CN219424345U - On-line dehydration equipment for continuous reaction - Google Patents

Abstract

The utility model provides on-line dehydration equipment for continuous reaction. The on-line dehydration equipment for continuous reaction comprises: at least one dehydration module and an evacuating device disposed on one side of the at least one dehydration module, each dehydration module comprising: the reaction device is provided with a raw material feeding hole and a product discharging hole which are communicated with the reaction cavity, and the product discharging hole is positioned above the raw material feeding hole in the longitudinal direction; a heating structure provided at the outer periphery of the reaction device; a dehydration film tube, at least a portion of which is positioned in the reaction chamber, and defines a receiving chamber in communication with the reaction chamber; the vacuumizing device is communicated with the accommodating cavity and is used for providing a negative pressure environment for the dehydration membrane tube so that free water in the reaction cavity flows to the accommodating cavity under the action of pressure difference. The technical scheme of the utility model can complete continuous reaction through an online dehydration process, and has higher efficiency.

Description

On-line dehydration equipment for continuous reaction

Technical Field

The utility model relates to the technical field of chemical industry, in particular to on-line dehydration equipment for continuous reaction.

Background

The separation process plays a role in the chemical and pharmaceutical industries, accounting for 40% -70% of the capital and operating costs, and in the chemical and pharmaceutical industries, in organic synthesis reactions (such as esterification reaction, etherification reaction, condensation reaction, acid anhydride preparation and amide preparation), a certain amount of free water is often generated along with the reaction, so that the smooth reaction and the purity of the product are seriously affected, and therefore, continuous and efficient dehydration treatment is a critical ring for continuous reaction, not only can the reaction efficiency be improved, but also the product can be collected in time. The reaction dehydration technology mainly comprises rectification dehydration, azeotropic dehydration and dehydrating agent dehydration, the methods generally consume higher energy, secondary pollution is easy to form, the membrane separation technology can realize separation tasks which are difficult to complete by traditional methods such as distillation, extraction and adsorption with lower energy consumption, a large amount of energy consumption is reduced, and the separation requirements which are difficult or impossible to realize by the conventional method are realized, so that the method has wide application prospect. The method has the characteristics of simple process, high safety coefficient, compact structure, low investment, high efficiency and energy conservation.

At present, the existing reaction dehydration equipment comprises a reaction kettle and a dehydration membrane pipe arranged in the reaction kettle, wherein the dehydration membrane pipe is positioned at the top of a cavity of the reaction kettle, a feed hole is formed in the top of the reaction kettle, a discharge hole is formed in the bottom of the reaction kettle, the discharge hole is closed, raw materials are input into the reaction kettle through the feed hole, fall to the bottom of the reaction kettle under the action of gravity and react at the bottom of the reaction kettle, water generated by the reaction moves upwards after vaporization and contacts with the dehydration membrane pipe to carry out dehydration, and after the dehydration is completed, the feed hole is closed again, the discharge hole is opened, and products are discharged; and after the product is discharged, continuously inputting the raw materials for the next round of reaction.

That is, in the existing reaction dehydration equipment, four steps of feeding, reacting, dehydrating and collecting the product are needed to complete one reaction dehydration process, and the dehydration process is performed after the reaction is completed, so that continuous reaction cannot be completed by on-line dehydration, and the time and efficiency of the reaction dehydration are long and low.

Disclosure of Invention

The utility model mainly aims to provide on-line dehydration equipment for continuous reaction, which solves the problems that the continuous reaction cannot be completed by on-line dehydration due to the sequential reaction process and dehydration process in the prior art, and the efficiency is lower.

In order to achieve the above object, the present utility model provides an on-line dehydration apparatus for continuous reaction, comprising: at least one dehydration module and an evacuating device disposed on one side of the at least one dehydration module, each dehydration module comprising: the reaction device is provided with a raw material feeding hole and a product discharging hole which are communicated with the reaction cavity, and the product discharging hole is positioned above the raw material feeding hole in the longitudinal direction; a heating structure provided at the outer periphery of the reaction device; a dehydration film tube, at least a portion of which is positioned in the reaction chamber, and defines a receiving chamber in communication with the reaction chamber; the vacuumizing device is communicated with the accommodating cavity and is used for providing a negative pressure environment for the dehydration membrane tube so that free water in the reaction cavity flows to the accommodating cavity under the action of pressure difference.

Further, the on-line dehydration device for continuous reaction further comprises: a cold trap; one end of the liquid outlet pipeline is communicated with the accommodating cavity, the other end of the liquid outlet pipeline is communicated with the cold trap, and the vacuumizing device is communicated with the cold trap.

Further, the heating structure includes a heating cartridge defining a heating cavity for storing a heating medium.

Further, a heating medium feeding hole and a heating medium discharging hole are formed in the heating cylinder, and the heating medium discharging hole is located above the heating medium feeding hole in the longitudinal direction.

Further, the on-line dehydration apparatus for continuous reaction further comprises a product discharge pipe, one end of which is communicated with the product discharge hole, and the other end of which is configured to be capable of communicating with the product collecting device.

Further, the online dehydration equipment for continuous reaction further comprises a first thermometer arranged on the product discharging pipeline, wherein the first thermometer is used for measuring the temperature of materials in the product discharging pipeline; and/or the online dehydration equipment for continuous reaction further comprises a first pressure gauge and a first product discharge valve, wherein the first pressure gauge is arranged on the product discharge pipeline and is used for measuring the pressure of the material in the product discharge pipeline, and the first product discharge valve is configured to be opened or closed so as to adjust the flow rate of the material in the product discharge pipeline.

Further, the on-line dehydration apparatus for continuous reaction further comprises a raw material feed valve provided at the raw material feed hole, the raw material feed valve being for opening or closing the raw material feed hole; and/or the reaction device is arranged at the periphery of at least part of the dewatering film pipe, and the heating structure is arranged at the periphery of at least part of the reaction device.

Further, the on-line dehydration equipment for continuous reaction comprises a plurality of dehydration assemblies connected in series and at least one communication pipeline, wherein the product discharge hole of one dehydration assembly is communicated with the raw material feed hole of the other dehydration assembly through the communication pipeline in two adjacent dehydration assemblies.

Further, the online dehydration equipment for continuous reaction also comprises a second thermometer arranged on the communicating pipeline, wherein the second thermometer is used for measuring the temperature of materials in the communicating pipeline; and/or the on-line dehydration equipment for continuous reaction further comprises a second pressure gauge and a second product discharge valve, wherein the second pressure gauge is arranged on the communicating pipeline and is used for measuring the pressure of the materials in the communicating pipeline, and the second product discharge valve is configured to be opened or closed so as to regulate the flow rate of the materials in the communicating pipeline.

Further, the dehydration component comprises a plurality of dehydration membrane pipes connected in parallel, at least part of the structure of each dehydration membrane pipe is positioned in the reaction cavity, and the accommodating cavity of each dehydration membrane pipe is communicated with the vacuumizing device.

By applying the technical scheme of the utility model, the heating structure can heat the reaction device and the materials in the reaction device, so as to provide a reaction environment for the materials in the reaction device; the vacuuming device can provide power for the free water generated by the reaction to pass through the dehydration film pipe. Raw materials enter the reaction device through the raw material feed hole, and react in the reaction device, the reaction generates required products and partial free water, under the action of the vacuumizing device, the dehydration membrane tube generates a negative pressure environment, and under the action of pressure difference, the free water in the reaction cavity can enter the accommodating cavity through the dehydration membrane tube, so that the dehydration effect is realized. The on-line dehydration equipment for continuous reaction integrates chemical reaction and dehydration of the dehydration membrane tube, has high integration level, and can realize on-line dehydration while reacting, thereby realizing continuous reaction, avoiding the problem of long reaction dehydration time caused by dividing the reaction and the dehydration into two steps, and improving the reaction efficiency; because the raw material feeding hole is positioned below the product discharging hole, raw materials enter the reaction cavity from the raw material feeding hole, the raw materials can fully react in the process of moving to the product discharging hole, and the raw materials in the reaction process can fully contact with the dehydration membrane tube during the reaction, so that the reaction and the dehydration are simultaneously carried out, that is, the reaction dehydration process can be completed through one-time feeding without multiple circulating reactions, thus the online dehydration continuous reaction can be realized, and the reaction efficiency is improved; meanwhile, the problem that the product discharge hole is closed when feeding and the product is collected again after the reaction is completed, so that continuous reaction cannot be performed in the prior art is avoided.

Drawings

The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model. In the drawings:

fig. 1 shows a schematic structural view of an embodiment of an on-line dehydration apparatus for continuous reaction according to the present utility model.

Wherein the above figures include the following reference numerals:

1. a dewatering film tube; 2. a reaction device; 3. a heating structure; 31. a heating cylinder; 4. a raw material feed line; 5. a product discharge pipeline; 8. a liquid outlet pipeline; 9. a cold trap; 11. a second thermometer; 12. a second pressure gauge; 13. a first thermometer; 14. a first pressure gauge; 15. a vacuum pumping device; 16. a communication pipeline; 61. a first heating medium feed line; 62. a second heating medium feed line; 71. a first heating medium discharge line; 72. a second heating medium discharge pipeline; 1001. a raw material feed valve; 1002. a second product discharge valve; 1003. a first heating medium feed valve; 1004. a first heating medium discharge valve; 2001. a reactant feed valve; 2002. a first product discharge valve; 2003. a second heating medium feed valve; 2004. a second heating medium discharge valve; 3001. a first liquid outlet valve; 3002. a second liquid outlet valve; 3003. and a pipeline on-off valve.

Detailed Description

It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The utility model will be described in detail below with reference to the drawings in connection with embodiments.

In the embodiments of the present utility model, "on-line dehydration" means that dehydration is completed simultaneously with the reaction.

In the prior art (application number 201120024242.6) known by the inventor, a reaction dehydration device comprises a reaction kettle and a dehydrator, wherein the dehydration process is to dehydrate a reaction product through azeotropic rectification separation of a ternary system, and the device has the defects of high energy consumption, large equipment investment and the like, and is not suitable for continuous fine chemical and pharmaceutical reactions due to high energy consumption and high cost. In another prior art known by the inventor, the application number 201210045573.7 provides a method for removing water generated by reaction in situ by adopting an acid-resistant molecular sieve membrane pervaporation device, permeation steam enters a cold trap under the pushing of negative pressure and is rapidly condensed and collected by liquid nitrogen, and as the mixed reaction liquid after primary reaction separation fails to completely react, the mixed reaction liquid after the separation of a membrane component needs to be returned into a reaction tank to continuously participate in the reaction after being cooled by a condenser, namely the reactant needs to be continuously circulated to achieve the purpose of completing the reaction, and continuous reaction cannot be realized because the reactant can not be completely reacted after being circulated for many times, and a great amount of heat energy is consumed because the reactant is continuously heated and condensed; the device divides the reaction and the dehydration into two steps which are sequentially carried out, the reaction dehydration time is prolonged, and the integration level of the device is not high.

That is, the conventional reaction dehydration apparatus fails to achieve continuous reaction in the case of performing esterification reaction, etherification reaction, condensation reaction, acid anhydride production, amide production; and because the catalyst, reactant or product adopted in the reaction is mostly acidic, the equipment is easy to corrode. Accordingly, the present application provides an apparatus system that is acid resistant to achieve continuous reaction on-line dehydration.

As shown in fig. 1, an embodiment of the present utility model provides an on-line dehydration apparatus for continuous reactions. The on-line dehydration equipment for continuous reaction comprises: at least one dehydration module and a vacuum-pumping device 15 disposed at one side of the at least one dehydration module, each dehydration module comprising: the reaction device 2 is used for defining a reaction cavity, a raw material feeding hole and a product discharging hole which are communicated with the reaction cavity are formed in the reaction device 2, and the product discharging hole is positioned above the raw material feeding hole in the longitudinal direction; a heating structure 3 provided on the outer periphery of the reaction device 2; a dehydration film tube 1, at least part of the dehydration film tube 1 is positioned in the reaction cavity, and the dehydration film tube 1 defines a containing cavity communicated with the reaction cavity; the vacuumizing device 15 is communicated with the accommodating cavity, and the vacuumizing device 15 is used for providing a negative pressure environment for the dehydration membrane tube 1 so that free water in the reaction cavity flows to the accommodating cavity under the action of pressure difference.

In the above technical solution, the reaction device 2 is located outside the dehydration film tube 1 and surrounds part of the dehydration film tube 1, the heating structure 3 is located outside the reaction device 2 and surrounds part of the reaction device 2, and the heating structure 3 can heat the reaction device 2 and the materials located in the reaction device 2 to provide a reaction environment for the materials in the reaction device 2; the evacuation device 15 is capable of providing the free water produced by the reaction with the power to pass through the dehydration film tube 1. Raw materials enter the reaction device through the raw material feed hole, and react in the reaction device, the reaction generates required products and partial free water, under the action of the vacuumizing device 15, the dehydration membrane tube 1 generates a negative pressure environment, and under the action of pressure difference, the free water in the reaction cavity can enter the accommodating cavity through the dehydration membrane tube 1, so that the dehydration effect is realized.

Through the arrangement, the on-line dehydration equipment for continuous reaction integrates chemical reaction and dehydration of the dehydration membrane tube 1, has high integration level, and can realize on-line dehydration while reacting, thereby realizing continuous reaction, avoiding the problem of long reaction dehydration time caused by dividing the reaction and the dehydration into front and rear steps, and improving the reaction efficiency; because the raw material feeding hole is positioned below the product discharging hole, raw materials enter the reaction cavity from the raw material feeding hole, the raw materials can fully react in the process of moving to the product discharging hole, and the raw materials in the reaction process can fully contact with the dehydration membrane tube 1 during the reaction, so that the reaction and the dehydration are simultaneously carried out, that is, the reaction dehydration process can be completed through one-time feeding without multiple circulating reactions, thus the online dehydration continuous reaction can be realized, and the reaction efficiency is improved; meanwhile, the problem that the product discharge hole is closed when feeding and the product is collected again after the reaction is completed, so that continuous reaction cannot be performed in the prior art is avoided.

In addition, compared with the scheme that the water carrying agent or the water removing/absorbing material is needed to be used for dehydration in the prior art, the method and the device have the advantages that negative pressure is generated through vacuumizing, dehydration is realized by utilizing pressure difference, the steps of separating and recycling the water carrying agent and regenerating the water removing/absorbing material in the follow-up process are reduced, the product with higher purity can be obtained through simple fractionation, the operation flow of the reaction and the follow-up treatment difficulty are shortened, the organic solvent obtained after the product is fractionated can be recycled, and the three-waste emission is reduced. Meanwhile, the reaction condition is mild, the product yield is high, and the energy consumption in the reaction process is greatly reduced. The dehydration membrane tube 1 used in the application can be used for a long time and multiple times, and the production cost can be obviously reduced.

Because the water carrying agent or the water removing/absorbing material is not needed, the water carrying agent or the water removing/absorbing agent is not needed to be separated by additionally adding a vaporization-liquefaction step, and the dehydration membrane tube 1 can be dehydrated in a liquid state, so that the energy consumption can be greatly reduced, the steps of dehydration and liquefaction after the material vaporization and then the reaction are reduced, and the reaction can be continuously carried out.

In one embodiment of the utility model, the dehydration membrane tube 1 is an acid-resistant dehydration membrane tube. The acid-resistant dehydration membrane tube is formed by growing an acid-resistant molecular sieve membrane on a porous ceramic tubular support body, wherein the average pore diameter of the porous ceramic tubular support body is 0.5-5 nm, the outer diameter of the acid-resistant dehydration membrane tube is 5-14 mm, and the wall thickness of the acid-resistant dehydration membrane tube is 1-3 mm. Because the specific structure of the acid-resistant dewatering membrane tube is the prior art, the detailed description is omitted here.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction comprises a plurality of dehydration modules connected in series and at least one communication pipe 16, wherein the product discharge hole of one dehydration module is communicated with the raw material feed hole of the other dehydration module through the communication pipe 16 in two adjacent dehydration modules.

Preferably, the on-line dehydration device for continuous reaction comprises two dehydration components connected in series and 1 communication pipeline 16, as shown in fig. 1, the dehydration component on the left side is a first dehydration component, the dehydration component on the right side is a second dehydration component, one end of the communication pipeline 16 is communicated with a product discharge hole of the first dehydration component, the other end of the communication pipeline 16 is communicated with a raw material feed hole of the second dehydration component, and a reactant feed valve 2001 is further arranged at the connection part of the communication pipeline 16 and the raw material feed hole of the second dehydration component. The on-line dehydration equipment for continuous reaction further comprises a raw material feeding pipeline 4 communicated with the raw material feeding hole of the first dehydration component and a product discharging pipeline 5 communicated with the product discharging hole of the second dehydration component. The dehydration film pipes 1 of the first dehydration module and the second dehydration module are communicated with a vacuumizing device 15.

By the arrangement, the two dehydration assemblies are connected in series, so that the raw materials can be completely reacted in the equipment under the condition of one-time feeding, and the repeated circulating feeding is not needed, thereby further ensuring continuous reaction.

In another embodiment of the utility model, three or more dewatering modules may be selected in series depending on the reaction times of the different reactions.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further includes a second thermometer 11 disposed on the communication line 16, and the second thermometer 11 is used for measuring the temperature of the material in the communication line 16. In this way, the temperature of the material in the communication pipeline 16 can be obtained, when the measured value of the second thermometer 11 is lower than the temperature required by the reaction, that is, the condition required by the reaction is not met, the reaction in the reaction cavity may be incomplete, and the heating temperature of the heating structure 3 can be adjusted according to the measured value of the second thermometer 11, so that the reaction is further ensured to be complete.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further includes a second pressure gauge 12 and a second product discharge valve 1002 provided on the communication line 16, the second pressure gauge 12 being used to measure the pressure of the material in the communication line 16, the second product discharge valve 1002 being configured to be opened or closed to adjust the flow rate of the material in the communication line 16. In this way, the pressure value of the material in the communication line 16 can be obtained, and when the measured value of the second pressure gauge 12 is lower than the required pressure, the second product discharge valve 1002 is closed to raise the pressure of the material in the communication line 16.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further comprises: a cold trap 9; the liquid outlet pipeline 8, one end of the liquid outlet pipeline 8 is communicated with the accommodating cavity, the other end of the liquid outlet pipeline 8 is communicated with the cold trap 9, and the vacuumizing device 15 is communicated with the cold trap 9.

In the above technical solution, the on-line dehydration device for continuous reaction includes two liquid outlet pipelines 8, wherein one liquid outlet pipeline 8 is used for communicating the first dehydration component and the cold trap 9, and the other liquid outlet pipeline 8 is used for communicating the second dehydration component and the cold trap 9. The cold trap 9 is used for collecting the water vapor flowing out of the dehydration assembly and liquefying the water vapor, so that free water removed by the dehydration assembly is prevented from directly entering the vacuumizing device 15, the vacuumizing device 15 is protected, and the service life is prolonged; at the same time, the water vapor is collected by the cold trap 9, and the reaction state in the dehydration module can be observed at any time.

As shown in fig. 1, in an embodiment of the present utility model, the heating structure 3 includes a heating cartridge 31, and the heating cartridge 31 defines a heating chamber for storing a heating medium.

In the above technical solution, the heating cylinder 31 is provided with a heating medium feeding hole and a heating medium discharging hole, the heating medium discharging hole is located above the heating medium feeding hole in the longitudinal direction, the heating medium enters the heating cavity from the heating medium feeding hole and flows to the heating medium discharging hole, and in the flowing process, the heating medium can be fully contacted with the outer wall of the reaction device 2 to heat the reaction device 2 and the materials located in the reaction device, so as to provide the required energy for the reaction.

In one embodiment of the utility model, the heating medium is a thermal oil.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further includes a product discharge line 5, one end of the product discharge line 5 is communicated with the product discharge hole, and the other end of the product discharge line 5 is configured to be capable of communicating with the product collecting device.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further includes a first thermometer 13 disposed on the product discharge line 5, and the first thermometer 13 is used for measuring the temperature of the material in the product discharge line 5. In this way, the temperature of the material in the product discharging pipeline 5 can be obtained, when the measured value of the first thermometer 13 is lower than the temperature required by the reaction, that is, the condition required by the reaction is not met, the reaction in the reaction cavity may be incomplete, and the heating temperature of the heating structure 3 can be adjusted according to the measured value of the first thermometer 13, so that the reaction is further ensured to be complete.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further includes a first pressure gauge 14 provided on the product discharge line 5 and a first product discharge valve 2002, the first pressure gauge 14 for measuring the pressure of the material in the product discharge line 5, the first product discharge valve 2002 being configured to be opened or closed to adjust the flow rate of the material in the product discharge line 5. In this way, the pressure value of the material in the product take-off line 5 can be obtained, and when the measured value of the first pressure gauge 14 is lower than the desired pressure, the first product take-off valve 2002 is closed to increase the pressure of the material in the product take-off line 5.

As shown in fig. 1, in the embodiment of the present utility model, the on-line dehydration apparatus for continuous reaction further includes a raw material feed valve 1001 provided at the raw material feed hole, the raw material feed valve 1001 being for opening or closing the raw material feed hole. The raw material feed valve 1001 is disposed on the raw material feed line 4, and the on-line dehydration apparatus for continuous reaction further includes a first heating medium feed line 61, a first heating medium discharge line 71, a second heating medium feed line 62, and a second heating medium discharge line 72, wherein the first heating medium feed line 61 and the first heating medium discharge line 71 are respectively communicated with the heating medium feed hole of the first dehydration component and the heating medium discharge hole of the first dehydration component, and the second heating medium feed line 62 and the second heating medium discharge line 72 are respectively communicated with the heating medium feed hole of the second dehydration component and the heating medium discharge hole of the second dehydration component. The on-line dehydration apparatus for continuous reaction further includes a first heating medium feed valve 1003 provided on the first heating medium feed line 61, a first heating medium discharge valve 1004 provided on the first heating medium discharge line 71, a second heating medium feed valve 2003 provided on the second heating medium feed line 62, and a second heating medium discharge valve 2004 provided on the second heating medium discharge line 72.

With the above arrangement, in actual use, the raw material feed valve 1001 is first closed, the first heating medium feed valve 1003, the first heating medium discharge valve 1004, the second heating medium feed valve 2003, and the second heating medium discharge valve 2004 are opened, and the heating medium is fed through the first heating medium feed line 61 and the second heating medium feed line 62, so that the reaction apparatus 2 is heated to the temperature required for the reaction, and then the raw material feed valve 1001 is opened to allow the complete reaction of the materials.

As shown in fig. 1, in the embodiment of the present utility model, the reaction device 2 is provided at least partially on the outer periphery of the dehydration film tube 1, and the heating structure 3 is provided at least partially on the outer periphery of the reaction device 2.

In the above-described embodiments, the reaction device 2 is provided on the outer periphery of the partial dehydration membrane tube 1, and the heating structure 3 is provided on the outer periphery of the partial reaction device 2, that is, the lengths of the heating structure 3, the reaction device 2, and the dehydration membrane tube 1 are sequentially increased.

In another embodiment of the present utility model, the lengths of the heating structure 3, the reaction device 2 and the dehydration film pipe 1 may be the same, or the dehydration film pipe 1 may be disposed inside the reaction device 2.

In another embodiment of the utility model, a plurality of continuous reactions can be arranged in parallel by using on-line dehydration equipment or in the same dehydration component according to the reaction yield requirements of different reactions, so as to meet the requirement of yield improvement. Specifically, when a plurality of dehydration film pipes 1 are arranged in the same dehydration module, the dehydration module comprises a plurality of dehydration film pipes 1 connected in parallel, at least part of the structure of each dehydration film pipe 1 is positioned in a reaction cavity, and the accommodating cavity of each dehydration film pipe 1 is communicated with a vacuumizing device 15.

In one embodiment of the utility model, according to the actual requirement, the reactants can be circulated for a plurality of times after a single group of continuous reaction is used in the on-line dehydration equipment, so as to achieve the aim of completing the reaction.

In another embodiment of the utility model, the molecular sieve can be dehydrated in the continuous reaction on-line dehydration equipment, and the molecular sieve can be regenerated after the reaction is completed in the reaction process, so that the aim of completing the reaction is fulfilled.

As shown in fig. 1, in the embodiment of the present utility model, a first liquid outlet valve 3001 and a second liquid outlet valve 3002 are further respectively disposed on the two liquid outlet pipelines 8, the cold trap 9 is communicated with the vacuumizing device 15 through pipelines, and pipeline on-off valves 3003 are disposed on the pipelines.

The following describes the operation of the continuous dehydration for chemical industry according to the present utility model:

1. the first heating medium feed valve 1003, the first heating medium discharge valve 1004, the second heating medium feed valve 2003, and the second heating medium discharge valve 2004 are opened, and a heating medium of a certain temperature is introduced into the heating chamber through the first heating medium feed line 61 and the second heating medium feed line 62, so that the reaction chamber of the reaction apparatus 2 is heated to a certain temperature, and the energy required for the reaction is supplied.

2. The raw material feed valve 1001, the second product discharge valve 1002, the reactant feed valve 2001, and the first product discharge valve 2002 are opened, and after the raw materials are sufficiently mixed in the early stage, the raw materials enter the reaction chamber through the raw material feed line 4, and the chemical reaction is started.

3. The first liquid outlet valve 3001, the second liquid outlet valve 3002 and the pipeline on-off valve 3003 are opened, free water is generated in the chemical reaction process, and under the action of pressure difference, the free water passes through the dewatering film pipe 1 to reach the accommodating cavity and is collected by the cold trap 9 through the liquid outlet pipeline 8.

4. Reactants continuously enter the reaction cavity to react through the raw material feeding pipeline 4, water generated by the continuous removal reaction is used for the continuous reaction by the on-line dehydration equipment, the reaction is propelled to proceed, and the product is obtained through the first product discharging valve 2002 and the pipeline.

In one application case of the utility model, the continuous reaction is used for synthesizing ketal by using the on-line dehydration equipment, 1.2 eq acetone, 2 eq propanol and 0.01 eq p-toluenesulfonic acid are fully mixed, the reaction temperature is 100 ℃, the reaction pressure is 0.8 MPa, the raw materials react for 1h in the continuous reaction by using the on-line dehydration equipment to complete the reaction, the reaction time is reduced by 75 percent, the raw material conversion rate is 95 percent, the reaction yield is 92 percent, the dehydration speed in the reaction process is 16g/h, and 20 percent of acetone can be recovered for recovery and application after the post-treatment.

In another application case of the utility model, the continuous reaction is used for synthesizing ethyl acetate by using the on-line dehydration equipment, 1 eq acetic acid, 1.2 eq ethanol and 0.01 eq p-toluenesulfonic acid are fully mixed, the reaction temperature is 105 ℃, the reaction pressure is 0.8 MPa, the raw materials react for 0.75h in the continuous reaction on-line dehydration equipment to complete the reaction, compared with the reaction time of the prior art, the raw material conversion rate is reduced by 60%, the reaction yield is 94%, the dehydration speed in the reaction process is 16g/h, and the ethanol with 15% can be recovered for recycling after the post-treatment.

Compared with the prior art, the on-line dehydration equipment for continuous reaction can realize continuous reaction and continuous dehydration, has shorter reaction time and higher raw material conversion rate, and can recycle and reuse the organic solvent obtained after the product is fractionated.

From the above description, it can be seen that the above embodiments of the present utility model achieve the following technical effects: the heating structure can heat the reaction device and the materials in the reaction device, so as to provide a reaction environment for the materials in the reaction device; the vacuuming device can provide power for the free water generated by the reaction to pass through the dehydration film pipe. Raw materials enter the reaction device through the raw material feed hole, and react in the reaction device, the reaction generates required products and partial free water, under the action of the vacuumizing device, the dehydration membrane tube generates a negative pressure environment, and under the action of pressure difference, the free water in the reaction cavity can enter the accommodating cavity through the dehydration membrane tube, so that the dehydration effect is realized. The on-line dehydration equipment for continuous reaction integrates chemical reaction and dehydration of the dehydration membrane tube, has high integration level, can realize on-line continuous dehydration while reacting, and avoids the problem of long reaction dehydration time caused by dividing the reaction and the dehydration into two steps, thereby improving the reaction efficiency; because the raw material feeding hole is positioned below the product discharging hole, raw materials enter the reaction cavity from the raw material feeding hole, and can fully react in the process of moving the raw materials to the product discharging hole, namely, the reaction dehydration process can be completed through one-time feeding without multiple circulating reactions, so that continuous feeding and continuous reactions can be realized, and the reaction efficiency is improved; meanwhile, the problem that the product discharge hole is closed when feeding and the product is collected again after the reaction is completed, so that continuous reaction cannot be performed in the prior art is avoided.

The above is only a preferred embodiment of the present utility model, and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.

Claims (10)

1. An on-line dewatering apparatus for continuous reactions, characterized by comprising at least one dewatering module and a vacuum-pumping device (15) arranged on one side of at least one of said dewatering modules, each of said dewatering modules comprising:

the reaction device (2) is used for defining a reaction cavity, a raw material feeding hole and a product discharging hole which are communicated with the reaction cavity are formed in the reaction device (2), and the product discharging hole is positioned above the raw material feeding hole in the longitudinal direction;

a heating structure (3) provided on the outer periphery of the reaction device (2);

a dehydration membrane tube (1), at least part of the dehydration membrane tube (1) is positioned in the reaction cavity, and the dehydration membrane tube (1) defines a containing cavity communicated with the reaction cavity;

the vacuumizing device (15) is communicated with the accommodating cavity, and the vacuumizing device (15) is used for providing a negative pressure environment for the dehydration membrane tube (1) so that free water in the reaction cavity flows to the accommodating cavity under the action of pressure difference.

2. The on-line dehydration apparatus for continuous reaction according to claim 1, further comprising:

a cold trap (9);

the liquid outlet pipeline (8), one end of the liquid outlet pipeline (8) is communicated with the accommodating cavity, the other end of the liquid outlet pipeline (8) is communicated with the cold trap (9), and the vacuumizing device (15) is communicated with the cold trap (9).

3. The on-line dewatering equipment for continuous reactions according to claim 1, characterized in that the heating structure (3) comprises a heating cartridge (31), the heating cartridge (31) defining a heating chamber for storing a heating medium.

4. An in-line dewatering apparatus for continuous reactions as claimed in claim 3, characterized in that the heating cylinder (31) is provided with a heating medium feed hole and a heating medium discharge hole, the heating medium discharge hole being located above the heating medium feed hole in the longitudinal direction.

5. The on-line dewatering apparatus for continuous reactions according to any of claims 1 to 4 further comprising a product offtake piping (5), one end of the product offtake piping (5) being in communication with the product offtake hole, the other end of the product offtake piping (5) being configured to be capable of communicating with a product collection device.

6. The on-line dewatering equipment for continuous reactions according to claim 5, characterized in that it further comprises a first thermometer (13) arranged on the product take-off line (5), the first thermometer (13) being used for measuring the temperature of the material in the product take-off line (5); and/or the number of the groups of groups,

the on-line dehydration device for continuous reaction further comprises a first pressure gauge (14) and a first product discharge valve (2002) which are arranged on the product discharge pipeline (5), wherein the first pressure gauge (14) is used for measuring the pressure of materials in the product discharge pipeline (5), and the first product discharge valve (2002) is configured to be capable of being opened or closed so as to regulate the flow rate of the materials in the product discharge pipeline (5).

7. The online dewatering apparatus for continuous reaction according to any one of claims 1 to 4, further comprising a raw material feed valve (1001) provided at the raw material feed hole, the raw material feed valve (1001) being for opening or closing the raw material feed hole; and/or the number of the groups of groups,

the reaction device (2) is arranged at the periphery of at least part of the dewatering film pipe (1), and the heating structure (3) is arranged at the periphery of at least part of the reaction device (2).

8. The on-line dewatering apparatus for continuous reactions according to any of claims 1 to 4, characterized in that it comprises a plurality of said dewatering modules connected in series and at least one communication line (16), the product discharge hole of one of said dewatering modules being in communication with the raw material feed hole of the other dewatering module through said communication line (16) in adjacent two of said dewatering modules.

9. The on-line dewatering equipment for continuous reactions according to claim 8, characterized in that it further comprises a second thermometer (11) arranged on the communication line (16), the second thermometer (11) being used for measuring the temperature of the material in the communication line (16); and/or the number of the groups of groups,

the on-line dewatering device for continuous reaction further comprises a second pressure gauge (12) and a second product discharge valve (1002) which are arranged on the communication pipeline (16), wherein the second pressure gauge (12) is used for measuring the pressure of materials in the communication pipeline (16), and the second product discharge valve (1002) is configured to be capable of being opened or closed so as to regulate the flow rate of the materials in the communication pipeline (16).

10. The on-line dewatering equipment for continuous reactions according to any of claims 1 to 4, characterized in that the dewatering assembly comprises a plurality of parallel connected dewatering membrane tubes (1), at least part of the structure of each dewatering membrane tube (1) is located in the reaction chamber, and the receiving chamber of each dewatering membrane tube (1) is in communication with the evacuating device (15).