CN206553428U - The ethynylation system of synthesizing methyl butynol - Google Patents
The ethynylation system of synthesizing methyl butynol Download PDFInfo
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- CN206553428U CN206553428U CN201720244345.0U CN201720244345U CN206553428U CN 206553428 U CN206553428 U CN 206553428U CN 201720244345 U CN201720244345 U CN 201720244345U CN 206553428 U CN206553428 U CN 206553428U
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- hole plate
- auxiliary reactor
- methyl butynol
- ethynylation
- synthesizing methyl
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Abstract
The utility model is related to a kind of production equipment of methyl butynol, specifically discloses a kind of ethynylation system of synthesizing methyl butynol, and the system includes the stirred autoclave, auxiliary reactor and termination blender being sequentially connected, and auxiliary reactor bottom is provided with hole plate.The utility model has the advantages that：1) agitator is substituted with hole plate, material is set to be mixed in the form of meeting acetylene, acetone reaction rule and methyl butynol productive prospecting, ensure that all materials entered in auxiliary reactor have the reaction time of abundance and faster reaction rate, improve methyl butynol yield.2) device structure is simple, beneficial to industrially promoting.
Description
Technical field
The utility model is related to a kind of production equipment of methyl butynol, in especially a kind of methyl butynol production process
Reaction unit used in ethynylation step.
Background technology
Methyl butynol, CAS 115-19-5, molecular formula：C5H8O.It is mainly used as synthesis medicine and agricultural chemicals, terpenes is fragrant
Expect intermediate, acid inhibition inhibitor, viscosity stabiliser, viscosity reductant, nickel plating or copper-plated glazing agent etc..Also act as silicon rubber
The polymerization inhibitor of middle platinum catalysis hydrosilylation.In addition it is also serving as being used as solvent, the stabilization of chlorinated solvents.
The method of industrial synthesizing methyl butynol mainly includes two steps of ethynylation and separation.
Ethynylation step is that, using acetylene, acetone as raw material, solid (mostly powdered) potassium hydroxide is catalyst, or liquid hydrogen
Sodium oxide molybdena makees catalyst, ethynylation occurs in ethynylation device ethynylation mixture is made.Its reaction equation is such as
Under：
HC ≡ CH+NaOH=HC ≡ CHNaOH
The complex compound of generation and water decomposition, generate methyl butynol：
Separating step is then that separating-purifying goes out methyl butynol from ethynylation mixture, generally main to include flash distillation, saltout
The steps such as dehydration, rectifying.
In ethynylation step, the ethynylation of acetylene and acetone is generally carried out in stirred autoclave, in stirred autoclave
In, alkynes, alcohol/ketone mixtures are to lower and upper flowing, and catalyst flows from top to bottom, mixed in the axial direction by density contrast, radially then
Mainly by the stirring action mixing of agitator, because the temperature difference, the concentration difference of reaction system are larger, therefore the methyl in stirred autoclave
The yield of butynol is only capable of reaching 60% or so (please check).To improve the yield of methyl butynol, conventional way is at present
One auxiliary reactor is set again after stirred autoclave, material is carried out primary first-order equation again in auxiliary reactor, so as to improve
The yield of methyl butynol.
Conventional auxiliary reactor structure is the reaction vessels such as the reactor with agitating device, reaction tower, reaction tube, its typical case
Structure is as shown in Figure 1.In auxiliary reactor, unreacted material carries out hybrid reaction again in the presence of agitator, so that
Improve the yield of methyl butynol.Finally, the reaction stream in auxiliary reactor is passed through in termination blender with reaction terminating agent
Mix and terminating reaction, obtain ethynylation mixture.After further being reacted by auxiliary reactor, the yield of methyl butynol can reach
85% or so (please check).
Utility model content
Further to improve the yield of methyl butynol, the utility model provides a kind of ethynylation of synthesizing methyl butynol
Reaction system.
The technical scheme that the utility model is used is：The ethynylation system of synthesizing methyl butynol, including stirring are anti-
Answer kettle, auxiliary reactor and termination blender；The stirred autoclave is connected by overflow pipe with auxiliary reactor, the auxiliary reactor
It is connected by discharge nozzle with terminating blender, material feeding tube and catalyst charge pipe is communicated with the stirred autoclave；Institute
State auxiliary reactor bottom and be provided with hole plate, the overflow pipe is communicated on the side reaction wall below hole plate.
It is as follows because local acetone can excessively cause occur side reaction generation dimethylhexyne glycol：
So must assure that the material in auxiliary reactor is sufficiently mixed uniformly, therefore the setting of agitator is considered as necessary
's.
By taking the ethynylation system of the methyl butynol shown in Fig. 1 as an example, it has been recognised by the inventors that limitation methyl butynol yield
The problem of raising, essentially consists in, in existing reaction system, and material after initial reaction, passes through overflow pipe in stirred autoclave
Into auxiliary reactor bottom, hybrid reaction is being carried out again under the immixture of agitator.As material is constantly from overflow pipe
Flow into, material is gradually advanced from reactor lower part toward top in auxiliary reactor, and material constantly completes reaction during traveling, most
Enter eventually from upper outlet pipe and terminate blender.In the process, because the stirring of agitator causes liquid acutely to disturb so that
The product that auxiliary reactor top more fully react is mixed with the unreacted material that bottom is newly entered from overflow pipe, makes production
Thing is mixed into unreacted material, reduces the reaction rate of unreacted material.Also cause the unreacted for having just enter into auxiliary reactor simultaneously
Material quickly flow to auxiliary reactor top because of the violent flow-disturbing that stirring is formed, and reaction is not in time for also and is just flowed into eventually from discharging opening
Only blender.
On the other hand, during the material for entering auxiliary reactor from overflow pipe flings auxiliary reactor from auxiliary reactor bottom, shape
Into the uneven fluid of flow velocity form bias current and dead angle in the reactor, it is impossible to ensure that all materials have in reactor and fill
The reaction time of foot and faster reaction rate, while also increasing the degree of side reaction generation.
For solve the above the problem of, inventor by auxiliary reactor agitator cancel, be replaced with hole plate so that from overflow
Flow tube flow into auxiliary reactor material by auxiliary reactor bottom hole plate stop, the fast fluid of flow velocity to both sides horizontal proliferation,
And be formed down vortex and disturb, play the effect for being well mixed material.Then bottom material is past by the hole of hole plate
Upper to advance, hole serves the effect for being uniformly distributed fluid, it is to avoid bias current and dead angle are produced.Hole plate upper flow is upward simultaneously
The unreacted material just entered during propulsion with hole plate bottom from overflow pipe is in opposing spaced apart state, and (fluid is acutely disturbed
It is dynamic to be concentrated in hole plate bottom, it is ensured that hole plate upper flow is uniformly up advanced all the time, without flowing back to
Hole plate bottom), the fluid more fully reacted on auxiliary reactor top can be prevented effectively from and mixed with unreacted material, or newly
Enter unreacted material and quickly flow to auxiliary reactor top.So as to ensure that all materials have the reaction of abundance in auxiliary reactor
Time and quick reaction rate, and then realize the purpose for improving methyl butynol yield.
As further improvement of the utility model, the overflow pipe is communicated in auxiliary reactor bottom, new according to this practicality
The mentality of designing of type, mesh of the present utility model is can be achieved as long as overflow pipe is communicated on the side reaction wall below hole plate
's.But in order that the material mixing of hole plate bottom is evenly, and hole plate top material forms fluid evenly, preferably
Overflow pipe is communicated in auxiliary reactor bottom, this also complies with the custom connected mode in industry.
As further improvement of the utility model, hole on the hole plate is can make the fluid by hole plate
The mode for producing disturbance on hole plate top is set.Hole on hole plate can be conducive to the shape that fluid is evenly distributed with any
Formula is set, most typical such as equally distributed circular aperture, or other shapes aperture, and or uniformly or non-uniformly set
The diversified forms such as thin seam.But still can not in order that obtaining lower flow and passing through after hole plate during the traveling of hole plate top
The disturbance and mixing of disconnected generation appropriateness, further the local acetone of reduction excessively occur side reaction or form dead angle and bias current
May, the hole on hole plate be able to can be made to set by way of the fluid of hole plate produces disturbance on hole plate top
Put.Hole can be for example set to the inclined circular aperture arranged according to certain rules, or be similar to turbine blade shape
Gap etc..So that fluid formed during through hole plate on hole plate top under the water conservancy diversion of hole appropriate vortex or
Disturbance, promotes hole plate upper flow further to mix.
As further improvement of the utility model, the hole plate setting height(from bottom) is the distance apart from auxiliary reactor bottom
For 15~40cm.The setting height(from bottom) of hole plate is too high or too low all to cause hole plate bottom material to be difficult to form stronger disturbance
(such as hole plate be installed on close to auxiliary reactor medium position even upper position when will be unable to realize mesh of the present utility model
), mixed effect is poor.Inventor draws through overtesting, it is generally the case that hole plate installation site and auxiliary reactor bottom
Effect is preferable when distance is 15~40cm.In addition, the specific installation site of hole plate also with auxiliary reactor specification, overflow pipe material
The factors such as flow velocity, flow are relevant.Therefore the number range is only preferred values under normal circumstances, and concrete numerical value scope can be according to reality
Border situation is adjusted.
Distance additionally, due to general auxiliary reactor bottom head welding position and auxiliary reactor bottom is about 20~30cm,
Therefore can be directly by hole plate weld in end socket weld, in order to the installation and plant maintenance of hole plate.
The beneficial effects of the utility model are：1) agitator is substituted with hole plate, makes material and reacted with meeting acetylene, acetone
Rule and the form of methyl butynol productive prospecting are mixed, it is ensured that all materials entered in auxiliary reactor have abundance
Reaction time and faster reaction rate, it is demonstrated experimentally that using production system of the present utility model, first in ethynylation mixture can be made
Base butynol yield reaches 95% or so.2) device structure is simple, beneficial to industrially promoting.
Brief description of the drawings
Fig. 1 is the structural representation of the ethynylation system of synthesizing methyl butynol in the prior art.
Fig. 2 is structural representation of the present utility model.
Fig. 3 is the hole plate structure schematic diagram of embodiment one.
Fig. 4 is the hole plate structure schematic diagram of embodiment two.
Fig. 5 is Fig. 4 a to fragmentary, perspective view.
Fig. 6 is the hole plate structure schematic diagram of embodiment three.
Fig. 7 is Fig. 6 a to fragmentary, perspective view.
Marked in figure：1- stirred autoclaves, 2- auxiliary reactors, 3- terminates blender, 4- overflow pipes, 5- discharge nozzles, 6-
Material feeding tube, 7- catalyst charge pipes, 8- agitators, 9- hole plates, 9a, 9b, 9c- hole.
Embodiment
As shown in Figure 2 to 7, the ethynylation system of synthesizing methyl butynol of the present utility model, including stirring reaction
Kettle 1, auxiliary reactor 2 and termination blender 3；The barrel diameter of auxiliary reactor 2 is 800mm, is highly 1200mm, end socket is highly
300mm, stirred autoclave 1 is connected by its top overflow pipe 4 with the bottom of auxiliary reactor 2, and auxiliary reactor 2 passes through its upper outlet
Pipe 5 is connected with terminating blender 3, and material feeding tube 6 and catalyst charge pipe 7, auxiliary reactor 2 are communicated with stirred autoclave 1
Bottom head weld is provided with hole plate 9.
The utility model is further illustrated with reference to the accompanying drawings and examples.
Embodiment one：
Fig. 2, Fig. 3 are illustrated in the first embodiment of the present utility model, the program on auxiliary reactor hole plate
Pore structure is size, circular aperture arranged in a uniform, and the fluid for entering auxiliary reactor from overflow pipe is stopped by hole plate, in hole
Gap plate bottom produces disturbance, is well mixed material.Then bottom material penetrates into hole by the uniform aperture on hole plate
Gap plate top, is evenly distributed as uniform fluid by aperture, and upper flow and the fluid of hole plate bottom is in relatively
Segmented state.Uniform fluid is slowly advanced on hole plate top toward auxiliary reactor top, step-reaction in material traveling process
Completely, all materials have the residence time of abundance in auxiliary reactor, finally from the discharging opening for being arranged at auxiliary reactor top
Into termination blender, and terminating reaction is mixed with terminator, obtain ethynylation mixture.
Embodiment two：
Fig. 2, Fig. 4, Fig. 5 illustrate another embodiment of the present utility model, are not both with embodiment one, this implementation
Circular aperture on the plate of example mesopore is arranged according to certain rules, and in vertical direction is inclined on hole plate
, all apertures are obliquely installed according to certain rule, make hole plate that a flow guide system is integrally formed.Hole plate bottom
Fluid by the way that the liquid stream of appropriateness disturbance is formed on hole plate top during hole plate under the guide functions of aperture, make material through
Continue to mix during advancing toward auxiliary reactor top after hole plate, the degree that further reduction side reaction occurs.
It should be understood readily by those skilled in this art that the present embodiment mesopore plate should possess certain thickness, to reach
The purpose of this programme.
Embodiment three：
Fig. 2, Fig. 6, Fig. 7 illustrate the third embodiment of the present utility model, the hole on the embodiment mesopore plate
Gap is strip crevice, as shown in fig. 7, the strip crevice in the vertical direction is obliquely installed, and leading with certain radian
Flow ramp.The program can play the effect similar with embodiment two and effect.
Claims (7)
1. the ethynylation system of synthesizing methyl butynol, including stirred autoclave (1), auxiliary reactor (2) and termination blender
(3)；The stirred autoclave (1) is connected by overflow pipe (4) with auxiliary reactor (2), and the auxiliary reactor (2) passes through discharge nozzle
(5) it is connected with terminating blender (3), material feeding tube (6) and catalyst charge pipe is communicated with the stirred autoclave (1)
(7)；It is characterized in that：Auxiliary reactor (2) bottom is provided with hole plate (9), and the overflow pipe (4) is communicated in hole plate
(9) on the side reaction wall below.
2. the ethynylation system of synthesizing methyl butynol according to claim 1, it is characterised in that：The overflow pipe
(4) it is communicated in auxiliary reactor (2) bottom.
3. the ethynylation system of synthesizing methyl butynol according to claim 2, it is characterised in that：The hole plate
(9) hole on is can make to set by way of the fluid of hole plate (9) produces disturbance on hole plate (9) top.
4. the ethynylation system of synthesizing methyl butynol according to claim 2, it is characterised in that：The hole plate
(9) setting height(from bottom) is apart from auxiliary reactor (2) 15~40cm of bottom.
5. the ethynylation system of the synthesizing methyl butynol according to any claim in Claims 1 to 4, its feature
It is：Hole on the hole plate (9) is circular port.
6. the ethynylation system of the synthesizing methyl butynol according to any claim in Claims 1 to 4, its feature
It is：The hole plate (9) is installed on auxiliary reactor (2) bottom head weld.
7. the ethynylation system of the synthesizing methyl butynol according to any claim in Claims 1 to 4, its feature
It is：The catalyst charge pipe (7) is communicated in stirred autoclave (1) top, and material feeding tube (6) is communicated in stirred autoclave
(1) bottom.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201720244345.0U CN206553428U (en) | 2017-03-14 | 2017-03-14 | The ethynylation system of synthesizing methyl butynol |
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| CN201720244345.0U CN206553428U (en) | 2017-03-14 | 2017-03-14 | The ethynylation system of synthesizing methyl butynol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831332A (en) * | 2017-03-14 | 2017-06-13 | 四川泸州巨宏化工有限责任公司 | The ethynylation system of synthesizing methyl butynol |
| CN107827711A (en) * | 2017-10-31 | 2018-03-23 | 西南化工研究设计院有限公司 | A kind of system and technique of coproducing methyl butynol and dimethylhexyne glycol |
-
2017
- 2017-03-14 CN CN201720244345.0U patent/CN206553428U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831332A (en) * | 2017-03-14 | 2017-06-13 | 四川泸州巨宏化工有限责任公司 | The ethynylation system of synthesizing methyl butynol |
| CN107827711A (en) * | 2017-10-31 | 2018-03-23 | 西南化工研究设计院有限公司 | A kind of system and technique of coproducing methyl butynol and dimethylhexyne glycol |
| CN107827711B (en) * | 2017-10-31 | 2023-09-29 | 西南化工研究设计院有限公司 | System and process for coproducing methyl butynol and dimethyl hexynediol |
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