An ethyl acetate production device and a production method

By designing the split box and circulating hoisting mechanism in the ethyl acetate production equipment, efficient stirring and moisture removal of impurity adsorbents are achieved, the problem of insufficient utilization of adsorbents is solved, and the purification quality and purity of ethyl acetate is improved.

CN117504360BActive Publication Date: 2025-07-22ZHUHAI QIANXIN NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202311499581.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-13
Publication Date
2025-07-22
Estimated Expiration
2043-11-13

AI Technical Summary

Technical Problem

During the existing ethyl acetate production process, the utilization rate of adsorbent in the inner layer of the adsorbent cage is insufficient, which affects the purification quality.

Method used

An ethyl acetate production equipment including a fixed and connected liquid storage tank and purification cylinder is designed, and the reciprocating screw and spiral blades are used to drive the reciprocating screw and spiral blade to stir the impurity adsorbent, and the position exchange and impurity pouring of the impurity adsorbent are controlled by gravity passively, and the water content is reduced in combination with the water absorbing layer.

Benefits of technology

It improves the utilization rate of impurity adsorbents, improves the purification effect of ethyl acetate, and reduces the water content in the product.

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Abstract

The present invention discloses an ethyl acetate production device and a production method, which relate to the technical field of ethyl acetate production. The present invention includes a liquid storage tank and a purification cylinder that are fixedly connected. A reciprocating screw is rotatably arranged on the inner top wall of the purification cylinder. A rotating shaft is fixedly arranged on the reciprocating screw. A spiral blade is fixedly arranged on the outer peripheral surface of the rotating shaft. A shunt box for controlling the rotation of the reciprocating screw is vertically slidably arranged in the purification cylinder. The purification cylinder is filled with an impurity adsorbent. A circulating lifting mechanism for passively controlling the reciprocating movement of the shunt box is fixedly arranged on the purification cylinder. The spiral blade is driven to rotate passively by the gravity of the shunt box, thereby stirring the impurity adsorbent. The feeding amount is passively controlled by the up and down movement of the shunt box, so as to achieve the effect of pouring a part of crude ethyl acetate on the impurity adsorbent every time the impurity adsorbent is stirred. The water content of ethyl acetate at the bottom of the purification cylinder is reduced through a water removal pipe.
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Description

Technical Field

[0001] The present invention relates to the technical field of ethyl acetate production, and specifically relates to an ethyl acetate production device and a production method. Background Art

[0002] Ethyl acetate, also known as acetic acid ethyl ester, has the molecular formula: C4H8O2. It is a colorless, transparent, and flammable liquid with fluidity. It has a fruity fragrance and is volatile. Ethyl acetate is a very important chemical solvent with wide applications. The methods for preparing ethyl acetate include: ① the method of synthesizing acetic acid and ethanol catalyzed by phosphomolybdic acid, ② the method of dehydrogenating and oxidizing ethanol, ③ the method of adding ethylene to acetic acid, ④ the method of producing acetaldehyde catalyzed by aluminum triethanolate, etc.; currently, the acetaldehyde condensation method is widely used to produce ethyl acetate. This production method has the advantages of low unit consumption of raw materials, simple process, little corrosion of equipment, and low discharge of three wastes, and is widely applied.

[0003] For example, in the Chinese invention patent with the authorization announcement number CN112299999B, the authorization announcement date of July 13, 2021, and the name "A Refining Method of High-Purity Ethyl Acetate", the main steps of its purification and refining are: S1. Adsorption and impurity removal: Coarse ethyl acetate is put into a mixed adsorbent, adsorbed and filtered to obtain ethyl acetate after preliminary impurity removal; S2. Atmospheric distillation: The ethyl acetate after preliminary impurity removal is added to a high-efficiency distillation column for atmospheric distillation reflux to obtain ethyl acetate after atmospheric distillation; S3. Precision filtration: The ethyl acetate after atmospheric distillation is filtered twice to obtain high-purity ethyl acetate.

[0004] When preparing ethyl acetate by the acetaldehyde condensation method, it is necessary to use distilled water to destroy the excess catalyst. Therefore, in the prepared crude ethyl acetate, in addition to impurities, it also contains part of distilled water. Currently, the first step in purifying and purifying ethyl acetate is to carry out adsorption and impurity removal on ethyl acetate. During adsorption and impurity removal, granular adsorbent is used for adsorption and impurity removal. Specifically, the adsorbent is filled in an adsorption mesh box and then immersed in an adsorption pool filled with ethyl acetate for adsorption and impurity removal. When the adsorption mesh box adsorbs impurities, the adsorbent on the outer layer of the adsorption mesh box comes into contact with the crude ethyl acetate first, and the ethyl acetate that comes into contact with the adsorbent on the inner layer of the adsorption mesh box has been purified by the outer layer adsorbent. This will result in insufficient utilization rate of the adsorbent on the inner layer of the adsorption mesh box and affect the purification quality of ethyl acetate. Summary of the Invention

[0005] The purpose of the present invention is to provide an ethyl acetate production device and a production method to solve the above deficiencies in the prior art.

[0006] To achieve the above object, the present invention provides the following technical solution: An ethyl acetate production device, comprising a liquid storage tank and a purification cylinder that are fixedly connected and communicated. A reciprocating screw is rotatably arranged on the inner top wall of the purification cylinder. A rotating shaft is fixedly arranged on the reciprocating screw. A spiral blade is fixedly arranged on the outer peripheral surface of the rotating shaft. A shunt box for controlling the rotation of the reciprocating screw is vertically slidably arranged in the purification cylinder. An impurity adsorbent is filled in the purification cylinder. A circulating lifting mechanism for passively controlling the reciprocating movement of the shunt box is fixedly arranged on the purification cylinder.

[0007] Preferably, the circulating lifting mechanism includes two hydraulic tanks fixedly arranged on the outer wall of the purification cylinder. A counterweight block is slidably arranged in each hydraulic tank. A linkage cylinder is fixedly arranged in the purification cylinder. A lifting rod is slidably arranged in each linkage cylinder. A communicating pipe is fixedly connected and communicated between each linkage cylinder and each hydraulic tank in a one-to-one correspondence. Each lifting rod is fixedly connected to the bottom wall of the shunt box.

[0008] Preferably, two fixing frames are fixedly arranged on the inner bottom wall of the shunt box. A permanent magnet plate is slidably arranged in each fixing frame. A sliding rod is fixedly arranged on each permanent magnet plate. Two top plates are fixedly arranged on the inner wall of the purification cylinder.

[0009] Preferably, a sieve mesh is fixedly arranged on the shunt box. Two groups of push plates are fixedly arranged on the sieve mesh. Two sliding plates are slidably arranged on the inner top wall of the purification cylinder. A sliding frame is fixedly arranged on the side wall of each sliding plate. Two push wheels are rotatably arranged on each sliding frame.

[0010] Preferably, fixing plates are slidably arranged on both sides of each sliding plate. Each fixing plate is fixedly connected to the inner top wall of the purification cylinder. A rotating rod is rotatably arranged between two adjacent fixing plates. A pulling rope is fixedly arranged on each sliding frame. One end of each pulling rope away from the sliding frame is fixedly connected to the sieve mesh after passing around each rotating rod in a one-to-one correspondence.

[0011] Preferably, a buffer mesh is fixedly arranged in the purification cylinder.

[0012] Preferably, two water discharge pipes are fixedly arranged at the bottom of the purification cylinder. An absorbent layer is arranged in each water discharge pipe.

[0013] Preferably, a lifting frame is fixedly arranged on each counterweight block. A connecting rod is fixedly arranged at the bottom of each lifting frame. A piston is fixedly arranged at one end of each connecting rod away from the lifting frame. An outer sleeve is fixedly connected and communicated with each water discharge pipe. Each piston is slidably arranged in each outer sleeve in a one-to-one correspondence.

[0014] Preferably, a plugging cap is threadedly connected to one end of each water discharge pipe away from the purification cylinder.

[0015] A method for producing ethyl acetate, based on the above production equipment, includes the following steps:

[0016] S1: Prepare ethyl acetate through the condensation reaction of acetaldehyde;

[0017] S2: Remove the catalyst. Add distilled water into the body of a kettle reactor to destroy the excess catalyst;

[0018] S3: Adsorb and remove impurities: Put crude ethyl acetate into the above-mentioned ethyl acetate production equipment for adsorption and filtration to obtain ethyl acetate after preliminary impurity removal, and then distill out the crude ethyl acetate through an evaporator;

[0019] S4: Rectify and purify. Pass through three rectification towers, namely a deacetaldehyde tower, a deethanol tower, and a de-heavy component tower, to remove acetaldehyde, ethanol, and acetal from the crude ethyl acetate respectively. In the above technical solution, the present invention provides an ethyl acetate production equipment and a production method, which have the following beneficial effects: 1. By injecting crude ethyl acetate into the shunt box, the shunt box is driven to move up and down passively through the cooperation of the gravity of the shunt box and the counterweight, thereby driving the spiral blade to rotate passively, and then stirring the impurity adsorbent in the purification cylinder to exchange the positions of the upper and lower layers of the impurity adsorbent, greatly improving the utilization rate of the impurity adsorbent; 2. Control the movement of the slider through the up and down movement of the shunt box, and then passively control the opening and closing of the connection between the liquid storage tank and the purification cylinder, thereby controlling the feeding amount of the liquid storage tank each time, and then achieving the effect of pouring a part of the crude ethyl acetate on the impurity adsorbent every time it is stirred; 3. Absorb and discharge the liquid with a large water content at the bottom of the purification cylinder through the up and down movement of the counterweight, and cooperate with the water absorption layer to reduce the water content of the ethyl acetate in the purification cylinder. Description of the Drawings

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required in the embodiments. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings.

[0021] Figure 1 It is a schematic diagram of the overall structure provided by the embodiment of the present invention;

[0022] Figure 2 It is a schematic diagram of the structure of the shunt box provided by the embodiment of the present invention;

[0023] Figure 3 It is a schematic diagram of the structure of the reciprocating screw provided by the embodiment of the present invention;

[0024] Figure 4 It is a schematic diagram of the structure of the water absorption layer provided by the embodiment of the present invention;

[0025] Figure 5 The enlarged view of the structure at A in Figure 3 this embodiment of the present invention;

[0026] Figure 6 The schematic structural diagram of the piston provided by this embodiment of the present invention;

[0027] Figure 7 The schematic structural diagram of the permanent magnet plate provided by this embodiment of the present invention;

[0028] Figure 8 The schematic structural diagram of the push plate provided by this embodiment of the present invention;

[0029] Figure 9 The schematic structural diagram of the counterweight provided by this embodiment of the present invention;

[0030] Figure 10 The schematic structural diagram of the push wheel provided by this embodiment of the present invention.

[0031] Explanation of reference numerals: 1, liquid storage tank; 2, purification cylinder; 3, rotating shaft; 4, spiral blade; 5, reciprocating screw; 6, shunt box; 7, screen; 8, buffer screen; 10, hydraulic tank; 11, counterweight; 12, jacking rod; 13, linkage cylinder; 14, connecting pipe; 15, lifting frame; 16, outer sleeve; 17, piston; 18, connecting rod; 19, round rod; 21, water discharge pipe; 22, plugging cap; 23, water absorption layer; 24, switch valve; 31, fixing frame; 32, sliding rod; 33, top plate; 34, permanent magnet plate; 41, push plate; 42, sliding plate; 43, fixing plate; 44, rotating rod; 45, sliding frame; 46, push wheel; 47, pull rope. Detailed implementation manners

[0032] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further introduced in detail below with reference to the accompanying drawings.

[0033] Please refer to Figures 1-10, An ethyl acetate production device, comprising a liquid storage tank 1 and a purification cylinder 2 that are fixedly connected. A reciprocating screw 5 is rotatably arranged on the inner top wall of the purification cylinder 2. A rotating shaft 3 is fixedly arranged on the reciprocating screw 5. A spiral blade 4 is fixedly arranged on the outer peripheral surface of the rotating shaft 3. A shunt box 6 for controlling the rotation of the reciprocating screw 5 is vertically slidably arranged in the purification cylinder 2. The purification cylinder 2 is filled with an impurity adsorbent. A circulating lifting mechanism for passively controlling the reciprocating movement of the shunt box 6 is fixedly arranged on the purification cylinder 2; the liquid storage tank 1 is used to place the prepared crude ethyl acetate. The bottom of the liquid storage tank 1 is fixedly connected to the top of the purification cylinder 2. The purification cylinder 2 is filled with an appropriate amount of impurity adsorbent. The impurity adsorbent is composed of a mixture of activated carbon and activated alumina. The reciprocating screw 5 is rotatably connected to the inner top wall of the purification cylinder 2. The rotating shaft 3 is fixedly arranged at one end of the reciprocating screw 5 away from the inner bottom wall of the purification cylinder 2. The shunt box 6 is annular. A contact ball matching with the thread groove of the reciprocating screw 5 is fixedly arranged on the inner wall of the inner ring of the shunt box 6. When the shunt box 6 moves up and down through the contact ball, the reciprocating screw 5 is driven to rotate, and then the rotating shaft 3 and the spiral blade 4 are driven to rotate. When the spiral blade 4 rotates, the impurity adsorbent in the purification cylinder 2 can be stirred, so that the impurity adsorbent at the bottom of the purification cylinder 2 is gradually turned to the upper part, so that the impurity adsorbents in different layers in the purification cylinder 2 can all be in full contact with the unpurified crude ethyl acetate, thereby improving the utilization rate of the impurity adsorbent and the purification effect of ethyl acetate.

[0034] Further, the circulating lifting mechanism includes two hydraulic tanks 10 fixedly arranged on the outer wall of the purification cylinder 2. A counterweight 11 is slidably arranged in each hydraulic tank 10. A linkage cylinder 13 is fixedly arranged in the purification cylinder 2. A lifting rod 12 is slidably arranged in each linkage cylinder 13. A communicating pipe 14 is fixedly connected in one-to-one correspondence between each linkage cylinder 13 and each hydraulic tank 10. Each lifting rod 12 is fixedly connected to the bottom wall of the shunt box 6; two liquid leakage holes (not marked in the figure) are opened at the bottom of the shunt box 6. Hydraulic oil is placed in each hydraulic tank 10. During use, crude ethyl acetate is discharged from the liquid storage tank 1 into the shunt box 6. When the shunt box 6 is filled with ethyl acetate, the weight of the shunt box 6 increases, and the shunt box 6 slides downward as the weight increases. When the shunt box 6 slides downward, the lifting rod 12 is driven to move downward. When the lifting rod 12 moves downward, the hydraulic oil in the linkage cylinder 13 is squeezed, so that the counterweight 11 in the hydraulic tank 10 moves upward. When the shunt box 6 moves downward, the reciprocating screw 5 is driven to rotate, and then the spiral blade 4 stirs the impurity adsorbent. When the shunt box 6 moves downward to a certain position, the liquid in the shunt box 6 flows from the shunt box 6 to the impurity adsorbent in the purification cylinder 2 through the two liquid leakage holes. At this time, the ethyl acetate left in the shunt box 6 comes into contact with the relatively clean impurity adsorbent, thereby improving the utilization rate of the impurity adsorbent.

[0035] Furthermore, two fixing frames 31 are fixedly arranged on the inner bottom wall of the flow splitting box 6. A permanent magnet plate 34 is slidably arranged in each fixing frame 31. A sliding rod 32 is fixedly arranged on each permanent magnet plate 34. Two top plates 33 are fixedly arranged on the inner wall of the purification cylinder 2. The top wall of the fixing frame 31 is made of magnetic material. Each fixing frame 31 is fixedly arranged on each liquid leakage hole correspondingly. In the initial state, each permanent magnet plate 34 abuts against the inner bottom wall of the flow splitting box 6 under the action of gravity, so as to block the two liquid leakage holes and prevent the crude ethyl acetate from leaking out of the liquid leakage holes. As the ethyl acetate in the flow splitting box 6 increases, the flow splitting box 6 moves downward. During the downward movement of the flow splitting box 6, the sliding rod 32 penetrating the permanent magnet plate 34 will abut against the top plate 33. Through the cooperation of the top plate 33 and the sliding rod 32, each permanent magnet plate 34 slides along the vertical direction towards the top wall of the fixing frame 31. When the permanent magnet plate 34 contacts the top wall of the fixing frame 31, the permanent magnet plate 34 and the top wall of the fixing frame 31 are adsorbed together. At this time, each liquid leakage hole is opened, and the crude ethyl acetate in the liquid storage tank 1 no longer discharges into the flow splitting box 6. As the liquid leakage hole is opened, the ethyl acetate in the flow splitting box 6 gradually flows onto the impurity adsorbent in the purification cylinder 2. As the ethyl acetate in the flow splitting box 6 decreases, the counterweight 11 extrudes the hydraulic oil in the hydraulic tank 10 and jacks up the flow splitting box 6 through the jacking rod 12. When the flow splitting box 6 moves upward to a certain position, the permanent magnet plate 34 is separated from the top wall of the fixing frame 31 by the sliding rod 32 penetrating the permanent magnet plate 34 abutting against the inner top wall of the purification cylinder 2. At this time, the permanent magnet plate 34 blocks the liquid leakage hole again due to gravity, and ethyl acetate is injected into the flow splitting box 6 again, and the flow splitting box 6 moves downward again, so that the flow splitting box 6 moves up and down passively, and then drives the spiral blade 4 to rotate passively. The whole device does not need to be provided with a driving source.

[0036] In another embodiment of the present invention: A screen 7 is fixedly arranged on the flow splitting box 6. Two groups of push plates 41 are fixedly arranged on the screen 7. Two sliding plates 42 are slidably arranged on the inner top wall of the purification cylinder 2. A sliding frame 45 is fixedly arranged on the side wall of each sliding plate 42. Two push wheels 46 are rotatably arranged on each sliding frame 45. The communication between the liquid storage tank 1 and the purification cylinder 2 is blocked by the sliding plate 42, so as to control the injection of ethyl acetate from the liquid storage tank 1 into the purification cylinder 2. The crude ethyl acetate discharged from the liquid storage tank 1 is purified for the first time through the screen 7, and the impurities with larger particles in the crude ethyl acetate are filtered out through the screen 7. The number of each group of push plates 41 is two, and each push plate 41 is arranged in a trapezoid shape. When the flow splitting box 6 moves upward to be close to the inner top wall of the purification cylinder 2, each push plate 41 abuts against the push wheel 46 on each sliding frame 45 correspondingly. By pushing the push plate 41, each sliding frame 45 and the corresponding sliding plate 42 are moved, so as to open the communication between the liquid storage tank 1 and the purification cylinder 2, and facilitate the injection of the liquid in the liquid storage tank 1 into the purification cylinder 2.

[0037] Specifically, fixing plates 43 are slidably arranged on both sides of each slide plate 42. Each fixing plate 43 is fixedly connected to the inner top wall of the purification cylinder 2. A rotating rod 44 is rotatably arranged between two adjacent fixing plates 43. A pull rope 47 is fixedly arranged on each sliding frame 45. One end of each pull rope 47 away from the sliding frame 45 is correspondingly wound around each rotating rod 44 and fixedly connected to the sieve mesh 7. When the shunt box 6 moves upward, the corresponding push wheels 46 are pushed by the respective push plates 41 to move the slide plate 42, thereby opening the communication between the liquid storage tank 1 and the purification cylinder 2. When the shunt box 6 moves downward by a certain distance, each slide plate 42 is moved towards the reciprocating screw rod 5 through the respective pull ropes 47, thereby blocking the communication between the liquid storage tank 1 and the purification cylinder 2. At this time, ethyl acetate in the liquid storage tank 1 no longer flows into the shunt box 6, which facilitates the upward movement of the shunt box 6. By controlling the rotation of the spiral blade 4 and the movement of the slide plate 42 through the up and down movement of the shunt box 6, the effect of pouring a part of crude ethyl acetate on the impurity adsorbent every time some impurity adsorbents are turned is achieved, making full use of the impurity adsorbent.

[0038] Further, a buffer mesh 8 is fixedly arranged inside the purification cylinder 2. The buffer mesh 8 is fixedly arranged between the linkage cylinder 13 and the spiral blade 4. The ethyl acetate flowing down from the shunt box 6 first falls on the buffer mesh 8 and then is dispersed by the buffer mesh 8 and falls on the impurity adsorbent inside the purification cylinder 2.

[0039] In another embodiment of the present invention: Two water discharge pipes 21 are fixedly arranged at the bottom of the purification cylinder 2. An absorbent layer 23 is arranged inside each water discharge pipe 21. The absorbent layer 23 is filled with molecular sieves with a pore size of 3A. A barrier net is provided between the water discharge pipe 21 and the purification cylinder 2 to prevent the molecular sieves from entering the purification cylinder 2. The water is absorbed by the molecular sieves, and the absorbed molecular sieves can be recycled by heating. Since the density of ethyl acetate is less than that of water, when there is crude ethyl acetate in the purification cylinder 2, the water in the ethyl acetate will sink to the bottom of the purification cylinder 2. The water sinking to the bottom of the purification cylinder 2 is absorbed by the absorbent layer 23 in the two water discharge pipes 21, thereby reducing the water content in the crude ethyl acetate.

[0040] Furthermore, a lifting frame 15 is fixedly arranged on each counterweight 11, a connecting rod 18 is fixedly arranged at the bottom of each lifting frame 15, a piston 17 is fixedly arranged at one end of each connecting rod 18 away from the lifting frame 15, an outer sleeve 16 is fixedly communicated with each water discharge pipe 21, and each piston 17 is slidably arranged in each outer sleeve 16 in a one-to-one correspondence; a round rod 19 is fixedly arranged on each counterweight 11, one end of each round rod 19 away from the counterweight 11 is fixedly connected with the lifting frame 15, and each lifting frame 15 is fixedly connected with the counterweight 11 through the round rod 19. When the counterweight 11 moves up and down, it drives the counterweight 11 to move up and down, thereby driving the piston 17 to move up and down through the connecting rod 18. When the piston 17 moves upward, a negative pressure is generated in the outer sleeve 16, so as to suck the ethyl acetate with a large water content at the bottom of the purification cylinder 2 into the water discharge pipe 21, and the water content in the ethyl acetate at the bottom of the purification cylinder 2 is reduced through the water absorption layer 23 in the water discharge pipe 21. When the piston 17 moves downward, the ethyl acetate in the water discharge pipe 21 and the outer sleeve 16 is discharged from the water discharge pipe 21.

[0041] Even further, a plugging cap 22 is threadedly connected to one end of each water discharge pipe 21 away from the purification cylinder 2; a switching valve 24 is arranged at the bottom of the purification cylinder 2, and the opening and closing of the bottom of the purification cylinder 2 are controlled through the switching valve 24, so as to facilitate the discharge of the ethyl acetate in the purification cylinder 2. The water discharge pipe 21 is plugged through the plugging cap 22. When the water absorption layer 23 needs to be replaced, the plugging cap 22 is opened to facilitate the replacement of the filler in the water absorption layer 23.

[0042] An ethyl acetate production method, which is based on the above production equipment, includes the following steps:

[0043] S1: Prepare ethyl acetate through the condensation reaction of acetaldehyde; this is the prior art and will not be elaborated here one by one;

[0044] S2: Remove the catalyst, and add distilled water to a kettle reactor body to destroy the excess catalyst;

[0045] S3: Adsorb and remove impurities: Put the crude ethyl acetate into the above ethyl acetate production equipment for adsorption and filtration to obtain the preliminarily purified ethyl acetate. Then, the crude ethyl acetate is distilled out through an evaporator, and the aluminum hydroxide residue liquid is discharged from the bottom. Then, the residue liquid is further separated from aluminum hydroxide through a separator, and the liquid part will be returned to the evaporator again. The alcohol and the crude ethyl acetate are sent to the distillation process together:

[0046] S4: Rectification and purification. The crude ethyl acetate is passed through three rectification towers, namely the acetaldehyde removal tower, the ethanol removal tower, and the heavy component removal tower in sequence to remove acetaldehyde, ethanol, and acetal in the crude ethyl acetate respectively. Working principle: The prepared crude ethyl acetate is placed in the liquid storage tank 1. In the initial state, the connection between the liquid storage tank 1 and the purification cylinder 2 is open. At this time, the crude ethyl acetate in the liquid storage tank 1 flows into the shunt box 6 in the purification cylinder 2. As the ethyl acetate in the shunt box 6 increases, the weight of the shunt box 6 is greater than the weight of the counterweight 11. At this time, the shunt box 6 moves downward, thereby driving the reciprocating screw 5 and the spiral blade 4 to rotate. When the shunt box 6 moves down to the slide bar 32 abuts against the top plate 33, the connection between the liquid storage tank 1 and the purification cylinder 2 is blocked by pulling the slide plate 42 through the pull rope 47. The permanent magnet plate 34 is pushed upward by the slide bar 32 and attracted to the fixed frame 31. At this time, the crude ethyl acetate in the shunt box 6 flows onto the impurity adsorbent. As the ethyl acetate in the shunt box 6 flows out, the weight of the shunt box 6 gradually becomes less than the weight of the counterweight 11. At this time, the shunt box 6 moves upward. When the push plate 41 on the shunt box 6 abuts against the push wheel 46, the slide plate 42 moves again, and the crude ethyl acetate in the liquid storage tank 1 flows into the shunt box 6 again, so that the shunt box 6 moves downward again. When the counterweight 11 moves up and down, it can drive the piston 17 to move up and down, and then suck the crude ethyl acetate with a large water content at the bottom of the purification cylinder 2 into the water removal pipe 21, thereby reducing the water content of the ethyl acetate. This device does not require a separate drive source and can automatically adsorb and remove impurities from the crude ethyl acetate. Only some exemplary embodiments of the present invention have been described by way of illustration. Undoubtedly, for those of ordinary skill in the art, the described embodiments can be modified in various different ways without departing from the spirit and scope of the present invention. Therefore, the above 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. An ethyl acetate production device, comprising a liquid storage tank (1) and a purification cylinder (2) that are fixedly connected and communicated, characterized in that, A reciprocating screw (5) is rotatably arranged on the inner top wall of the purification cylinder (2). A rotating shaft (3) is fixedly arranged on the reciprocating screw (5). A spiral blade (4) is fixedly arranged on the outer peripheral surface of the rotating shaft (3). A flow dividing box (6) for controlling the rotation of the reciprocating screw (5) is vertically slidably arranged in the purification cylinder (2). The purification cylinder (2) is filled with an impurity adsorbent. A circulating lifting mechanism for passively controlling the reciprocating movement of the flow dividing box (6) is fixedly arranged on the purification cylinder (2). The circulating lifting mechanism includes two hydraulic boxes (10) fixedly arranged on the outer wall of the purification cylinder (2). A counterweight block (11) is slidably arranged in each hydraulic box (10). A linkage cylinder (13) is fixedly arranged in the purification cylinder (2). A lifting rod (12) is slidably arranged in each linkage cylinder (13). A communicating pipe (14) is fixedly connected in a one-to-one correspondence between each linkage cylinder (13) and each hydraulic box (10). Each lifting rod (12) is fixedly connected to the bottom wall of the flow dividing box (6). Two fixing frames (31) are fixedly arranged on the inner bottom wall of the flow dividing box (6). A permanent magnet plate (34) is slidably arranged in each fixing frame (31). A sliding rod (32) is fixedly arranged on each permanent magnet plate (34). Two top plates (33) are fixedly arranged on the inner wall of the purification cylinder (2). Two liquid leakage holes are formed at the bottom of the flow dividing box (6). Each fixing frame (31) is fixedly arranged on each liquid leakage hole in a one-to-one correspondence.

2. The ethyl acetate production equipment according to claim 1, wherein, A screen (7) is fixedly arranged on the flow dividing box (6). Two groups of push plates (41) are fixedly arranged on the screen (7). Two sliding plates (42) are slidably arranged on the inner top wall of the purification cylinder (2). A sliding frame (45) is fixedly arranged on the side wall of each sliding plate (42). Two push wheels (46) are rotatably arranged on each sliding frame (45).

3. An ethyl acetate production device according to claim 2, characterized in that, Fixing plates (43) are slidably arranged on both sides of each sliding plate (42). Each fixing plate (43) is fixedly connected to the inner top wall of the purification cylinder (2). A rotating rod (44) is rotatably arranged between two adjacent fixing plates (43). A pull rope (47) is fixedly arranged on each sliding frame (45). One end of each pull rope (47) away from the sliding frame (45) is fixedly connected to the screen (7) after bypassing each rotating rod (44) in a one-to-one correspondence.

4. An ethyl acetate production device according to claim 1, characterized in that, A buffer screen (8) is fixedly arranged in the purification cylinder (2).

5. An ethyl acetate production device according to claim 4, characterized in that, Two drain pipes (21) are fixedly arranged at the bottom of the purification cylinder (2). An absorbent layer (23) is arranged in each drain pipe (21).

6. The ethyl acetate production equipment according to claim 5, characterized in that, A lifting frame (15) is fixedly arranged on each counterweight block (11). A connecting rod (18) is fixedly arranged at the bottom of each lifting frame (15). A piston (17) is fixedly arranged at one end of each connecting rod (18) away from the lifting frame (15). A sleeve (16) is fixedly connected to each drain pipe (21). Each piston (17) is slidably arranged in each sleeve (16) in a one-to-one correspondence.

7. An ethyl acetate production device according to claim 6, characterized in that, A plug cap (22) is threadedly connected to one end of each drain pipe (21) away from the purification cylinder (2).

8. A method for producing ethyl acetate, which is realized by the ethyl acetate production equipment described in any one of claims 1-7, comprising the following steps: S1: Prepare ethyl acetate through the condensation reaction of acetaldehyde; S2: Remove the catalyst. Add distilled water to the body of a kettle reactor to destroy the excess catalyst; S3: Adsorb and remove impurities: Put the crude ethyl acetate into the above-mentioned ethyl acetate production equipment for adsorption and filtration to obtain the preliminarily purified ethyl acetate, and then distill out the crude ethyl acetate through an evaporator; S4: Rectify and purify. Pass through three rectifying towers, namely a deacetaldehyde tower, a deethanol tower and a deheavy component tower in sequence to remove acetaldehyde, ethanol and acetal in the crude ethyl acetate respectively.

Citation Information

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  • A method for purifying high-purity ethyl acetate

    CN112299999B

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    CN113750941A

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