CN205999303U - A kind of device of 2,2 bipyridyls of synthesis - Google Patents
A kind of device of 2,2 bipyridyls of synthesis Download PDFInfo
- Publication number
- CN205999303U CN205999303U CN201620892235.0U CN201620892235U CN205999303U CN 205999303 U CN205999303 U CN 205999303U CN 201620892235 U CN201620892235 U CN 201620892235U CN 205999303 U CN205999303 U CN 205999303U
- Authority
- CN
- China
- Prior art keywords
- reactor
- bipyridyl
- synthesis
- catalyst
- drawing mechanism
- 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.)
- Expired - Fee Related
Links
Landscapes
- Pyridine Compounds (AREA)
Abstract
The utility model discloses a kind of 2,2 bipyridyl devices of synthesis, belong to field of fine chemical.The device includes preheater, reactor, drawing mechanism, wherein inside reactor is liquid distribution trough, beds, catalyst supporting plate from top to bottom successively and unloads catalyst-assembly, gas distributor, drawing mechanism includes regulating valve, and after-treatment device is evaporimeter.Its technique enters into reactor for pyridine by preheater, through liquid distribution trough, is uniformly spread across beds, then pass through regulating valve after reacting, discharging, unreacted pyridine are applied mechanically through evaporimeter Distillation recovery, steam the residue after pyridine and be 2,2 bipyridyls.
Description
Technical field
The utility model belongs to field of fine chemical, and in particular to a kind of device of synthesis 2,2- bipyridyl.
Background technology
2,2- bipyridyls are a kind of important fine chemical materials, are widely used in the works such as medicine, agricultural chemicals, analysis, plating
In industry, can such as produce diquat dibromide, for copper plating additive, developer of analyzing metal elements etc..
2,2- bipyridyl traditional processing technologies are with 2- chloropyridine as raw material, are coupled through catalyst and form, tradition
Technique has that catalyst amount is big, a large amount of waste water and dregs, high cost serious to equipment corrosion the shortcomings of, GB899015,
The documents such as GB948956, GB1014076, US4966972, US315237, US3053846 are mentioned direct with catalyst pyridine
Be coupled and prepare 2,2 ' -2,2- bipyridyl, this technique has that Atom economy is good, three wastes, to equipment not burn into catalyst amount
Less, can with continuous operation high degree of automation the advantages of, in these documents equipment therefor be immersion type fixed bed liquid-solid reaction,
So there are some shortcomings：1. pyridine utilization rate is not high, because only that the pyridine contacted with catalyst could participate in reaction, and urges
Most pyridines in agent space can not participate in reaction, so as to cause bipyridyl concentration very low, in turn result in very big
Separating pressure；2. contain Toxic in reactant liquor, if catalyst is immersed in reactant liquor always, catalyst poisoning can be caused.
Utility model content
For above-mentioned problem, the utility model provides a kind of device of synthesis 2,2- bipyridyl, and this practicality is new
Type is flowed downward after reaction in time using the method for spraying, and so reaction can be removed in time and avoid catalyst poisoning, can carry again
High 2,2- bipyridyl concentration.
The purpose of this utility model can be achieved through the following technical solutions：
A kind of device of synthesis 2.2- bipyridyl, the device include preheater, at least one reactor, drawing mechanism and after
Processing meanss, the top of described reactor are provided with liquid distribution trough, and middle part is provided with reactor catalyst bed, the reactor
The lower section of beds is sequentially provided with catalyst supporting plate, is provided with gas distributor below the catalyst supporting plate, and described is pre-
The top of hot device is connected with the top of reactor, and the bottom of described reactor is connected with drawing mechanism, described drawing mechanism
It is connected with after-treatment device.
Described catalyst supporting plate is made up of two semicircular orifice plates, covers filter screen or sintered plate on orifice plate.Two and half
Circular orifice plate is connected in fixing axle by hinge, and described fixing axle is fixed on the lower section of reactor catalyst bed, orifice plate
Lower section has the catalyst pallet stand that can be moved up and down to support two pieces of orifice plates to rotate upwardly and downwardly with fixing axle as axle.When dress catalyst
When two semicircular orifice plates be in 180 degree, when catalyst is unloaded, two pieces of orifice plates rotate down inclination, facilitate catalyst to draw off.
In technical solutions of the utility model：Described after-treatment device is evaporimeter.
In technical solutions of the utility model：Catalyst pallet stand is additionally provided with below catalyst supporting plate.
In technical solutions of the utility model：The preheater is tubular heat exchanger.
In technical solutions of the utility model：Drawing mechanism includes pipeline and regulating valve.
In technical solutions of the utility model：Described reactor lower part is provided with low head liquid level gauge, and described regulating valve
Chain with low head liquid level gauge.
In some preferred technical schemes：The device of described synthesis 2,2- bipyridyl includes two reactors.
A kind of method for realizing synthesis 2,2- bipyridyl using said apparatus, the method are that pyridine is anti-by preheater entrance
Device is answered, through liquid distribution trough, is uniformly sprinkled upon on the catalyst in beds, pyridine is kept by controlling pyridine liquid air speed
Liquid film rather than immersion are formed in catalyst surface, the pyridine flow down for reacting passes through catalyst supporting plate, then through going out
Material device discharging, after discharging, unreacted pyridine reclaims pyridine by evaporimeter and applies mechanically, and residue is 2,2- bipyridyl.
In the method for above-mentioned synthesis 2,2- bipyridyl：In the heating-up temperature of preheater and entrance reactor, reaction temperature is
115～250 DEG C, the 0.1～2.0Mpa of pressure in reactor, pyridine liquid air speed are 0.1～10, beds used catalyst
For Raney's nickel or fixed-bed Raney nickel.It is preferred that reaction temperature is 150～250 in the heating-up temperature of preheater and entrance reactor
DEG C, the 0.6～1.7Mpa of pressure in reactor, pyridine liquid air speed are 2～4h-1.
The beneficial effects of the utility model：
2, the 2- bipyridyl device facilitates the handling of catalyst, is easy to control reaction condition, improves the stability of system；Should
2,2- bipyridyl techniques, atom economy are good, low cost, are the 50% of traditional handicraft, friendly to equipment, environmentally friendly, continuously
Change automated production, it is ensured that the stability of product quality.
Description of the drawings
Fig. 1 is the installation drawing for synthesizing 2,2- bipyridyl.
Wherein, 1 it is, the first ball valve, 2, be the second ball valve, 3, be the 3rd ball valve, 4 is the 4th ball valve, and 5 is the 5th ball valve, 6
For the 6th ball valve, 7 is the 7th ball valve, and 8 is the first regulating valve, and 9 is the second regulating valve, and 10 is preheater, and 11 is reactor catalysis
Agent bed, 12 is reactor, and 13 is evaporimeter, and 14 is liquid level gauge, and 15 is catalyst supporting plate, and 16 is gas distributor, and 17 for urging
Agent pallet stand, 18 is liquid distribution trough.
Specific embodiment
The utility model is described further with reference to embodiment, but protection domain of the present utility model is not limited to
This：
As Fig. 1, a kind of device of synthesis 2,2- bipyridyl, the device include preheater (10), two reactors (12), go out
Material device and after-treatment device, the top of described reactor (12) are provided with liquid distribution trough (18), and middle part is provided with reactor and urges
Agent bed (11), the lower section of the beds are sequentially provided with catalyst supporting plate (15), under catalyst supporting plate (15)
Side is provided with gas distributor (16), and the top of described preheater (10) is connected with the top of reactor (12), described reaction
The bottom of device (12) is connected with drawing mechanism, and described drawing mechanism is connected with after-treatment device.Described after-treatment device is
Evaporimeter (13).Catalyst pallet stand (17) is additionally provided with below catalyst supporting plate (15).Described preheater (10) are shell and tube
Heat exchanger.Described catalyst supporting plate (15) is made up of two semicircular orifice plates, covers filter screen or sintered plate on orifice plate.Two
Individual semicircular orifice plate is connected in fixing axle by hinge, and described fixing axle is fixed under reactor catalyst bed (11)
Side, has the catalyst pallet stand (17) that can be moved up and down to support two pieces of orifice plates to turn with fixing axle up and down as axle below orifice plate
Dynamic.The drawing mechanism of two reactors all includes pipeline and regulating valve.Described reactor (12) bottom is provided with low head liquid level
Meter (14), regulating valve (8) and regulating valve (9) are all chain with low head liquid level gauge (14).First ball valve (1) and the second ball valve (2)
For controlling the charging of pyridine, the 3rd ball valve (3) and the 6th ball valve (6) for unloading carried catalyst, the 4th ball valve (4) and the 7th ball
Valve (7) is used for controlling the connection between drawing mechanism and after-treatment device.
Embodiment 1-4
2,2- bipyridyl synthesis techniques are the conveyings of pyridine pump, through preheater, are heated to reaction temperature, enter reaction
Device, on liquid distribution trough, the catalyst fixed bed Raney's nickel of uniform drip washing to beds, pyridine liquid air 2～4h of speed-1, after reaction, pyridine flow down passes through catalyst supporting plate, discharges through regulating valve, and reactant liquor enters evaporimeter distillation pyridine, returns
Receipts are applied mechanically, and residue is 2,2- bipyridyl.The reaction condition of embodiment 1-4 and pyridine conversion per pass are shown in Table 1.
1 2,2- bipyridyl compound experiment data of table
| Embodiment | Reaction temperature/DEG C | Pressure/MPa | Pyridine liquid air speed/h-1 | Conversion per pass |
| 1 | 150 | 0.6 | 3 | 5.73% |
| 2 | 180 | 1.0 | 3 | 6.36% |
| 3 | 200 | 1.7 | 2 | 7.57% |
| 4 | 230 | 1.5 | 4 | 6.79% |
Claims (8)
1. a kind of device of synthesis 2.2- bipyridyl, it is characterised in that：The device includes preheater (10), at least one reactor
(12), drawing mechanism and after-treatment device, the top of described reactor (12) are provided with liquid distribution trough (18), and middle part is provided with instead
The lower section of device beds (11), reactor catalyst bed (11) is answered to be sequentially provided with catalyst supporting plate (15), described
Gas distributor (16), the described top of preheater (10) and the top of reactor (12) is provided with below catalyst supporting plate (15)
It is connected, the bottom of described reactor (12) is connected with drawing mechanism, and described drawing mechanism is connected with after-treatment device.
2. the device of synthesis 2.2- bipyridyl according to claim 1, it is characterised in that：Described after-treatment device is for steaming
Send out device (13).
3. the device of synthesis 2.2- bipyridyl according to claim 1, it is characterised in that：Below catalyst supporting plate (15) also
It is provided with catalyst pallet stand (17).
4. the device of synthesis 2.2- bipyridyl according to claim 1, it is characterised in that：Described preheater (10) are tubulation
Formula heat exchanger.
5. the device of synthesis 2.2- bipyridyl according to claim 1, it is characterised in that：Described catalyst supporting plate (15)
It is made up of two semicircular orifice plates, on orifice plate, covers filter screen or sintered plate.
6. the device of synthesis 2.2- bipyridyl according to claim 5, it is characterised in that：Two semicircular orifice plates pass through
Hinge is connected in fixing axle, and described fixing axle is fixed on the lower section of reactor catalyst bed (11), is had permissible below orifice plate
The catalyst pallet stand (17) for moving up and down supports two pieces of orifice plates to rotate upwardly and downwardly with fixing axle as axle.
7. according to claim 1 synthesis 2,2- bipyridyl device, it is characterised in that：Drawing mechanism includes pipeline and tune
Section valve.
8. according to claim 7 synthesis 2,2- bipyridyl device, it is characterised in that：Described reactor (12) bottom
Low head liquid level gauge (14) is provided with, and described regulating valve is chain with low head liquid level gauge (14).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620892235.0U CN205999303U (en) | 2016-08-17 | 2016-08-17 | A kind of device of 2,2 bipyridyls of synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620892235.0U CN205999303U (en) | 2016-08-17 | 2016-08-17 | A kind of device of 2,2 bipyridyls of synthesis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205999303U true CN205999303U (en) | 2017-03-08 |
Family
ID=58198975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620892235.0U Expired - Fee Related CN205999303U (en) | 2016-08-17 | 2016-08-17 | A kind of device of 2,2 bipyridyls of synthesis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205999303U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117121A (en) * | 2016-08-17 | 2016-11-16 | 南京红太阳生物化学有限责任公司 | A kind of device and method of synthesis 2,2 bipyridyls |
| CN111659329A (en) * | 2019-03-07 | 2020-09-15 | 江西福特化工新材料有限公司 | Condensation reaction device |
-
2016
- 2016-08-17 CN CN201620892235.0U patent/CN205999303U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117121A (en) * | 2016-08-17 | 2016-11-16 | 南京红太阳生物化学有限责任公司 | A kind of device and method of synthesis 2,2 bipyridyls |
| CN111659329A (en) * | 2019-03-07 | 2020-09-15 | 江西福特化工新材料有限公司 | Condensation reaction device |
| CN111659329B (en) * | 2019-03-07 | 2022-05-24 | 江西福特化工新材料有限公司 | Condensation reaction device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN205999303U (en) | A kind of device of 2,2 bipyridyls of synthesis | |
| CN106117121A (en) | A kind of device and method of synthesis 2,2 bipyridyls | |
| CN104098474B (en) | Nitrotoluene Continuous Liquid Phase catalytic hydrogenating reduction produces the device and method of monomethylaniline | |
| CN201710990U (en) | Variable aperture dual-flow sieve-plate tower | |
| CN101941720A (en) | Tube furnace ammonia evaporation process and equipment | |
| CN201988366U (en) | Continuous subcritical water tube type reaction apparatus | |
| CN110256334A (en) | A kind of process for catalytic synthesis and preparation facilities of penta chloropyridine | |
| CN103045276A (en) | Pyrolyzing furnace for powdered coal | |
| CN100460384C (en) | Process for synthesizing methyl acryloyl-(N,N-dimethyl propylene diamine) and device therefor | |
| CN201653071U (en) | Dipping and drying tower of vinyl acetate catalyst synthesized from acetylene in gas phase | |
| CN205886831U (en) | Gather methoxy dimethyl ether synthesis fixed bed reactor | |
| CN210559368U (en) | Preparation facilities of hydrogen chloride and ammonia | |
| CN206229322U (en) | A kind of processing system of catalyst for producing propylene with methanol | |
| CN105859505A (en) | Reaction system and method for removing green oil to prepare ethylene and method | |
| CN201906595U (en) | Cracking reactor | |
| CN205886832U (en) | It is listed as reactor to gather methoxy dimethyl ether synthesis | |
| CN104772102A (en) | Injection reaction device | |
| CN105237357B (en) | A kind of hydrogenation reaction device | |
| CN205797166U (en) | A kind of powder gas-solid reaction device | |
| CN206045989U (en) | A kind of response system of utilization prepared in slurry bed reactor for ethylene | |
| CN205700485U (en) | A kind of paste state bed reactor preparing ethylene | |
| CN220048079U (en) | Online regeneration system of fixed bed furfural hydrogenation catalyst | |
| CN218372319U (en) | Fluidized bed for preparing biodiesel by enzyme method | |
| CN108031426A (en) | A kind of board-like continuous flow Dow Chemical reactor | |
| CN110204412B (en) | Pretreatment device and treatment process for fixed bed catalytic hydrogenation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190701 Address after: 225000 room 103, Wanke golden street, East Road, Szeto temple, Yangzhou, Jiangsu, 103 Patentee after: Jiangsu Huadong culture and technology Financing Leasing Co., Ltd. Address before: 210048 No. 168 aromatics South Road, Nanjing chemical industry park, Jiangsu Patentee before: Nanjing Red Sun Biological Chemical Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170308 Termination date: 20190817 |