Purification device and purification process for production of electronic-grade acetic ether

Abstract

The invention relates to the technical field of ethyl acetate purification, in particular to a purification device and process for electronic grade ethyl acetate production, the device comprises a treatment kettle, a driving rod is movably arranged in the treatment kettle, a plurality of fan-shaped pieces are movably arranged at the bottom end of the driving rod, and a plurality of through holes capable of being opened and closed are formed in the fan-shaped pieces; the floating ring is assembled to be used in the following two states: in the first state, the multiple fanning strips are in the vertical state, the through holes in the fanning strips are closed, the floating ring sinks to the bottom of the treatment kettle, and the driving rod drives the fanning strips to rotate and reciprocate in the vertical direction. The driving rod drives the fanning strips to rotate so as to mix mixed liquid in the treatment kettle, the floating ring determines layering of acetic ether and an aqueous solution, the floating ring is matched with the fanning strips to separate the interior of the treatment kettle, the aqueous solution on the lower portion is discharged, and only the acetic ether on the upper portion is reserved.

Description

Technical Field

[0001] This invention relates to the field of ethyl acetate purification technology, and more specifically to a purification apparatus and process for the production of electronic-grade ethyl acetate. Background Technology

[0002] Industrially, ethyl acetate is mostly produced by the direct esterification of acetic acid and ethanol, with sulfuric acid as a catalyst. Ethyl acetate produced in this way will have residual acidic substances and needs to be purified before it can be used.

[0003] Chinese patent publication number CN112500292B discloses a method for purifying ethyl acetate.

[0004] In the prior art, including the aforementioned patent, the purification of ethyl acetate generally involves first adding a saturated sodium carbonate solution to the ethyl acetate to wash away residual acidic substances. After standing and allowing the layers to separate, the lower aqueous solution is drained, retaining only the upper ethyl acetate. Next, a saturated brine solution is added to the ethyl acetate to remove residual sodium carbonate. The layers are then allowed to separate again, the lower aqueous solution is drained, and only the upper ethyl acetate is retained. A saturated calcium chloride solution is then added to the ethyl acetate to dissolve residual ethanol and further remove water. The layers are then allowed to separate again, the lower aqueous solution is drained, and only the upper ethyl acetate is retained. Finally, the mixture is washed, dried, and distilled. This process requires multiple layers and draining operations, often requiring experienced personnel to control the amount of lower aqueous solution drained, making it difficult to control the purity and yield of the purified ethyl acetate. Summary of the Invention

[0005] The purpose of this invention is to provide a purification apparatus and process for the production of electronic-grade ethyl acetate, in order to solve the above-mentioned problems.

[0006] To achieve the above objectives, the present invention provides a purification apparatus for the production of electronic-grade ethyl acetate, comprising a processing vessel, wherein the processing vessel contains: A drive rod, the bottom end of which is movably provided with multiple sector-shaped plates, and the sector-shaped plates are provided with multiple openable and closable through holes; A floating ring, which is assembled for use in the following two states: In the first state, the multiple fan-shaped plates are in a vertical state with their through holes closed, the floating ring sinks to the bottom of the processing vessel, and the driving rod drives the fan-shaped plates to rotate and reciprocate in the vertical direction; In the second state, the floating ring floats at the interface between the aqueous solution and ethyl acetate, and multiple fan-shaped plates are combined to form a septum with its through holes open. The septum moves down and couples with the floating ring to close its through holes.

[0007] Preferably, the floating ring is provided with an air bladder, and the air pressure inside the processing vessel is increased to cause the air bladder to contract.

[0008] Preferably, the processing vessel has a U-shaped air passage with both ends connected to the airbag and the processing vessel, respectively.

[0009] Preferably, a first piston and a second piston are fixedly connected in the parallel portion of the air passage.

[0010] Preferably, a plurality of sliding plates are slidably disposed in the floating ring, and the spacer is coupled to the floating ring so that the sliding plates move outward and push against the sealing ring.

[0011] Preferably, a slide bar is slidably disposed in the drive rod, and the slide bar moves relative to the drive rod to cause the sector plate to move relative to the drive rod.

[0012] Preferably, the sector-shaped plate is provided with a locking block embedded in the drive rod, and the bottom of the slide rod is provided with a top block for pushing the locking block.

[0013] Preferably, the top block is provided with a rack, and the top block is moved to a predetermined position to couple the rack with the sector plate.

[0014] Preferably, the sector-shaped piece is movably provided with a sealing plate having multiple through holes thereon, and the sealing plate moves relative to the sector-shaped piece to open and close the through holes on the sector-shaped piece.

[0015] A purification process for producing electronic-grade ethyl acetate, based on the purification apparatus for producing electronic-grade ethyl acetate in the above-mentioned scheme, further includes the following steps: S1. Ethyl acetate is injected into the treatment vessel, and then saturated sodium carbonate solution is injected into the treatment vessel. At this time, the floating ring and the fan-shaped plate are in the first state, and the drive rod drives the fan-shaped plate to stir the mixed liquid. S2. The mixed liquid is allowed to stand and separate into layers. The floating ring and fan-shaped plate switch to the second state, and the septum moves down while the ethyl acetate moves up to the septum. S3. The septum is coupled to the floating ring to separate ethyl acetate and the aqueous solution, and then the aqueous solution below is drained. S4. Switch the floating ring and sector plate to the first state, add saturated brine and repeat the above steps, then add saturated calcium chloride solution and repeat the above steps, and finally wash with water, dry and distill to obtain pure ethyl acetate.

[0016] In the above technical solution, the purification device and purification process for producing electronic-grade ethyl acetate provided by the present invention have the following beneficial effects: During operation, the floating ring and the fan-shaped plate are in the first state. Ethyl acetate is injected into the processing vessel through the feed pipe, and then saturated sodium carbonate solution is injected into the processing vessel through another feed pipe. The motor operates, outputting positive and negative torques to drive the gear to rotate forward and backward. The gear, through a meshing drive ring and a synchronizing block, drives the drive rod to rotate. The drive rod drives the fan-shaped plate to rotate and reciprocate vertically along the threaded through-hole on the movable block. The fan-shaped plate stirs the mixture in the processing vessel, causing the saturated sodium carbonate solution to react with the residual acidic substances in the ethyl acetate. After stirring for a period of time, the operation stops. Multiple fan-shaped plates move relative to the drive rod to form a partition. After standing for a period of time, the ethyl acetate... The ester and aqueous solution separate into layers. The floating ring floats to the separation point between the ethyl acetate and aqueous solution. The motor drives the drive rod and the partition plate to move slowly downwards. Ethyl acetate moves from the through-hole on the partition plate and the gap between the partition plate and the inner wall of the treatment vessel to the top of the partition plate until the partition plate couples with the floating ring. The partition plate, together with the floating ring, separates the treatment vessel from the separation point between the ethyl acetate and aqueous solution. At this point, the lower discharge pipe can be opened to discharge the aqueous solution below. Then, the discharge pipe is closed, and the floating ring and the fan-shaped plate switch to the first state. Saturated brine is injected into the treatment vessel through another feed pipe. The above operation is repeated to remove residual sodium carbonate from the mixed liquid. Saturated calcium chloride solution is injected into the treatment vessel. The above operation is repeated to remove residual ethanol from the mixed liquid. Then, water washing is performed, and ethyl acetate is discharged. Finally, ethyl acetate is dried and distilled to obtain pure ethyl acetate. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this invention. For those skilled in the art, other drawings can be obtained based on these drawings.

[0018] Figure 1 This is a schematic diagram of the overall structure provided in an embodiment of the present invention; Figure 2 This is a schematic diagram of the internal structure provided in an embodiment of the present invention; Figure 3 for Figure 2 Enlarged view of point A in the middle; Figure 4 This is a schematic diagram of the internal structure of the drive rod provided in an embodiment of the present invention; Figure 5 for Figure 4 Enlarged view at point B in the middle; Figure 6 for Figure 4 Enlarged view at point C; Figure 7 This is a schematic diagram of the airway structure provided in an embodiment of the present invention; Figure 8 for Figure 7 Enlarged view at point D; Figure 9 This is a schematic diagram of the structure of the floating ring provided in an embodiment of the present invention; Figure 10 This is a schematic diagram of the internal structure of the floating ring provided in an embodiment of the present invention; Figure 11 This is a schematic diagram of the push ring provided in an embodiment of the present invention; Figure 12 This is a schematic diagram of the internal structure of the fan-shaped piece provided in an embodiment of the present invention; Figure 13 This is a schematic diagram of the slide bar provided in an embodiment of the present invention; Figure 14 This is a schematic diagram of the guide groove provided in an embodiment of the present invention.

[0019] Explanation of reference numerals in the attached figures: 1. Processing vessel; 11. Drive rod; 111. Mounting block; 112. Sector-shaped blade; 113. Connecting rod; 114. Locking block; 115. Wedge block; 116. Sealing plate; 117. Toothed rod; 118. Drive ring; 119. Synchronizing block; 12. Floating ring; 121. Airbag; 122. Push ring; 123. Sealing ring; 124. Movable plate; 125. Air passage; 126. Connecting pipe; 127. First piston; 128. Second piston; 129. Partition plate; 13. Movable block; 131. Magnetic ring; 132. Pulley block; 133. Slide rod; 134. Pulley rod; 135. Push block; 136. Rack; 137. Clamping rod; 138. Cable; 139. Sealing plug; 14. Feed pipe; 141. Tenon rod; 142. Second V-groove; 143. Vent hole; 144. Vent groove; 145. First V-groove; 15. Discharge pipe. Detailed Implementation

[0020] To enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0021] Example 1 like Figure 1-14 As shown, a purification apparatus and process for producing electronic-grade ethyl acetate includes a processing vessel 1, in which: The drive rod 11 has multiple fan-shaped pieces 112 movably arranged at its bottom end, and multiple openable and closable through holes are provided on the fan-shaped pieces 112. Floating ring 12, the floating ring 12 is assembled for the following two states: In the first state, multiple sector-shaped plates 112 are in a vertical state with their through holes closed, the floating ring 12 sinks to the bottom of the processing vessel 1, and the drive rod 11 drives the sector-shaped plates 112 to rotate and reciprocate in the vertical direction. In the second state, the floating ring 12 floats at the interface between the aqueous solution and ethyl acetate. Multiple fan-shaped pieces 112 are combined to form a septum 129 with its through holes open. The septum 129 moves down and couples with the floating ring 12 to close its through holes.

[0022] Specifically, the top of the processing vessel 1 is provided with multiple feed pipes 14 corresponding to various materials, and the bottom is provided with a discharge pipe 15. The top of the processing vessel 1 is rotatably provided with a drive ring 118, and the drive ring 118 is provided with a synchronization block 119 extending into the drive rod 11. The drive rod 11 is provided with a sliding groove adapted to the synchronization block 119. The processing vessel 1 is provided with a bidirectional motor, and the output end of the motor is provided with a gear that meshes with the drive ring 118. The processing vessel 1 is slidably provided with a square movable block 13, and the outer wall of the drive rod 11 is provided with a threaded protrusion. The movable block 13 is provided with a threaded through hole adapted to the drive rod 11.

[0023] In the above technical solution, during operation, the floating ring 12 and the sector plate 112 are in the first state. Ethyl acetate feed pipe 14 is injected into the treatment vessel 1, and then saturated sodium carbonate solution is injected into the treatment vessel 1 from another feed pipe 14. The motor operates, outputting positive and negative torques to drive the gear to rotate in the forward and reverse directions. The gear drives the drive rod 11 to rotate through the drive ring 118 and the synchronizing block 119 meshing with it. The drive rod 11 drives the sector plate 112 to rotate and reciprocate vertically along the threaded through hole on the movable block 13. The sector plate 112 stirs the mixture in the treatment vessel 1, causing the saturated sodium carbonate solution to react with the acidic substances remaining in the ethyl acetate. After stirring for a period of time, the operation stops. Multiple sector plates 112 move relative to the drive rod 11 to form a partition 129. After standing for a period of time, the ethyl acetate and aqueous solution separate into layers, and the floating ring 12 floats to the ethyl acetate layer. At the stratification point of the ester and aqueous solution, the motor drives the drive rod 11 and the partition 129 to move slowly downwards. Ethyl acetate moves from the through hole on the partition 129 and the gap between the partition 129 and the inner wall of the treatment vessel 1 to the top of the partition until the partition 129 couples with the floating ring 12. The partition 129, in conjunction with the floating ring 12, separates the treatment vessel 1 from the stratification point of the ester and aqueous solution. At this point, the lower discharge pipe can be opened to discharge the aqueous solution below. Then, the discharge pipe 15 is closed, and the floating ring 12 and the fan-shaped plate 112 switch to the first state. Saturated brine is injected into the treatment vessel 1 from another feed pipe 14. The above operation is repeated to remove the residual sodium carbonate in the mixed liquid. Saturated calcium chloride solution is injected into the treatment vessel 1. The above operation is repeated to remove the residual ethanol in the mixed liquid. Then, water washing is performed, and the ethyl acetate is discharged. Finally, the ethyl acetate is dried and distilled to obtain pure ethyl acetate.

[0024] As a further embodiment of the present invention, an air bladder 121 is provided on the floating ring 12, and the air pressure inside the processing vessel 1 is increased to cause the air bladder 121 to contract.

[0025] Specifically, carbon dioxide is generated during the reaction of sodium carbonate with acid and sodium chloride with sodium carbonate. Calcium chloride reacts with ethanol to generate chloroethane. Both the generated carbon dioxide and chloroethane will cause the internal pressure of the treatment vessel 1 to increase. At this time, the higher pressure will cause the air bladder 121 on the floating ring 12 to contract, reducing the buoyancy of the floating ring 12. The floating ring 12 will sink to the bottom of the treatment vessel 1 to prevent the floating ring 12 from interfering with the drive rod 11 and causing the fan-shaped plate 112 to move.

[0026] As a further embodiment of the present invention, a U-shaped air passage 125 is provided on the processing vessel 1, with both ends connected to the air bag 121 and the processing vessel 1 respectively. A first piston 127 and a second piston 128 are respectively fixedly connected in the parallel part of the air passage 125.

[0027] Specifically, a flexible connecting pipe 126 is provided between the air passage 125 and the air bag 121, an exhaust port 143 is provided on the top of the processing vessel 1, a sealing plug 139 adapted to the exhaust port 143 is provided on the top of the movable block 13, an exhaust groove 144 is provided on the side wall of the movable block 13, and an electric telescopic rod is provided between the movable block 13 and the processing vessel 1.

[0028] Furthermore, when the internal gas pressure in the treatment vessel 1 increases, some of the gas in the treatment vessel 1 will enter the U-shaped gas passage 125 and push the first piston 127 to move. The gas inside the gas passage 125 is compressed, and the first piston 127 drives the second piston 128 to move synchronously, forming a negative pressure on the air bag 121 and the connecting pipe 126. The air bag 121 contracts to reduce the buoyancy of the floating ring 12, and the floating ring 12 moves downward. After the reaction is completed, the electric telescopic rod extends to push the movable block 13 downward, the sealing plug 139 separates from the exhaust port 143, the exhaust port 143 opens, the gas in the treatment vessel 1 is discharged, the gas pressure returns to normal, the gas inside the gas passage 125 pushes the first piston 127 and the second piston 128 to reset, the air bag 121 re-inflates, so that the floating ring 12 can float to the connection between ethyl acetate and the aqueous solution.

[0029] As another embodiment of the present invention, a plurality of sliding plates are slidably disposed in the floating ring 12, and the spacer 129 is coupled to the floating ring 12 so that the sliding plates move outward and push against the sealing ring 123.

[0030] Specifically, the inner side of the floating ring 12 is stepped, a push ring 122 is slidably arranged on the floating ring 12, a slope is provided at the bottom of the push ring 122, a sealing ring 123 is provided on the outer wall of the partition plate 129, a clamping rod 137 is symmetrically slidably arranged inside the processing vessel 1, a pull cable 138 is provided between the clamping rod 137 and the movable block 13, and a spring is provided between the clamping rod 137 and the processing vessel 1.

[0031] Furthermore, after the ethyl acetate and aqueous solution separate, the electric telescopic rod drives the movable block 13 to move downward, the vent 143 opens, the internal air pressure of the treatment vessel 1 returns to normal, the floating ring 12 floats to the separation point of the ethyl acetate and aqueous solution, the movable block 13 continues to move downward, the cable 138 is released, and the clamping rod 137 moves towards the middle of the treatment vessel 1 under the push of the spring and clamps on the outer wall of the floating ring 12, fixing the floating ring 12. Then, the drive rod 11 drives the partition plate 129 to move downward, the partition plate 129 engages with the floating ring 12 and squeezes the push ring 122, the push ring 122 moves downward, and the slope at the bottom of the push ring 122 pushes the movable piece 124 to move away from the middle of the floating ring 12 and pushes the sealing ring 123, so that the sealing ring 123 contacts the inner wall of the treatment vessel 1, sealing the gap between the floating ring 12 and the treatment vessel 1, reducing the leakage of ethyl acetate during the drainage process.

[0032] As another embodiment of the present invention, a slide rod 133 is slidably disposed in the drive rod 11, and the slide rod 133 moves relative to the drive rod 11 to make the sector piece 112 move relative to the drive rod 11.

[0033] Specifically, a mounting block 111 is provided at the bottom of the drive rod 11, a fan-shaped piece 112 is movably mounted on the mounting block 111, and a lever 134 extending to the outside of the drive rod 11 is provided on the slide rod 133.

[0034] Furthermore, as the drive rod 11 moves the sector piece 112 upward, the lever 134 on the slide rod 133 contacts the movable block 13. The movable block 13 pushes the slide rod 133 downward through the lever 134, and the slide rod 133 moves the sector piece 112 relative to the mounting block 111, so that the sector piece 112 switches from the second state to the first state.

[0035] As another embodiment of the present invention, a locking block 114 embedded in the drive rod 11 is provided on the fan-shaped plate 112, and a top block for pushing the locking block 114 is provided at the bottom of the slide rod 133. A rack 136 is provided on the top block, and the top block moves to a predetermined position to couple the rack 136 with the fan-shaped plate 112.

[0036] Specifically, the top block has an isosceles trapezoidal cross-section. A connecting rod 113 is provided between the sector plate 112 and the locking block 114. The locking block 114 is provided with a toothed bar 117 that meshes with the rack 136. The mounting block 111 has a groove adapted to the locking block 114 and a cavity for the locking block 114 to rotate inside. A spring is provided between the sector plate 112 and the mounting block 111. A magnetic ring 131 (ring magnet) that attracts the lever 134 is provided on the movable block 13. A lever 132 extending to the outside of the movable block 13 is provided on the magnetic ring 131. A spring is provided between the lever 132 and the movable block 13.

[0037] Furthermore, when the movable block 13 is in a lower position, as the movable block 13 and the sector piece 112 move closer to the movable block 13, the magnetic ring 131 retracts inside the movable block 13 under the action of the spring. At this time, the lever 134 moves towards the bottom of the movable block 13 and is blocked by the movable block 13. The lever 134 drives the slide bar 133 to move downward relative to the drive rod 11. The ramp of the push block 135 pushes against the toothed rod 117 to move the sector piece 112 away from the mounting block 111. The fan-shaped pieces 112 have a certain gap between them. When the rack 117 contacts the vertical surface of the push block 135, it engages with the rack 136. The locking block 114 separates from the groove on the mounting block 111 and enters the cavity inside the mounting block 111. The spring between the fan-shaped pieces 112 and the mounting block 111 is stretched, accumulating elastic potential energy. The slide bar 133 and the rack 136 continue to move downwards. The rack 136 pushes the rack 117 and the fan-shaped pieces 112 to rotate, causing them to move from the water... When the horizontal position changes to a vertical position, the slide bar 133 continues to move downwards, and the rack 117 moves to the end of the tooth on the rack 136. The rack 117 and rack 136 no longer mesh, and the end of the rack 117 contacts the ramp above the push block 135. The spring pulls the sector piece 112 towards the mounting block 111, and the locking block 114 is embedded in the groove on the mounting block 111, fixing the sector piece 112 to the mounting block 111 together. When the movable block 13 is in a higher position... As the movable block 13 and the sector 112 approach the movable block 13, the pusher block 132 is pushed against the top of the processing vessel 1, and the magnetic ring 131 protrudes from the bottom of the movable block 13. The slide bar 133 is at its lowest point relative to the mounting block 111. The magnetic ring 131 is attracted to the pusher bar 134. Then the drive rod 11 moves downward, and the magnetic ring 131 drives the slide bar 133 to move upward relative to the mounting block 111 through the pusher bar 134, so that the sector 112 switches from a vertical state to a horizontal state.

[0038] As another embodiment of the present invention, a sealing plate 116 with multiple through holes is movably disposed in the fan-shaped plate 112. The sealing plate 116 moves relative to the fan-shaped plate 112 to open and close the through holes on the fan-shaped plate 112.

[0039] Specifically, the inside of the fan-shaped plate 112 is provided with a spring for pushing against the sealing plate 116, and the sealing plate 116 is provided with a wedge 115 extending to the outside of the fan-shaped plate 112. The fan-shaped plate 112 is provided with a notch for the wedge 115 to move.

[0040] Furthermore, when the sector-shaped plate 112 is in a vertical state, the sealing plate 116 moves relative to the sector-shaped plate 112 under the action of gravity, causing the through holes on the sector-shaped plate 112 to be misaligned with the through holes on the sealing plate 116, at which point the through holes on the sector-shaped plate 112 are in a closed state; when the sector-shaped plate 112 is in a horizontal state, multiple springs inside the sector-shaped plate 112 push the sealing plate 116 to move relative to the sector-shaped plate 112, causing the through holes on the sealing plate 116 to be aligned with the through holes on the sector-shaped plate 112. Yes, at this time, the through holes on the sector plate 112 are in an open state; as the partition plate 129 composed of sector plates 112 approaches the floating ring 12, the inclined surface of the wedge block 115 on the sealing plate 116 contacts the floating ring 12, and the floating ring 12 pushes the wedge block 115 to retract into the sector plate 112, thereby driving the sealing plate 116 to move relative to the sector plate 112. The through holes on the sealing plate 116 are misaligned with the through holes on the sealing plate 116, and at this time the through holes on the sector plate 112 are in a closed state.

[0041] As another embodiment of the present invention, a guide groove composed of an inclined first V groove 145 and an inclined second V groove 142 is provided on the side wall of the processing vessel 1, and a tenon rod 141 adapted to the guide groove is horizontally slidably provided on the movable block 13.

[0042] Specifically, during the process of the electric telescopic rod driving the movable block 13 to move from a low point to a high point, the tenon 141 moves along the right side of the first V-groove 145 (with... Figure 14 The movable block 13 moves upwards, and the tenon 141 slides laterally relative to the movable block 13. After moving to the highest point, the movable block 13 moves down a short distance, and the tenon 141 moves along the right side of the second V-groove 142 to the lowest point of the second V-groove 142, supporting the movable block 13 and reducing the burden on the electric telescopic rod. During the process of the movable block 13 moving from the high position to the low position, the movable block 13 first moves up a short distance, and the tenon 141 moves along the left side of the second V-groove 142 to the highest point. Then the movable block 13 moves down, and the tenon 141 moves along the left side of the first V-groove 145 to the lowest point of the first V-groove 145, supporting the movable block 13.

[0043] Example 2 A purification process for producing electronic-grade ethyl acetate, based on a purification apparatus for producing electronic-grade ethyl acetate in Example 1, further includes the following steps: S1. Ethyl acetate is injected into the treatment vessel 1, and then saturated sodium carbonate solution is injected into the treatment vessel 1. At this time, the floating ring 12 and the sector plate 112 are in the first state. The motor works and outputs positive torque and reverse torque to drive the gear to rotate in the forward and reverse directions. The gear drives the drive rod 11 to rotate through the drive ring 118 and the synchronizing block 119 that mesh with it. The drive rod 11 drives the sector plate 112 to rotate and move back and forth in the vertical direction along the threaded through hole on the movable block 13. The sector plate 112 stirs the mixture in the treatment vessel 1, so that the saturated sodium carbonate solution reacts with the acidic substances remaining in the ethyl acetate. S2. After stirring for a period of time, the work is stopped. Multiple fan-shaped plates 112 move relative to the drive rod 11 to form a partition 129. After standing for a period of time, ethyl acetate and aqueous solution separate into layers. The floating ring 12 floats to the layering point of ethyl acetate and aqueous solution. The motor drives the drive rod 11 and the partition 129 to move slowly downward. Ethyl acetate moves from the through hole on the partition 129 and the gap between the partition 129 and the inner wall of the treatment vessel 1 to the top of the partition plate until the partition 129 is coupled with the floating ring 12. The partition 129, together with the floating ring 12, separates the treatment vessel 1 from the layering point of ethyl acetate and aqueous solution. At this time, the discharge pipe below can be opened to discharge the aqueous solution below. Then the discharge pipe 15 is closed. S4, the floating ring 12 and the sector plate 112 are switched to the first state, saturated brine is added and the above steps are repeated, then saturated calcium chloride solution is added and the above steps are repeated, and finally the mixture is washed with water, dried and distilled to obtain pure ethyl acetate.

[0044] The foregoing has only described certain exemplary embodiments of the present invention by way of illustration. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the foregoing drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A purification apparatus for the production of electronic-grade ethyl acetate, characterized in that, Includes a processing vessel (1), wherein the processing vessel (1) is movably provided with: A drive rod (11) has multiple fan-shaped pieces (112) movably arranged at its bottom end, and multiple openable and closable through holes are provided on the fan-shaped pieces (112). A floating ring (12) is assembled for use in the following two states: In the first state, the multiple fan-shaped plates (112) are in a vertical state and their through holes are closed. The floating ring (12) is submerged at the bottom of the processing vessel (1). The driving rod (11) drives the fan-shaped plates (112) to rotate and reciprocate in the vertical direction. In the second state, the floating ring (12) floats at the interface between the aqueous solution and ethyl acetate, and multiple fan-shaped pieces (112) are combined to form a septum (129) with its through holes open. The septum (129) moves down and couples with the floating ring (12) to close its through holes.

2. The purification apparatus for producing electronic-grade ethyl acetate according to claim 1, characterized in that, An air bladder (121) is provided on the floating ring (12), and the internal air pressure of the processing vessel (1) is increased to cause the air bladder (121) to contract.

3. The purification apparatus for producing electronic-grade ethyl acetate according to claim 2, characterized in that, The processing vessel (1) has a U-shaped air passage (125) with both ends connected to the airbag (121) and the processing vessel (1).

4. The purification apparatus for producing electronic-grade ethyl acetate according to claim 3, characterized in that, The parallel portion of the air passage (125) is provided with a first piston (127) and a second piston (128) that are fixedly connected.

5. The purification apparatus for producing electronic-grade ethyl acetate according to claim 1, characterized in that, Multiple sliding plates are slidably disposed in the floating ring (12), and the partition (129) is coupled to the floating ring (12) to make the sliding plates move outward and push against the sealing ring (123).

6. The purification apparatus for producing electronic-grade ethyl acetate according to claim 1, characterized in that, A slide rod (133) is slidably disposed in the drive rod (11), and the slide rod (133) moves relative to the drive rod (11) to move the sector plate (112) relative to the drive rod (11).

7. The purification apparatus for producing electronic-grade ethyl acetate according to claim 6, characterized in that, The fan-shaped plate (112) is provided with a locking block (114) embedded in the drive rod (11), and the bottom of the slide rod (133) is provided with a top block for pushing the locking block (114).

8. The purification apparatus for producing electronic-grade ethyl acetate according to claim 7, characterized in that, The top block is provided with a rack (136), and the top block is moved to a predetermined position so that the rack (136) is coupled with the sector plate (112).

9. The purification apparatus for producing electronic-grade ethyl acetate according to claim 1, characterized in that, A sealing plate (116) with multiple through holes is movably disposed in the fan-shaped plate (112). The sealing plate (116) moves relative to the fan-shaped plate (112) to open and close the through holes on the fan-shaped plate (112).

10. A purification process for the production of electronic-grade ethyl acetate, based on the purification apparatus for the production of electronic-grade ethyl acetate according to any one of claims 1-9, characterized in that, It also includes the following steps: S1. Ethyl acetate is injected into the treatment vessel (1), and then saturated sodium carbonate solution is injected into the treatment vessel (1). At this time, the floating ring (12) and the fan-shaped plate (112) are in the first state, and the driving rod (11) drives the fan-shaped plate (112) to stir the mixed liquid. S2, the mixed liquid is allowed to stand and separate into layers, the floating ring (12) and the fan-shaped plate (112) switch to the second state, and the partition plate (129) moves down and the ethyl acetate moves above the partition plate (129); S3, the septum (129) is coupled to the floating ring (12) to separate ethyl acetate and aqueous solution, and then the aqueous solution below is drained; S4, the floating ring (12) and the sector plate (112) are switched to the first state, saturated brine is added and the above steps are repeated, then saturated calcium chloride solution is added and the above steps are repeated, and finally the mixture is washed with water, dried and distilled to obtain pure ethyl acetate.

Images