CN106892802A - A kind of device of preparing benzaldehyde by oxidizing toluene - Google Patents
A kind of device of preparing benzaldehyde by oxidizing toluene Download PDFInfo
- Publication number
- CN106892802A CN106892802A CN201710213490.7A CN201710213490A CN106892802A CN 106892802 A CN106892802 A CN 106892802A CN 201710213490 A CN201710213490 A CN 201710213490A CN 106892802 A CN106892802 A CN 106892802A
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- CN
- China
- Prior art keywords
- autoclave
- valve
- pipeline
- toluene
- oxygen cylinder
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- 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.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
- C07C45/34—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds
- C07C45/36—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in compounds containing six-membered aromatic rings
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of device of preparing benzaldehyde by oxidizing toluene, including：Autoclave, agitator, oxygen cylinder, air bottle, sampler, temperature control equipment；The direction vertically downward of pipeline is provided with probe tube between the autoclave and oxygen cylinder, and the probe tube is provided with the 3rd valve, and the sampler is arranged on the probe tube lower section；Principle of device of the invention is simple, used suitable for laboratory, the present invention uses autoclave as the reactor of toluene oxidation, interacted the pressure controlled in reactor by air bottle and oxygen cylinder, the present invention is poor using external and internal pressure simultaneously, can automatic sampling, the second valve is opened after the completion of sampling, the sample in pipeline is set to return in reactor and enter into sampler on a small quantity, n.s residual in pipeline, it is ensured that the accuracy of lower sub-sampling, apparatus of the present invention can be with grab sampling, facilitate many sub-samplings, significantly improve conventional efficient.
Description
Technical field
The present invention relates to technical field of chemical, and in particular to a kind of device of preparing benzaldehyde by oxidizing toluene.
Background technology
Benzaldehyde is medical in cosmetics as a kind of important organic synthesis raw material, agricultural chemicals, the industry such as spices and dyestuff
On be widely used.The commercial run for preparing benzaldehyde at present mainly has three major types：The direct oxygen of chlorination toluene Hydrolyze method, toluene
Change method, benzyl alcohol oxidation method.Wherein toluene under gas phase or liquid-phase condition direct oxidation generation benzaldehyde be it is relatively inexpensive and
The method of environmental protection；The installation cost of current preparing benzaldehyde by oxidizing toluene is too high, complex operation and laboratory installation is in experiment
During, typically all can many sub-samplings be analyzed research, there is presently no a kind of toluene oxidation for being suitable to laboratory research and development
Prepare the device of benzaldehyde.
The content of the invention
It is an object of the invention to regarding to the issue above, there is provided a kind of device of preparing benzaldehyde by oxidizing toluene, this hair
Bright apparatus structure is simple, and easy to operate, security performance is high, poor using external and internal pressure, can automatic sampling, pass through after the completion of sampling
Control valve, in the sample in pipeline is returned to reactor, n.s residual in pipeline, it is ensured that the accuracy of lower sub-sampling, side
Just many sub-samplings.
The present invention provide technical scheme be：
A kind of device of preparing benzaldehyde by oxidizing toluene, including：Autoclave, agitator, oxygen cylinder, air bottle, take
Sample device, temperature control equipment；
One end of wherein described agitator is arranged in autoclave, for reaction stirred, the autoclave
It is connected with oxygen cylinder, air bottle successively by pipeline, and is provided with the first valve, the second valve, first valve and the second valve
Door is in parallel, the first Valve controlling oxygen cylinder, and the second Valve controlling air bottle, wherein one end of pipeline are deeply to reaction under high pressure
Bottom portion；Wherein autoclave is used for preparing benzaldehyde by oxidizing toluene, and wherein toluene and catalyst is added to autoclave
In, control to stir rotation by agitator, then be passed through oxygen by oxygen cylinder carries out oxidation reaction with toluene, also by oxygen cylinder
Control the pressure in autoclave simultaneously with air bottle；
The direction vertically downward of pipeline is provided with probe tube between the autoclave and oxygen cylinder, is set on the probe tube
There is the 3rd valve, the sampler is arranged on the probe tube lower section, and probe tube can go deep into sampler cavity；It is wherein described
Sampler is the container that can contain liquid, such as beaker, measuring cup, and preferably container transparent has scale, due to autoclave
Interior pressure is more than atmospheric pressure, closes first, second valve, opens the 3rd valve, due to inside and outside differential pressure, sample can it is automatic from
In flowing to sampler by pipeline, probe tube in reactor, after sample takes, the second valve of opening causes back flow of sample in pipeline
To in autoclave and a small amount of into sampler, n.s residual in pipeline turns off the 3rd valve, opens the first valve
Door, then reacted；
The temperature control equipment is provided with recirculated cooling water device, heater, temperature inductor, wherein the circulating cooling
Water installations are arranged on autoclave outer wall surrounding, and the heater is arranged on autoclave inwall, the temperature sense
Device is arranged on parallel with the agitating shaft of agitator in autoclave and does not contact agitator, is controlled by temperature control equipment high
Temperature in pressure reactor.
Preferably, also include：Device for recovering tail gas, the device for recovering tail gas is provided with aspiration pump, tail gas recycle tank, institute
Aspiration pump is stated to be connected with autoclave, after the completion of preparing benzaldehyde by oxidizing toluene, the recovery of tail gas in autoclave.
Preferably, pressure gauge is additionally provided with the pipeline, the pressure gauge is arranged near autoclave, testing tube
Road pressure, improves security performance.
Preferably, booster pump is additionally provided with the pipeline, the booster pump is arranged in pressure gauge and autoclave
Between, booster pump can quickly increase pressure in autoclave.
Beneficial effects of the present invention are as follows：
Principle of device of the invention is simple, it is adaptable to used in laboratory, and the present invention is using autoclave as toluene
The reactor of oxidation, interacted the pressure controlled in reactor by air bottle and oxygen cylinder, while the present invention is using inside and outside
Pressure differential, can automatic sampling, the second valve is opened after the completion of sampling, the sample in pipeline is returned in reactor and a small amount of entrance
To in sampler, n.s residual in pipeline, it is ensured that the accuracy of lower sub-sampling, apparatus of the present invention can be convenient with grab sampling
Many sub-samplings, significantly improve conventional efficient.
Brief description of the drawings
Fig. 1 is the installation drawing of preparing benzaldehyde by oxidizing toluene of the present invention；
Identified in figure：1 is autoclave, and 2 is agitator, and 3 is oxygen cylinder, and 4 is air bottle, and 5 is temperature control equipment,
6 is sampler, and 7 is tail gas recycle tank, and 8 is aspiration pump, and 9 is pressure gauge, and 10 is booster pump, and 11 is fixator, and 21 is agitating shaft,
31 is the first valve, and 41 is the second valve, and 51 is recirculated cooling water device, and 52 is heater, and 53 is temperature inductor, and 61 is the
Three valves, 62 is probe tube.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
As shown in figure 1, a kind of device of preparing benzaldehyde by oxidizing toluene, including：Autoclave 1, agitator 2, oxygen
Bottle 3, air bottle 4, sampler 6, temperature control equipment 5；
One end of wherein described agitator 2 is arranged in autoclave 1, for reaction stirred, the reaction under high pressure
Kettle 1 is connected with oxygen cylinder 3, air bottle 4 successively by pipeline, and is provided with the first valve 31, the second valve 41, first valve
31 is in parallel with the second valve 41, and first valve 31 controls oxygen cylinder 3, the control air bottle 4 of the second valve 41 to open the first valve
Oxygen in 31 oxygen cylinders 3 of door is just passed into autoclave 1, and wherein one end of pipeline is deeply to the bottom of autoclave 1；
Wherein autoclave 1 is used for preparing benzaldehyde by oxidizing toluene, and wherein toluene and catalyst is added in autoclave 1, leads to
Cross the control stirring of agitator 2 to rotate, then be passed through oxygen by oxygen cylinder 3 carries out oxidation reaction with toluene, also by the He of oxygen cylinder 3
Air bottle 4 controls the pressure in autoclave 1 simultaneously, and the bottom of autoclave 1 is provided with fixator 21, for fixing reaction under high pressure
Kettle 1；
The direction vertically downward of pipeline is provided with probe tube 62, the probe tube between the autoclave 1 and oxygen cylinder 3
62 are provided with the 3rd valve 61, and the sampler 6 is arranged on the lower section of the probe tube 62；Preparing benzaldehyde by oxidizing toluene typically exists
Reacted under conditions of high pressure, therefore pressure in autoclave 1 is more than atmospheric pressure, closes the first valve 31, the second valve
41, the 3rd valve 61 is opened, due to inside and outside differential pressure, sample automatic can be flowed to from autoclave 1 by pipeline, probe tube 62
In sampler 6, after sample takes, open air stream in the air bottle of the second valve 41 send as an envoy in pipeline back flow of sample it is anti-to high pressure
Answer in kettle 1 and it is a small amount of enter in sampler 6, turn off the 3rd valve 61, the first valve 31 is opened, then reacted, in pipeline
N.s are remained, and do not interfere with sub-sampling under sample；
The temperature control equipment 5 is provided with recirculated cooling water device 51, heater 52, temperature inductor 53, wherein described
Recirculated cooling water device 51 is arranged on the outer wall surrounding of autoclave 1, and the heater 52 is arranged on the inwall of autoclave 1
On, the temperature inductor 53 is arranged on parallel with the agitating shaft 21 of agitator 2 in autoclave 1 and does not contact agitator 2,
By temperature in the control autoclave 1 of temperature control equipment 5.
Wherein another implementation method, also includes：Device for recovering tail gas, the device for recovering tail gas is provided with aspiration pump 8, tail gas
Recycling can 7, the aspiration pump 8 is connected with autoclave 1, for preparing benzaldehyde by oxidizing toluene after the completion of, by aspiration pump 7
By the recovery of tail gas in autoclave 1, then discharge after treatment, be conducive to the safety and not contaminated air of experiment, green
Environmental protection,.
Another implementation method, is additionally provided with pressure gauge 9 on the pipeline, it is attached that the pressure gauge 9 is arranged on autoclave 1
Closely, pipeline pressure is tested, experiment safety is improved.
Another implementation method, is additionally provided with booster pump 10 on the pipeline, the booster pump 10 is arranged on pressure gauge 9 and high pressure
In the middle of reactor 1, booster pump can quickly increase pressure in autoclave, and booster pump is arranged near autoclave, subtracts
The pressure in education and correction for juvenile offenders road and can quickly increase pressure in autoclave, improve the security of experiment.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and implementation method
With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the embodiment with description.
Claims (4)
1. a kind of device of preparing benzaldehyde by oxidizing toluene, it is characterised in that including：Autoclave, agitator, oxygen cylinder,
Air bottle, sampler, temperature control equipment；
Wherein, one end of agitator is arranged in autoclave, and for reaction stirred, the autoclave passes through pipeline
It is connected with oxygen cylinder, air bottle successively, and is provided with the first valve, the second valve, first valve and the second valve in parallel, institute
The first Valve controlling oxygen cylinder is stated, the second Valve controlling air bottle, wherein one end of pipeline are deeply to high pressure reactor bottom；
The direction vertically downward of pipeline is provided with probe tube between the autoclave and oxygen cylinder, and the probe tube is provided with
Three valves, the sampler is arranged on the probe tube lower section；
The temperature control equipment is provided with recirculated cooling water device, heater, temperature inductor, wherein the recirculated cooling water is filled
Put and be arranged on autoclave outer wall surrounding, the heater is arranged on autoclave inwall, and the temperature inductor sets
Put parallel with the agitating shaft of agitator in autoclave and do not contact agitator.
2. the device of preparing benzaldehyde by oxidizing toluene as claimed in claim 1, it is characterised in that also include：Tail gas recycle is filled
Put, the device for recovering tail gas is provided with aspiration pump, tail gas recycle tank, and the aspiration pump is connected with autoclave, for toluene
After the completion of preparing benzaldehyde by oxidizing, the recovery of tail gas in autoclave.
3. the device of preparing benzaldehyde by oxidizing toluene as claimed in claim 1, it is characterised in that pressure is additionally provided with the pipeline
Power table, the pressure gauge is arranged near autoclave.
4. the device of preparing benzaldehyde by oxidizing toluene as claimed in claim 3, it is characterised in that increasing is additionally provided with the pipeline
Press pump, the booster pump is arranged in the middle of pressure gauge and autoclave.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710213490.7A CN106892802A (en) | 2017-03-29 | 2017-03-29 | A kind of device of preparing benzaldehyde by oxidizing toluene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710213490.7A CN106892802A (en) | 2017-03-29 | 2017-03-29 | A kind of device of preparing benzaldehyde by oxidizing toluene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106892802A true CN106892802A (en) | 2017-06-27 |
Family
ID=59192713
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710213490.7A Withdrawn CN106892802A (en) | 2017-03-29 | 2017-03-29 | A kind of device of preparing benzaldehyde by oxidizing toluene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106892802A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114558532A (en) * | 2022-03-04 | 2022-05-31 | 连云港市工投集团利海化工有限公司 | Production method and equipment of environment-friendly benzaldehyde |
-
2017
- 2017-03-29 CN CN201710213490.7A patent/CN106892802A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114558532A (en) * | 2022-03-04 | 2022-05-31 | 连云港市工投集团利海化工有限公司 | Production method and equipment of environment-friendly benzaldehyde |
| CN114558532B (en) * | 2022-03-04 | 2023-02-17 | 连云港市工投集团利海化工有限公司 | Production method and equipment of environment-friendly benzaldehyde |
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| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170627 |