CN118236960B - Three-kettle serial continuous DMM esterification reaction device and method - Google Patents
Three-kettle serial continuous DMM esterification reaction device and method Download PDFInfo
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- CN118236960B CN118236960B CN202410666578.4A CN202410666578A CN118236960B CN 118236960 B CN118236960 B CN 118236960B CN 202410666578 A CN202410666578 A CN 202410666578A CN 118236960 B CN118236960 B CN 118236960B
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 235
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 190
- 230000001360 synchronised effect Effects 0.000 claims abstract description 48
- 239000000463 material Substances 0.000 claims abstract description 45
- 238000005192 partition Methods 0.000 claims abstract description 37
- 230000032050 esterification Effects 0.000 claims abstract description 21
- 238000009833 condensation Methods 0.000 claims abstract description 11
- 230000005494 condensation Effects 0.000 claims abstract description 11
- 238000004891 communication Methods 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 53
- 238000003860 storage Methods 0.000 claims description 46
- 238000003756 stirring Methods 0.000 claims description 40
- 238000001816 cooling Methods 0.000 claims description 39
- 238000007789 sealing Methods 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 20
- 238000009834 vaporization Methods 0.000 claims description 19
- 238000009826 distribution Methods 0.000 claims description 18
- 230000008016 vaporization Effects 0.000 claims description 18
- 239000012295 chemical reaction liquid Substances 0.000 claims description 13
- 125000006850 spacer group Chemical group 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 abstract description 16
- 238000012545 processing Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000012824 chemical production Methods 0.000 abstract description 2
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000010517 secondary reaction Methods 0.000 description 10
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- XREKLQOUFWBSFH-UHFFFAOYSA-N dimethyl 2-acetylbutanedioate Chemical compound COC(=O)CC(C(C)=O)C(=O)OC XREKLQOUFWBSFH-UHFFFAOYSA-N 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MHKKFFHWMKEBDW-UHFFFAOYSA-N dimethyl 2,5-dioxocyclohexane-1,4-dicarboxylate Chemical compound COC(=O)C1CC(=O)C(C(=O)OC)CC1=O MHKKFFHWMKEBDW-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical production, in particular to a three-kettle serial continuous DMM esterification reaction device and method, comprising a vertical support frame, wherein a continuous reaction kettle is vertically arranged in the middle of the vertical support frame, and the device further comprises: the grading division plates are horizontally arranged in the continuous reaction kettle, two grading division plates are arranged in parallel in the continuous reaction kettle, and divide the internal space of the continuous reaction kettle into three independent closed reaction bins. According to the invention, the two grading partition plates are arranged in parallel in the integral continuous reaction kettle, so that the interior of the continuous reaction kettle is sequentially divided into the first-stage reaction bin, the second-stage reaction bin and the third-stage reaction bin at intervals from bottom to top, three-stage continuous reaction processing is realized, vaporized hydrated methanol can be directly used for the next-stage esterification without condensation, the synchronous control reaction is facilitated, the quantity of materials needing condensation and heating steam are reduced, and the energy consumption is reduced.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a three-kettle serial continuous DMM esterification reaction device and method.
Background
Dimethyl maleate (DMM), a chemical, a colorless transparent oily liquid, can be used as a reactive plasticizer. And the DMM is used as a main raw material of dimethyl succinate (DMS) and dimethyl acetylsuccinate (DMAS), the quality and the yield of the DMM directly determine the quality and the yield of DMAS and DMS and even DMSS, and an esterification kettle is generally required for esterification production during DMM production.
In the existing esterification production, the esterification is a single kettle intermittent reaction, the steam consumption is high, the condensation amount of vaporized hydrated methanol is high, and the vaporized hydrated methanol of a plurality of esterification kettles is required to be condensed by condensers and then fed into a storage tank during production, but the esterification kettles are distilled at the same time, so that the pressure and the requirements on the condensers are high, a large amount of heat is required to be cooled and conducted in a short time, the condensed water temperature of a cooling tower required by condensation can be overhigh, especially in summer, the operation of a plurality of kettles is performed at the same time, the misoperation is easy, the energy consumption is high, and the methanol dripping amount is large.
Disclosure of Invention
In view of the above, the invention aims to provide a three-kettle serial continuous DMM esterification reaction device and method, which are used for solving the problems that all hydrated methanol vaporized by a plurality of esterification kettles needs to be condensed by a condenser and then fed into a storage tank, but the plurality of esterification kettles are distilled at the same time, the pressure and the requirement on the condenser are high, a large amount of heat is required to be cooled and conducted in a short time, and the condensing temperature of a cooling tower required for condensation is too high.
Based on the above purpose, the invention provides a three-kettle serial continuous DMM esterification reaction device, which comprises a vertical support frame, wherein a continuous reaction kettle is vertically arranged in the middle of the vertical support frame, and the three-kettle serial continuous DMM esterification reaction device further comprises:
the continuous reaction kettle is characterized by comprising a continuous reaction kettle, wherein the continuous reaction kettle is provided with a first-stage reaction bin, a second-stage reaction bin and a third-stage reaction bin;
the raw material input pipe is connected and arranged at the top of the continuous reaction kettle, the vaporization output pipe is further connected and arranged above the three-stage reaction bin, the bottoms of the raw material input pipe and the vaporization output pipe are communicated with the three-stage reaction bin, the bottom of the continuous reaction kettle is connected and provided with the material output pipe, and the material output pipe is communicated with the first-stage reaction bin;
the first-stage reaction bin, the second-stage reaction bin and the third-stage reaction bin are communicated with each other sequentially through a communication conveying pipe, and a one-way conveying valve is arranged in the middle of the communication conveying pipe;
the annular distribution groove is circumferentially and uniformly arranged in the grading partition plate, the top surface of the grading partition plate is circumferentially and uniformly provided with a plurality of vaporization conveying holes in a surrounding mode, the annular distribution groove is communicated with the upper side of the grading partition plate through the vaporization conveying holes, the outer side of the annular distribution groove is connected and provided with an inverted U-shaped conveying pipe, and the outer end of the inverted U-shaped conveying pipe is communicated with the top of a reaction bin positioned on the lower side of the grading partition plate of the annular distribution groove;
The constant pressure drip is arranged at the top of the primary reaction bin, and a methanol conveying pipe is connected with the outer side of the constant pressure drip.
Further, the one-way conveying valve comprises a communication channel, a conical sealing block is arranged on the inner side of the communication channel in a jogged sliding mode, a conical interface is arranged at the top of the communication channel, the conical interface and the conical sealing blocks are matched with each other in size, a sealing spring is arranged below the conical sealing block, and the sealing spring pushes the conical sealing block to be embedded into the conical interface so as to seal the communication channel.
Further, the center department of continuous reation kettle's top center department and the center department of classifying partition board all run through and are provided with the center uide bushing, the inside nested slip of center uide bushing is provided with the center connecting rod, the inside of one-level reaction chamber, second grade reaction chamber and tertiary reaction chamber is all horizontal gomphosis slip and is provided with the interval delivery board, the interval delivery board is divided into upper and lower two parts with the reaction chamber interval, the centre of interval delivery board runs through and is provided with a plurality of intercommunication solenoid valves, all interval delivery boards all with center connecting rod fixed connection, the center connecting rod drives all interval delivery boards and reciprocates synchronous movement.
Further, the top of vertical support frame is provided with vertical guide way, the top connection of center connecting rod is provided with synchronous crane, synchronous crane passes through vertical guide way and vertical support frame sliding connection, synchronous crane's outside connection is provided with the lift swivel nut, the inboard nest of lift swivel nut is provided with the lift screw, the axle head connection of lift screw is provided with elevator motor.
Further, the inside of one-level reaction storehouse, second grade reaction storehouse and tertiary reaction storehouse all is provided with synchronous stirring frame, synchronous stirring frame's outside is encircled and is provided with the stirring go-between, synchronous stirring frame passes through the stirring go-between and is connected with reaction storehouse inner wall rotation, synchronous stirring frame's below is circumference form evenly around being provided with a plurality of vertical stirring vane, the centre of interval delivery plate corresponds and is provided with a plurality of direction sliding sleeves, interval delivery plate passes through direction sliding sleeve and vertical stirring vane sliding connection, interval delivery plate passes through direction sliding sleeve and drives all vertical stirring vane and synchronous stirring frame synchronous rotation, be provided with rotatory adapter sleeve between center connecting rod and the synchronous lifting frame, center connecting rod passes through rotatory adapter sleeve and synchronous lifting frame rotation to be connected, rotatory adapter sleeve's top connection is provided with agitator motor, agitator motor with synchronous lifting frame fixed connection.
Further, the constant pressure dropwise add ware is including fixed dropwise add ring, be the circumference form in the middle of fixed dropwise add ring and evenly encircle and be provided with a plurality of ration liquid storage tanks, the vertical fixed dropwise add ring setting that runs through of ration liquid storage tank, the upper and lower both ends of ration liquid storage tank all are provided with the intercommunication opening, the inside and outside both sides of ration liquid storage tank all encircle the interval and are provided with cooling channel, are connected respectively in the middle of cooling channel's the left and right sides and are provided with cooling conveyer pipe and cooling back flow, cooling conveyer pipe with methanol conveyer pipe intercommunication each other, be connected between cooling conveyer pipe and the methanol conveyer pipe and be provided with the circulation delivery pump, the outside nestification of fixed dropwise add ring is provided with the interval insulation cover.
Further, the top rotation connection of fixed dropwise add ring is provided with rotatory conveying ring, the centre of rotatory conveying ring is the even annular and is provided with a plurality of dropwise add open grooves and unit conveyer pipe that encircle of circumference, the vertical rotatory conveying ring setting that runs through of dropwise add open groove, dropwise add open groove and unit conveyer pipe set up in turn, dropwise add open groove and unit conveyer pipe with correspond each other between the ration reservoir and set up, the bottom of unit conveyer pipe is provided with the delivery opening, rotatory conveying ring drives the open groove of dropwise add and delivery opening and the ration reservoir between the circulation coincide each other and the mismatch when rotating.
Further, the top connection of unit conveyer pipe is provided with the rotation conveying ring, the outside of rotation conveying ring with cooling back flow interconnect, the cooling back flow passes through rotation conveying ring and all unit conveyer pipes intercommunication each other, the cooling back flow passes through rotation conveying ring and all unit conveyer pipes rotate to be connected.
Further, the below rotation connection of fixed dropwise add ring is provided with rotatory dropwise add ring, rotatory dropwise add ring with rotatory conveying ring is fixed connection each other, rotatory dropwise add ring with rotatory conveying ring synchronous rotation, the centre of rotatory dropwise add ring is circumference form evenly and encircles and be provided with a plurality of dropwise add openings, the vertical rotatory dropwise add ring setting that runs through of dropwise add opening, the dropwise add opening with correspond each other between the ration reservoir and set up, the dropwise add opening with the open groove of dropwise add sets up on same vertical central line, it coincides each other and the mistake to drive the circulation between dropwise add opening and the ration reservoir when rotatory dropwise add ring rotates.
A three-kettle serial continuous DMM esterification reaction method comprises the following steps:
Three batches of dissolved materials are sequentially added into three reaction chambers through a raw material input pipe, then methanol is dripped into the first-stage reaction chamber through a methanol conveying pipe and a constant pressure dripper for esterification reaction, vaporized hydrated methanol in the first-stage reaction chamber is conveyed to an annular distribution groove of a grading partition plate at the bottom of the second-stage reaction chamber through an inverted U-shaped conveying pipe connected with the top of the first-stage reaction chamber, and is further uniformly conveyed into materials in the second-stage reaction chamber through a vaporization conveying hole, the esterification reaction is participated in the second-stage reaction chamber, the vaporized hydrated methanol is further conveyed into the third-stage reaction chamber to participate in the esterification reaction, the vaporized hydrated methanol is directly used for the next-stage esterification without condensation, after the esterification of the first-stage reaction chamber is output through a material output pipe, the reaction liquid in the second-stage reaction chamber and the third-stage reaction chamber is respectively and sequentially transferred into the first-stage reaction chamber through a communication conveying pipe and a one-way conveying valve, the emptied third-stage reaction chamber is added with a new batch of dissolved materials through a raw material input pipe, and is continuously dripped after heating, and the steps are circulated, so that the continuous reaction processing of three stages is realized.
The invention has the beneficial effects that: according to the three-kettle serial continuous DMM esterification reaction device, two grading partition plates are arranged in parallel in the integral continuous reaction kettle, the interior of the continuous reaction kettle is sequentially divided into a first-stage reaction bin, a second-stage reaction bin and a third-stage reaction bin at intervals from bottom to top, the three reaction bins are sequentially connected with each other through a communicating conveying pipe on the grading partition plates, and the on-off of the communicating conveying pipe can be controlled through a one-way conveying valve, so that three batches of dissolved materials can be simultaneously added into the three reaction bins during production, then methanol is dropwise added from the first-stage reaction bin during esterification, vaporized hydrated methanol can be conveyed to enter the second-stage reaction bin through an inverted U-shaped conveying pipe for esterification reaction, the hydrated methanol vaporized from the second-stage reaction bin is further conveyed to the third-stage reaction bin for esterification reaction, after the esterification of the first-stage reaction bin is completed, the reaction liquid in the second-stage reaction bin and the third-stage reaction bin can be sequentially transferred into the first-stage reaction bin and the third-stage reaction bin through the communicating conveying pipe and the one-way conveying valve respectively, the emptied third-stage reaction bin can be simultaneously added into the first-stage reaction bin and the third-stage reaction bin through the communicating conveying pipe, the new-stage conveying pipe can be continuously heated, the heating up can be continuously controlled, the continuous heating of the materials can be reduced, the continuous heating and the continuous heating of the materials can be realized, the continuous heating and the continuous heating of the materials can be continuously cooled, and the continuous heating process of the steam can be realized, and the continuous heating and the steam can be reduced, and the continuous heating and the heating can be conveniently cooled.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of the internal structure of a continuous reactor according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a front structure of an embodiment of the present invention;
FIG. 3 is a schematic view of a back structure of an embodiment of the present invention;
FIG. 4 is a schematic view showing a lifting state of a spacer transport plate according to an embodiment of the present invention;
FIG. 5 is a schematic structural view of a continuous reactor according to an embodiment of the present invention;
FIG. 6 is a schematic view of a hierarchical spacer plate according to an embodiment of the present invention;
FIG. 7 is a schematic view of a one-way transfer valve according to an embodiment of the present invention;
FIG. 8 is a schematic view of a spacer transport plate according to an embodiment of the present invention;
FIG. 9 is a schematic view showing the structure of a constant pressure drip in accordance with an embodiment of the present invention;
FIG. 10 is a schematic view of a stationary drip ring according to an embodiment of the present invention;
FIG. 11 is a schematic view showing a structure of a cooling channel according to an embodiment of the present invention;
Fig. 12 is a schematic structural view of a rotary conveying ring according to an embodiment of the present invention.
Marked in the figure as:
1. A continuous reaction kettle; 101. grading division plates; 102. a center guide sleeve; 103. an annular distribution groove; 104. vaporization delivery aperture; 105. an inverted U-shaped conveying pipe; 106. an electromagnetic on-off valve; 2. a communicating conveying pipe; 201. a one-way delivery valve; 202. a communication passage; 203. a conical interface; 204. locking the electromagnet; 205. a conical sealing block; 206. a seal spring; 207. locking the magnetic ring; 3. a vertical support frame; 301. a vertical guide groove; 302. lifting screw rods; 303. a lifting motor; 304. a synchronous lifting frame; 305. lifting the screw sleeve; 306. rotating the connecting sleeve; 307. a stirring motor; 4. a first-stage reaction bin; 401. a second-stage reaction bin; 402. a third-stage reaction bin; 403. a raw material input pipe; 404. a material output pipe; 405. a vaporisation output tube; 406. an air pressure regulating valve; 5. a center connecting rod; 501. a spacing conveying plate; 502. a communication electromagnetic valve; 503. a guide sliding sleeve; 504. a synchronous stirring frame; 505. stirring the connecting ring; 506. a vertical stirring blade; 6. a constant pressure drip; 601. a methanol delivery pipe; 602. a circulating delivery pump; 603. an arc-shaped toothed ring; 604. a rotary gear; 605. dropping a motor; 7. fixing a dripping ring; 701. a quantitative liquid storage tank; 702. a communication opening; 703. a cooling channel; 704. cooling the conveying pipe; 705. a cooling return pipe; 706. a spacer insulation sleeve; 8. rotating the conveying ring; 801. dripping an open groove; 802. a unit conveying pipe; 803. a delivery opening; 804. rotating the conveying ring; 805. rotating the dropping ring; 806. the opening was added dropwise.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, fig. 6, fig. 7 and fig. 8, a three-kettle serial continuous DMM esterification reaction device includes a vertical support frame 3, a continuous reaction kettle 1 is vertically arranged in the middle of the vertical support frame 3, and the device further includes:
the grading division plates 101 are horizontally arranged in the continuous reaction kettle 1, two grading division plates 101 are arranged in parallel in the continuous reaction kettle 1, the two grading division plates 101 divide the internal space of the continuous reaction kettle 1 into three independent closed reaction chambers, and the three reaction chambers are a first-stage reaction chamber 4, a second-stage reaction chamber 401 and a third-stage reaction chamber 402 from bottom to top in sequence;
The raw material input pipe 403 is connected and arranged at the top of the continuous reaction kettle 1, the vaporization output pipe 405 is also connected and arranged above the three-stage reaction bin 402, the bottoms of the raw material input pipe 403 and the vaporization output pipe 405 are communicated with the three-stage reaction bin 402, the bottom of the continuous reaction kettle 1 is connected and provided with the material output pipe 404, and the material output pipe 404 is communicated with the first-stage reaction bin 4;
The communication conveying pipe 2 is arranged in the middle of the grading partition plate 101, the first-stage reaction bin 4, the second-stage reaction bin 401 and the third-stage reaction bin 402 are communicated with each other sequentially through the communication conveying pipe 2, and a one-way conveying valve 201 is arranged in the middle of the communication conveying pipe 2;
The annular distribution groove 103 is circumferentially and uniformly arranged in the grading division plate 101, a plurality of vaporization conveying holes 104 are circumferentially and uniformly circumferentially formed in the top surface of the grading division plate 101, the annular distribution groove 103 is mutually communicated with the upper side of the grading division plate 101 through the vaporization conveying holes 104, an inverted U-shaped conveying pipe 105 is connected and arranged on the outer side of the annular distribution groove 103, and the outer end of the inverted U-shaped conveying pipe 105 is mutually communicated with the top of a reaction bin positioned on the lower side of the grading division plate 101 of the annular distribution groove 103;
the constant pressure drip 6 is arranged at the top of the first-stage reaction bin 4, and a methanol delivery pipe 601 is connected with the outer side of the constant pressure drip 6.
In the embodiment, the device is characterized in that two grading partition plates 101 are arranged in parallel in the integral continuous reaction kettle 1, the interior of the continuous reaction kettle 1 is sequentially divided into a first-stage reaction chamber 4, a second-stage reaction chamber 401 and a third-stage reaction chamber 402 at intervals from bottom to top, the three reaction chambers are sequentially connected with each other through a communication conveying pipe 2 on the grading partition plates 101, the on-off of the communication conveying pipe 2 can be controlled through a one-way conveying valve 201 so as to seal or conduct the two corresponding reaction chambers, when in production, three batches of dissolved materials can be sequentially added into the three reaction chambers through a raw material input pipe 403, then methanol can be dripped into the first-stage reaction chamber 4 through a methanol conveying pipe 601 and a constant pressure dripper 6 for esterification reaction, vaporized hydrated methanol in the first-stage reaction chamber 4 is conveyed to an annular distribution groove 103 of the grading plate 101 at the bottom of the second-stage reaction chamber 401 through an inverted U-shaped conveying pipe 105 connected at the top of the first-stage reaction chamber 4, and further evenly conveying the mixture to the materials in the secondary reaction bin 401 through the vaporization conveying hole 104 so as to lead the secondary reaction bin 401 to carry out esterification reaction, an electromagnetic on-off valve 106 is arranged in the middle of the inverted U-shaped conveying pipe 105, so that the conveying amount is convenient to control, the hydrated methanol which is esterified and gasified in the secondary reaction bin 401 is also further conveyed to the tertiary reaction bin 402 to carry out esterification reaction, after the esterification reaction liquid in the primary reaction bin 4 is output through the material output pipe 404, the reaction liquid in the secondary reaction bin 401 and the tertiary reaction bin 402 can be respectively and sequentially transferred into the primary reaction bin 4 and the secondary reaction bin 401 through the communication conveying pipe 2 and the one-way conveying valve 201, the vacated tertiary reaction bin 402 is added with a new batch of dissolved materials through the raw material input pipe 403, and methanol is continuously added dropwise after heating, therefore, three-level continuous reaction processing is realized, vaporized hydrated methanol can be directly used for lower-level esterification without condensation, the synchronous control reaction is convenient, the quantity of materials which need to be condensed and the steam for heating are reduced, the energy consumption is reduced, and meanwhile, the methanol is directly conveyed and utilized, so that the methanol dripping use amount in the whole reaction production process can be reduced, and the production cost is reduced.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, fig. 6, fig. 7 and fig. 8, preferably, the unidirectional conveying valve 201 of the device comprises a communication channel 202, a conical sealing block 205 is arranged on the inner side of the communication channel 202 in a jogged sliding manner, a conical interface 203 is arranged on the top of the communication channel 202, the conical interface 203 and the conical sealing block 205 are mutually matched in size, a sealing spring 206 is arranged below the conical sealing block 205, the sealing spring 206 pushes the conical sealing block 205 to be embedded into the conical interface 203 so as to seal the communication channel 202, materials can only be conveyed from top to bottom, and a locking electromagnet 204 and a locking magnetic ring 207 are correspondingly arranged between the conical interface 203 and the conical sealing block 205, the conical sealing block 205 can be locked through the locking electromagnet 204 and the locking magnetic ring 207, and the opening force of the conical sealing block 205 is adjusted, so that the device is more convenient and flexible in use, and the air pressure regulating valve 406 is independently arranged on the top of the side wall of the three-stage reaction bin 402, and the internal air pressure of the reaction bin can be regulated through the air pressure regulating valve 406, so that the conical sealing block 205 can be pushed down to move to open from top to bottom through the locking electromagnet 204, and the three-stage materials can be conveyed from top to bottom.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, fig. 6, fig. 7 and fig. 8, preferably, the center of the top of the continuous reaction kettle 1 and the center of the grading partition plate 101 of the device are respectively provided with a central guide sleeve 102 in a penetrating way, the inner sides of the central guide sleeves 102 are provided with central connecting rods 5 in a nested sliding way, the insides of the primary reaction bin 4, the secondary reaction bin 401 and the tertiary reaction bin 402 are respectively provided with a partition conveying plate 501 in a horizontally embedded sliding way, the partition conveying plates 501 divide the reaction bin into an upper part and a lower part, the middle of the partition conveying plates 501 are respectively provided with a plurality of communication electromagnetic valves 502 in a penetrating way, all the partition conveying plates 501 are fixedly connected with the central connecting rods 5, the central connecting rods 5 drive all the partition conveying plates 501 to move synchronously up and down, the tops of the vertical supporting frames 3 are provided with vertical guide grooves 301, the tops of the central connecting rods 5 are connected with synchronous lifting frames 304, the synchronous lifting frame 304 is in sliding connection with the vertical supporting frame 3 through the vertical guide groove 301, the outer side of the synchronous lifting frame 304 is connected with a lifting screw sleeve 305, the inner side of the lifting screw sleeve 305 is nested to be provided with a lifting screw rod 302, the shaft end of the lifting screw rod 302 is connected with a lifting motor 303, so that the lifting motor 303 can drive the synchronous lifting frame 304 to move up and down along the vertical guide groove 301 through the lifting screw rod 302 and the lifting screw sleeve 305, and further drive all interval conveying plates 501 to move up and down synchronously through a central connecting rod 5, when the reaction is carried out, a communication electromagnetic valve 502 is opened, the central connecting rod 5 drives all interval conveying plates 501 to move up and down synchronously so as to stir the internal materials up and down, the reaction uniformity and the production quality are improved, when the reaction liquid transfer is required to be carried out after the reaction is completed, the interval conveying plates 501 move to be above the internal liquid level and the communication electromagnetic valve 502 is closed, so that the interval conveying plates 501 form a piston interval, the upper side and the lower side of the interval, and then the central connecting rod 5 drives all the interval conveying plates 501 to synchronously move downwards so as to downwards press the liquid below into the reaction bin of the next stage through the communication conveying pipe 2 and the one-way conveying valve 201, and the liquid pressed by the reaction bin of the previous stage is temporarily stored and isolated above the interval conveying plates 501 until the liquid is completely conveyed, and then the communication electromagnetic valve 502 is opened, so that synchronous material transfer can be realized, pressure and heat loss is reduced, and the integral continuous reaction production efficiency of the device is improved.
As shown in fig. 1,2, 3, 4,5,6,7 and 8, preferably, synchronous stirring frames 504 are arranged in the primary reaction chamber 4, the secondary reaction chamber 401 and the tertiary reaction chamber 402 of the device, stirring connection rings 505 are arranged on the outer sides of the synchronous stirring frames 504 in a surrounding manner, the synchronous stirring frames 504 are rotationally connected with the inner wall of the reaction chamber through the stirring connection rings 505, a plurality of vertical stirring blades 506 are uniformly arranged on the lower part of the synchronous stirring frames 504 in a surrounding manner in a circumferential manner, a plurality of guiding sliding sleeves 503 are correspondingly arranged in the middle of the interval conveying plates 501, the interval conveying plates 501 are in sliding connection with the vertical stirring blades 506 through the guiding sliding sleeves 503, the interval conveying plates 501 drive all the vertical stirring blades 506 and the synchronous stirring frames 504 to synchronously rotate through the guiding sliding sleeves 503, be provided with rotatory adapter sleeve 306 between center connecting rod 5 and the synchronous lifting frame 304, center connecting rod 5 rotates with synchronous lifting frame 304 through rotatory adapter sleeve 306 and is connected, the top connection of rotatory adapter sleeve 306 is provided with agitator motor 307, agitator motor 307 and synchronous lifting frame 304 fixed connection, thereby agitator motor 307 can drive center connecting rod 5 rotation, and center connecting rod 5 then drives all interval delivery boards 501 and rotates, interval delivery boards 501 further drive all vertical stirring vane 506 and synchronous stirring frame 504 synchronous rotation through direction sliding sleeve 503, in order to stir the inside material from top to bottom, improve reaction uniformity and production quality, and can realize the synchronous stirring processing of all reaction warehouses, be convenient for synchronous control reaction, improve the reaction uniformity.
As shown in fig. 1, 2,3, 4, 5, 6, 7, 8, 9, 10, 11 and 12, preferably, the constant pressure drip 6 of the device comprises a fixed drip ring 7, a plurality of quantitative liquid storage tanks 701 are uniformly and circumferentially arranged in the middle of the fixed drip ring 7 in a surrounding manner, the quantitative liquid storage tanks 701 vertically penetrate through the fixed drip ring 7, communication openings 702 are respectively arranged at the upper end and the lower end of the quantitative liquid storage tanks 701, a rotary conveying ring 8 is rotatably connected above the fixed drip ring 7, a plurality of drip open grooves 801 and unit conveying pipes 802 are uniformly and circumferentially arranged in the middle of the rotary conveying ring 8 in a surrounding manner, The dripping open groove 801 vertically penetrates through the rotary conveying ring 8, the dripping open groove 801 and the unit conveying pipe 802 are alternately arranged, the dripping open groove 801, the unit conveying pipe 802 and the quantitative liquid storage groove 701 are correspondingly arranged, the bottom end of the unit conveying pipe 802 is provided with a conveying opening 803, the rotary conveying ring 8 drives the dripping open groove 801, the conveying opening 803 and the quantitative liquid storage groove 701 to be overlapped and staggered circularly when rotating, meanwhile, a rotary dripping ring 805 is rotationally connected below the fixed dripping ring 7, the rotary dripping ring 805 is fixedly connected with the rotary conveying ring 8, the rotary dripping ring 805 and the rotary conveying ring 8 synchronously rotate, A plurality of dripping openings 806 are uniformly and circumferentially arranged in the middle of the rotary dripping ring 805 in a surrounding manner, the dripping openings 806 vertically penetrate through the rotary dripping ring 805, the dripping openings 806 and the quantitative liquid storage tanks 701 are correspondingly arranged, the dripping openings 806 and the dripping open tanks 801 are arranged on the same vertical central line, the rotary dripping ring 805 rotates to drive the dripping openings 806 and the quantitative liquid storage tanks 701 to be circularly overlapped and staggered, so that when the rotary conveying ring 8 and the rotary dripping ring 805 rotate, firstly, the conveying openings 803 arranged at the bottom ends of the unit conveying pipes 802 are overlapped with the communicating openings 702 above the quantitative liquid storage tanks 701, At this time, the communication opening 702 below the quantitative liquid storage tank 701 is closed by the rotary dropping ring 805, methanol is delivered to the inside of the quantitative liquid storage tank 701, then the rotary delivery ring 8 and the rotary dropping ring 805 continue to rotate by a certain angle, the unit delivery pipe 802 and the communication opening 702 above the quantitative liquid storage tank 701 are staggered with each other, the dropping open groove 801 and the communication opening 702 above the quantitative liquid storage tank 701 coincide with each other, and simultaneously the communication opening 702 below the quantitative liquid storage tank 701 and the dropping opening 806 coincide with each other, so that the communication openings 702 on the upper and lower sides of the quantitative liquid storage tank 701 are simultaneously opened, the pressure is balanced, the methanol in the quantitative liquid storage tank 701 naturally drops from the lower communication opening 702 and the dropping opening 806 by gravity, then the rotary conveying ring 8 and the rotary dropping ring 805 reversely rotate by the same angle, the communication openings 702 on the upper side and the lower side of the quantitative liquid storage tank 701 are simultaneously closed until the unit conveying pipe 802 and the communication opening 702 above the quantitative liquid storage tank 701 are overlapped again to complete a working cycle, the rotary conveying ring 8 and the rotary dropping ring 805 are connected with each other through the arc-shaped toothed ring 603 arranged on the inner side, the inner side of the arc-shaped toothed ring 603 is also meshed with the rotary gear 604, the shaft end of the rotary gear 604 is connected with the dropping motor 605, The dropping motor 605 is fixedly connected with the top of the three-stage reaction bin 402, the dropping motor 605 can drive the continuous circulation forward and reverse rotation of the rotary conveying ring 8 and the rotary dropping ring 805 through the rotary gear 604 and the arc-shaped toothed ring 603 to finish the quantitative dropping work of the methanol, the influence of the internal pressure of the reaction bin can be reduced when the methanol is dropped through the constant pressure dropping device 6, the slow dropping of the methanol is avoided, even the dropping can not be carried out, the quantitative dropping of the methanol can be realized, the reaction precision is convenient to control, and the overall reaction efficiency and the overall reaction quality are improved.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, fig. 6, fig. 7, fig. 8, fig. 9, fig. 10, fig. 11 and fig. 12, preferably, cooling channels 703 are arranged on the inner side and the outer side of the quantitative liquid storage tank 701 of the device at intervals, a cooling conveying pipe 704 and a cooling return pipe 705 are respectively connected between the left side and the right side of the cooling channels 703, the cooling channels 703 on the inner side and the outer side are mutually communicated, the cooling conveying pipe 704 is mutually communicated with the methanol conveying pipe 601, a circulating conveying pump 602 is connected between the cooling conveying pipe 704 and the methanol conveying pipe 601, a spacing heat insulation sleeve 706 is nested on the outer side of the fixed dropping ring 7, a rotary conveying ring 804 is connected on the top of the unit conveying pipe 802, the outer side of the rotary conveying ring 8 is mutually connected with the cooling return pipe 705, the cooling return pipe 705 is mutually communicated with all the unit conveying pipes 802 through the rotary conveying ring 804, the cooling return pipe 705 is rotationally connected with all unit conveying pipes 802 through a rotary conveying ring 804, methanol is conveyed to a cooling channel 703 through the cooling conveying pipe 704 to cool the quantitative liquid storage tank 701, then conveyed to the rotary conveying ring 8 through the cooling return pipe 705, and further conveyed to all unit conveying pipes 802 through the rotary conveying ring 8 uniformly, so that when the communication openings 702 on the upper side and the lower side of the quantitative liquid storage tank 701 are closed at the same time, the quantitative liquid storage tank 701 is cooled, high-pressure steam entering the quantitative liquid storage tank 701 is cooled and liquefied, the internal pressure of the quantitative liquid storage tank 701 is reduced, the subsequent unit conveying pipes 802 are convenient for conveying the methanol into the quantitative liquid storage tank 701, the influence of the internal pressure of a reaction bin is further reduced, meanwhile, the conveyed raw material methanol forms a circulating cooling medium, the heat is brought back again after the methanol is dripped, so as to reduce heat loss, maintain reaction temperature, further facilitate control of reaction precision and improve overall reaction efficiency and quality.
When in use, corresponding pipelines of the device are connected, three batches of dissolved materials are sequentially added into three reaction chambers through a raw material input pipe 403, then methanol is conveyed to a constant-pressure drip feeder 6 in a first-stage reaction chamber 4 through a methanol conveying pipe 601, a circulating conveying pump 602 is conveyed to a cooling channel 703 through a cooling conveying pipe 704 to cool a quantitative liquid storage tank 701, then conveyed to a rotary conveying ring 8 through a cooling return pipe 705, a drip motor 605 drives the rotary conveying ring 8 and a rotary drip ring 805 to continuously circulate forward and reversely rotate through a rotary gear 604 and an arc toothed ring 603, a conveying opening 803 arranged at the bottom end of a unit conveying pipe 802 is mutually overlapped with a communicating opening 702 above the quantitative liquid storage tank 701, At this time, the communication opening 702 below the quantitative liquid storage tank 701 is closed by the rotary dropping ring 805, methanol is delivered to the inside of the quantitative liquid storage tank 701, then the rotary delivery ring 8 and the rotary dropping ring 805 continue to rotate by a certain angle, the unit delivery pipe 802 and the communication opening 702 above the quantitative liquid storage tank 701 are staggered with each other, the dropping open groove 801 and the communication opening 702 above the quantitative liquid storage tank 701 coincide with each other, and simultaneously the communication opening 702 below the quantitative liquid storage tank 701 and the dropping opening 806 coincide with each other, so that the communication openings 702 on the upper and lower sides of the quantitative liquid storage tank 701 are simultaneously opened, the pressure is balanced, The methanol in the quantitative liquid storage tank 701 naturally drops by the lower communication opening 702 and the dropping opening 806 under the gravity, then the rotary conveying ring 8 and the rotary dropping ring 805 reversely rotate by the same angle, the communication openings 702 on the upper side and the lower side of the quantitative liquid storage tank 701 are simultaneously closed until the unit conveying pipe 802 is overlapped with the communication opening 702 above the quantitative liquid storage tank 701 again, the methanol drops into the first-stage reaction bin 4 for esterification reaction during the cyclic rotation, the vaporized hydrated methanol in the first-stage reaction bin 4 is conveyed to the annular distribution groove 103 of the grading partition plate 101 at the bottom of the second-stage reaction bin 401 through the inverted U-shaped conveying pipe 105 connected with the top of the first-stage reaction bin 4, And further evenly conveying the mixture to the materials in the secondary reaction bin 401 through the vaporization conveying holes 104, wherein esterification reaction is participated in the secondary reaction bin 401, and the hydrated methanol which is esterified and gasified in the secondary reaction bin 401 is also further conveyed to the tertiary reaction bin 402 to participate in the esterification reaction, the gasified hydrated methanol is directly used for the next-stage esterification without condensation, when the reaction liquid after the esterification of the primary reaction bin 4 is output through the material output pipe 404, the lifting motor 303 drives the synchronous lifting frame 304 to move up and down along the vertical guide groove 301 through the lifting screw 302 and the lifting screw sleeve 305, and further drives all the interval conveying plates 501 to move up and down synchronously through the central connecting rod 5, The interval conveying plate 501 moves to the upper part of the inner liquid level and closes the communication electromagnetic valve 502, so that the interval conveying plate 501 forms a piston interval, the upper side and the lower side are separated, then the central connecting rod 5 drives all the interval conveying plates 501 to synchronously move downwards, so that the liquid below is downwards pressed into the reaction chamber of the next stage through the communication conveying pipe 2 and the one-way conveying valve 201, the liquid pressed by the reaction chamber of the previous stage is temporarily stored and isolated above the interval conveying plate 501 until the liquid is completely conveyed, the communication electromagnetic valve 502 is opened again, the synchronous transfer of materials is realized, the reaction liquid inside the second-stage reaction chamber 401 and the third-stage reaction chamber 402 is respectively transferred into the first-stage reaction chamber 4 and the second-stage reaction chamber 401 in sequence through the communication conveying pipe 2 and the one-way conveying valve 201, And the new batch of dissolved materials is added into the vacated three-stage reaction bin 402 through the raw material input pipe 403, methanol is continuously added dropwise after the temperature is raised, and the steps are circulated, so that three-stage continuous reaction processing is realized.
A three-kettle serial continuous DMM esterification reaction method comprises the following steps:
Three batches of dissolved materials are sequentially added into three reaction bins through a raw material input pipe 403, then methanol is dripped into a first-stage reaction bin 4 through a methanol conveying pipe 601 and a constant pressure dripper 6 for esterification reaction, vaporized hydrated methanol in the first-stage reaction bin 4 is conveyed to an annular distribution groove 103 of a grading partition plate 101 at the bottom of a second-stage reaction bin 401 through an inverted U-shaped conveying pipe 105 connected with the top of the first-stage reaction bin 4, and is further uniformly conveyed into materials in the second-stage reaction bin 401 through a vaporization conveying hole 104, the esterification reaction is participated in the second-stage reaction bin 401, the esterified vaporized hydrated methanol in the second-stage reaction bin 401 is also further conveyed to a third-stage reaction bin 402 for esterification reaction, the vaporized hydrated methanol is directly used for next-stage esterification without condensation, after the esterification reaction liquid in the first-stage reaction bin 4 is output through a material output pipe 404, the reaction liquid in the second-stage reaction bin 401 and the third-stage reaction bin 402 is sequentially transferred to the first-stage reaction bin 4 and the second-stage reaction bin 401 through a communication conveying pipe 201 respectively, the emptied third-stage reaction bin 402 is added with a new dissolved material through a raw material input pipe 403, and then the esterification reaction is dripped, and the continuous processing steps are realized.
The three-kettle serial continuous DMM esterification reaction device provided by the invention is characterized in that two grading partition boards 101 are arranged in parallel in the integral continuous reaction kettle 1, the interior of the continuous reaction kettle 1 is sequentially divided into a first-stage reaction bin 4, a second-stage reaction bin 401 and a third-stage reaction bin 402 at intervals from bottom to top, the three reaction bins are sequentially connected with each other through a communicating conveying pipe 2 on the grading partition boards 101, and the communicating conveying pipe 2 is controlled to be on-off through a one-way conveying valve 201, so that three batches of dissolved materials can be simultaneously added into the three reaction bins during production, then methanol is dripped into the first-stage reaction bin 4 during esterification, vaporized hydrated methanol can be conveyed into the second-stage reaction bin 401 through an inverted U-shaped conveying pipe 105 for esterification reaction, and the hydrated methanol which is esterified and gasified in the second-stage reaction bin 401 is further conveyed to the third-stage reaction bin 402 for esterification reaction, after the reaction liquid which is esterified in the first-stage reaction bin 4 is output through the material output pipe 404, the reaction liquid in the second-stage reaction bin 401 and the third-stage reaction bin 402 can be respectively and sequentially transferred into the first-stage reaction bin 4 and the second-stage reaction bin 401 through the communication conveying pipe 2 and the one-way conveying valve 201, a new batch of dissolved materials is added into the vacated third-stage reaction bin 402 through the raw material input pipe 403, and methanol is continuously added dropwise after heating, so that three-stage continuous reaction processing is realized, the gasified hydrated methanol can be directly used for lower-stage esterification without condensation, the synchronous control reaction is facilitated, the material quantity and heating steam which are required to be condensed at the same time are reduced, and the energy consumption is reduced.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity. Any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. Three cauldron series connection serialization DMM esterification reaction device, including vertical support frame (3), the vertical continuous reation kettle (1) that is provided with in centre of vertical support frame (3), its characterized in that still includes:
The device comprises a continuous reaction kettle (1), a grading partition plate (101), a first-stage reaction bin (4), a second-stage reaction bin (401) and a third-stage reaction bin (402), wherein the grading partition plate (101) is horizontally arranged in the continuous reaction kettle (1), two grading partition plates (101) are arranged in parallel in the continuous reaction kettle (1), and the two grading partition plates (101) divide the internal space of the continuous reaction kettle (1) into three independent closed reaction bins from bottom to top;
the raw material input pipe (403) is connected and arranged at the top of the continuous reaction kettle (1), the vaporization output pipe (405) is further connected and arranged above the three-stage reaction bin (402), the bottoms of the raw material input pipe (403) and the vaporization output pipe (405) are communicated with the three-stage reaction bin (402), the bottom of the continuous reaction kettle (1) is connected and provided with the material output pipe (404), and the material output pipe (404) is communicated with the first-stage reaction bin (4);
The first-stage reaction bin (4), the second-stage reaction bin (401) and the third-stage reaction bin (402) are communicated with each other sequentially through the communication conveying pipe (2), and a one-way conveying valve (201) is arranged in the middle of the communication conveying pipe (2);
The annular distribution groove (103) is circumferentially and uniformly arranged in the grading partition plate (101), a plurality of vaporization conveying holes (104) are circumferentially and uniformly formed in the top surface of the grading partition plate (101), the annular distribution groove (103) is mutually communicated with the upper side of the grading partition plate (101) through the vaporization conveying holes (104), an inverted U-shaped conveying pipe (105) is connected and arranged on the outer side of the annular distribution groove (103), and the outer end of the inverted U-shaped conveying pipe (105) is mutually communicated with the top of a reaction bin positioned on the lower side of the grading partition plate (101) of the annular distribution groove (103);
the constant pressure dropwise add ware (6) set up in the top of one-level reaction storehouse (4), the outside connection of constant pressure dropwise add ware (6) is provided with methyl alcohol conveyer pipe (601).
2. The three-kettle serial continuous DMM esterification reaction device according to claim 1, wherein the one-way conveying valve (201) comprises a communication channel (202), a conical sealing block (205) is arranged on the inner side of the communication channel (202) in a jogged sliding manner, a conical interface (203) is arranged on the top of the communication channel (202), the conical interface (203) and the conical sealing block (205) are mutually matched in size, a sealing spring (206) is arranged below the conical sealing block (205), and the sealing spring (206) pushes the conical sealing block (205) to be embedded into the conical interface (203) so as to seal the communication channel (202).
3. The three-kettle serial continuous DMM esterification reaction device according to claim 1, wherein a central guide sleeve (102) is arranged at the center of the top of the continuous reaction kettle (1) and the center of the grading partition plate (101) in a penetrating manner, a central connecting rod (5) is arranged on the inner side of the central guide sleeve (102) in a nested sliding manner, a partition conveying plate (501) is arranged in the first-stage reaction bin (4), the second-stage reaction bin (401) and the third-stage reaction bin (402) in a horizontally embedded sliding manner, the partition conveying plate (501) divides the reaction bin into an upper part and a lower part, a plurality of communication electromagnetic valves (502) are arranged in the middle of the partition conveying plate (501) in a penetrating manner, and all the partition conveying plates (501) are fixedly connected with the central connecting rod (5), and all the partition conveying plates (501) are driven to move up and down synchronously by the central connecting rod (5).
4. The three-kettle serial continuous DMM esterification reaction device according to claim 3, wherein a vertical guide groove (301) is formed in the top of the vertical support frame (3), a synchronous lifting frame (304) is connected to the top of the central connecting rod (5), the synchronous lifting frame (304) is slidably connected with the vertical support frame (3) through the vertical guide groove (301), a lifting screw sleeve (305) is connected to the outer side of the synchronous lifting frame (304), a lifting screw (302) is nested in the inner side of the lifting screw sleeve (305), and a lifting motor (303) is connected to the shaft end of the lifting screw (302).
5. The three-kettle serial continuous DMM esterification reaction device according to claim 4, wherein the first-stage reaction bin (4), the second-stage reaction bin (401) and the third-stage reaction bin (402) are respectively provided with a synchronous stirring frame (504), a stirring connecting ring (505) is arranged on the outer side of the synchronous stirring frame (504) in a surrounding manner, the synchronous stirring frame (504) is rotationally connected with the inner wall of the reaction bin through the stirring connecting ring (505), a plurality of vertical stirring blades (506) are uniformly arranged on the lower side of the synchronous stirring frame (504) in a surrounding manner in a circumferential manner, a plurality of guiding sliding sleeves (503) are correspondingly arranged in the middle of the interval conveying plate (501), the interval conveying plate (501) is in sliding connection with the vertical stirring blades (506) through the guiding sliding sleeves (503), the interval conveying plate (501) drives all the vertical stirring blades (506) and the synchronous stirring frame (504) to synchronously rotate through the guiding sliding sleeves (503), a rotary connecting sleeve (306) is arranged between the central connecting rod (5) and the synchronous lifting frame (304), the central connecting rod (5) is connected with the rotary connecting sleeve (306) through the rotary connecting sleeve (307), the stirring motor (307) is fixedly connected with the synchronous lifting frame (304).
6. The three-kettle serial continuous DMM esterification reaction device according to claim 1, wherein the constant pressure dropwise add ware (6) is including fixed dropwise add ring (7), the centre of fixed dropwise add ring (7) is circumference form evenly and encircles and be provided with a plurality of ration reservoir (701), the setting of fixed dropwise add ring (7) is run through vertically to ration reservoir (701), the upper and lower both ends of ration reservoir (701) all are provided with intercommunication opening (702), the inside and outside both sides of ration reservoir (701) all encircle the interval and are provided with cooling channel (703), the left and right sides intermediate junction of cooling channel (703) is provided with cooling conveyer pipe (704) and cooling back flow (705) respectively, cooling conveyer pipe (704) with be connected between methanol conveyer pipe (601) and be provided with circulation delivery pump (602), the outside nested of fixed dropwise add ring (7) is provided with spacer sleeve (706).
7. The three-kettle serial continuous DMM esterification reaction device according to claim 6, wherein a rotary conveying ring (8) is rotatably connected above the fixed dropping ring (7), a plurality of dropping open grooves (801) and unit conveying pipes (802) are uniformly and circumferentially arranged in the middle of the rotary conveying ring (8) in a surrounding mode, the dropping open grooves (801) vertically penetrate through the rotary conveying ring (8), the dropping open grooves (801) and the unit conveying pipes (802) are alternately arranged, the dropping open grooves (801), the unit conveying pipes (802) and the quantitative liquid storage tanks (701) are correspondingly arranged, conveying openings (803) are formed in the bottom ends of the unit conveying pipes (802), and the rotary conveying ring (8) drives the dropping open grooves (801), the conveying openings (803) and the quantitative liquid storage tanks (701) to be overlapped and staggered in a circulating mode when rotated.
8. The three-kettle serial continuous DMM esterification reaction device according to claim 7, wherein a rotary conveying ring (804) is connected to the top of the unit conveying pipe (802), the outer side of the rotary conveying ring (8) is connected with the cooling return pipe (705), the cooling return pipe (705) is communicated with all the unit conveying pipes (802) through the rotary conveying ring (804), and the cooling return pipe (705) is connected with all the unit conveying pipes (802) through the rotary conveying ring (804) in a rotary mode.
9. The three-kettle serial continuous DMM esterification reaction device according to claim 8, wherein a rotary drip ring (805) is rotatably connected below the fixed drip ring (7), the rotary drip ring (805) is fixedly connected with the rotary conveying ring (8), the rotary drip ring (805) and the rotary conveying ring (8) synchronously rotate, a plurality of drip openings (806) are uniformly and circumferentially arranged in the middle of the rotary drip ring (805) in a surrounding manner, the drip openings (806) vertically penetrate through the rotary drip ring (805), the drip openings (806) and the quantitative liquid storage tanks (701) are correspondingly arranged, the drip openings (806) and the drip opening tanks (801) are arranged on the same vertical central line, and the rotary drip ring (805) drives the drip openings (806) and the quantitative liquid storage tanks (701) to be overlapped and staggered in a circulating manner when rotating.
10. A three-kettle serial continuous DMM esterification reaction method according to any one of claims 1 to 9, comprising the steps of:
Three batches of dissolved materials are sequentially added into three reaction bins through a raw material input pipe (403), then methanol is dripped into a first-stage reaction bin (4) through a methanol conveying pipe (601) and a constant-pressure dripper (6) for esterification, vaporized hydrated methanol in the first-stage reaction bin (4) is conveyed to an annular distribution groove (103) of a grading partition plate (101) at the bottom of a second-stage reaction bin (401) through an inverted U-shaped conveying pipe (105) connected with the top of the first-stage reaction bin (4), the materials are further uniformly conveyed into the second-stage reaction bin (401) through a vaporization conveying hole (104), the esterification reaction is participated in the second-stage reaction bin (401), the hydrated methanol which is esterified and vaporized in the second-stage reaction bin (401) is also further conveyed into a third-stage reaction bin (402) for esterification reaction, the vaporized hydrated methanol is directly used for next-stage esterification without condensation, after the esterification reaction liquid in the first-stage reaction bin (4) is output through a material output pipe (404), the reaction liquid in the second-stage reaction bin (401) and the third-stage reaction bin (402) is conveyed into the first-stage reaction bin (201) through a communication conveying pipe (201) and a one-way valve respectively, the materials are continuously processed and the materials are dripped out from the first-stage reaction bin (401) through the first-stage reaction bin (401), and the new-stage reaction bin (4) are continuously processed, and the raw materials are continuously and the materials are continuously dripped out and processed.
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| CN203683140U (en) * | 2013-12-19 | 2014-07-02 | 宜兴新威利成稀土有限公司 | Multifunctional reaction kettle for preparing ultrafine yttrium oxide |
| CN117504783A (en) * | 2023-11-10 | 2024-02-06 | 贝鸿湖北能源科技有限公司 | Reaction kettle for regenerating fuel oil by using waste rubber plastic |
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| CN203683140U (en) * | 2013-12-19 | 2014-07-02 | 宜兴新威利成稀土有限公司 | Multifunctional reaction kettle for preparing ultrafine yttrium oxide |
| CN117504783A (en) * | 2023-11-10 | 2024-02-06 | 贝鸿湖北能源科技有限公司 | Reaction kettle for regenerating fuel oil by using waste rubber plastic |
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