CN206188686U - Device of butyraldehyde oxidation preparation butyric acid - Google Patents
Device of butyraldehyde oxidation preparation butyric acid Download PDFInfo
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- CN206188686U CN206188686U CN201621206708.3U CN201621206708U CN206188686U CN 206188686 U CN206188686 U CN 206188686U CN 201621206708 U CN201621206708 U CN 201621206708U CN 206188686 U CN206188686 U CN 206188686U
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- butyric acid
- heat exchanger
- water heat
- cooling water
- rectifying column
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The utility model discloses a device of butyraldehyde oxidation preparation butyric acid, initial response ware even catalyst prepare jar, and initial response ware top is first cooling water heat exchanger even, and the bottom is second cooling water heat exchanger even, and second cooling water heat exchanger is the second reactor even, and third cooling water heat exchanger is connected on second reactor top, and water heat exchanger is cooled off with the fourth in the bottom even first pump of sending outside, and the first pump of sending outside links first butyric acid rectifying column, first butyric acid rectification top of the tower is the 5th cooling water heat exchanger, a liquid receiving tank, the 2nd outer circulating pump even, and the 2nd outer circulating pump connects butyraldehyde raw material input pipeline and first butyric acid rectifying column, and second butyric acid rectifying column is connected to first butyric acid rectifying column bottom, N -butyric acie outlet line and second butyric acid rectifying column are connected to the 6th cooling water heat exchanger of second butyric acid rectifying column top polyphone, the 2nd liquid receiving tank, backwash pump, backwash pump, and second butyric acid rectifying column bottom is connected the second and is sent the pump outside. The utility model discloses the process route is simple, and the production control is convenient, and the product yield is high.
Description
Technical field
The utility model is related to a kind of deep processing and utilization device of the butyraldehyde produced in octyl alconyl process units production process,
In particular, it is a kind of be related to butyraldehyde oxidation to prepare butyric acid device and method.
Background technology
N-butyric acie is a kind of important synthetic perfume and the raw material of other fine chemical products, is mainly used in n-butyric acie ester
The synthesis of class and n-butyric acie cellulose.N-butyric acie esters are widely used in essence, food additives, medicine and other fields.Synthesis
The method of n-butyric acie mainly has three kinds：N-butyl alcohol oxidation method, agricultural byproducts fermentation method and hutanal oxidizing process.Agricultural byproducts ferment
Method is low because of product yield, and post processing amount has been synthesized greatly method substitution.From the oxidizing process of n-butanol, its intermediate product is also fourth
Aldehyde, with the development of propenecarbonyl technology, directly has that process route is simple, production control using butyraldehyde oxidation production n-butyric acie
The advantages of system is convenient, raw material is single, product yield is high.
Utility model content
The purpose of this utility model is to overcome deficiency of the prior art, there is provided a kind of process route is simple, production
The butyraldehyde oxidation high of easy to control, product yield prepares the device of butyric acid.
The purpose of this utility model can be achieved through the following technical solutions.
A kind of butyraldehyde oxidation prepares the device of butyric acid, including is connected with oxygen input tube line and butyraldehyde raw material intake pipeline
First reactor, the first reactor is connected with catalyst preparation tank, the first reactor by catalyst intake pipeline
Top is connected with the first cooling water heat exchanger of formed circulation loop, and the first reactor bottom is connected with formed
Second cooling water heat exchanger of circulation loop, second cooling water heat exchanger is also associated with what is be connected with oxygen input tube line
Second reactor, second reactor top is connected with the 3rd cooling water heat exchanger of formed circulation loop, and described the
Three cooling water heat exchangers and the first cooling water heat exchanger are respectively connected with tail gas absorber, and the second reactor bottom is connected with
One sends pump and the 4th cooling water heat exchanger connected with second reactor outside, and described first sends pump output terminal outside is also associated with first
Butyric acid rectifying column；
The first butyric acid rectifying column top is connected with the 5th cooling water heat exchanger, the first submerged soil, the second outer circulation pump,
The second outer circulation pump output terminal is connected with butyraldehyde raw material intake pipeline and the first butyric acid rectifying column, the first butyric acid rectifying
Tower bottom sends pump outside and connects the second butyric acid rectifying column by the 3rd；
The second butyric acid rectifying column top is connected with the 6th cooling water heat exchanger, the second submerged soil, reflux pump, institute successively
State backflow pump output terminal and be connected with n-butyric acie export pipeline and the second butyric acid rectifying column, the second butyric acid rectifier bottoms connection
There is second to send pump outside, described second sends pump output terminal outside is connected with bottom of towe heavy constituent export pipeline and catalyst intake pipeline.
The catalyst preparation tank is connected with n-butyric acie intake pipeline and manganese acetate intake pipeline.
The first submerged soil bottom connects organic wastewater export pipeline.
The first butyric acid rectifier bottoms are connected with the low-pressure steam heater of formed circulation loop；
The second butyric acid rectifier bottoms are connected with the middle pressure steam heater of formed circulation loop；
The catalyst intake pipeline is provided with catalyst pump；The second cooling water heat exchanger input is provided with first
Outer circulation pump.
Compared with prior art, the beneficial effect that the technical solution of the utility model is brought is：
The utility model is to react to be made by dioxygen oxidation as raw material with butyraldehyde, and course of reaction belongs to continuous operation, raw
Product process is recycled using mutually equal catalyst, post catalyst reaction, and the cymogene acid after oxidation reaction is obtained by distillation system
Butyric acid product；The utility model has that process route is simple, it is easy to control to produce, using butyraldehyde direct oxidation, by rectifying skill
Art deviates from the heavy constituent that unoxidized butyraldehyde and butyraldehyde raw band come, and the purity of product, fourth are improve compared with biological fermentation process
In aldehyde oxidation process, not oxidized butyraldehyde returns re-oxidation in reactor by reflux pump, improves product yield.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
Reference:1 butyraldehyde raw material intake pipeline；2 oxygen input tube lines；3 first reactors；4 catalyst intake pipelines；
5 catalyst pumps；6 catalyst preparation tanks；7 n-butyric acie intake pipelines；8 manganese acetate intake pipelines；9 first cooling water heat exchangers；10
First outer circulation pump；11 second cooling water heat exchangers；12 second reactors；13 the 3rd cooling water heat exchangers；14 the 4th cooling waters
Heat exchanger；15 first send pump outside；16 tail gas absorbers；17 first butyric acid rectifying columns；18 the 5th cooling water heat exchangers；19 first receive
Liquid bath；20 second outer circulation pumps；21 organic wastewater export pipelines；22 low-pressure steam heaters；23 the 3rd send pump outside；24 second fourths
Sour rectifying column；25 the 6th cooling water heat exchangers；26 second submerged soils；27 reflux pumps；28 n-butyric acie export pipelines；29 middle pressure steams
Heater；30 second send pump outside；31 bottom of towe heavy constituent export pipelines.
Specific embodiment
The utility model will be further described below in conjunction with the accompanying drawings.
As shown in figure 1, a kind of butyraldehyde oxidation of the present utility model prepares the device of butyric acid, including it is connected with oxygen input tube
The first reactor 3 of line 2 and butyraldehyde raw material intake pipeline 1, the first reactor 3 is connected with by catalyst intake pipeline 4
Catalyst preparation tank 6, the catalyst preparation tank 6 is connected with n-butyric acie intake pipeline 7 and manganese acetate intake pipeline 8, described to urge
Agent intake pipeline 4 is provided with catalyst pump 5.The top of the first reactor 3 is connected with the first of formed circulation loop
Cooling water heat exchanger 9, the bottom of the first reactor 3 is connected with the second cooling water heat exchanger 11 of formed circulation loop,
The input of second cooling water heat exchanger 11 is provided with the first outer circulation pump 10, the output end of the second cooling water heat exchanger 11
It is also associated with second reactor 12.The second reactor 12 is connected with oxygen input tube line 2, and the second reactor 12 is pushed up
Portion is connected with the 3rd cooling water heat exchanger 13 of formed circulation loop, and the 3rd cooling water heat exchanger 13 and first is cooled down
Water- to-water heat exchanger 9 is respectively connected with tail gas absorber 16.The bottom of the second reactor 12 is connected with first, and to send pump 15 and the 4th outside cold
But water- to-water heat exchanger 14, the output end of the 4th cooling water heat exchanger 14 is connected to form circulation loop with second reactor 12.
Described first sends the output end of pump 15 outside is connected with the first butyric acid rectifying column 17, the top of the first butyric acid rectifying column 17
The 5th cooling water heat exchanger 18, the first submerged soil 19 and the second outer circulation pump 20 are connected with, the bottom of the first submerged soil 19 connects
Connect organic wastewater export pipeline 21, the output end of the second outer circulation pump 20 respectively with the first butyric acid rectifying column 17 and butyraldehyde raw material
Intake pipeline 1 is connected.The bottom of first butyric acid rectifying column 17 is connected with the low-pressure steam heating of formed circulation loop
Device 22, the bottom of the first butyric acid rectifying column 17 is also associated with the 3rd and sends pump 23 outside, and the described 3rd sends the connection of the output end of pump 23 outside
Second butyric acid rectifying column 24.The top of the second butyric acid rectifying column 24 is connected with the 6th cooling water heat exchanger 25, second receives successively
Liquid bath 26 and reflux pump 27, the output end of the reflux pump 27 connect the second butyric acid rectifying column 24 and n-butyric acie export pipeline respectively
28.The bottom of second butyric acid rectifying column 24 is connected with the middle pressure steam heater 29 of formed circulation loop, described second
The bottom of butyric acid rectifying column 24 is also associated with second and sends pump 30 outside, and described second sends the output end of pump 30 and catalyst intake pipeline 4 outside
It is connected, and described second sends the output end of pump 30 outside and is also associated with bottom of towe heavy constituent export pipeline 31.
Operating procedure using the present apparatus is as follows：
Step one, by the unoxidized fourth from the butyraldehyde in butyraldehyde head tank and the overhead extraction of the first butyric acid rectifying column 17
Aldehyde is delivered to first reactor 3, and under catalyst action, pressure enters for the oxygen of 0.55MPa after decompression with from space division station
Row oxidation reaction, releases heat in butyraldehyde oxidizing process, the mixing gaseous phase materials that tower top is obtained are cold through the first cooling water heat exchanger 9
But after, condensate liquid is back to first reactor 3, after not solidifying waste gas is absorbed into tail gas absorber 16, emptying；Tower reactor is obtained
Blended liquid phase material through the second cooling water heat exchanger 11 cool down after, a part after be back to first reactor 3, to first reaction
Material in device 3 is lowered the temperature, it is ensured that material reaction temperature is 55~60 DEG C in first reactor 3, Stress control 0.45~
0.5Mpa, another part enters second reactor 12.
The configuration of the catalyst：Manganese acetate and n-butyric acie are pressed 1:4 ratio is added in catalyst preparation tank 6, temperature
At 30~40 DEG C, agitated device mixing is allowed to be completely dissolved uniformly for control.
Step 2, the blended liquid phase material into second reactor 12 is with from space division station pressure after decompression
The oxygen of 0.55MPa proceeds oxidation reaction；After the mixing gaseous phase materials of top of tower are cooled down through the 3rd cooling water heat exchanger 13,
Condensate liquid is back to second reactor 12, after not solidifying waste gas is absorbed into tail gas absorber 16, emptying；Containing catalysis in tower reactor
The cymogene acid mixed liquor of agent mother liquor is sent pump 15 outside and is pumped out and is divided into two parts through first, and a part drops through the 4th cooling water heat exchanger 14
Second reactor 12 is back to after temperature, it is ensured that in second reactor 12 material reaction temperature be 55~60 DEG C, pressure be 0.35~
0.4Mpa, another part enters the first butyric acid rectifying column 17.
Step 3, heats through low-pressure steam heater 22 into the cymogene acid mixed liquor in the first butyric acid rectifying column 17 and steams
Hair, realizes that the tower top temperature of the first butyric acid rectifying column 17 is 86~89 DEG C, and column bottom temperature is 102 DEG C -104 DEG C, and Stress control is 0.3
~0.35MPa；The unoxidized butyraldehyde and water vapour of overhead extraction are condensed to 35 DEG C -40 DEG C through the 5th cooling water heat exchanger 18,
Sedimentation separation is carried out into the first submerged soil 19, wherein unoxidized butyraldehyde delivers to first by the part of the second outer circulation pump 20
Reactor 3, another part is back to the first butyric acid rectifying column 17, and organic wastewater is conveyed by export pipeline 21 and collected；Tower reactor is adopted
The butyric acid mixed liquor for going out sends pump 23 outside and pumps into the second butyric acid rectifying column 24 through the 3rd.
Step 4, into the butyric acid mixed liquor in the second butyric acid rectifying column 24 through the heating evaporation of middle pressure steam heater 29,
Tower top temperature is set to control at 168.5~172 DEG C, bottom temperature is controlled at 183~185 DEG C, and liquid level is 50%, tower pressure interior force control
In 0.085~0.09Mpa.The n-butyric acie of the top of the second butyric acid rectifying column 24 extraction, is cooled to through the 6th cooling water heat exchanger 25
35 DEG C~40 DEG C, into after the second submerged soil 26, through reflux pump, 27 points is two parts, and a part is back to the second butyric acid rectifying column
24, prevent the heavy constituents such as catalyst mother liquor from rising, it is ensured that the n-butyric acie purity of extraction reaches more than 99.5%, and another part is carried out
The extraction of n-butyric acie, delivers to finished product tank field, can subsequently carry out certified products and defective work inspection-classification.The second butyric acid rectifying
The restructuring that catalyst mother liquor, butyraldehyde raw band in tower 24 come grades from the discharge of its bottom, and it is two to send 30 points of pump outside through second
Point, a part is delivered to catalyst intake pipeline 4, is back to first reactor 3, and another part is delivered to heavy constituent tank field, enters
Row is collected.
Although being described to function of the present utility model and the course of work above, the utility model is not limited to
Above-mentioned concrete function and the course of work, above-mentioned specific embodiment are only schematical, rather than restricted, ability
The those of ordinary skill in domain can also make many forms under enlightenment of the present utility model, belong to guarantor of the present utility model
Within shield.
Claims (6)
1. a kind of butyraldehyde oxidation prepares the device of butyric acid, it is characterised in that former including being connected with oxygen input tube line (2) and butyraldehyde
The first reactor (3) of material intake pipeline (1), the first reactor (3) is connected with catalysis by catalyst intake pipeline (4)
Agent preparing tank (6), first reactor (3) top is connected with first cooling water heat exchanger (9) of formed circulation loop,
First reactor (3) bottom is connected with second cooling water heat exchanger (11) of formed circulation loop, and described second is cold
But water- to-water heat exchanger (11) is also associated with the second reactor (12) being connected with oxygen input tube line (2), the second reactor
(12) top is connected with the 3rd cooling water heat exchanger (13) of formed circulation loop, the 3rd cooling water heat exchanger (13)
Tail gas absorber (16) is respectively connected with the first cooling water heat exchanger (9), second reactor (12) bottom is connected with first
Send pump (15) and the 4th cooling water heat exchanger (14) connected with second reactor (12) outside, described first sends pump (15) output outside
End is also associated with the first butyric acid rectifying column (17)；
First butyric acid rectifying column (17) top is connected with the 5th cooling water heat exchanger (18), the first submerged soil (19), second
Outer circulation pump (20), the second outer circulation pump (20) output end is connected with butyraldehyde raw material intake pipeline (1) and the first butyric acid essence
Tower (17) is evaporated, the first butyric acid rectifying column (17) bottom sends pump (23) outside and connects the second butyric acid rectifying column (24) by the 3rd；
The second butyric acid rectifying column (24) top be connected with successively the 6th cooling water heat exchanger (25), the second submerged soil (26),
Reflux pump (27), reflux pump (27) output end is connected with n-butyric acie export pipeline (28) and the second butyric acid rectifying column (24),
Second butyric acid rectifying column (24) bottom is connected with second and sends pump (30) outside, and described second sends pump (30) output end outside is connected with
Bottom of towe heavy constituent export pipeline (31) and catalyst intake pipeline (4).
2. butyraldehyde oxidation according to claim 1 prepares the device of butyric acid, it is characterised in that the catalyst preparation tank
(6) n-butyric acie intake pipeline (7) and manganese acetate intake pipeline (8) are connected with.
3. butyraldehyde oxidation according to claim 1 prepares the device of butyric acid, it is characterised in that first submerged soil (19)
Bottom connects organic wastewater export pipeline (21).
4. butyraldehyde oxidation according to claim 1 prepares the device of butyric acid, it is characterised in that the first butyric acid rectifying column
(17) bottom is connected with the low-pressure steam heater (22) of formed circulation loop.
5. butyraldehyde oxidation according to claim 1 prepares the device of butyric acid, it is characterised in that the second butyric acid rectifying column
(24) bottom is connected with the middle pressure steam heater (29) of formed circulation loop.
6. butyraldehyde oxidation according to claim 1 prepares the device of butyric acid, it is characterised in that the catalyst intake pipeline
(4) it is provided with catalyst pump (5)；Second cooling water heat exchanger (11) input is provided with the first outer circulation pump (10).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621206708.3U CN206188686U (en) | 2016-11-09 | 2016-11-09 | Device of butyraldehyde oxidation preparation butyric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621206708.3U CN206188686U (en) | 2016-11-09 | 2016-11-09 | Device of butyraldehyde oxidation preparation butyric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206188686U true CN206188686U (en) | 2017-05-24 |
Family
ID=58734940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201621206708.3U Withdrawn - After Issue CN206188686U (en) | 2016-11-09 | 2016-11-09 | Device of butyraldehyde oxidation preparation butyric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206188686U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106431884A (en) * | 2016-11-09 | 2017-02-22 | 天津渤化永利化工股份有限公司 | Device and method for preparing butyric acid through butyraldehyde oxidation |
| CN114956981A (en) * | 2022-05-31 | 2022-08-30 | 鲁西化工集团股份有限公司 | System and process for continuously producing butyric acid |
-
2016
- 2016-11-09 CN CN201621206708.3U patent/CN206188686U/en not_active Withdrawn - After Issue
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106431884A (en) * | 2016-11-09 | 2017-02-22 | 天津渤化永利化工股份有限公司 | Device and method for preparing butyric acid through butyraldehyde oxidation |
| CN114956981A (en) * | 2022-05-31 | 2022-08-30 | 鲁西化工集团股份有限公司 | System and process for continuously producing butyric acid |
| CN114956981B (en) * | 2022-05-31 | 2024-01-26 | 鲁西化工集团股份有限公司 | System and process for continuously producing butyric acid |
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|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20170524 Effective date of abandoning: 20190830 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20170524 Effective date of abandoning: 20190830 |