loop heat exchanger (3) is provided with a refrigerant inlet (3-1), a refrigerant outlet (3-2), a steam inlet (3-3) and a softened water outlet (3-4), air is replaced by inert gas in the reactor (1), and the reactor (1) discharges tail gas through a condenser.
5. A loop reactor for amination of prochloraz products according to claim 1, wherein a sampling port i (9) is connected to a connecting pipeline of the loop heat exchanger (3) and the circulating pump (4) through a sampling pipeline and a sampling valve; and a pipeline connected with the bottom end of the reactor (1) by the circulating pump (4) is connected with a sampling port II (10) through a sampling pipeline and a sampling valve.
6. A loop reactor for amination reaction of prochloraz product according to claim 1, wherein a pressure gauge i (11) is arranged on a material pipeline between the feeding pump (7) and the feeding port (5) of the reactor (1), a pressure gauge ii (12), a temperature gauge (13) and a liquid level gauge (14) are respectively arranged outside the reactor (1), and a pressure gauge iii (15) is arranged on a connecting pipeline of the loop heat exchanger (3) and the circulating pump (4).
7. A loop reactor for amination of prochloraz products according to claim 1, wherein said loop heat exchanger (3) is an external tube heat exchanger or plate heat exchanger.
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CN202021452628.2U CN212942832U (en) | 2020-07-22 | 2020-07-22 | Loop reactor for amination reaction of prochloraz product |
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CN202021452628.2U CN212942832U (en) | 2020-07-22 | 2020-07-22 | Loop reactor for amination reaction of prochloraz product |
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Denomination of utility model: A loop reactor for amination of prochloraz products Effective date of registration: 20221013 Granted publication date: 20210413 Pledgee: Industrial Bank Co.,Ltd. Jiujiang Branch Pledgor: Jiangxi Hui He Chemical Co.,Ltd. Registration number: Y2022980018283 |