CN107954929A - A kind of process units of 8-hydroxyquinoline halides - Google Patents
A kind of process units of 8-hydroxyquinoline halides Download PDFInfo
- Publication number
- CN107954929A CN107954929A CN201711413456.0A CN201711413456A CN107954929A CN 107954929 A CN107954929 A CN 107954929A CN 201711413456 A CN201711413456 A CN 201711413456A CN 107954929 A CN107954929 A CN 107954929A
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- China
- Prior art keywords
- methacrylaldehyde
- kettle
- tank
- inlet tube
- synthesis reactor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/16—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D215/20—Oxygen atoms
- C07D215/24—Oxygen atoms attached in position 8
- C07D215/26—Alcohols; Ethers thereof
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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 process units of 8 oxyquinoline halides, including synthesis reactor, neutralize kettle, suction filtration tank, refining kettle, centrifuge, filter press, waste water treatment tank and dryer, feed inlet, catalyst inlet, sulfuric acid and methacrylaldehyde inlet tube, sulfuric acid and methacrylaldehyde inlet flow rate feedback regulation control valve and methacrylaldehyde air entrainment pipe are equipped with the top of the synthesis reactor, methacrylaldehyde measuring tank is equipped with above the feedback regulation control valve.Of the invention specially to set material inlet tube and bottoms material distributor pipe improvement reaction effect obvious in synthesis reactor, most effective scattered, reduction accessory substance and tar growing amount can be obtained in time into the raw material in kettle by allowing, reaction yield significantly improves, tar reduce, allow below refining effect it is more preferable, the technical process three wastes significantly reduce, raw materials consumption substantially reduces, especially soda acid consumption reduces obvious, and wastewater flow rate reduces 80%, and drying system is higher than conventionally used drier efficiency, time is short, and moisture drying is thorough.
Description
Technical field
Quinoline compound production equipment technology of the present invention, more particularly to a kind of production dress of 8-hydroxyquinoline halides
Put.
Background technology
8-hydroxyquinoline is an important organic synthesis intermediate, and the preparation of its synthesis technique and derivative, biology are living
Property research be current chemistry, one of Hot Contents of pharmacy and medical field.8-hydroxyquinoline as excellent performance metal from
Sub- chelating agent, metallic element chemical analysis, the extraction of metal ion, the light being widely used in metallurgical industry and analytical chemistry
Degree analysis and anti-corrosion of metal.Since most of 8-hydroxyquinoline and derivative have bioactivity, in medical industry field
Application it is also quite varied.8-hydroxyquinoline is directly used as disinfectant, its halide derivative, nitrification and N- oxides is to close
Into the raw material of medicine, the also intermediate as synthetic pesticide, dyestuff and other functional materials.Due to preparing 8- hydroxyls in the prior art
Base quinoline device structure is simple, and raw material timely and effective cannot disperse, and synthetic effect unobvious, can produce a large amount of byproducts and Jiao
Oil, can to it is follow-up it is refined produce a very large impact, and existing process units raw material consumptive material is more, produces a large amount of waste water, dry system
Also drying is slower for system, produces dry the problems such as being not thorough, and therefore, the present invention provides a kind of production dress of 8-hydroxyquinoline halides
Put.
The content of the invention
In view of the deficiencies of the prior art, the present invention proposes a kind of process units of 8-hydroxyquinoline halides, including synthesis
Kettle, neutralize kettle, suction filtration tank, refining kettle, centrifuge, filter press, waste water treatment tank and dryer, be equipped with the top of the synthesis reactor into
Material mouth, catalyst inlet, sulfuric acid and methacrylaldehyde inlet tube, sulfuric acid and methacrylaldehyde inlet flow rate feedback regulation control valve and methacrylaldehyde
Air entrainment pipe, the feedback regulation control valve top are equipped with methacrylaldehyde measuring tank, methacrylaldehyde are equipped with above methacrylaldehyde measuring tank
Storage tank, the methacrylaldehyde measuring tank connect methacrylaldehyde storage tank, and the synthesis reactor bottom is equipped with discharge port, the discharge port and neutralization
Kettle is connected, and the neutralization kettle is equipped with liquid caustic soda inlet tube, and flux of alkaline liquor control valve, flux of alkaline liquor are set on the liquid caustic soda inlet tube
Lye measuring tank is equipped with above control valve, lye storage tank is equipped with above lye measuring tank, lye import pipe connects lye measuring tank,
The lye measuring tank is connected with lye storage tank, and the neutralization bottom portion, which is equipped with, neutralizes discharge port, the neutralization discharge port connection
To suction filtration tank, the suction filtration tank is laid with filter aid filter cloth filled layer, suction filtration mouth connection suction filtration machine, the suction filtration tank and wastewater treatment
Groove connects, and the suction filtration tank discharging goes to refining kettle, refining kettle outlet connection centrifuge and filter press, and centrifugate outlet connection is useless
Water treatment trough.
Further improvement lies in that：Methacrylaldehyde feed distribution mechanism is equipped with the synthesis reactor, the distribution apparatus includes half
The hole that annulus inlet tube and distributor pipe are opened downwards point, the annulus inlet tube are fixed on synthesis reactor top and methacrylaldehyde inlet tube
Connection, methacrylaldehyde inlet tube lower section are connected to compressed air hose, are passed through air and play scattered charging and prevent reaction solution from blocking charging
Pipe, the distribution apparatus distribution hole are evenly distributed on semicircular ring inlet tube, and distribution hole count is six.
Further improvement lies in that：The drying machine is improved flow rotation drying machine, is equipped with and adds below the drying machine
Hot device, the side of the heater are equipped with mixing chamber, and described dryer inner is equipped with dryer section, and the dryer section outlet is equipped with rotation
Turn separator, the drying machine top side is equipped with air pulse vibrator, and the wet stock that the filter press is sent out passes through drying
Discharged after the combination drying structure drying of machine.
Further improvement lies in that：Special Resin filler is set in the wastewater treatment kettle, and the filter press is plate compression
Manhole and visor etc. are all additionally provided with the top of machine, the synthesis reactor and neutralization kettle and refining kettle routinely to configure.
Beneficial effects of the present invention：
It is obvious that the present invention specially sets material inlet tube and bottoms material distributor pipe to improve reaction effect in synthesis reactor, allows entrance
Raw material in kettle can obtain most effective scattered in time, reduce accessory substance and tar growing amount, reaction yield significantly improve, tar subtracts
It is few, allow below refining effect it is more preferable, color and luster is obviously improved, and the technical process three wastes significantly reduce, and raw materials consumption substantially reduces, especially
Its soda acid consumption reduces substantially, and wastewater flow rate reduces 80%, and drying system is higher than conventionally used drier efficiency, and the time is short, moisture content
It is dry thorough.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention.
Fig. 2 is production procedure schematic diagram of the present invention.
Fig. 3 is methacrylaldehyde feed distribution mechanism schematic diagram of the present invention.
Wherein：1- synthesis reactors, in 2- and kettle, 3- suction filtration tanks, 4- refining kettles, 5- centrifuges, 6- filter presses, 7- wastewater treatments
Groove, 8- dryers, 9- feed inlets, 10- catalyst inlets, 11- sulfuric acid and methacrylaldehyde inlet tube, 12- feedback regulation control valves,
13- methacrylaldehyde air entrainment pipe, 14- methacrylaldehyde measuring tanks, 15- methacrylaldehyde storage tanks, 16- discharge ports, 17- liquid caustic soda inlet tubes, 18-
Flux of alkaline liquor control valve, 19- lye measuring tanks, 20- lye storage tanks, in 21- and discharge port, 22- filter aid filter cloth filled layers,
23- methacrylaldehyde feed distribution mechanisms, 24- compressed air hoses, 25- heaters, 26- mixing chambers, 27- dryer sections, 28- rotating separations
Device, 29- air pulse vibrators, 30- Special Resin fillers.
Embodiment
In order to deepen the understanding of the present invention, the present invention is further described below in conjunction with embodiment, the present embodiment
It is only used for explaining the present invention, is not intended to limit the scope of the present invention..
A kind of process units of 8-hydroxyquinoline halides according to Fig. 1,2,3, including synthesis reactor 1, neutralize kettle 2,
Suction filtration tank 3, refining kettle 4, centrifuge 5, filter press 6, waste water treatment tank 7 and dryer 8, the top of synthesis reactor 1 are equipped with charging
Mouth 9,12 and of catalyst inlet 10, sulfuric acid and methacrylaldehyde inlet tube 11, sulfuric acid and methacrylaldehyde inlet flow rate feedback regulation control valve
Methacrylaldehyde air carries pipe 13 secretly, and the top of feedback regulation control valve 12 is equipped with methacrylaldehyde measuring tank 14, methacrylaldehyde measuring tank 14
Top is equipped with methacrylaldehyde storage tank 15, and the methacrylaldehyde measuring tank 14 connects methacrylaldehyde storage tank 15, and 1 bottom of synthesis reactor is equipped with out
Material mouth 16, the discharge port 16 are connected with kettle 2 is neutralized, and the neutralization kettle 2 is equipped with liquid caustic soda inlet tube 17, the liquid caustic soda import
Set flux of alkaline liquor control valve 18 on pipe 17, the top of flux of alkaline liquor control valve 18 is equipped with lye measuring tank 19, on lye measuring tank 19
Side is equipped with lye storage tank 20, and lye import pipe 17 connects lye measuring tank 19, and the lye measuring tank 19 connects with lye storage tank 20
Logical, 2 bottom of the neutralization kettle, which is equipped with, neutralizes discharge port 21, and the neutralization discharge port 21 is communicated to suction filtration tank 3, the suction filtration tank 3
Filter aid filter cloth filled layer 22, suction filtration mouth connection suction filtration machine are laid with, the suction filtration tank 3 is connected with waste water treatment tank 7, the suction filtration
The discharging of groove 3 goes to refining kettle 4, the outlet of refining kettle 4 connection centrifuge 5 and filter press 6, and centrifugate outlet connects waste water treatment tank 7,
Methacrylaldehyde feed distribution mechanism 23 is equipped with the synthesis reactor 1, the distribution apparatus 23 includes semicircular ring inlet tube and distributor pipe
The hole opened point downwards, the annulus inlet tube are fixed on 1 top of synthesis reactor and are connected with methacrylaldehyde inlet tube 11, methacrylaldehyde import
The lower section of pipe 11 is connected to compressed air hose 24, is passed through air and plays scattered charging and prevent reaction solution from blocking feed pipe, the distribution
23 distribution hole of device is evenly distributed on semicircular ring inlet tube, and distribution hole count is six, and the drying machine 8 revolves for improved air-flow
Turn drying machine, the lower section of drying machine 8 is equipped with heater 25, and the side of the heater 25 is equipped with mixing chamber 26, described drying
Machine 8 is internally provided with dryer section 27, and the outlet of dryer section 27 is equipped with rotary separator 28, and 8 top side of drying machine is equipped with
Air pulse vibrator 29, is discharged after the combination drying structure drying that the wet stock that the filter press 6 is sent out passes through drying machine 8,
Special Resin filler 30 is set in the wastewater treatment kettle 7, and the filter press 6 is plate and frame filter press, and the synthesis reactor 1, neutralize
Manhole and visor etc. is designed with the top of kettle 2 and refining kettle routinely to configure.
Beneficial effect：The present invention is specially provided with distribution apparatus 23, and the material inlet of distribution apparatus 23 in synthesis reactor 1
Pipe and bottoms material distributor pipe improvement reaction effect are obvious, and most effective scattered, reduction can be obtained in time into the raw material in kettle by allowing
Accessory substance and tar growing amount, reaction yield significantly improve, tar reduce, allow below refining effect it is more preferable, color and luster is obviously improved,
The technical process three wastes significantly reduce, and raw materials consumption substantially reduces, and especially soda acid consumption reduces obvious, and wastewater flow rate reduces 80%,
Drying system 8 is higher than conventionally used drier efficiency, and the time is short, and moisture drying is thorough.
First catalyst and raw material are added in synthesis reactor 1, methacrylaldehyde storage tank 15 passes through sulfuric acid and methacrylaldehyde inlet tube 11
Cooperation compressed air hose 11 is passed through methacrylaldehyde and sulfuric acid is carried secretly into a small amount of air, passes through 23 upper semi-circle of methacrylaldehyde feed distribution mechanism
Ring inlet tube and distribution hole methacrylaldehyde are uniformly added in synthesis reactor 1, then are stirred synthesis, by semi-finished stock after synthesis
It is passed through and neutralizes in kettle 2, corresponding annex solution aqueous slkali stirring discharges into raw material in suction filtration tank 3 after neutralizing, and passes through filter aid filter cloth
Filled layer 22 carries out filtration treatment, then is refined raw material feeding refining kettle 4 by suction filter pump, then passes through centrifuge 5 again
Being handled with filter press 6, be finally sent into drying machine 8 accordingly, air is heated by filter in heater 25, with
Contact from the wet stock that filter press 6 is sent and mixed in mixing chamber 26, material is dried in dryer section 27, and dry raw material is revolving
Turn to be separated and collected in separator 28, the waste water wherein produced in synthesis reactor 1, suction filtration tank 3, centrifuge 5 passes through wastewater treatment kettle 7
Interior setting Special Resin filler 30 handled, and liquid phase water solvent portions, which then return, in suction filtration tank 3 neutralizes in kettle 2.
Claims (4)
- A kind of 1. process units of 8-hydroxyquinoline halides, it is characterised in that：Including synthesis reactor（1）, neutralize kettle（2）, filter Groove（3）, refining kettle（4）, centrifuge（5）, filter press（6）, waste water treatment tank（7）And dryer（8）, the synthesis reactor（1）Top Portion is equipped with feed inlet（9）, catalyst inlet（10）, sulfuric acid and methacrylaldehyde inlet tube（11）, sulfuric acid and methacrylaldehyde inlet flow rate it is anti- Present adjusting control valve（12）Carry secretly and manage with methacrylaldehyde air（13）, the feedback regulation control valve（12）Top is equipped with methacrylaldehyde meter Measuring tank（14）, methacrylaldehyde measuring tank（14）Top is equipped with methacrylaldehyde storage tank（15）, the methacrylaldehyde measuring tank（14）Connect propylene Aldehyde storage tank（15）, the synthesis reactor（1）Bottom is equipped with discharge port（16）, the discharge port（16）With neutralization kettle（2）It is connected, institute State neutralization kettle（2）It is equipped with liquid caustic soda inlet tube（17）, the liquid caustic soda inlet tube（17）On set flux of alkaline liquor control valve（18）, lye Flow control valve（18）Top is equipped with lye measuring tank（19）, lye measuring tank（19）Top is equipped with lye storage tank（20）, lye Inlet tube（17）Connect lye measuring tank（19）, the lye measuring tank（19）With lye storage tank（20）Connection, the neutralization kettle （2）Bottom, which is equipped with, neutralizes discharge port（21）, the neutralization discharge port（21）It is communicated to suction filtration tank（3）, the suction filtration tank（3）It is laid with Filter aid filter cloth filled layer（22）, suction filtration mouth connection suction filtration machine, the suction filtration tank（3）With waste water treatment tank（7）Connection, the pumping Filter pocket（3）Discharging goes to refining kettle（4）, refining kettle（4）Outlet connection centrifuge（5）And filter press（6）, centrifugate outlet connection Waste water treatment tank（7）.
- A kind of 2. process units of 8-hydroxyquinoline halides according to claim 1, it is characterised in that：The synthesis reactor （1）It is interior to be equipped with methacrylaldehyde feed distribution mechanism（23）, the distribution apparatus（23）It is downward including semicircular ring inlet tube and distributor pipe The hole opened point, the annulus inlet tube are fixed on synthesis reactor（1）Top and methacrylaldehyde inlet tube（11）Connection, methacrylaldehyde import Pipe（11）Lower section is connected to compressed air hose（24）, it is passed through air and plays scattered charging and prevent reaction solution from blocking feed pipe, it is described Distribution apparatus（23）Distribution hole is evenly distributed on semicircular ring inlet tube, and distribution hole count is six.
- A kind of 3. process units of 8-hydroxyquinoline halides according to claim 1, it is characterised in that：The drying machine （8）For improved flow rotation drying machine, the drying machine（8）Lower section is equipped with heater（25）, the heater（25）One Side is equipped with mixing chamber（26）, described drying machine（8）It is internally provided with dryer section（27）, the dryer section（27）Outlet is equipped with rotation point From device（28）, the drying machine（8）Top side is equipped with air pulse vibrator（29）, the filter press（6）The wet thing sent out Material passes through drying machine（8）Combination drying structure drying after discharge.
- A kind of 4. process units of 8-hydroxyquinoline halides according to claim 1, it is characterised in that：At the waste water Manage kettle（7）Interior setting Special Resin filler（30）, the filter press（6）For plate and frame filter press, the synthesis reactor（1）, neutralize kettle （2）Routinely configured with manhole and visor etc. is designed with the top of refining kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711413456.0A CN107954929A (en) | 2017-12-24 | 2017-12-24 | A kind of process units of 8-hydroxyquinoline halides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711413456.0A CN107954929A (en) | 2017-12-24 | 2017-12-24 | A kind of process units of 8-hydroxyquinoline halides |
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| Publication Number | Publication Date |
|---|---|
| CN107954929A true CN107954929A (en) | 2018-04-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711413456.0A Pending CN107954929A (en) | 2017-12-24 | 2017-12-24 | A kind of process units of 8-hydroxyquinoline halides |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267943A (en) * | 2011-07-29 | 2011-12-07 | 江苏力达宁化工有限公司 | Method for preparing 5-chloro-8-hydroxyquinoline |
| ES2525114A1 (en) * | 2013-06-18 | 2014-12-18 | Universidad De Burgos | Colorimetric iron sensor in aqueous and biological media, such as industrial water, wine and blood (Machine-translation by Google Translate, not legally binding) |
| CN106986824A (en) * | 2017-05-08 | 2017-07-28 | 宜兴市宏博精细化工有限公司 | A kind of 8 oxyquinoline preparation facilities |
| CN107029642A (en) * | 2017-05-08 | 2017-08-11 | 宜兴市宏博精细化工有限公司 | A kind of oxyquinoline preparation facilities of 5 chlorine 8 |
-
2017
- 2017-12-24 CN CN201711413456.0A patent/CN107954929A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267943A (en) * | 2011-07-29 | 2011-12-07 | 江苏力达宁化工有限公司 | Method for preparing 5-chloro-8-hydroxyquinoline |
| ES2525114A1 (en) * | 2013-06-18 | 2014-12-18 | Universidad De Burgos | Colorimetric iron sensor in aqueous and biological media, such as industrial water, wine and blood (Machine-translation by Google Translate, not legally binding) |
| CN106986824A (en) * | 2017-05-08 | 2017-07-28 | 宜兴市宏博精细化工有限公司 | A kind of 8 oxyquinoline preparation facilities |
| CN107029642A (en) * | 2017-05-08 | 2017-08-11 | 宜兴市宏博精细化工有限公司 | A kind of oxyquinoline preparation facilities of 5 chlorine 8 |
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Application publication date: 20180424 |