A production process for continuous photochlorination of ethylene carbonate

By using a continuous process and a multi-stage reactor in the photochlorination reaction of vinyl carbonate, combined with an ultraviolet lamp to promote the reaction and the recycling of the chloride liquid, the problems of uneven reactions and low chlorine utilization in the existing process are solved, and the production of high-purity chlorinated vinyl carbonate and the efficient utilization of chlorine are achieved.

CN115569620BActive Publication Date: 2025-03-21ZHEJIANG SORBO CHEM CO LTD
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Patent Information

Application Number
CN202211346894.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-10-31
Publication Date
2025-03-21
Estimated Expiration
2042-10-31

AI Technical Summary

Technical Problem

The existing photochlorination reaction process of vinyl carbonate has intermittent operation of single reactors, resulting in uneven heating, many by-products, low chlorine utilization, and thus low purity of chlorinated vinyl carbonate and excessive consumption of chlorine.

Method used

The continuous process is adopted, and the continuous reaction between vinyl carbonate and chlorine is achieved through a multi-stage reactor in series, and the photochlorination reaction is promoted by ultraviolet lamps, and the recycling and storage of the chloride liquid is realized through the pumping module.

Benefits of technology

The purity of chlorinated vinyl carbonate is improved, the consumption of chlorine is reduced, the reaction efficiency and product quality is enhanced, and the production cost is reduced through recycling.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of chemical industry, and particularly relates to a production process for continuous photochlorination reaction of ethylene carbonate, comprising the following steps: S1, adding a mixture of ethylene carbonate and an inert organic solvent prepared in advance according to metering into a primary reactor through an ethylene carbonate feeding pipe, and heating a jacket on the reactor; S2, after the temperature in the reactor rises to the reaction temperature, turning on an ultraviolet lamp in the primary reactor, and introducing chlorine into the primary reactor through a chlorine feeding pipe; S3, after the ethylene carbonate in the primary reactor reaches a certain amount, overflowing into a secondary reactor through a chlorinated liquid material pipe, and then turning on the ultraviolet lamp in the secondary reactor, during which the chlorine in the primary reactor enters into the secondary reactor through a chlorine residual gas pipe; and by adding a fourth-stage reactor, the purity of the reaction product chloroethylene carbonate is improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of chemical industry, and in particular relates to a production process for continuous photochlorination reaction of ethylene carbonate. Background Art

[0002] The chemical name of chloroethylene carbonate is 4-chloro-1,3-dioxolane-2-one; English name: Chloroethylen carbonate, UPAC name: 4-Chloro-1,3-dioxolan-2-one; CAS: 3967-54-2; molecular formula: C3H3ClO3; physical properties: colorless to light yellow liquid; density: 1.504 g / mL (25°C); boiling point: 121-123°C / 2.4 kPa; flash point: >113°C; refractive index (n20 / D): 1.454 (lit.). The structural formula is as follows

[0003]

[0004] Chloroethylene carbonate is primarily used as an electrolyte additive for lithium batteries and as an intermediate in organic synthesis, such as in the synthesis of vinylene carbonate and fluoroethylene carbonate. Due to the limited purity of commercially available chloroethylene carbonate, its scope and volume of use have remained largely unchanged. Therefore, the preparation of high-purity chloroethylene carbonate remains a pressing challenge for organic synthetic chemists and a key technical challenge awaiting resolution by relevant chemical companies.

[0005] Currently, there are two main industrial production methods for ethylene carbonate: 1) dissolving ethylene carbonate in an inert organic solvent such as carbon tetrachloride, introducing chlorine gas under ultraviolet light irradiation for chlorination, and then removing the solvent and performing vacuum distillation to obtain the ethylene carbonate product; 2) dissolving ethylene carbonate in an inert solvent such as carbon tetrachloride, then adding sulfonyl chloride and an initiator, heating under reflux, and after the reaction is completed, vacuum distillation is performed to obtain the ethylene carbonate product.

[0006] Above-mentioned two schemes, because the second kind uses the residual meeting of initiator, therefore can have a negative effect on the application of follow-up ethylene chlorocarbonate, and most of manufacturers use first scheme at present, i.e. ethylene carbonate and chlorine, react and generate ethylene chlorocarbonate under the catalytic action of ultraviolet light.Yet the reactor that ethylene carbonate photochlorination is used at present, is single still batch operation, ethylene carbonate is long in reactor residence time, causes being heated unevenly, by-product high yield rate is low, and the residence time of chlorine institute is shorter, exists to contact insufficient, consumes the problems such as large, utilization rate is low, and then causes ethylene chlorocarbonate purity to be no more than 80% in the reaction mixture, and the consumption of chlorine is more than 2 times of theoretical value. Summary of the Invention

[0007] Summary of the invention The object of the present invention is to provide a kind of production technology of continuous photochlorination reaction of ethylene carbonate, to solve the problem of raising in above-mentioned background technology.

[0008] To achieve the above object, the present invention provides the following technical solution: a production process for continuous photochlorination of ethylene carbonate, comprising the following steps:

[0009] S1. Adding a pre-measured mixture of ethylene carbonate and an inert organic solvent into a primary reactor through an ethylene carbonate feed pipe, and heating the jacket of the primary reactor;

[0010] S2. After the temperature in the reactor rises to the reaction temperature, the ultraviolet lamp in the first-stage reactor is turned on, and chlorine is introduced into the first-stage reactor through the chlorine feed pipe;

[0011] S3, after the ethylene carbonate in the primary reactor reaches a certain amount, it overflows into the secondary reactor through the chlorinated liquid material pipe, and then the ultraviolet lamp in the secondary reactor is turned on. During this process, the chlorine in the primary reactor enters the secondary reactor through the chlorine residual gas pipe;

[0012] S4, after the ethylene carbonate in the secondary reactor reaches a certain amount, it overflows into the tertiary reactor through the chlorinated liquid material pipe, and then the ultraviolet lamp in the tertiary reactor is turned on. During this process, the chlorine in the secondary reactor enters the tertiary reactor through the chlorine residual gas pipe;

[0013] S5, after the ethylene carbonate in the third-stage reactor reaches a certain amount, it overflows into the fourth-stage reactor through the chlorinated liquid material pipe, and then the ultraviolet lamp in the fourth-stage reactor is turned on. During this process, the chlorine in the third-stage reactor enters the fourth-stage reactor through the chlorine residual gas pipe;

[0014] S6. After the amount of ethylene carbonate in the fourth-stage reactor reaches a certain level, the chlorinated liquid containing ethylene carbonate is transported to the first-stage reactor through the chlorinated liquid material pipe and the pumping assembly connected to the chlorinated liquid material pipe to continue the reaction;

[0015] S7. After detecting that the ethylene carbonate in the fourth-stage reactor has completely reacted, the chlorinated liquid material pipe and the pumping assembly connected to the chlorinated liquid material pipe pump the chlorinated liquid into the chlorinated liquid storage tank;

[0016] S8. Adjust the feed flow rate in the ethylene carbonate feed pipe on the first-stage reactor and the air intake flow in the chlorine pipe to achieve continuous pumping of the reaction product chloroethylene carbonate in the fourth-stage reactor to the chlorinated liquid storage tank.

[0017] In the above technical solution, further, during step S6, when the chlorinated liquid overflowing from the fourth-stage reactor is transported to the first-stage reactor, the control valve in the ethylene carbonate feed pipe is disconnected.

[0018] In any of the above technical solutions, further, the chlorinated liquid material pipe on the four-stage reactor is divided into a discharge main pipe and a first branch pipe and a second branch pipe connected to the discharge main pipe, and the discharge main pipe is connected to the discharge port of the four-stage reactor;

[0019] The pumping assembly includes:

[0020] A circulating plunger pump, the feed end of which is connected to the first distribution pipe through a first connecting pipe, and the discharge end of which is connected to the second feed port on the first reactor through a circulating pipe;

[0021] and a receiving plunger pump; the feed end of which is connected to the second material distribution pipe through a second connecting pipe, and the discharge end of which is connected to the second feed port of the chlorinated liquid storage tank through a receiving pipe;

[0022] Among them, when the circulating plunger pump is working, the receiving plunger pump stops working;

[0023] When the circulating plunger pump stops working, the receiving plunger pump starts working.

[0024] In any of the above technical solutions, further, the circulation plunger pump and the receiving plunger pump have the same structure and both include:

[0025] a pump housing having a first piston chamber therein;

[0026] a first piston slidably disposed in the first piston chamber;

[0027] The pumping assembly also includes:

[0028] Motor;

[0029] A transmission part, used to connect the motor with the first piston of the circulation plunger pump and the first piston of the receiving plunger pump;

[0030] Among them, when the motor rotates, the transmission part is used to drive the circulation plunger pump to work and the receiving plunger pump stops working; when the motor rotates in the opposite direction, the transmission part is used to drive the receiving plunger pump to work and the circulation plunger pump stops working.

[0031] In any of the above technical solutions, further, the transmission unit includes:

[0032] Main transmission gear, the main transmission gear is arranged on the main shaft of the motor;

[0033] A first turntable is rotatably arranged on the side of the main transmission gear;

[0034] a first crank, one end of which is arranged at an eccentric position of the first rotary disk, and the other end of which is arranged on the first piston of the circulating plunger pump;

[0035] A first claw disc is fixed on the first rotating disc;

[0036] A first slave transmission gear is rotatably disposed between the first rotating disk and the first claw disk and meshes with the main transmission gear;

[0037] The second turntable is rotatably arranged on the side of the main transmission gear and is symmetrical with the first turntable;

[0038] A second crank, one end of which is arranged at an eccentric position of the second rotary disk, and the other end of which is arranged on the first piston of the receiving plunger pump;

[0039] A second claw plate is fixed on the second rotating plate;

[0040] A second slave transmission gear is rotatably disposed between the second rotating disk and the second claw disk and meshes with the main transmission gear;

[0041] The first slave transmission gear is provided with a first ratchet, the second slave transmission gear is provided with a second ratchet, and the direction of the tooth grooves on the first ratchet is opposite to the direction of the tooth grooves on the second ratchet. The claws on the first claw plate are provided in the tooth grooves of the first ratchet, and the claws on the second claw plate are provided in the tooth grooves of the second ratchet.

[0042] When the motor drives the main transmission gear to rotate forward, the first slave transmission gear and the second slave transmission gear rotate, the claw on the first claw plate slides in the tooth groove of the first ratchet wheel, the first claw plate does not rotate, the first rotary disk is in a stationary state, the claw on the second claw plate is limited in the tooth groove of the second ratchet wheel, the second claw plate rotates, and drives the second rotary disk to rotate;

[0043] When the motor drives the main transmission gear to rotate in the opposite direction, the first slave transmission gear and the second slave transmission gear rotate, the pawl on the first pawl plate is limited in the tooth groove of the first ratchet wheel, the first pawl plate rotates, and drives the first turntable to rotate, the pawl on the second pawl plate slides in the tooth groove of the second ratchet wheel, the second pawl plate does not rotate, and the second turntable is in a stationary state.

[0044] In any of the above technical solutions, further, the first material distribution pipe and the second material distribution pipe are respectively connected to a first storage part and a second storage part;

[0045] When the circulating plunger pump is working, the second storage part is used to quickly extract the chlorinated liquid that does not contain ethylene carbonate in the discharge main pipe and temporarily store it, and output it to the second connecting pipe when the receiving plunger pump is working;

[0046] When the receiving plunger pump is working, the first storage part is used to quickly extract the chlorinated liquid containing ethylene carbonate in the discharge main pipe and temporarily store it, and output it to the first connecting pipe when the circulating plunger pump is working.

[0047] In any of the above technical solutions, further, the first storage unit and the second storage unit have the same structure, and both include:

[0048] The storage chamber has an inlet and outlet port, and the inlet and outlet port is used to be connected to the first distribution pipe or the second distribution pipe;

[0049] The second piston is slidably disposed in the storage chamber.

[0050] a piston rod, one end of which is disposed on the second piston and the other end of which passes through and extends out of the storage chamber;

[0051] A working chamber is provided on the outer shell of the storage chamber, and is provided with a first port and a second port;

[0052] A third piston is slidably disposed in the working chamber and separates the first port from the second port; one end of the piston rod extending out of the storage chamber extends into the working chamber and is connected to the third piston;

[0053] Oil tank;

[0054] an oil pump, the oil inlet end of which is connected to the oil tank;

[0055] A three-position, four-way electromagnetic directional control valve, whose working oil port A is connected to the first port, the working oil port B is connected to the second port, the oil inlet P is connected to the oil outlet of the oil pump, and the oil return port T is connected to the oil tank;

[0056] And the control unit controls the status of the three-position four-way electromagnetic reversing valve and the oil pump according to the operating status of the circulating plunger pump and the receiving plunger pump.

[0057] In any of the above technical solutions, further, the control method of the control unit is specifically as follows:

[0058] At the moment when the working states of the circulating plunger pump and the receiving plunger pump are switched, when the circulating plunger pump is turned on and the receiving plunger pump is turned off, the control unit controls the three-position four-way solenoid reversing valve on the first storage part to connect its working oil port A with the oil inlet P and its working oil port B with the oil return port T, the oil pump is started, and the chlorinated liquid in the first storage chamber is sent into the first connecting pipe; and controls the three-position four-way solenoid reversing valve on the second storage part to connect its working oil port B with the oil inlet P and its working oil port A with the oil return port T, the oil pump is started, and the second storage part extracts the chlorinated liquid in the discharge main pipe and temporarily stores it; after the first storage part and the second storage part have completed half of their actions, the control unit controls the two three-position four-way solenoid reversing valves to disconnect and controls the two oil pumps to stop running;

[0059] At the moment when the working states of the circulating plunger pump and the receiving plunger pump are switched, when the circulating plunger pump is turned off and the receiving plunger pump is turned on, the control unit controls the three-position four-way solenoid reversing valve on the first storage part so that its working oil port B is connected to the oil inlet P, and the working oil port A is connected to the oil return port T, the oil pump is started, and the first storage part extracts the chlorinated liquid in the discharge main pipe and temporarily stores it; and controls the three-position four-way solenoid reversing valve on the second storage part so that its working oil port A is connected to the oil inlet P, and the working oil port B is connected to the oil return port T, the oil pump is started, and the chlorinated liquid in the second storage chamber is sent to the second connecting pipe; after the first storage part and the second storage part have completed half of the action, the control unit controls the two three-position four-way solenoid reversing valves to disconnect, and controls the two oil pumps to stop running.

[0060] Additional aspects and beneficial effects of the present invention will be described in detail with reference to the embodiments to make the effects apparent. BRIEF DESCRIPTION OF THE DRAWINGS

[0061] Figure 1 It is a structural schematic diagram of the present invention;

[0062] Figure 2 It is a structural schematic diagram of the chlorine distributor of the present invention;

[0063] Figure 3 It is a schematic diagram of the connection structure of the pumping assembly of the present invention;

[0064] Figure 4 It is a schematic structural diagram of the pumping assembly of the present invention;

[0065] Figure 5 It is a structural schematic diagram of the transmission part of the present invention;

[0066] Figure 6 Schematic diagram of the connection structure between the first storage unit and the second storage unit of the present invention;

[0067] Figure 7 It is a structural diagram of the first storage unit of the present invention;

[0068] The accompanying drawings are marked as follows: 10, ethylene carbonate feed pipe; 20, chlorine feed pipe; 30, chlorinated liquid material pipe; 31, discharge main pipe; 32, first distribution pipe; 33, second distribution pipe; 34, first connecting pipe; 35, second connecting pipe; 40, chlorine residual gas pipe; 100, first reactor; 110, ultraviolet lamp; 120, chlorine distributor; 200, second reactor; 300, third reactor; 400, fourth reactor; 500, pumping assembly; 510, circulating plunger pump; 511, pump housing; 512, first piston; 520, receiving plunger pump; 530, motor; 540, transmission unit; 541, main Transmission gear; 542, first turntable; 543, first crank; 544, first claw plate; 545, first slave transmission gear; 5451, first ratchet; 546, second turntable; 547, second crank; 548, second claw plate; 549, second slave transmission gear; 5491, second ratchet; 600, chlorine liquid storage tank; 700, exhaust gas absorption device; 800, first storage part; 810, storage chamber; 820, second piston; 830, piston rod; 840, working chamber; 850, third piston; 860, oil tank; 870, oil pump; 880, three-position four-way solenoid reversing valve; 900, second storage part. DETAILED DESCRIPTION

[0069] The following will be combined with the accompanying drawings in the embodiments of the present application to clearly describe the technical solutions in the embodiments of the present application. Obviously, the embodiments described are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field are within the scope of protection of this application.

[0070] In the description of this application, it should be noted that the terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the exemplary embodiments according to this application. For ease of description, the dimensions of the various parts shown in the drawings are not drawn according to the actual proportional relationship. Technologies, methods and equipment known to ordinary technicians in the relevant fields may not be discussed in detail, but where appropriate, technologies, methods and equipment should be considered as part of the authorization specification. In all examples shown and discussed here, any specific values ​​should be interpreted as merely exemplary and not as limitations. Therefore, other examples of the exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following figures, so once an item is defined in one figure, it does not need to be further discussed in subsequent figures.

[0071] It should be noted that the terms "first," "second," etc. in the specification and claims of this application are used to distinguish similar objects, and are not used to describe a specific order or sequence. It should be understood that the data used in this way are interchangeable where appropriate, so that the embodiments of this application can be implemented in an order other than those illustrated or described herein, and that the objects distinguished by "first," "second," etc. are generally of the same type, and do not limit the number of objects. For example, the first object can be one or more. In addition, "and / or" in the specification and claims represents at least one of the connected objects, and the character " / " generally indicates that the objects associated with each other are in an "or" relationship.

[0072] It should be noted that, in the description of this application, the directions or positional relationships indicated by directional terms such as "front, back, up, down, left, right", "horizontal, vertical, vertical, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing this application and simplifying the description. Unless otherwise specified, these directional terms do not indicate or imply that the device or element referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of this application; the directional terms "inside and outside" refer to the inside and outside relative to the outline of each component itself.

[0073] It should be noted that, in the present application, the terms "comprise", "include" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, an element defined by the statement "comprises a ..." does not exclude the presence of other identical elements in the process, method, article or device comprising the element. In addition, it should be pointed out that the scope of the methods and devices in the embodiments of the present application is not limited to performing functions in the order shown or discussed, and may also include performing functions in a substantially simultaneous manner or in the opposite order according to the functions involved. For example, the described method may be performed in an order different from that described, and various steps may also be added, omitted, or combined. In addition, the features described with reference to certain examples may be combined in other examples.

[0074] Example 1:

[0075] like Figure 1 As shown, this embodiment provides a production process for continuous photochlorination of ethylene carbonate, comprising the following steps:

[0076] S1. Adding a pre-measured mixture of ethylene carbonate and an inert organic solvent into the primary reactor 100 through the ethylene carbonate feed pipe 10, and heating the jacket of the primary reactor 100;

[0077] S2. After the temperature in the reactor rises to the reaction temperature, the ultraviolet lamp 110 in the primary reactor 100 is turned on, and chlorine gas is introduced into the primary reactor 100 through the chlorine feed pipe 20;

[0078] S3, after the ethylene carbonate in the primary reactor 100 reaches a certain amount, it overflows into the secondary reactor 200 through the chlorinated liquid material pipe 30, and then the ultraviolet lamp 110 in the secondary reactor 200 is turned on. During this process, the chlorine gas in the primary reactor 100 enters the secondary reactor 200 through the chlorine residual gas pipe 40;

[0079] S4. After the ethylene carbonate in the secondary reactor 200 reaches a certain amount, it overflows into the tertiary reactor 300 through the chlorinated liquid material pipe 30. Then, the ultraviolet lamp 110 in the tertiary reactor 300 is turned on. During this process, the chlorine gas in the secondary reactor 200 enters the tertiary reactor 300 through the chlorine gas residual pipe 40.

[0080] S5. After the ethylene carbonate in the tertiary reactor 300 reaches a certain amount, it overflows into the quaternary reactor 400 through the chlorinated liquid material pipe 30. Then, the ultraviolet lamp 110 in the quaternary reactor 400 is turned on. During this process, the chlorine gas in the tertiary reactor 300 enters the quaternary reactor 400 through the chlorine gas residual pipe 40.

[0081] S6. After the amount of ethylene carbonate in the fourth-stage reactor 400 reaches a certain level, the chlorinated liquid containing ethylene carbonate is transported to the first-stage reactor 100 through the chlorinated liquid material pipe 30 and the pumping assembly 500 connected to the chlorinated liquid material pipe 30 to continue the reaction;

[0082] S7. After detecting that the ethylene carbonate in the fourth-stage reactor 400 has completely reacted, the chlorinated liquid material pipe 30 and the pumping assembly 500 connected to the chlorinated liquid material pipe 30 pump the chlorinated liquid into the chlorinated liquid storage tank 600;

[0083] S8. Adjust the feed flow rate in the ethylene carbonate feed pipe 10 on the primary reactor 100 and the air intake flow in the chlorine pipe to achieve continuous pumping of the reaction product ethylene carbonate in the fourth reactor 400 to the chlorinated liquid storage tank 600.

[0084] In the technical scheme, for the photochlorination of ethylene carbonate, for improving yield, for this reason, be provided with 4 reactors side by side, and each reactor links to each other successively.In primary reactor 100, feed chlorine and ethylene carbonate by chlorine pipeline and ethylene carbonate pipeline, under the effect of the ultraviolet lamp 110 in primary reactor 100, carry out photochlorination then, because ethylene carbonate is to add in primary reactor 100 continuously, therefore the chlorated liquid in primary reactor 100 can increase gradually, after reaching the maximum amount that can be carried, can flow to secondary reactor 200 by overflow pipe, corresponding chlorine also can enter in secondary reactor 200, therefore also carry out photochlorination in secondary reactor 200, so, photochlorination also takes place in three-level reactor 300, level 4 reactor 400, thereby realize making full use of chlorine, and to greatest extent, improve the purity of the chloro-carbonated ethylene in chlorated liquid.

[0085] Regarding the setting of the reactor, it was found in the experiment that the benefit was the highest when the reactor was set to four levels, that is, the purity of ethylene chloride in the chlorinated liquid would be greatly improved. If additional reactors were added, the production cost would increase, which would be detrimental to controlling the production cost.

[0086] In this embodiment, during step S6 , when the chlorinated liquid overflowing from the fourth-stage reactor 400 is transported to the first-stage reactor 100 , the control valve in the ethylene carbonate feed pipe 10 is disconnected.

[0087] In the present technical solution, when the chlorinated liquid of ethylene carbonate that has not been completely reacted is recycled, in order to avoid an increase in the amount of ethylene carbonate entering the primary reactor 100, the ethylene carbonate feed pipe 10 needs to be disconnected. After the ethylene carbonate in the fourth-stage reactor 400 has been completely reacted and is no longer recycled, the ethylene carbonate feed pipe 10 is opened to achieve a continuous reaction.

[0088] Example 2:

[0089] This embodiment provides a production process for continuous photochlorination of ethylene carbonate, which, in addition to the technical solutions of the above embodiments, also has the following technical features.

[0090] like Figure 1 and Figure 2 As shown, in this embodiment, each reactor is further provided with a chlorine distributor 120, and chlorine is discharged from the chlorine distributor 120. The chlorine distributor 120 is disc-shaped and horizontally arranged on the lower side of the reactor cavity.

[0091] In this technical solution, by disposing a chlorine distributor 120 in each reactor, the chlorine can be evenly distributed in each reactor, thereby improving the reaction efficiency of chlorine and ethylene carbonate.

[0092] Example 3:

[0093] This embodiment provides a production process for continuous photochlorination of ethylene carbonate, which, in addition to the technical solutions of the above embodiments, also has the following technical features.

[0094] like Figure 1 As shown, in this embodiment, a tail gas absorption device 700 is further included, which is connected to the four-stage reactor 400.

[0095] In the present technical solution, in order to speed up the efficiency of the photochlorination reaction, generally speaking, an excessive amount of chlorine will be introduced. Therefore, the amount of chlorine in the four-stage reactor 400 will also be large. In order to avoid the chlorine being directly discharged from the four-stage reactor 400 and affecting the environment, an absorption device is also provided for it, and the excess chlorine is absorbed by the tail gas absorption device 700.

[0096] Example 4:

[0097] This embodiment provides a production process for continuous photochlorination of ethylene carbonate, which, in addition to the technical solutions of the above embodiments, also has the following technical features.

[0098] In this embodiment, the chlorinated liquid material pipe 30 on the four-stage reactor 400 is divided into a discharge main pipe 31 and a first branch pipe 32 and a second branch pipe 33 connected to the discharge main pipe 31. The discharge main pipe 31 is connected to the discharge port of the four-stage reactor 400.

[0099] The pumping assembly 500 includes:

[0100] A circulating plunger pump 510, whose feed end is connected to the first distribution pipe 32 via the first connecting pipe 34, and whose discharge end is connected to the second feed port on the first reactor via a circulating pipe;

[0101] and a receiving plunger pump 520; its feed end is connected to the second feed pipe 33 via a second connecting pipe 35, and its discharge end is connected to the second feed port of the chlorinated liquid storage tank 600 via a receiving pipe;

[0102] When the circulating plunger pump 510 is working, the receiving plunger pump 520 stops working;

[0103] When the circulation plunger pump 510 stops working, the receiving plunger pump 520 starts working.

[0104] In this technical solution, the pumping assembly 500 includes a circulating plunger pump 510 and a receiving plunger pump 520. With the cooperation of the two plunger pumps, the chlorinated liquid of ethylene carbonate that has completely reacted can be sent into the liquid storage tank, and the chlorinated liquid of ethylene carbonate that has not completely reacted can be sent into the first reactor. The practical effect is good, and there will be no interference during transportation.

[0105] In this embodiment, the circulation plunger pump 510 and the receiving plunger pump 520 are optimized to have the same structure and both include:

[0106] a pump housing 511 having a first piston 512 chamber therein;

[0107] a first piston 512 slidably disposed in the first piston 512 chamber;

[0108] The pumping assembly 500 also includes:

[0109] Motor 530;

[0110] The transmission part 540 is used to connect the motor 530 with the first piston 512 of the circulation plunger pump 510 and the first piston 512 of the receiving plunger pump 520;

[0111] Among them, when the motor 530 rotates, the transmission part 540 is used to drive the circulation plunger pump 510 to work and the material receiving plunger pump 520 stops working; when the motor 530 rotates in the opposite direction, the transmission part 540 is used to drive the material receiving plunger pump 520 to work and the circulation plunger pump 510 stops working.

[0112] In this technical solution, the pumping assembly 500 includes a circulating plunger pump 510 and a receiving plunger pump 520. With the cooperation of the two plunger pumps, the chlorinated liquid of ethylene carbonate that has completely reacted can be sent into the liquid storage tank, and the chlorinated liquid of ethylene carbonate that has not completely reacted can be sent into the first reactor. The practical effect is good, and there will be no interference during transportation.

[0113] Example 5:

[0114] This embodiment provides a production process for continuous photochlorination of ethylene carbonate, which, in addition to the technical solutions of the above embodiments, also has the following technical features.

[0115] In this embodiment, the transmission unit 540 includes:

[0116] A main transmission gear 541 is provided on the main shaft of the motor 530;

[0117] A first rotating disk 542 is rotatably disposed on the side of the main transmission gear 541;

[0118] A first crank 543 , one end of which is disposed at an eccentric position of the first rotary disk 542 , and the other end of which is disposed on the first piston 512 of the circulating plunger pump 510 ;

[0119] The first claw plate 544 is fixed on the first rotating plate 542;

[0120] The first slave transmission gear 545 is rotatably disposed between the first rotating disk 542 and the first claw disk 544 and meshes with the main transmission gear 541;

[0121] The second rotating disk 546 is rotatably disposed on the side of the main transmission gear 541 and is symmetrical with the first rotating disk 542;

[0122] A second crank 547 , one end of which is disposed at an eccentric position of the second rotary disk 546 , and the other end of which is disposed on the first piston 512 of the receiving plunger pump 520 ;

[0123] The second claw plate 548 is fixed on the second rotating plate 546;

[0124] The second slave transmission gear 549 is rotatably disposed between the second rotating disk 546 and the second claw disk 548 and meshes with the main transmission gear 541;

[0125] Among them, a first ratchet 5451 is provided on the first slave transmission gear, and a second ratchet 5491 is provided on the second slave transmission gear, and the direction of the tooth groove on the first ratchet 5451 is opposite to the direction of the tooth groove on the second ratchet 5491, the claw on the first claw plate 544 is provided in the tooth groove of the first ratchet 5451, and the claw on the second claw plate 548 is provided in the tooth groove of the second ratchet 5491.

[0126] In the present technical solution, specifically, after the detection unit in the last reactor does not detect that there is still ethylene carbonate in the chlorinated liquid above the reactor, the chlorinated liquid discharged from the discharge main pipe 31 needs to be discharged from the receiving plunger pump 520 to the liquid storage tank. At this time, the motor 530 is controlled to rotate forward. When the motor 530 drives the main transmission gear 541 to rotate forward, the first slave transmission gear 545 and the second slave transmission gear 549 rotate, and the claw on the first claw plate 544 slides in the tooth groove of the first ratchet 5451. The first claw plate 544 does not rotate, the first turntable 542 is in a stationary state, the claws on the second claw plate 548 are limited in the tooth grooves of the second ratchet 5491, the second claw plate 548 rotates, and drives the second turntable 546 to rotate; thereby causing the second crank 547 to swing, causing the piston in the receiving plunger pump 520 to reciprocate, and the chlorinated liquid flowing out of the discharge main pipe 31 flows to the second distribution pipe 33, flows into the receiving plunger pump 520, and is discharged, and finally transported to the liquid storage tank through the receiving pipe.

[0127] After the detection unit in the last reactor detects that there is still ethylene carbonate in the chlorinated liquid above the reactor, the chlorinated liquid discharged from the discharge main pipe 31 needs to be discharged from the circulation plunger pump 510 to the first reactor. At this time, the control motor 530 rotates in the reverse direction. When the motor 530 drives the main transmission gear 541 to rotate in the reverse direction, the first slave transmission gear 545 and the second slave transmission gear 549 rotate, and the claw on the first claw plate 544 is limited in the tooth groove of the first ratchet 5451. The first claw plate 544 is in the tooth groove of the first ratchet 5451. The claw plate 544 rotates and drives the first turntable 542 to rotate. The claws on the second claw plate 548 slide in the tooth grooves of the second ratchet 5491. The second claw plate 548 does not rotate, and the second turntable 546 is in a stationary state; thereby, the first crank 543 swings, causing the piston in the circulating plunger pump 510 to reciprocate, and the chlorinated liquid flowing out of the discharge main pipe 31 flows to the first distribution pipe 32, flows into the circulating plunger pump 510, and is discharged, and finally transported to the first reactor through the circulation pipe.

[0128] Example 6:

[0129] This embodiment provides a production process for continuous photochlorination of ethylene carbonate, which, in addition to the technical solutions of the above embodiments, also has the following technical features.

[0130] In this embodiment, the first material distribution pipe 32 and the second material distribution pipe 33 are further connected to a first storage part 800 and a second storage part 900 respectively;

[0131] When the circulating plunger pump 510 is working, the second storage part 900 is used to quickly extract the chlorinated liquid that does not contain ethylene carbonate in the discharge main pipe 31 and temporarily store it, and output it to the second connecting pipe 35 when the receiving plunger pump 520 is working;

[0132] When the receiving plunger pump 520 is working, the first storage part 800 is used to quickly extract the chlorinated liquid containing ethylene carbonate in the discharge main pipe 31 and temporarily store it, and output it to the first connecting pipe 34 when the circulation plunger pump 510 is working.

[0133] In the present technical solution, whether the ethylene carbonate in the chlorinated liquid in the fourth-stage reactor 400 has reacted completely is determined by whether the circulating plunger pump 510 or the receiving plunger pump 520 is in operation. Specifically, a detection unit capable of detecting the content of ethylene carbonate is provided above the fourth-stage reactor 400, and the determination is made by the detection unit. Of course, due to the volatility of the reaction, the ethylene carbonate in the chlorinated liquid in the fourth-stage reactor 400 is often in a state of complete reaction or incomplete reaction, which causes the circulating plunger pump 510 and the receiving plunger pump 520 to constantly switch. For the discharge main pipe 31, the first branch pipe, and the second branch pipe, when the circulating plunger pump 510 and the receiving plunger pump 520 are switched, the chlorinated liquid inside them will not be immediately fed into the circulation pipe or the receiving pipe.

[0134] Therefore, when the detection component in the four-stage reactor 400 detects ethylene carbonate, the motor 530 will change from forward to reverse, that is, the receiving plunger pump 520 will change from working to non-working, and the circulating plunger pump 510 will change from non-working to working. At this time, the chlorinated liquid in the discharge main pipe 31 and the second branch pipe does not contain ethylene carbonate; on the contrary, after the detection component in the four-stage reactor 400 does not detect ethylene carbonate, the chlorinated liquid in the discharge main pipe 31 and the second branch pipe does contain ethylene carbonate. In order to prevent the chlorinated liquid containing ethylene carbonate from remaining in the discharge main pipe 31, a first storage part 800 is provided for this purpose. The first storage part 800 is used to absorb the chlorinated liquid containing ethylene carbonate remaining in the discharge main pipe 31, and the second storage part 900 is provided to absorb the chlorinated liquid without ethylene carbonate remaining in the discharge main pipe 31, thereby improving the purity of the chloroethylene carbonate in the liquid storage tank.

[0135] Example 7:

[0136] This embodiment provides a production process for continuous photochlorination of ethylene carbonate, which, in addition to the technical solutions of the above embodiments, also has the following technical features.

[0137] In this embodiment, the first storage unit 800 and the second storage unit 900 have the same structure, and both include:

[0138] The storage chamber 810 has an inlet and outlet port, which is used to connect to the first distribution pipe 32 or the second distribution pipe 33;

[0139] The second piston 820 is slidably disposed in the storage chamber 810.

[0140] A piston rod 830, one end of which is disposed on the second piston 820, and the other end of which passes through and extends out of the storage chamber 810;

[0141] The working chamber 840 is provided on the outer shell of the storage chamber 810 and is provided with a first port and a second port;

[0142] The third piston 850 is slidably disposed in the working chamber 840 and separates the first port from the second port; one end of the piston rod 830 extending from the storage chamber 810 extends into the working chamber 840 and is connected to the third piston 850;

[0143] Oil tank 860;

[0144] an oil pump 870 , the oil inlet of which is connected to the oil tank 860 ;

[0145] A three-position, four-way electromagnetic directional control valve, whose working oil port A is connected to the first port, the working oil port B is connected to the second port, the oil inlet P is connected to the oil outlet of the oil pump 870, and the oil return port T is connected to the oil tank 860;

[0146] The control unit controls the status of the three-position four-way electromagnetic reversing valve 880 and the oil pump 870 according to the operating status of the circulation plunger pump 510 and the receiving plunger pump 520.

[0147] In this technical solution, the control method of the control unit is as follows:

[0148] At the moment when the working states of the circulating plunger pump 510 and the receiving plunger pump 520 are switched, when the circulating plunger pump 510 is turned on and the receiving plunger pump 520 is turned off, the control unit controls the three-position four-way solenoid reversing valve 880 on the first storage section 800, so that its working oil port A is connected to the oil inlet P, and the working oil port B is connected to the oil return port T, the oil pump 870 is started, and the chlorinated liquid in the first storage chamber 810 is sent to the first connecting pipe 34; and controls the three-position four-way solenoid reversing valve 880 on the second storage section 900, so that its working oil port B is connected to the oil inlet P, and the working oil port A is connected to the oil return port T, the oil pump 870 is started, and the second storage section 900 extracts the chlorinated liquid in the discharge main pipe 31 and temporarily stores it; after the first storage section 800 and the second storage section 900 have completed half of the action, the control unit controls the two three-position four-way solenoid reversing valves 880 to be disconnected, and controls the two oil pumps 870 to stop running;

[0149] At the moment when the working states of the circulating plunger pump 510 and the receiving plunger pump 520 are switched, when the circulating plunger pump 510 is turned off and the receiving plunger pump 520 is turned on, the control unit controls the three-position four-way solenoid reversing valve 880 on the first storage section 800 to connect its working oil port B with the oil inlet P and its working oil port A with the oil return port T, and the oil pump 870 is started. The first storage section 800 extracts the chlorinated liquid from the discharge main pipe 31 and temporarily stores it. The control unit also controls the three-position four-way solenoid reversing valve 880 on the second storage section 900 to connect its working oil port A with the oil inlet P and its working oil port B with the oil return port T, and the oil pump 870 is started. The chlorinated liquid in the second storage chamber 810 is sent to the second connecting pipe 35. After both the first storage section 800 and the second storage section 900 complete half of their operations, the control unit controls the two three-position four-way solenoid reversing valves 880 to disconnect and the two oil pumps 870 to stop operating.

[0150] The embodiments of the present application are described above in conjunction with the accompanying drawings. Unless there is a conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application is not limited to the above-mentioned specific implementation methods. The above-mentioned specific implementation methods are merely illustrative and not restrictive. Under the guidance of this application, ordinary technicians in this field can also make many forms without departing from the purpose of this application and the scope of protection of the claims, all of which are within the protection of this application.

Claims

1. A production process for the photochlorination of ethylene carbonate, characterized in that: The following steps are involved: S1, adding a mixture of ethylene carbonate and an inert organic solvent prepared in advance according to metering into a primary reaction kettle (100) through an ethylene carbonate feeding pipe (10), and heating the jacket on the primary reaction kettle (100); S2. After the temperature in the reactor rises to the reaction temperature, the ultraviolet lamp (110) in the primary reactor (100) is turned on, and chlorine gas is introduced into the primary reactor (100) through the chlorine gas feed pipe (20); S3, when the amount of ethylene carbonate in the primary reactor (100) reaches a certain amount, the ethylene carbonate overflows into the secondary reactor (200) through the chlorinated liquid material pipe (30), and then the ultraviolet lamp (110) in the secondary reactor (200) is turned on. During this process, the chlorine gas in the primary reactor (100) enters the secondary reactor (200) through the chlorine gas residual pipe (40); S4, when the amount of ethylene carbonate in the secondary reactor (200) reaches a certain amount, the ethylene carbonate overflows into the tertiary reactor (300) through the chlorinated liquid material pipe (30), and then the ultraviolet lamp (110) in the tertiary reactor (300) is turned on. During this process, the chlorine gas in the secondary reactor (200) enters the tertiary reactor (300) through the chlorine gas residual pipe (40); S5, when the ethylene carbonate in the tertiary reactor (300) reaches a certain amount, the ethylene carbonate overflows into the quaternary reactor (400) through the chlorinated liquid material pipe (30), and then the ultraviolet lamp (110) in the quaternary reactor (400) is turned on. During this process, the chlorine gas in the tertiary reactor (300) enters the quaternary reactor (400) through the chlorine gas residual pipe (40); S6, after the amount of ethylene carbonate in the fourth-stage reactor (400) reaches a certain amount, the chlorinated liquid containing ethylene carbonate is transported to the first-stage reactor (100) through the chlorinated liquid material pipe (30) and a pumping assembly (500) connected to the chlorinated liquid material pipe (30) to continue the reaction; S7, after detecting that the ethylene carbonate in the fourth-stage reactor (400) is completely reacted, the chlorinated liquid material pipe (30) and the pumping assembly (500) connected to the chlorinated liquid material pipe (30) pump the chlorinated liquid into the chlorinated liquid storage tank (600); S8, adjusting the feed flow rate in the ethylene carbonate feed pipe (10) on the primary reactor (100) and the air intake flow rate in the chlorine pipe to achieve continuous pumping of the reaction product ethylene carbonate in the fourth reactor (400) to the chlorinated liquid storage tank (600); The chlorinated liquid material pipe (30) on the four-stage reactor (400) is divided into a discharge main pipe (31) and a first material distribution pipe (32) and a second material distribution pipe (33) connected to the discharge main pipe (31); the discharge main pipe (31) is connected to the discharge port of the four-stage reactor (400); The pumping assembly (500) comprises: A circulating plunger pump (510), whose feeding end is connected to the first material distribution pipe (32) through a first connecting pipe (34), and whose discharging end is connected to the second feeding port on the first reactor through a circulating pipe; and a receiving plunger pump (520); the feeding end of which is connected to the second material distribution pipe (33) via a second connecting pipe (35), and the discharging end of which is connected to the second feeding port of the chlorinated liquid storage tank (600) via a receiving pipe; Wherein, when the circulating plunger pump (510) is working, the receiving plunger pump (520) stops working; When the circulating plunger pump (510) stops working, the receiving plunger pump (520) starts working; The first material distribution pipe (32) and the second material distribution pipe (33) are respectively connected to a first storage part (800) and a second storage part (900); Wherein, when the circulating plunger pump (510) is working, the second storage part (900) is used to quickly extract the chlorinated liquid that does not contain ethylene carbonate in the discharge main pipe (31), temporarily store it, and output it to the second connecting pipe (35) when the receiving plunger pump (520) is working; When the receiving plunger pump (520) is working, the first storage part (800) is used to quickly extract the chlorinated liquid containing ethylene carbonate in the discharge main pipe (31), temporarily store it, and output it to the first connecting pipe (34) when the circulating plunger pump (510) is working.

2. The production process of a continuous photochlorination reaction of ethylene carbonate according to claim 1, characterized in that: The first storage unit (800) and the second storage unit (900) have the same structure, and both include: A storage chamber (810) having an inlet and outlet port, the inlet and outlet port being used to be connected to the first distribution pipe (32) or the second distribution pipe (33); The second piston (820) is slidably disposed in the chamber of the storage chamber (810). A piston rod (830), one end of which is disposed on the second piston (820), and the other end of which penetrates and extends out of the storage chamber (810); A working chamber (840) is disposed on the outer shell of the storage chamber (810), and a first port and a second port are provided on the working chamber (840); The third piston (850) is slidably disposed in the working chamber (840) and separates the first port from the second port; one end of the piston rod (830) extending out of the storage chamber (810) extends into the working chamber (840) and is connected to the third piston (850); Oil tank (860); An oil pump (870), whose oil inlet end is connected to the oil tank (860); A three-position four-way electromagnetic reversing valve, wherein the working oil port A is connected to the first port, the working oil port B is connected to the second port, the oil inlet P is connected to the oil outlet of the oil pump (870), and the oil return port T is connected to the oil tank (860); And a control unit controls the states of a three-position four-way electromagnetic reversing valve (880) and an oil pump (870) according to the operating states of a circulating plunger pump (510) and a receiving plunger pump (520).

3. The production process of a continuous photochlorination reaction of ethylene carbonate according to claim 1, characterized in that: During step S6, when the chlorinated liquid overflowing from the fourth-stage reactor (400) is transported to the first-stage reactor (100), the control valve in the ethylene carbonate feed pipe (10) is disconnected.

4. The production process of a continuous photochlorination reaction of ethylene carbonate according to claim 1, characterized in that: The circulation plunger pump (510) and the receiving plunger pump (520) have the same structure and both include: A pump housing (511) having a first piston (512) chamber therein; A first piston (512) is slidably disposed in a first piston (512) chamber; The pumping assembly (500) further comprises: Motor (530); A transmission part (540) is used to connect the motor (530) with the first piston (512) of the circulation plunger pump (510) and the first piston (512) of the receiving plunger pump (520); When the motor (530) rotates, the transmission part (540) is used to drive the circulating plunger pump (510) to work, and the receiving plunger pump (520) stops working; when the motor (530) rotates in the opposite direction, the transmission part (540) is used to drive the receiving plunger pump (520) to work, and the circulating plunger pump (510) stops working.

5. The production process of a continuous photochlorination reaction of ethylene carbonate according to claim 4, characterized in that: The transmission part (540) comprises: A main transmission gear (541), wherein the main transmission gear (541) is arranged on a main shaft of the motor (530); A first rotating disk (542) is rotatably disposed on the side of the main transmission gear (541); A first crank (543), one end of which is arranged at an eccentric position of the first rotating disk (542), and the other end of which is arranged on the first piston (512) of the circulating plunger pump (510); A first claw plate (544) fixed on the first rotating plate (542); A first slave transmission gear (545) is rotatably disposed between the first rotating disk (542) and the first claw disk (544), and is meshed with the main transmission gear (541); A second rotating disk (546) is rotatably disposed on the side of the main transmission gear (541) and is symmetrical with the first rotating disk (542); A second crank (547), one end of which is disposed at an eccentric position of the second rotating disk (546), and the other end of which is disposed on the first piston (512) of the receiving plunger pump (520); A second claw plate (548) fixed on the second rotating plate (546); A second slave transmission gear (549) is rotatably disposed between the second rotating disk (546) and the second claw disk (548), and is meshed with the main transmission gear (541); The first slave transmission gear (545) is provided with a first ratchet (5451), the second slave transmission gear (549) is provided with a second ratchet (5491), and the tooth groove direction on the first ratchet (5451) is opposite to the tooth groove direction on the second ratchet (5491), the claw on the first claw plate (544) is provided in the tooth groove of the first ratchet (5451), and the claw on the second claw plate (548) is provided in the tooth groove of the second ratchet (5491); When the motor (530) drives the main transmission gear (541) to rotate in the forward direction, the first slave transmission gear (545) and the second slave transmission gear (549) rotate, the claws on the first claw plate (544) slide in the tooth grooves of the first ratchet (5451), the first claw plate (544) does not rotate, the first rotating disk (542) is in a stationary state, the claws on the second claw plate (548) are limited in the tooth grooves of the second ratchet (5491), the second claw plate (548) rotates, and drives the second rotating disk (546) to rotate; When the motor (530) drives the main transmission gear (541) to rotate in the opposite direction, the first slave transmission gear (545) and the second slave transmission gear (549) rotate, the claw on the first claw plate (544) is limited in the tooth groove of the first ratchet (5451), the first claw plate (544) rotates, and drives the first rotating disk (542) to rotate, the claw on the second claw plate (548) slides in the tooth groove of the second ratchet (5491), the second claw plate (548) does not rotate, and the second rotating disk (546) is in a stationary state.

6. The production process of a continuous photochlorination reaction of ethylene carbonate according to claim 2, characterized in that: The control method of the control unit is specifically as follows: At the moment when the working states of the circulating plunger pump (510) and the receiving plunger pump (520) are switched, when the circulating plunger pump (510) is turned on and the receiving plunger pump (520) is turned off, the control unit controls the three-position four-way electromagnetic reversing valve (880) on the first storage part (800) so that its working oil port A is connected to the oil inlet port P, and the working oil port B is connected to the oil return port T, and the oil pump (870) is started, and the chlorinated liquid in the first storage chamber (810) is sent to the first connecting pipe (34); and the second storage chamber (800) is controlled to be connected to the second storage chamber (800). The three-position four-way electromagnetic reversing valve (880) on the first storage part (900) is turned on to connect its working oil port B with the oil inlet port P, and the working oil port A with the oil return port T, and the oil pump (870) is started, and the second storage part (900) extracts the chlorinated liquid in the discharge main pipe (31) and temporarily stores it; after the first storage part (800) and the second storage part (900) have completed half of the action, the control unit controls the two three-position four-way electromagnetic reversing valves (880) to be disconnected, and controls the two oil pumps (870) to stop running; At the moment when the working states of the circulating plunger pump (510) and the receiving plunger pump (520) are switched, when the circulating plunger pump (510) is turned off and the receiving plunger pump (520) is turned on, the control unit controls the three-position four-way electromagnetic reversing valve (880) on the first storage unit (800) so that its working oil port B is connected to the oil inlet port P, and the working oil port A is connected to the oil return port T, the oil pump (870) is started, and the first storage unit (800) extracts the chlorinated liquid in the discharge main pipe (31) and temporarily stores it; and The three-position four-way electromagnetic reversing valve (880) on the second storage part (900) is controlled so that its working oil port A is connected to the oil inlet port P, and the working oil port B is connected to the oil return port T, the oil pump (870) is started, and the chlorinated liquid in the second storage chamber (810) is sent to the second connecting pipe (35); after the first storage part (800) and the second storage part (900) have completed half of the action, the control unit controls the two three-position four-way electromagnetic reversing valves (880) to be disconnected, and controls the two oil pumps (870) to stop running.

Citation Information

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