CN205199011U - Methyl acetoacetate rectifier unit - Google Patents

Methyl acetoacetate rectifier unit Download PDF

Info

Publication number
CN205199011U
CN205199011U CN201520884202.7U CN201520884202U CN205199011U CN 205199011 U CN205199011 U CN 205199011U CN 201520884202 U CN201520884202 U CN 201520884202U CN 205199011 U CN205199011 U CN 205199011U
Authority
CN
China
Prior art keywords
tower
layer
methyl acetoacetate
packing layer
packing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201520884202.7U
Other languages
Chinese (zh)
Inventor
丁彩峰
朱小刚
刘芳
姚俊生
张伟
朱双双
徐晶晶
徐子云
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nantong Acetic Acid Chemical Co Ltd
Original Assignee
Nantong Acetic Acid Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nantong Acetic Acid Chemical Co Ltd filed Critical Nantong Acetic Acid Chemical Co Ltd
Priority to CN201520884202.7U priority Critical patent/CN205199011U/en
Application granted granted Critical
Publication of CN205199011U publication Critical patent/CN205199011U/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The utility model provides a rectifying column (3) that methyl acetoacetate rectifier unit, including tower skirt (1), tower cauldron (2) and set up on tower skirt (1) rectifying column (1) first layer packing layer (4), second floor packing layer (5) and third layer packing layer (6) of establishing ties by the pipeline constitute. The utility model discloses a methyl acetoacetate rectifier unit, the flow is simple, and rectification tower packing adopts the combination formula to pack, and it is big to have a flux, and material dwell time is short, and methyl acetoacetate is difficult to decompose among the distillation process. The rectification yield is more than 98.5 percent, and finished product content reaches more than 99.8 percent.

Description

Methyl acetoacetate rectifier unit
Technical Field
The utility model belongs to the chemical industry field, concretely relates to methyl acetoacetate rectifier unit.
Background
Rectification is a distillation method for separating a liquid mixture with high purity by utilizing reflux, is the separation operation of the liquid mixture with the widest industrial application, and is widely applied to the departments of petroleum, chemical industry, light industry, food, metallurgy and the like. The rectification operations are classified in different ways. According to the operation mode, the method can be divided into continuous rectification and batch rectification.
In the production process of methyl acetoacetate, in order to obtain high-purity methyl acetoacetate, crude methyl acetoacetate obtained after esterification reaction of crude diketene and methanol needs to be rectified. Wherein the crude diketene is diketene with the purity of 90-95%. However, the crude methyl acetoacetate produced after the esterification reaction contains many impurities, including low-boiling components such as methanol, acetone and methyl acetate, medium-boiling components such as acetic anhydride, and part of high-boiling components. High-quality methyl acetoacetate cannot be obtained by using common rectifying tower packing, so that better packing combination is required to obtain high-quality methyl acetoacetate.
The invention application with application number "201410086572.6", which discloses "a process for preparing methyl acetoacetate": adding a catalyst once, continuously adding diketene and a methanol solution, continuously adding an extracting agent, simultaneously adding two materials into a reactive extraction rectifying tower, heating, carrying out total reflux reactive extraction rectifying tower to obtain the methanol solution at the top of the tower, wherein the tower kettle is a mixed solution of methyl acetoacetate, the catalyst and the extracting agent, feeding the mixed solution into a reduced pressure extraction tower, and obtaining a finished product of methyl acetoacetate at the top of the tower. The process is relatively complex, the energy consumption is high, the bisethylmethyl ester is easy to decompose, the purity is low, and the production cost is high.
SUMMERY OF THE UTILITY MODEL
For providing a flow simple, the flux is big, the rectifier unit that material dwell time is short, the utility model discloses a modular filler structure provides a methyl acetoacetate rectifier unit, and its technical scheme specifically as follows:
the utility model provides a methyl acetoacetate rectifier unit, including tower skirt (1), tower cauldron (2) and set up rectifying column (3) on tower skirt (1), its characterized in that:
the rectifying tower (1) is composed of a first layer packing layer (4), a second layer packing layer (5) and a third layer packing layer (6) which are connected in series through pipelines,
and a pipeline gas outlet end is arranged on the tower kettle and is connected to a pipeline gas inlet end of the first packing layer of the rectifying tower through a pipeline.
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
the acetoacetyl methyl ester rectifying device also comprises a condenser (7), a low boiling tank (8) and a finished product tank (9),
the gas inlet end pipelines of the low-boiling tank (8) and the finished product tank (9) are connected in parallel to the gas outlet end of the condenser (7),
and the gas inlet end pipeline of the condenser (7) is connected with the gas outlet end of the third packing layer (6) of the rectifying tower.
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
and the gas outlet end pipeline of the low-boiling tank (8) is connected to the tower kettle (2).
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
a tower kettle stirrer (10) is arranged in the tower kettle (2).
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
a reboiler (11) is arranged in the tower kettle (2).
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
a thermometer (T1) is arranged in the tower kettle (2);
a thermometer (T2) is arranged at the joint of the first packing layer of the rectifying tower of the tower skirt (1);
a thermometer (T3) is arranged at the joint of the first packing layer of the rectifying tower and the second packing layer of the rectifying tower;
a thermometer (T4) is arranged at the joint of the second layer packing layer of the rectifying tower and the third layer packing layer of the rectifying tower;
a thermometer (T5) is arranged at the top of the rectifying tower (3).
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
a pressure gauge (P1) is arranged in the tower kettle (2);
a pressure gauge (P2) is arranged at the top of the rectifying tower (3).
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
a pressure gauge (P3) is arranged in the low-boiling tank (8);
a pressure gauge (P4) is arranged in the finished product groove (9);
and a thermometer (T6) is arranged at the air outlet end of the condenser (7).
According to the utility model discloses a methyl acetoacetate rectifier unit, its characterized in that:
the first layer of packing layer of the rectifying tower is filled with metal saddle ring packing, and the packing layer is favorable for liquid distribution and increase of civil gas channels;
the second layer of packing layer of the rectifying tower is filled with metal Intel rock packing, the geometric bodies outside the packing layer are not interlocked or entangled, the optimal randomness and the internal area of the bed packing are ensured, and the internal claws, the arched doors and the blades promote the gas/liquid contact or the wind tide with the optimal interface at the minimum resistance. The lower reflux ratio reduces the energy consumption, is beneficial to shortening the height of the packed bed, has high liquid film surface renewal rate and generates high-quality transmission rate, thereby leading to larger capacity and efficiency, and a large number of contact points are the distribution of homogeneous liquid and gas;
the third layer of the packing layer of the rectifying tower is filled with wire mesh corrugated packing, and the packing layer has large specific surface area, large porosity and light weight; the inclination angle of the gas phase passage is small and regular, and the pressure is reduced; the radial diffusion is good, and the gas-liquid contact is sufficient.
The utility model discloses a methyl acetoacetate rectifier unit changes original single packing rectifying column inner structure, adopts the combination formula to pack, and it is big to reach the flux, and dwell time is effect such as short, reduces methyl acetoacetate and decomposes, improves content, and its flow is simple, and methyl acetoacetate is difficult to decompose in the rectification process. The rectification yield is more than 98.5 percent, and the content of the finished product is more than 99.8 percent.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure, 1 is a tower skirt; 2 is a tower kettle; 3 is a rectifying tower; 4 is a first packing layer of the rectifying tower; 5 is a second packing layer of the rectifying tower; 6 is a third packing layer of the rectifying tower; 7 is a condenser; 8 is a low-boiling tank; 9 is a finished product groove; 10 is a tower kettle stirrer; 11 is a reboiler; t1 to T6 are thermometers; P1-P4 are pressure gauges.
Detailed Description
The methyl acetoacetate rectification device of the present invention is further specifically described below with reference to the drawings and the detailed description.
As shown in figure 1, the methyl acetoacetate rectification device comprises a tower skirt (1), a tower kettle (2) and a rectification tower (3) arranged on the tower skirt (1), wherein the rectification tower (1) is composed of a first layer of packing layer (4), a second layer of packing layer (5) and a third layer of packing layer (6) which are connected in series through pipelines,
and a pipeline gas outlet end is arranged on the tower kettle and is connected to a pipeline gas inlet end of the first packing layer of the rectifying tower through a pipeline.
Wherein,
the acetoacetyl methyl ester rectifying device also comprises a condenser (7), a low boiling tank (8) and a finished product tank (9),
the gas inlet end pipelines of the low-boiling tank (8) and the finished product tank (9) are connected in parallel to the gas outlet end of the condenser (7),
and the gas inlet end pipeline of the condenser (7) is connected with the gas outlet end of the third packing layer (6) of the rectifying tower.
Wherein,
and the gas outlet end pipeline of the low-boiling tank (8) is connected to the tower kettle (2).
Wherein,
a tower kettle stirrer (10) is arranged in the tower kettle (2).
Wherein,
a reboiler (11) is arranged in the tower kettle (2).
Wherein,
a thermometer (T1) is arranged in the tower kettle (2);
a thermometer (T2) is arranged at the joint of the first packing layer of the rectifying tower of the tower skirt (1);
a thermometer (T3) is arranged at the joint of the first packing layer of the rectifying tower and the second packing layer of the rectifying tower;
a thermometer (T4) is arranged at the joint of the second layer packing layer of the rectifying tower and the third layer packing layer of the rectifying tower;
a thermometer (T5) is arranged at the top of the rectifying tower (3).
Wherein,
a pressure gauge (P1) is arranged in the tower kettle (2);
a pressure gauge (P2) is arranged at the top of the rectifying tower (3).
Wherein,
a pressure gauge (P3) is arranged in the low-boiling tank (8);
a pressure gauge (P4) is arranged in the finished product groove (9);
and a thermometer (T6) is arranged at the air outlet end of the condenser (7).
Wherein,
the first layer of packing layer of the rectifying tower is filled with metal saddle ring packing, and the packing layer is favorable for liquid distribution and increase of civil gas channels;
the second layer of packing layer of the rectifying tower is filled with metal Intel rock packing, the geometric bodies outside the packing layer are not interlocked or entangled, the optimal randomness and the internal area of the bed packing are ensured, and the internal claws, the arched doors and the blades promote the gas/liquid contact or the wind tide with the optimal interface at the minimum resistance. The lower reflux ratio reduces the energy consumption, is beneficial to shortening the height of the packed bed, has high liquid film surface renewal rate and generates high-quality transmission rate, thereby leading to larger capacity and efficiency, and a large number of contact points are the distribution of homogeneous liquid and gas;
the third layer of the packing layer of the rectifying tower is filled with wire mesh corrugated packing, and the packing layer has large specific surface area, large porosity and light weight; the inclination angle of the gas phase passage is small and regular, and the pressure is reduced; the radial diffusion is good, and the gas-liquid contact is sufficient.
Examples
The crude methyl acetoacetate (the content is about 90-95%) is directly fed into a tower still with a stirrer, wherein the tower still is provided with a thermometer T1 and a pressure gauge P1, the temperature is raised after stirring, and the rectification tower comprises: the tower comprises a tower skirt, a tower body, a metal saddle ring packing, a metal Intel rock packing and a wire mesh corrugated packing, wherein a thermometer T2 is arranged at the bottom of the tower, thermometers T3 and T4 are arranged between the packing layers of the tower body, a thermometer T5 and a pressure gauge P2 are arranged at the top of the tower, the thermometer T6 is arranged at the outlet of the condenser, a head and a middle-boiling tank are recycled and used, the pressure gauge P3 is arranged in the low-boiling tank, the final finished product is fed into a finished product tank R, and the finished product tank is provided with a pressure gauge P4. Packing of the rectifying tower: a first layer: metal intalox, second layer: metal intelox, third layer: wire mesh corrugated packing. Specification parameters are as follows
The utility model discloses a methyl acetoacetate rectifier unit, the flow is simple, and the rectifying column packs and adopts the combination formula to pack, and it is big to have a flux, and material dwell time is short, and methyl acetoacetate is difficult to decompose among the rectification process. The rectification yield is more than 98.5 percent, and the content of the finished product is more than 99.8 percent.

Claims (9)

1. The utility model provides a methyl acetoacetate rectifier unit, including tower skirt (1), tower cauldron (2) and set up rectifying column (3) on tower skirt (1), its characterized in that:
the rectifying tower (3) is composed of a first layer packing layer (4), a second layer packing layer (5) and a third layer packing layer (6) which are connected in series through pipelines,
and a pipeline gas outlet end is arranged on the tower kettle and is connected to a pipeline gas inlet end of the first packing layer of the rectifying tower through a pipeline.
2. A methyl acetoacetate rectification device according to claim 1, characterized in that:
the acetoacetyl methyl ester rectifying device also comprises a condenser (7), a low boiling tank (8) and a finished product tank (9),
the gas inlet end pipelines of the low-boiling tank (8) and the finished product tank (9) are connected in parallel to the gas outlet end of the condenser (7),
and the gas inlet end pipeline of the condenser (7) is connected with the gas outlet end of the third packing layer (6) of the rectifying tower.
3. A methyl acetoacetate rectification device according to claim 2, characterized in that:
and the gas outlet end pipeline of the low-boiling tank (8) is connected to the tower kettle (2).
4. A methyl acetoacetate rectification device according to claim 1, characterized in that:
a tower kettle stirrer (10) is arranged in the tower kettle (2).
5. A methyl acetoacetate rectification device according to claim 1, characterized in that:
a reboiler (11) is arranged in the tower kettle (2).
6. A methyl acetoacetate rectification device according to claim 1, characterized in that:
a thermometer (T1) is arranged in the tower kettle (2);
a thermometer (T2) is arranged at the joint of the first packing layer of the rectifying tower of the tower skirt (1);
a thermometer (T3) is arranged at the joint of the first packing layer of the rectifying tower and the second packing layer of the rectifying tower;
a thermometer (T4) is arranged at the joint of the second layer packing layer of the rectifying tower and the third layer packing layer of the rectifying tower;
a thermometer (T5) is arranged at the top of the rectifying tower (3).
7. A methyl acetoacetate rectification device according to claim 1, characterized in that:
a pressure gauge (P1) is arranged in the tower kettle (2);
a pressure gauge (P2) is arranged at the top of the rectifying tower (3).
8. A methyl acetoacetate rectification device according to claim 2, characterized in that:
a pressure gauge (P3) is arranged in the low-boiling tank (8);
a pressure gauge (P4) is arranged in the finished product groove (9);
and a thermometer (T6) is arranged at the air outlet end of the condenser (7).
9. A methyl acetoacetate rectification device according to claim 1, characterized in that:
metal intalox saddle ring packing is filled in the first layer of packing layer of the rectifying tower;
filling metal Intel rock filler in the second layer of filler layer of the rectifying tower;
and the third layer of packing layer of the rectifying tower is filled with wire mesh corrugated packing.
CN201520884202.7U 2015-11-06 2015-11-06 Methyl acetoacetate rectifier unit Active CN205199011U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201520884202.7U CN205199011U (en) 2015-11-06 2015-11-06 Methyl acetoacetate rectifier unit

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201520884202.7U CN205199011U (en) 2015-11-06 2015-11-06 Methyl acetoacetate rectifier unit

Publications (1)

Publication Number Publication Date
CN205199011U true CN205199011U (en) 2016-05-04

Family

ID=55836756

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201520884202.7U Active CN205199011U (en) 2015-11-06 2015-11-06 Methyl acetoacetate rectifier unit

Country Status (1)

Country Link
CN (1) CN205199011U (en)

Similar Documents

Publication Publication Date Title
CN102824890B (en) Catalytic distillation filler with alternative flow structure
CN101955187A (en) Method and apparatus for preparing trichlorosilane through reaction rectification by using proportionate reaction
CN103804124B (en) Preparation method of diethyl carbonate and methylethyl carbonate
CN106748651A (en) A kind of coal-ethylene glycol process for refining and system
CN102491341A (en) Reactive distillation device for preparing trichlorosilane from mixed chlorosilane and method for device
CN101219950B (en) System and method for producing n-butyl acetate by using methyl acetate and n-butyl alcohol ester exchange reaction
CN206624811U (en) The filling extract rectification separator of the picoline of high-purity 3
CN102134191B (en) Process method for producing ethyl acetate by catalytic rectification
CN102875328B (en) Catalyzing rectifying technology for synthesizing sec-butyl alcohol through ester exchange method and production equipment of catalyzing rectifying technology
CN205199011U (en) Methyl acetoacetate rectifier unit
CN101209955A (en) Methyl acetate hydrolysis catalysis reaction rectifying device and realization technique
CN105016974A (en) Separation method for optimizing butanol-octanol product structures
CN201807206U (en) High concentration methylal pressurizing rectifying tower
CN203090515U (en) External circular-reaction extractive distillation integrated device
CN202893314U (en) Catalyst filling structure of catalytic rectification tower
CN104592027A (en) Method for preparing methyl benzoate
CN103772084A (en) Ester-exchange reaction device
CN103755532B (en) Chloromethyl ether continuous production system and production process utilizing same
CN105561615B (en) catalytic distillation device and application
CN202427188U (en) Novel catalytic distillation equipment
CN102489220B (en) Continuous oxidation method and device for preparing oxalic acid
CN201930788U (en) Methyl trimethoxy silane purification device
CN201272776Y (en) Apparatus for continuous preparation of biodiesel by neutral grease
CN204356288U (en) A kind of weight hydrocarbon separation system
CN203700231U (en) Continuous manufacturing system for chloromethyl ether

Legal Events

Date Code Title Description
C14 Grant of patent or utility model
GR01 Patent grant