CN114159817B

CN114159817B - High-purity dimethyl ester batch distillation device

Info

Publication number: CN114159817B
Application number: CN202111413570.XA
Authority: CN
Inventors: 陈伟; 林绍辉; 陈双龙
Original assignee: Anhui Yishang Textile Technology Co ltd
Current assignee: Anhui Yishang Textile Technology Co ltd
Priority date: 2021-11-25
Filing date: 2021-11-25
Publication date: 2023-01-31
Anticipated expiration: 2041-11-25
Also published as: CN114159817A

Abstract

The invention discloses a high-purity dimethyl ester batch rectification device, and particularly relates to the technical field of distillation separation. The reciprocating swing mechanism is driven by the servo speed-reducing motor, so that the swing blades and the ratchet plates on the swing blades can swing in a reciprocating manner, dimethyl ester raw materials in the rectifying kettle can be uniformly mixed, the use of the stirring blades and the stirring paddles is matched, the dimethyl ester raw materials are guaranteed to be more sufficient and thorough in rectification, the utilization rate of the rectifying raw materials is improved, the upper clamping plate and the lower clamping plate are respectively pushed to move by the two micro cylinders, the rubber pad I and the rubber pad II are attached to the reaction cover and the outer wall surface of the rectifying kettle, the sealing performance of the reaction cover and the rectifying kettle is improved, the rectifying quality is improved, and the excessive waste heat gas generated by the heating plate is conveyed to the waste heat collecting box for recycling of the hot gas.

Description

High-purity dimethyl ester batch distillation device

Technical Field

The invention relates to the technical field of distillation separation, in particular to a high-purity dimethyl ester batch rectification device.

Background

Dimethyl sulfate is colorless or yellowish transparent oily liquid, is an important organic synthetic chemical raw material, is mainly used as a methylating agent, is used in the industries of medicines, pesticides and the like, and is also called batch rectification. FIG. 1 is a structural diagram of the prior art, the method of controlling the addition rate of formic acid to make formic acid almost completely react in the rectifying column without falling into the column bottom can not only effectively improve the conversion rate of esterification reaction, but also can easily recover the methanol in the column bottom after the reaction is completed, the semi-continuous reaction rectifying method of synthesizing methyl formate by adding formic acid into the column body can achieve the conversion rate of formic acid of more than 90%, which is nearly twenty percent higher than the traditional method of synthesizing methyl formate by directly adding formic acid and methanol into the column bottom, and the purity of the methyl formate generated by the method can achieve more than 95%.

The rectification method of dimethyl sulfate and methyl formate is the same, and in the actual rectification process of dimethyl, the dimethyl raw materials are not uniformly mixed, so that the raw materials are wasted, the time of the subsequent process is increased, the rectification effect is not ideal, and the fractionation efficiency is low.

Disclosure of Invention

The invention aims to provide a high-purity dimethyl ester intermittent rectification device.A fixed plate is driven by a servo speed-reducing motor, a rotating shaft and a limiting slide rod which are connected with the fixed plate rotate along with the rotating shaft, the limiting slide rod circularly moves around the rotating shaft and drives a slide seat to slide on the limiting slide rod in a limiting way, the slide seat and a transmission arm rod rotate through a pin shaft to drive the transmission arm rod and two swinging pieces to reciprocate on the fixed rod, and a swinging blade and a ratchet plate on the swinging blade reciprocate to uniformly mix dimethyl ester raw materials in a rectification kettle, so that the dimethyl ester raw materials are more fully and thoroughly rectified, the utilization rate of the rectification raw materials is improved, and the problems in the background technology are solved.

The invention can be realized by the following technical scheme: a high-purity dimethyl ester batch rectification device comprises a rectification kettle, wherein the top end of the rectification kettle is connected with a reaction cover, a fixed rod is fixedly arranged on the inner wall of the rectification kettle, and a reciprocating swing mechanism is sleeved outside the fixed rod;

reciprocating swing mechanism includes the oscillating piece, the equal fixedly connected with transmission armed lever in both ends of oscillating piece, the one end of transmission armed lever is rotated through the round pin axle and is connected with the slide, the surface of slide is run through and is provided with spacing slide bar, spacing slide bar and slide sliding connection, the equal fixedly connected with fixed plate of surface and the one end of spacing slide bar, and the other end of spacing slide bar is fixed and is provided with the separation blade, two one side that is close to spacing slide bar between the fixed plate is fixed and is provided with the axis of rotation, the axis of rotation is rotated and is installed on the roof in the reaction lid.

The invention has the further technical improvements that: the surface of the middle part of the top end of the reaction cover is provided with an air outlet, and two servo speed reduction motors are symmetrically arranged on two sides of the air outlet.

The invention has further technical improvements that: the bottom of the servo speed reducing motor is provided with a mounting seat fixedly connected with the outer surface of the reaction cover, and the end part of an output shaft of the servo speed reducing motor penetrates through the reaction cover in a sealing mode and is fixed with the rotating shaft.

The invention has the further technical improvements that: the surface of the swinging piece is provided with a through hole, the swinging piece is sleeved on the fixed rod in a sliding mode, the two ends of the bottom of the swinging piece are fixedly connected with swinging blades, and ratchet plates are arranged on the surfaces of the two sides of each swinging blade.

The invention has further technical improvements that: surface mounting has driving motor at the bottom middle part of rectifying still, and rectifying still's internally mounted cover establishes the epaxial stirring leaf of driving motor pivot, the below of stirring leaf is provided with the stirring rake the same with rectifying still bottom shape, one side that rectifying still's bottom surface is close to driving motor is provided with the liquid outlet.

The invention has further technical improvements that: the inner chamber of rectifying still is equipped with the heating chamber, the inside in heating chamber is provided with the hot plate, bottom one side of rectifying still be equipped with the communicating waste heat export in heating chamber, the one end of waste heat export is connected with the waste heat collecting box that is used for waste heat recovery to utilize.

The invention has further technical improvements that: the rectifying still is equipped with annular lagging with the junction cover of reaction lid, miniature cylinder is all installed to the top and the bottom of annular lagging, and the inner wall sliding connection of annular lagging has the last cardboard with the little cylinder piston rod tip rigid coupling in top, the laminating of the below of going up the cardboard is provided with the lower cardboard with the little cylinder piston rod tip rigid coupling in below.

The invention has further technical improvements that: the inner wall laminating of going up the cardboard is provided with cushion one, the inner wall laminating of cardboard is provided with cushion two down, cardboard and last cardboard all set up to L shape structure down, cushion one and cushion two laminate with the terminal surface of reaction lid and rectifying still respectively.

Compared with the prior art, the invention has the following beneficial effects:

1. the fixed plate is driven by a servo speed-reducing motor, the rotating shaft connected with the fixed plate and the limiting slide rod rotate along with the rotating shaft, the limiting slide rod moves circularly around the rotating shaft and drives the slide seat to slide on the limiting slide rod in a limiting way, the slide seat and the driving arm rod rotate through a pin shaft, the driving arm rod and the two swinging parts are driven to reciprocate on the fixed rod, the swinging blade and the ratchet plate on the swinging blade swing in a reciprocating way, and the stirring blade and the stirring paddle are used in a matching way, so that the dimethyl ester raw material in the rectifying kettle can be uniformly mixed, the dimethyl ester raw material is ensured to be more sufficient and thorough during rectification, and the utilization rate of the rectification raw material is improved;

2. the upper clamping plate and the lower clamping plate are respectively pushed to move by the upper micro cylinder and the lower micro cylinder, and the first rubber pad and the second rubber pad are respectively attached to the outer wall surfaces of the reaction cover and the rectifying still under the pushing action of the upper clamping plate and the lower clamping plate, so that the sealing property of the reaction cover and the rectifying still is increased, the gas leakage phenomenon during rectification is avoided, the rectification quality is improved, and the rectification purity of the dimethyl ester raw material is ensured;

3. the excessive hot gas that the hot plate produced can be discharged by the communicating waste heat export of heating chamber to carry to in the waste heat collecting box, the waste heat collecting box is used for the collection of steam, supplies the cyclic utilization of steam, reduces the waste of resource.

Drawings

To facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.

FIG. 1 is a schematic diagram of a prior art structure;

FIG. 2 is a schematic view of the structural connection of the present invention;

FIG. 3 is a schematic view of a portion of the structure of the reciprocating swing mechanism of the present invention;

FIG. 4 is a schematic connection diagram of a three-dimensional structure of the reciprocating swing mechanism of the present invention;

FIG. 5 is an enlarged view of a portion of the invention at A in FIG. 2;

fig. 6 is a schematic perspective view of the annular shroud of the present invention.

In the figure: 1. a rectifying still; 2. a reaction cover; 3. an air outlet; 4. a delivery conduit; 5. a servo deceleration motor; 6. a mounting seat; 7. a reciprocating swing mechanism; 8. a liquid outlet; 9. a drive motor; 10. stirring blades; 11. a stirring paddle; 12. swinging the blades; 13. a ratchet plate; 14. a waste heat collecting box; 15. a rectifying tower; 16. a filler layer; 17. fixing the rod; 18. a drive arm; 19. a fixing plate; 20. a rotating shaft; 21. a limiting slide bar; 22. a baffle plate; 23. a slide base; 24. a swinging member; 25. a through hole; 26. a connecting rod; 27. a waste heat outlet; 28. a heating chamber; 29. heating plates; 30. an annular race plate; 31. a micro cylinder; 32. an upper clamping plate; 33. a lower clamping plate; 34. a first rubber pad; 35. and a second rubber pad.

Detailed Description

To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, features and effects according to the present invention will be given with reference to the accompanying drawings and preferred embodiments.

Example 1

Referring to fig. 2 to 6, in an embodiment of the present invention, a high purity dimethyl ester batch rectification apparatus includes a rectification kettle 1, a reaction cover 2 is connected to a top end of the rectification kettle 1, a fixing rod 17 is fixedly disposed on an inner wall of the rectification kettle 1, and a reciprocating swing mechanism 7 is sleeved outside the fixing rod 17; the reciprocating swing mechanism 7 comprises a swing piece 24, both ends of the swing piece 24 are fixedly connected with transmission arm rods 18, one end of each transmission arm rod 18 is rotatably connected with a sliding seat 23 through a pin shaft, a limiting slide rod 21 penetrates through the surface of each sliding seat 23, and the limiting slide rods 21 are slidably connected with the sliding seats 23.

When the device is used, one end of the transmission arm rod 18 is movably connected with the sliding seat 23, the sliding seat 23 slides on the limiting slide rod 21 in a limiting manner, and then the transmission arm rod 18 is driven to move, so that the swinging piece 24 reciprocates, and the mixing and stirring of the dimethyl ester raw material in the rectifying still 1 are accelerated.

Referring to fig. 3-4, the outer surface and one end of the limiting slide bar 21 are fixedly connected with fixing plates 19, the other end of the limiting slide bar 21 is fixedly provided with a blocking plate 22, and a rotating shaft 20 is fixedly arranged between the two fixing plates 19 and on the side close to the limiting slide bar 21.

When the device is used, the blocking piece 22 is fixed with the tail end of the limiting slide rod 21, the blocking piece 22 can limit the position of the sliding seat 23, and the two fixing plates 19 drive the limiting slide rod 21 to make circular motion around the rotating shaft 20 under the rotation drive of the rotating shaft 20.

Referring to fig. 2-3, an air outlet 3 is disposed on the surface of the middle portion of the top end of the reaction cover 2, two servo deceleration motors 5 are symmetrically mounted on two sides of the air outlet 3, a mounting seat 6 fixedly connected with the outer surface of the reaction cover 2 is disposed at the bottom of the servo deceleration motor 5, and an end portion of an output shaft of the servo deceleration motor 5 penetrates the reaction cover 2 in a sealing manner and is fixed with the rotating shaft 20.

When the device is used, the two servo speed reducing motors 5 are fixed at the top end of the reaction cover 2 through the mounting seat 6, and the output shafts of the servo speed reducing motors 5 drive the fixing plate 19, so that the rotating shaft 20 connected with the fixing plate 19 and the limiting slide rod 21 do circular motion around the rotating shaft 20.

Referring to fig. 3-4, a through hole 25 is formed in the surface of the oscillating member 24, the oscillating member 24 slides on the outer surface of the fixing rod 17, the oscillating blades 12 are fixedly connected to both ends of the bottom of the oscillating member 24, the ratchet plates 13 are mounted on both side surfaces of the oscillating blades 12, two oscillating members 24 are provided, and the two oscillating members 24 are fixed by a connecting rod 26.

When the device is used, the swinging piece 24 reciprocates on the fixed rod 17 to drive the swinging blade 12 and the ratchet plate 13 on the swinging blade 12 to swing in a reciprocating mode, dimethyl ester raw materials in the rectifying still 1 can be uniformly mixed, the dimethyl ester raw materials are guaranteed to be more sufficient and thorough in rectification, and the utilization rate of the rectifying raw materials is improved.

When the device is used, the fixing plate 19 is driven by the servo reducing motor 5, the rotating shaft 20 and the limiting slide rod 21 connected with the fixing plate 19 rotate along with the rotating shaft 20, the limiting slide rod 21 circularly moves around the rotating shaft 20, the limiting slide rod 21 drives the slide seat 23 to slide on the limiting slide rod 21 while moving, the position of the slide seat 23 is limited by the blocking piece 22, the slide seat 23 rotates with the driving arm rod 18 through the pin shaft, the driving arm rod 18 and the two swinging pieces 24 reciprocate on the fixing rod 17, the swinging blade 12 and the ratchet plate 13 on the swinging blade 12 swing in a reciprocating mode, dimethyl ester raw materials in the rectifying still 1 can be uniformly mixed, the dimethyl ester raw materials are more fully and thoroughly rectified, and the utilization rate of the rectifying raw materials is improved.

Referring to fig. 2, a driving motor 9 is installed on the surface of the middle portion of the bottom end of the rectifying still 1, a stirring blade 10 sleeved on the rotating shaft of the driving motor 9 is installed inside the rectifying still 1, a stirring paddle 11 having the same shape as the bottom of the rectifying still 1 is arranged below the stirring blade 10, and a liquid outlet 8 is arranged on one side of the bottom surface of the rectifying still 1 close to the driving motor 9.

When the device is used, the driving motor 9 drives the rotating shaft to enable the stirring blades 10 and the stirring paddles 11 to rotate, and the reciprocating swing mechanism 7 is matched to move, so that the dimethyl ester raw material in the rectifying still 1 is more uniform and fine during rectification, the matching effect is good, and the rectification utilization rate of the rectification raw material can be fully improved.

Example 2

Referring to fig. 2, a heating cavity 28 is arranged in an inner cavity of the rectifying still 1, a heating plate 29 is arranged inside the heating cavity 28, a waste heat outlet 27 communicated with the heating cavity 28 is arranged at one side of the bottom of the rectifying still 1, and one end of the waste heat outlet 27 is connected with a waste heat collecting box 14 for waste heat recovery.

Referring to fig. 2, the top end of the gas outlet 3 is connected to a conveying pipeline 4, one end of the conveying pipeline 4 is connected to a rectifying tower 15, a packing layer 16 is disposed inside the rectifying tower 15, and the top end of the rectifying tower 15 is connected to a condenser through a pipeline.

When the heating device is used, the heating plate 29 heats the rectifying still 1 for temperature rise and rectification, gas generated by rectification enters the rectifying tower 15 through the gas outlet 3 and the conveying pipeline 4, passes through the packing layer 16 from bottom to top in the rectifying tower 15 for multiple fractionation and enters the condenser, excessive hot gas generated by the heating plate 29 can be conveyed to the waste heat collecting box 14 through the waste heat outlet 27, and the waste heat collecting box 14 is used for collecting hot gas for recycling of the hot gas, so that the waste of resources is reduced.

Example 3

Referring to fig. 2-6, an annular sleeve plate 30 is sleeved at a joint of the rectifying still 1 and the reaction cover 2, micro cylinders 31 are installed at the top end and the bottom end of the annular sleeve plate 30, an upper clamping plate 32 fixedly connected with the end of the piston rod of the upper micro cylinder 31 is slidably connected to the inner wall of the annular sleeve plate 30, and a lower clamping plate 33 fixedly connected with the end of the piston rod of the lower micro cylinder 31 is attached to the lower portion of the upper clamping plate 32.

During the use, annular lagging 30 can directly overlap in rectifying still 1 and the junction of reaction lid 2 to promote respectively by two upper and lower miniature cylinders 31 and go up cardboard 32 and lower cardboard 33 motion, go up cardboard 32 and lower cardboard 33 and laminate with the top of reaction lid 2 and the bottom of rectifying still 1 respectively, compactness when having increased reaction lid 2 and rectifying still 1 and being connected.

Referring to fig. 6, a first rubber mat 34 is attached to the inner wall of the upper clamping plate 32, a second rubber mat 35 is attached to the inner wall of the lower clamping plate 33, the lower clamping plate 33 and the upper clamping plate 32 are both of an L-shaped structure, and the first rubber mat 34 and the second rubber mat 35 are respectively attached to the outer wall surfaces of the reaction cover 2 and the rectifying still 1.

When the device is used, the first rubber cushion 34 and the second rubber cushion 35 are respectively attached to the outer wall surfaces of the reaction cover 2 and the rectifying still 1 under the pushing of the upper clamping plate 32 and the lower clamping plate 33, so that the tightness of the reaction cover 2 and the rectifying still 1 is improved, the phenomenon of gas leakage during rectification is avoided, the rectification quality is improved, and the rectification purity of the dimethyl ester raw material is ensured.

The working principle is as follows:

firstly, a fixing plate 19 is driven by a servo speed-reducing motor 5, a rotating shaft 20 and a limiting slide rod 21 which are connected with the fixing plate 19 rotate along with the rotating shaft 20, the limiting slide rod 21 circularly moves around the rotating shaft 20 and drives a slide seat 23 to slide on the limiting slide rod 21 in a limiting way, the slide seat 23 and a transmission arm rod 18 rotate through a pin shaft, the transmission arm rod 18 and two swinging pieces 24 are driven to reciprocate on a fixing rod 17, so that a swinging blade 12 and a ratchet plate 13 on the swinging blade 12 reciprocate, and the dimethyl ester raw material in a rectifying still 1 is uniformly mixed by matching with the use of a stirring blade 10 and a stirring paddle 11, the dimethyl ester raw material is more fully and thoroughly rectified, and the utilization rate of the rectifying raw material is improved;

the upper clamping plate 32 and the lower clamping plate 33 are respectively pushed to move by the upper micro cylinder 31 and the lower micro cylinder 31, the first rubber pad 34 and the second rubber pad 35 are respectively attached to the outer wall surfaces of the reaction cover 2 and the rectifying still 1 under the pushing of the upper clamping plate 32 and the lower clamping plate 33, the sealing performance of the reaction cover 2 and the rectifying still 1 is improved, the phenomenon of gas leakage during rectification is avoided, the rectification quality is improved, and the rectification purity of the dimethyl ester raw material is ensured;

the excessive hot air generated by the heating plate 29 can be discharged from the waste heat outlet 27 communicated with the heating cavity 28 and conveyed to the waste heat collection box 14, and the waste heat collection box 14 is used for collecting the hot air for recycling the hot air, so that the waste of resources is reduced.

Although the present invention has been described with reference to the preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but is intended to cover various modifications, equivalents and alternatives falling within the spirit and scope of the invention.

Claims

1. A high-purity dimethyl ester batch distillation device is characterized in that: the device comprises a rectifying kettle (1), wherein the top end of the rectifying kettle (1) is connected with a reaction cover (2), the middle surface of the top end of the reaction cover (2) is provided with an air outlet (3), the top end of the air outlet (3) is connected with a conveying pipeline (4), and one end of the conveying pipeline (4) is connected with a rectifying tower (15);

a fixed rod (17) is fixedly arranged on the inner wall of the rectifying still (1), and a reciprocating swing mechanism (7) is sleeved outside the fixed rod (17);

reciprocating swing mechanism (7) are including swing piece (24), the equal fixedly connected with in both ends of swing piece (24) drives armed lever (18), the one end of transmission armed lever (18) is rotated through the round pin axle and is connected with slide (23), the surface of slide (23) is run through and is provided with limit slide (21), limit slide (21) and slide (23) sliding connection, the equal fixedly connected with fixed plate (19) of surface and the one end of limit slide (21), and the other end of limit slide (21) is fixed and is provided with separation blade (22), two one side that is close to limit slide (21) between fixed plate (19) is fixed and is provided with axis of rotation (20), axis of rotation (20) are rotated and are installed on reaction lid (2) interior roof.

2. A high purity dimethyl ester batch distillation device according to claim 1, wherein two servo speed reducing motors (5) are symmetrically installed on two sides of the gas outlet (3), the bottom of each servo speed reducing motor (5) is provided with a mounting seat (6) fixedly connected with the outer surface of the reaction cover (2), and the end part of an output shaft of each servo speed reducing motor (5) penetrates through the reaction cover (2) in a sealing manner and is fixed with the rotating shaft (20).

3. The batch rectification device for the high-purity dimethyl ester according to claim 1, wherein a through hole (25) is formed in the surface of the swinging piece (24), the swinging piece (24) is slidably sleeved on the fixed rod (17), both ends of the bottom of the swinging piece (24) are fixedly connected with swinging blades (12), and ratchet plates (13) are mounted on the surfaces of both sides of the swinging blades (12).

4. A high-purity dimethyl ester batch rectification device as claimed in claim 1, characterized in that a driving motor (9) is installed on the surface of the middle of the bottom end of the rectifying still (1), a stirring blade (10) which is sleeved on the rotating shaft of the driving motor (9) is installed inside the rectifying still (1), a stirring paddle (11) which is the same as the bottom of the rectifying still (1) in shape is arranged below the stirring blade (10), and a liquid outlet (8) is arranged on one side of the bottom surface of the rectifying still (1) close to the driving motor (9).

5. A high-purity dimethyl ester batch rectification device according to claim 1, characterized in that the inner cavity of the rectifying still (1) is provided with a heating cavity (28), a heating plate (29) is arranged inside the heating cavity (28), one side of the bottom of the rectifying still (1) is provided with a waste heat outlet (27) communicated with the heating cavity (28), and one end of the waste heat outlet (27) is connected with a waste heat collecting box (14) for recycling waste heat.

6. The batch rectification device for high-purity dimethyl ester according to claim 1, wherein an annular sleeve plate (30) is sleeved at the joint of the rectifying still (1) and the reaction cover (2), micro cylinders (31) are mounted at the top end and the bottom end of the annular sleeve plate (30), an upper clamping plate (32) fixedly connected with the end part of a piston rod of the upper micro cylinder (31) is connected to the inner wall of the annular sleeve plate (30) in a sliding manner, and a lower clamping plate (33) fixedly connected with the end part of the piston rod of the lower micro cylinder (31) is attached to the lower part of the upper clamping plate (32).

7. A high-purity dimethyl ester batch rectification device as claimed in claim 6, wherein a first rubber pad (34) is attached to the inner wall of the upper clamping plate (32), a second rubber pad (35) is attached to the inner wall of the lower clamping plate (33), the lower clamping plate (33) and the upper clamping plate (32) are both arranged in an L-shaped structure, and the first rubber pad (34) and the second rubber pad (35) are respectively attached to the end faces of the reaction cover (2) and the rectification kettle (1).