CN206328318U - Reduction with sodium bisulfide produces the device of aminoanisole - Google Patents

Abstract

The utility model discloses the device that a kind of reduction with sodium bisulfide produces aminoanisole, including Nitroanisole storage tank, NaHS storage tank, liquid caustic soda storage tank, one-level reduction kettle, second-stage reduction kettle, three-level reduction kettle, discharging Liquid level tank, reducing solution cooler, reduction liquid/gas separator, aminoanisole storage tank, waste water tank, the one-level reduction kettle, second-stage reduction kettle, three-level reduction kettle structure are identical；The utility model realizes continuous production, and high degree of automation can improve production efficiency, reduce labor strength, reduce production cost, and equipment safety performance is improved, and accomplishes essential safety.

Description

Reduction with sodium bisulfide produces the device of aminoanisole

Technical field

The utility model belongs to chemical production field, and more particularly to a kind of reduction with sodium bisulfide produces the dress of aminoanisole Put.

Background technology

Aminoanisole（Predominantly o-aminoanisole or paraphenetidine）In being important dyestuff, spices and medicine Mesosome.Current domestic production aminoanisole mainly uses three kinds of sodium sulfide reducing, reduction with sodium bisulfide and catalytic hydrogenating reduction Production technology.Using vulcanization sodium reduction, waste water, useless solid amount are big, and production cost is high, and hydrogen is needed using catalytic hydrogenating reduction technique Resource, requires high, project investment is big to device fabrication, and uses reduction with sodium bisulfide technique, waste water, useless measures small, Er Qieguo admittedly The NaHS aboundresources of interior by-product, it is cheap, it is obvious using reduction with sodium bisulfide technology investment and cost advantage.

There is the producer using reduction with sodium bisulfide technique productions aminoanisole the country, but uses interval reduction apparatus Production, interval reduction apparatus production capacity is low, and operation labor intensity is big, and production cost is high.

Utility model content

The purpose of this utility model is to provide the device that a kind of reduction with sodium bisulfide produces aminoanisole.

The technical solution for realizing the utility model purpose is：A kind of reduction with sodium bisulfide produces the dress of aminoanisole Put and method, including Nitroanisole storage tank, NaHS storage tank, liquid caustic soda storage tank, one-level reduction kettle, second-stage reduction kettle, three-level Reduction kettle, discharging Liquid level tank, reducing solution cooler, reduction liquid/gas separator, aminoanisole storage tank, waste water tank, it is described One-level reduction kettle, second-stage reduction kettle, three-level reduction kettle structure are identical, and the one-level reduction kettle includes housing, transmission device, water conservancy diversion Cylinder, stirring vane, agitating shaft, heat exchange coil, the transmission device are fixed on case top by support, and guide shell passes through support It is suspended in housing, guide shell inwall is provided with radial direction baffle plate, stirring vane is connected by agitating shaft with transmission device, stirring vane It is suspended in guide shell, heat exchange coil is provided between housing and guide shell, the side wall of housing is provided with mixed liquor import, mixed liquor Outlet, is going out the inner side of the housing of mixture export side provided with discharging weir, the opened upper end on the weir that discharges, the bottom on the weir that discharges with Connected inside reactor, the case top is provided with Nitroanisole charging aperture, NaHS charging aperture, liquid caustic soda charging aperture, its Middle Nitroanisole charging aperture is connected with Nitroanisole feed conduit one end, and the Nitroanisole feed conduit other end, which is placed in, leads In flow cartridge, NaHS charging aperture is connected with NaHS feed conduit one end, and the NaHS feed conduit other end, which is placed in, leads In flow cartridge, liquid caustic soda charging aperture is connected with liquid caustic soda feed conduit one end, and the liquid caustic soda feed conduit other end is placed in guide shell；It is described to go back Stoste separator is provided with the import of separator mixed liquor, light liquid outlet, heavy liquid exit；

Wherein Nitroanisole storage tank is connected by pipeline with Nitroanisole measuring pump, and Nitroanisole measuring pump passes through Pipeline is connected with the Nitroanisole charging aperture of one-level reduction kettle, and NaHS storage tank is connected by pipeline and NaHS measuring pump Connect, NaHS measuring pump is connected by the NaHS charging aperture of pipeline and one-level reduction kettle, second-stage reduction kettle, three-level reduction kettle Connect, liquid caustic soda storage tank is connected by pipeline with liquid caustic soda measuring pump, liquid caustic soda measuring pump is fed by the liquid caustic soda of pipeline and one-level reduction kettle Mouth connection, the mixture export of one-level reduction kettle is connected by pipeline with the mixed liquor import of second-stage reduction kettle, second-stage reduction kettle Mixture export be connected by pipeline with the mixed liquor import of three-level reduction kettle, the mixture export of three-level reduction kettle passes through pipe Road is connected with discharging Liquid level tank, and discharging Liquid level tank is connected by pipeline with reducing solution cooler, reducing solution cooler Separator mixed liquor import by pipeline with reducing liquid/gas separator be connected, reduce the heavy liquid exit of liquid/gas separator by pipeline and Aminoanisole storage tank is connected, and the light liquid outlet of reduction liquid/gas separator is connected by pipeline with waste water tank.

Preferably, it is described reduction liquid/gas separator shell separator by front side board, left plate, right plate, with radian after Side plate, base plate, top board composition, dividing plate are provided with shell separator, dividing plate is sealedly and fixedly connected with front side board, base plate, dividing plate and Back side panel with radian leaves gap, and dividing plate will be divided into feed zone and sub-material area, feed zone and sub-material area inside shell separator Connected by gap, separator mixed liquor import is provided with the front side board of feed zone, provided with light on the front side board in sub-material area Liquid is exported and heavy liquid exit outlet, and light liquid outlet is higher than heavy liquid exit, and heavy liquid exit is connected with heavy-fluid pipeline upper end, heavy-fluid pipeline Lower end inside shell separator with connecting.

Preferably, the back side panel with radian is provided with separator drain.

Preferably, the one-level reduction kettle, second-stage reduction kettle, the case top of three-level reduction kettle are equipped with manhole, one-level Reduction kettle, second-stage reduction kettle, the housing sidewall of three-level reduction kettle are provided with thermometer mouthful, one-level reduction kettle, second-stage reduction kettle, three-level The housing bottom of reduction kettle is provided with reactor drain.

Preferably, the Nitroanisole measuring pump, NaHS measuring pump, liquid caustic soda measuring pump use plunger type metering pump Or diaphragm metering pump.

Preferably, connected at the top of the one-level reduction kettle by pipeline with second-stage reduction kettle top, at the top of second-stage reduction kettle By pipeline with being connected at the top of three-level reduction kettle.

Compared with prior art, its remarkable advantage is the utility model：1）Continuous production is realized, equipment volume is small, makes Valency is low, and installation area is small；2）Continuous production, easily realizes Automated condtrol, and production efficiency is high, labor strength It is small；3）Guide shell, the effect of guide shell are set in one-level reduction kettle, second-stage reduction kettle, three-level reduction kettle：Liquid can be improved Mixing efficiency, on the one hand improves the stirring extent to liquid, strengthens agitator and the direct mechanical shearing of liquid is acted on；Separately On the one hand all liq in device is made to reduce the chance that liquid walks short circuit by the strong mixed zone in guide shell.Water conservancy diversion Cylinder inwall can effectively prevent the circular motion of liquid in kettle provided with radial direction baffle plate；4）Set discharging Liquid level tank can between Connect the liquid level of control three-level reduction kettle, it is ensured that liquid level stabilizing in reduction kettle；5）Reduce liquid/gas separator close using linker and liquid The poor principle of degree, realizes aminoanisole and the continuous AUTOMATIC ZONING of waste water, and layered velocity is fast, and layered effect is good；6）Continuous metaplasia Production realizes that material component is stable in system, and technological parameter fluctuation is small, reacting balance, and equipment safety performance is improved, and accomplishes essential peace Entirely.

The utility model is described in further detail below in conjunction with the accompanying drawings.

Brief description of the drawings

Fig. 1 is the apparatus structure schematic diagram that utility model reduction with sodium bisulfide produces aminoanisole.

Fig. 2 is one-level reduction kettle structural representation.

Fig. 3 is reduction liquid/gas separator overlooking the structure diagram.

Fig. 4 is reduction liquid/gas separator side structure schematic view.

Embodiment

A kind of reduction with sodium bisulfide produces the device and method of aminoanisole, including the hydrogenation of Nitroanisole storage tank 1, sulphur Sodium storage tank 2, liquid caustic soda storage tank 3, one-level reduction kettle 4, second-stage reduction kettle 5, three-level reduction kettle 6, discharging Liquid level tank 7, reducing solution Cooler 8, reduction liquid/gas separator 9, aminoanisole storage tank 10, waste water tank 12, the one-level reduction kettle 4, second-stage reduction kettle 5th, the structure of three-level reduction kettle 6 is identical, and the one-level reduction kettle 4 includes housing 41, transmission device 42, guide shell 43, stirring vane 44th, agitating shaft 45, heat exchange coil 46, the transmission device 42 are fixed on the top of housing 41 by support, and guide shell 43 passes through branch Frame is suspended in housing 41, and the inwall of guide shell 43 is provided with radial direction baffle plate 47, and stirring vane 44 passes through agitating shaft 45 and transmission device 42 connections, stirring vane 44 is suspended in guide shell 43, and heat exchange coil 46 is provided between housing 41 and guide shell 43, housing 41 Side wall is provided with mixed liquor import 48, mixture export 49, is provided with out in the inner side for the housing 41 for going out the side of mixture export 49 Expect weir 50, the opened upper end on the weir 50 that discharges, the bottom on the weir 50 that discharges inside reactor with connecting, and the top of housing 41 is provided with nitre Base methyl phenyl ethers anisole charging aperture, NaHS charging aperture, liquid caustic soda charging aperture, wherein Nitroanisole charging aperture are fed with Nitroanisole Tube at one end is connected, and the Nitroanisole feed conduit other end is placed in guide shell 43, NaHS charging aperture and NaHS Feed conduit one end is connected, and the NaHS feed conduit other end is placed in guide shell 43, and liquid caustic soda charging aperture is led with liquid caustic soda charging Pipe one end is connected, and the liquid caustic soda feed conduit other end is placed in guide shell 43；The reduction liquid/gas separator 9 is provided with separator mixed liquor Import 91, light liquid outlet 92, heavy liquid exit 93；

Wherein Nitroanisole storage tank 1 is connected by pipeline with Nitroanisole measuring pump 11, Nitroanisole measuring pump 11 are connected by pipeline with the Nitroanisole charging aperture of one-level reduction kettle 4, and NaHS storage tank 2 passes through pipeline and NaHS Measuring pump 21 is connected, and NaHS measuring pump 21 passes through pipeline and one-level reduction kettle 4, second-stage reduction kettle 5, three-level reduction kettle 6 NaHS charging aperture is connected, and liquid caustic soda storage tank 3 is connected by pipeline with liquid caustic soda measuring pump 31, liquid caustic soda measuring pump 31 by pipeline and The liquid caustic soda charging aperture connection of one-level reduction kettle 4, the mixture export 49 of one-level reduction kettle 4 passes through pipeline and second-stage reduction kettle 5 Mixed liquor import is connected, and the mixture export of second-stage reduction kettle 5 is connected by pipeline with the mixed liquor import of three-level reduction kettle 6, The mixture export of three-level reduction kettle 6 is connected by pipeline with discharging Liquid level tank 7, and discharging Liquid level tank 7 passes through pipeline It is connected with reducing solution cooler 8, the separator mixed liquor import 91 that reducing solution cooler 8 passes through pipeline and reduction liquid/gas separator 9 Connection, the heavy liquid exit 93 of reduction liquid/gas separator 9 is connected by pipeline with aminoanisole storage tank 10, reduction liquid/gas separator 9 Light liquid outlet 92 is connected by pipeline with waste water tank 12.

The shell separator of liquid/gas separator 9 is reduced by front side board 94, left plate 95, right plate 96, the back side panel with radian 97th, base plate 98, top board 99 are constituted, and dividing plate 81 is provided with shell separator, and dividing plate 81 is fixed and connected with front side board 94, the sealing of base plate 98 Connect, dividing plate 81 leaves gap with the back side panel 97 with radian, and dividing plate 81 will be divided into feed zone and sub-material area inside shell separator, Feed zone is connected with sub-material area by gap, separator mixed liquor import 91 is provided with the front side board 94 of feed zone, in sub-material The front side board 94 in area is exported provided with light liquid outlet 92 and heavy liquid exit 93, and light night outlet 92 is higher than heavy liquid exit 93, and heavy-fluid goes out Mouth 93 is connected with the upper end of heavy-fluid pipeline 82, and the lower end of heavy-fluid pipeline 82 inside shell separator with connecting.

Back side panel 97 with radian is provided with separator drain 83.

One-level reduction kettle 4, second-stage reduction kettle 5, the case top of three-level reduction kettle 6 are equipped with manhole, one-level reduction kettle 4, Second-stage reduction kettle 5, the housing sidewall of three-level reduction kettle 6 are provided with thermometer mouthful, and one-level reduction kettle 4, second-stage reduction kettle 5, three-level are also The housing bottom of former kettle 6 is provided with reactor drain, is easy to repair and clear up reduction kettle.

The Nitroanisole measuring pump 11, NaHS measuring pump 21, liquid caustic soda measuring pump 31 use plunger type metering pump Or diaphragm metering pump.

The top of one-level reduction kettle 4 is connected by pipeline with the top of second-stage reduction kettle 5, and the top of second-stage reduction kettle 5 passes through The top of pipeline and three-level reduction kettle 6 connect, the pressure safety valve of each reduction kettle of cooperation can keep one-level reduction kettle 4, two grades The stable safety of reduction kettle 5, the internal pressure of three-level reduction kettle 5.

The aminoanisole production method of the device of reduction with sodium bisulfide production aminoanisole, comprises the following steps：

Added respectively by NaHS measuring pump 21 in step 1, one-level reduction kettle 4, second-stage reduction kettle 5, three-level reduction kettle 6 Enter the sodium hydrosulfide of the volume of reduction kettle 50%, uniform temperature is warming up in the case where stirring turns state；

Step 2, after design temperature is reached in one-level reduction kettle 4, second-stage reduction kettle 5, the housing of three-level reduction kettle 6 to one-level Reduction kettle 4 is continuously added to sodium hydrosulfide, liquid caustic soda, Nitroanisole, continue to keep one-level reduction kettle 4, second-stage reduction kettle 5, Temperature in the housing of three-level reduction kettle 6 reaches design temperature, while one-level reduction kettle 4 conveys mixed liquor, two to second-stage reduction kettle 5 Level reduction kettle 5 to three-level reduction kettle 6 convey mixed liquor, three-level reduction kettle 6 to discharging the continuous discharge of Liquid level tank 7；

Step 3, discharging Liquid level 7 reducing solution out of tank are cooled down by reducing solution cooler 8, then pass through reducing solution point From the isolated aminoanisole of device 9 and waste water, aminoanisole deposit aminoanisole storage tank 10, waste water flows into waste water tank 12。

Nitroanisole in step 2 can be ortho-nitroanisole or paranitroanisole or ortho-nitrophenyl The mixture of methyl ether and paranitroanisole arbitrary proportion.

NaHS is with Nitroanisole mol ratio in step 2：1.52~1.80, liquid caustic soda content 32%, liquid caustic soda（By hydrogen Sodium oxide molybdena meter）Mol ratio with Nitroanisole is：0.02~0.30：1.

One-level reduction kettle 4 in step 2, second-stage reduction kettle 5, the housing interior reaction temperature control of three-level reduction kettle 6 90~ 140℃。

Claims (6)

1. a kind of reduction with sodium bisulfide produces the device of aminoanisole, it is characterised in that including Nitroanisole storage tank（1）、 NaHS storage tank（2）, liquid caustic soda storage tank（3）, one-level reduction kettle（4）, second-stage reduction kettle（5）, three-level reduction kettle（6）, out-feed liquid Position control tank（7）, reducing solution cooler（8）, reduction liquid/gas separator（9）, aminoanisole storage tank（10）, waste water tank（12）, The one-level reduction kettle（4）, second-stage reduction kettle（5）, three-level reduction kettle（6）Structure is identical, the one-level reduction kettle（4）Including shell Body（41）, transmission device（42）, guide shell（43）, stirring vane（44）, agitating shaft（45）, heat exchange coil（46）, the transmission Device（42）Housing is fixed on by support（41）Top, guide shell（43）By holder suspension in housing（41）It is interior, guide shell （43）Inwall is provided with radial direction baffle plate（47）, stirring vane（44）Pass through agitating shaft（45）With transmission device（42）Connection, paddle Piece（44）It is suspended in guide shell（43）It is interior, housing（41）With guide shell（43）Between be provided with heat exchange coil（46）, housing（41）'s Side wall is provided with mixed liquor import（48）, mixture export（49）, going out mixture export（49）The housing of side（41）It is interior Side is provided with discharging weir（50）, discharge weir（50）Opened upper end, discharge weir（50）Bottom and reactor inside connect, the shell Body（41）Top is provided with Nitroanisole charging aperture, NaHS charging aperture, liquid caustic soda charging aperture, wherein Nitroanisole charging aperture It is connected with Nitroanisole feed conduit one end, the Nitroanisole feed conduit other end is placed in guide shell inner draft tube（43）, NaHS charging aperture is connected with NaHS feed conduit one end, and the NaHS feed conduit other end, which is placed in guide shell, leads Flow cartridge（43）, liquid caustic soda charging aperture is connected with liquid caustic soda feed conduit one end, and the liquid caustic soda feed conduit other end is placed in guide shell Inner guide Cylinder（43）；The reduction liquid/gas separator（9）Provided with separator mixed liquor import（91）, light liquid outlet（92）, heavy liquid exit（93）；

Wherein Nitroanisole storage tank（1）Pass through pipeline and Nitroanisole measuring pump（11）Connection, Nitroanisole measuring pump （11）Pass through pipeline and one-level reduction kettle（4）Nitroanisole charging aperture connection, NaHS storage tank（2）Pass through pipeline and sulphur Sodium hydride measuring pump（21）Connection, NaHS measuring pump（21）Pass through pipeline and one-level reduction kettle（4）, second-stage reduction kettle（5）、 Three-level reduction kettle（6）NaHS charging aperture connection, liquid caustic soda storage tank（3）Pass through pipeline and liquid caustic soda measuring pump（31）Connection, liquid Alkali measuring pump（31）Pass through pipeline and one-level reduction kettle（4）Liquid caustic soda charging aperture connection, one-level reduction kettle（4）Mixture export （49）Pass through pipeline and second-stage reduction kettle（5）Mixed liquor import connection, second-stage reduction kettle（5）Mixture export pass through pipeline With three-level reduction kettle（6）Mixed liquor import connection, three-level reduction kettle（6）Mixture export pass through pipeline with discharging liquid level control Tank processed（7）Connection, discharge Liquid level tank（7）Pass through pipeline and reducing solution cooler（8）Connection, reducing solution cooler（8）It is logical Piping and reduction liquid/gas separator（9）Separator mixed liquor import（91）Connection, reduces liquid/gas separator（9）Heavy liquid exit （93）Pass through pipeline and aminoanisole storage tank（10）Connection, reduces liquid/gas separator（9）Light liquid outlet（92）By pipeline with Waste water tank（12）Connection.

2. reduction with sodium bisulfide according to claim 1 produces the device of aminoanisole, it is characterised in that the reduction Liquid/gas separator（9）Shell separator by front side board（94）, left plate（95）, right plate（96）, the back side panel with radian（97）、 Base plate（98）, top board（99）Dividing plate is provided with composition, shell separator（81）, dividing plate（81）With front side board（94）, base plate（98） It is sealedly and fixedly connected, dividing plate（81）With the back side panel with radian（97）Leave gap, dividing plate（81）By part in shell separator Into feed zone and sub-material area, feed zone is connected with sub-material area by gap, in the front side board of feed zone（94）It is provided with separator Mixed liquor import（91）, the front side board in sub-material area（94）Provided with light liquid outlet（92）And heavy liquid exit（93）Outlet, light night Outlet（92）Higher than heavy liquid exit（93）, heavy liquid exit（93）With heavy-fluid pipeline（82）Upper end is connected, heavy-fluid pipeline（82）Lower end With being connected inside shell separator.

3. reduction with sodium bisulfide according to claim 2 produces the device of aminoanisole, it is characterised in that the band arc The back side panel of degree（97）It is provided with separator drain（83）.

4. reduction with sodium bisulfide according to claim 1 produces the device of aminoanisole, it is characterised in that the one-level Reduction kettle（4）, second-stage reduction kettle（5）, three-level reduction kettle（6）Case top be equipped with manhole, one-level reduction kettle（4）, two grades Reduction kettle（5）, three-level reduction kettle（6）Housing sidewall provided with thermometer mouthful, one-level reduction kettle（4）, second-stage reduction kettle（5）, three Level reduction kettle（6）Housing bottom be provided with reactor drain.

5. reduction with sodium bisulfide according to claim 1 produces the device of aminoanisole, it is characterised in that the nitro Methyl phenyl ethers anisole measuring pump（11）, NaHS measuring pump（21）, liquid caustic soda measuring pump（31）Using plunger type metering pump or diaphragm type meter Measure pump.

6. reduction with sodium bisulfide according to claim 1 produces the device of aminoanisole, it is characterised in that the one-level Reduction kettle（4）Top passes through pipeline and second-stage reduction kettle（5）Top is connected, second-stage reduction kettle（5）Top passes through pipeline and three-level Reduction kettle（6）Top is connected.