CN205199011U - Methyl acetoacetate rectifier unit - Google Patents
Methyl acetoacetate rectifier unit Download PDFInfo
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- 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
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- tower
- layer
- methyl acetoacetate
- packing layer
- packing
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- WRQNANDWMGAFTP-UHFFFAOYSA-N Methylacetoacetic acid Chemical compound COC(=O)CC(C)=O WRQNANDWMGAFTP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000012856 packing Methods 0.000 claims abstract description 70
- 238000009835 boiling Methods 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 10
- 239000011435 rock Substances 0.000 claims description 4
- -1 acetoacetyl methyl Chemical group 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 230000004907 flux Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 5
- WASQWSOJHCZDFK-UHFFFAOYSA-N diketene Chemical compound C=C1CC(=O)O1 WASQWSOJHCZDFK-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 210000000078 claw Anatomy 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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
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.
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) |
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2015
- 2015-11-06 CN CN201520884202.7U patent/CN205199011U/en active Active
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |