CN209143699U - A kind of oxidation reaction apparatus - Google Patents
A kind of oxidation reaction apparatus Download PDFInfo
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- CN209143699U CN209143699U CN201821203299.0U CN201821203299U CN209143699U CN 209143699 U CN209143699 U CN 209143699U CN 201821203299 U CN201821203299 U CN 201821203299U CN 209143699 U CN209143699 U CN 209143699U
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Abstract
A kind of oxidation reaction apparatus, including reactor 1, exhaust gas cooler 2, gas-liquid separator 3 and the supercharging equipment 4 being sequentially communicated；Wherein hydride entrance (11) are arranged in the reactor, oxygen-containing gas entrance (18) and oxidation solution outlet (19), offgas outlet (14) are arranged in the reactor head, the entrance of offgas outlet (14) connection exhaust gas cooler (2), the outlet gas-liquid separator (3) of the exhaust gas cooler, the gas-liquid separator is equipped with the gas-liquid separator offgas outlet (17) of condensate outlet (16) and top, the entrance of gas-liquid separator offgas outlet (17) connection supercharging equipment (4), the oxygen-containing gas entrance (18) of reactor described in the outlet of the supercharging equipment.Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, and process is simple, substantially reduces energy consumption, and not only safety and environmental protection but also saves organic solvent.
Description
Technical field
The utility model relates to a kind of oxidation reaction apparatus, are used for anthraquinone production peroxide more specifically to one kind
Change the oxidation reaction apparatus of hydrogen.
Background technique
Anthraquinone is the main stream approach of industrial hydrogen peroxide production, global industry hydrogen peroxide in terms of yield 99% or more
It is by anthraquinone production.Anthraquinone production process is: in the presence of a catalyst, under certain temperature and pressure, by alkyl anthracene
The anthraquinone in working solution that quinone and mixed organic solvents are made by a certain percentage is reacted with hydrogen, generates corresponding hydrogen anthraquinone, this
When working solution become hydride；Hydrogen anthraquinone in hydride is reacted with oxygen, generates anthraquinone and hydrogen peroxide, then hydride becomes oxygen
Change liquid；Aqueous hydrogen peroxide solution is obtained by extraction through pure water in oxidation solution, and raffinate is recycled back to hydrogenation process after processing.
Currently, oxidation reaction process mostly uses air as oxygen source.Organic solvent in working solution generally uses nonpolarity molten
Agent and polar solvent are made into, and wherein nonpolar solvent is mostly to have certain volatile high boiling aromatic hydrocarbons.So to reactor
In have a certain amount of high boiling aromatic hydrocarbons when blasting air and emit.On the one hand, it needs to recycle this part aromatic hydrocarbons, process
It is complicated, energy consumption is high, not environmentally.Operationally, it needs to utilize the aromatic hydrocarbons in temp-difference condensing recycling tail gas.Even tail gas is cooling
To 5 DEG C, heavy aromatics concentration of emission is still 2000mg/m3, greatly exceed the 120mg/m of national Specification3Requirement.Therefore,
In addition to cooling, further recycling and administration method, such as absorption process, turbine expansion method, absorption method are also taken oxidized tail gas.
It is the method for turbine expansion combination carbon fiber adsorption and catalytic combustion using more method at present.And activated carbon fibre will be periodically with steaming
Vapour regeneration, is hydrogen peroxide plant main stream exhaustion point.For 100,000 ton/year 27.5% of hydrogen peroxide plant, handle per hour
About 11000Nm3Tail gas.Annual tail gas causes aromatic hydrocarbons to lose about 10 tons, this also causes seriously to pollute to atmospheric environment.It is another
Aspect, there are explosion limits for aromatic hydrocarbons, the content and reaction temperature of strict control oxygen are needed when using air oxidation, otherwise easily
Explosion danger occurs.For example, the aerial explosion limit of trimethylbenzene is 0.9%~7%.Theoretically, when oxygen content down to certain
After one value, at any temperature, for any density of aromatic hydrocarbon, there is no explosion limits.This value is less than 21%.Therefore, mesh
Before use air as the oxidation technology of oxygen source, although Control for Oxygen Content in reactor tail gas is obtained relatively low, reacting
There are still security risks in device.So wanting limited reactions temperature to be no more than 55 DEG C toward contact.It reduce reaction efficiencies, cause oxygen
It is difficult to change reactor enlargement.The third aspect, oxidizing tower will discharge a part of water containing hydrogen peroxide from tower bottom per hour
Phase, referred to as oxidized residual liquid.Due to containing hydrogen peroxide, this partial oxidation raffinate is that long-term existence oxidation reactor bottom is endangered very much
Danger, needs timely discharge system, this causes the loss of device hydrogen peroxide again, reduces plant yield.This part water main source
It is the vapor that air is brought into.It is calculated with 4.5 ten thousand tons/year of devices, if 30 DEG C of ambient air temperature, brings the saturation of oxidizing tower into
All condensation can generate the condensed water of 722kg/h to vapor.Assuming that air compressor machine is isotherm compression, aoxidized after compression through air
Actual condensing capacity is 120.3 kg/h in tower.4th, it is rear into anti-that air need to be pressurized to 0.5MPa or so using air compressor machine
Device is answered to react.The loss of air compressor machine is the main energy consumption source of hydrogen peroxide plant.It can be seen that using air as anthraquinone life
Produce the oxygen source of hydrogen peroxide, energy consumption is high, not environmentally, there is also security risks, limit the development of China's hydrogen peroxide industry.
Utility model content
The technical problem to be solved by the present invention is to provide a kind of emission-free discharge, can without solvent recovery, oxygen content
Control, can reduce oxidized residual liquid amount process for prepairng hydrogen peroxide by anthraquinone oxidation reaction apparatus.Pass through the oxygen in control oxygen rich gas
Oxygen content in content and reactor in mixed gas, it is ensured that entire reaction system is run in safe range.
A kind of oxidation reaction apparatus, including reactor 1, exhaust gas cooler 2, gas-liquid separator 3 and the pressurization being sequentially communicated
Equipment 4；Wherein reactor setting hydride entrance 11, oxygen-containing gas entrance 18 and oxidation solution outlet 19, described is anti-
It answers and offgas outlet 14 is set at the top of device, the offgas outlet 14 is connected to the entrance of exhaust gas cooler 2, the exhaust gas cooler
Outlet gas-liquid separator 3, the gas-liquid separator tail gas that the gas-liquid separator is equipped with condensate outlet 16 and top goes out
Mouth 17, the gas-liquid separator offgas outlet 17 are connected to the entrance of supercharging equipment 4, the outlet institute of the supercharging equipment
The oxygen-containing gas entrance 18 for the reactor stated.
Oxidation reaction apparatus provided by the utility model is in use, the hydrogenated liquid entrance 11 of hydride, oxygenous
Body enters reactor 1 through oxygen-containing gas entrance 18, and oxidation reaction is carried out in reactor 1 and obtains the oxidation solution containing hydrogen peroxide
And tail gas.For oxidation solution through 19 discharge reactor of oxidation solution outlet, tail gas is laggard into the cooling of exhaust gas cooler 2 through offgas outlet 14
Enter gas-liquid separator 3, separate lime set and be discharged through condensate outlet 16, the tail gas separated enters through gas-liquid separator offgas outlet 17 to pass through
Supercharging equipment 4 is recycled back to reactor 1 after compressing.Wherein, oxygen-containing gas is the mixture of oxygen rich gas and nitrogen.
Oxidation reaction apparatus provided by the utility model has the beneficial effect that
For oxidation reaction apparatus provided by the utility model using oxygen containing mixed gas instead of air as oxygen source, tail gas can
It is recycled back to reactor, only need to fill into oxygen into reactor according to oxygen demand.1) this method has the advantage that without discharge, nothing
Solvent recovery operation is needed, the waste and environmental pollution of organic solvent is avoided, greatly reduces energy consumption；2) it can be mixed by adjusting
The concentration of oxygen improves the intrinsic safety of device to meet the requirement to oxygen content safety value in reactor in gas, can be with
Reaction temperature and reaction efficiency are properly increased, is conducive to device enlargement, can cancel and take heat in oxidation reactor, avoid recirculated water
The system of leaking into leads to the danger of decomposing hydrogen dioxide solution；3) oxygen containing mixed gas is unlike air is with very big humidity, it is possible to reduce
The discharge of oxidation reactor internal oxidition raffinate, safety and environmental protection improve the hydrogen peroxide yield of full device.4) it is pressurized using circulating air
Machine replaces air compressor machine, it is only necessary to provide system pressure drop, generally less than 0.2MPa, substantially reduce plant energy consumption.
Detailed description of the invention
Fig. 1 is the first embodiment schematic diagram of oxidation reaction apparatus provided by the utility model；
Fig. 2 is second of embodiment schematic diagram of oxidation reaction apparatus provided by the utility model；
Fig. 3 is the third embodiment schematic diagram of oxidation reaction apparatus provided by the utility model.
Wherein:
1- reactor；2- exhaust gas cooler；3- gas-liquid separator；4- supercharging equipment；11- hydride pipeline；12- is oxygen-enriched
Gas or pure oxygen pipeline；13- nitrogen pipeline；14,15,17,20- exhaust pipes；16- recycles lime set pipeline；18- is oxygen containing mixed
Close gas line；19- oxidation solution pipeline.
Specific embodiment
Specific embodiment of the present utility model described further below:
" top " for the container mentioned in specification is the position of the 0-10% of container from top to bottom, the container mentioned
" top " is the position of the 0-50% of container from top to bottom, and " lower part " of the container mentioned is the 50-100% of container from top to bottom
Position, " bottom " of the container mentioned is the position of the 90-100% of container from top to bottom.
A kind of oxidation reaction apparatus, including reactor 1, exhaust gas cooler 2, gas-liquid separator 3 and the pressurization being sequentially communicated
Equipment 4；Wherein reactor setting hydride entrance 11, oxygen-containing gas entrance 18 and oxidation solution outlet 19, described is anti-
It answers and offgas outlet 14 is set at the top of device, the offgas outlet 14 is connected to the entrance of exhaust gas cooler 2, the exhaust gas cooler
Outlet gas-liquid separator 3, the gas-liquid separator tail gas that the gas-liquid separator is equipped with condensate outlet 16 and top goes out
Mouth 17, the gas-liquid separator offgas outlet 17 are connected to the entrance of supercharging equipment 4, the outlet institute of the supercharging equipment
The oxygen-containing gas entrance 18 for the reactor stated.
Oxidation reaction apparatus provided by the utility model, it is preferable that the offgas outlet of the gas-liquid separator 3 is also through valve
It is connected to tail gas drain 20.
Oxidation reaction apparatus provided by the utility model, it is preferable that also set before the supercharging equipment or after supercharging equipment
It sets oxygen-containing gas and makes up line 12.
Oxidation reaction apparatus provided by the utility model in use, reactor 1 can be gas-liquid two-phase adverse current or
Gas-liquid two-phase cocurrent cooling operation.
In oxidation reaction apparatus provided by the utility model, the hydride entrance 11 is set to the reactor
Bottom, the oxidation solution outlet 19 are set to the top.Hydride can be entered by the bottom of reactor, oxygen containing mixed
It closes gas to be entered by the bottom of reactor, gas-liquid two-phase cocurrent cooling operation in reactor, the reacted device of the oxidation solution obtained after reaction
Top discharge.
In oxidation reaction apparatus provided by the utility model, the hydride entrance 11 is set to the reactor
Top, the oxidation solution outlet 19 are set to the bottom of the reactor.Hydride is entered by the top of reactor 1, is contained
The mixed gas of oxygen is entered by the bottom of reactor, gas-liquid two-phase counter-current operation in reactor, the oxidation solution obtained after reaction by
It flows out the bottom of reactor.
In oxidation reaction apparatus provided by the utility model, the supercharging device is the supercharging device of this field routine,
It can be compressor, supercharger etc., the utility model is not limited in this respect.
In oxidation reaction apparatus provided by the utility model, there is no any restriction to the reactor, can be this field
The reactor of any known form, such as stirred tank, packed tower, plate column.Filler, sieve plate, gas point can be installed in reactor
The gas-liquid distribution apparatus such as cloth device, liquid distribution trough.Gas-liquid contact mode can be fair current in reactor, be also possible to adverse current or wrong
Stream.Reactor can take the reaction heat of oxidation reaction generation away, with internal or external heat exchanger to avoid overtemperature in reactor.Instead
Answer device can within set or peripheral hardware gas-liquid separator, for oxidation solution and oxidized tail gas to be separated.
In reaction unit provided by the utility model, from the angle for preventing organic solvent from accumulating in tail gas, preferably
By partial tail gas interval discharge reactor.
Oxidation reaction apparatus provided by the utility model, it is preferable that the exhaust gas cooler 2 is located at the reactor
Inside as the heat transfer zone in reactor, the offgas outlet 14 of the reactor head and the gas-liquid separator 3 connect
It is logical.
Preferably, the heat transfer zone of the reactor is the 2-15%, more preferable 5-10% of the reactor.
The heat transfer zone of the inside reactor can be the form of tube side shell side, and wherein heat transferring medium walks shell side, reaction
Tail gas is discharged through offgas outlet upwards through tube side.It is preferred that heat transfer zone is the form of setting coil pipe or U-tube in reactor enclosure body,
Middle heat transferring medium walks tube side, and reaction end gas is discharged through offgas outlet upwards through shell side.
Preferably, the gas-liquid separator 3 also is located at the inside of the reactor.
Preferably, in the reactor, the height ratio of gas-liquid separation zone, heat transfer zone and the reactor is 0.08:
0.05:1.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, and hydride and oxygen-containing gas exist
Contact obtains the oxidation solution and tail gas containing hydrogen peroxide in reactor, the tail gas is returned after heat exchange cooling, pressurization anti-
Device is answered, before tail gas Returning reactor, is continuously mixed into oxygen rich gas thereto；Carrier of oxygen in the oxygen containing mixed gas
Product concentration is not more than 21%；Oxygen volumetric concentration is 40%-100% in the oxygen rich gas.
The rate that oxygen is consumed according to oxidation reaction, continuously fills into oxygen rich gas or pure into the tail gas before Returning reactor
Oxygen.It is consumed according to the dissolution of nitrogen, intermittently or serially fills into nitrogen into the tail gas before Returning reactor.Existed according to inert gas
The accumulation situation in mixed gas is recycled, through a small amount of interval emptying end gas of tail gas drain 20.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, oxygen in the oxygen rich gas
Volumetric concentration preferably 80%~100%, more preferable 90%~100%.The oxygen rich gas can be air-separating oxygen-making work
Oxygen product made from skill.For example, oxygen product concentration made from pressure swing absorption process is 90%~95.6%；By cryogenic air
It separates oxygen product volumetric concentration made from oxygen generation method and is more than or equal to 99.5%.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, the oxygen containing mixed gas
In in addition to containing also containing other gases, can be at least one of nitrogen, argon gas, helium and carbon dioxide outside oxygen rich gas
Gas, preferably nitrogen.It is consumed according to the dissolution of these gases, before tail gas Returning reactor, intermittently or serially to tail
Gas is filled into gas.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, and the tail gas can be first through cold
But device condensation enters back into supercharging equipment with after gas-liquid separator recovery section organic solvent.The organic solvent recycled and oxidation
Liquid enters subsequent handling together.Oxygen rich gas, intermittently or serially can continuously be filled into thereto before or after tail gas is pressurized
Fill into other gases.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, and the oxidation reaction condition does not have
It is particularly limited to, can be the conventional selection of this field.Generally, the oxidation reaction condition include: pressure be 0.1~
1.0MPa, preferably 0.2~0.5MPa；Temperature is 30~60 DEG C, preferably 40~55 DEG C.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, and the hydride is by working
Liquid in the presence of a catalyst, under certain temperature and pressure, react with hydrogen and the organic solution that generates.The working solution
Organic solvent is dissolved in for alkyl-anthraquinone to be formulated.Alkyl-anthraquinone preferably is selected from 2- alkyl -9,10- anthraquinone, and alkyl therein replaces
Base contains 1 to 5 carbon atoms, such as methyl, ethyl, sec-butyl, tert-butyl, tertiary pentyl and isopentyl and corresponding 5, and 6,7,
8 ,-four hydroperoxide derivatives, or it can also be selected from 9,10- dialkyl group anthraquinone, alkyl substituent therein can be identical or different, contains
1 to 5 carbon atoms, such as methyl, ethyl and tert-butyl, such as 1,3- dimethyl, Isosorbide-5-Nitrae-dimethyl, 2,7- dimethyl, 1,3- bis-
Ethyl, 2,7- bis- (tert-butyl), 2- ethyl -6- (tert-butyl) and corresponding 5,6,7,8,-four hydroperoxide derivatives.Organic solvent is excellent
What is selected is the mixture of non-polar compound and polar compound.Non-polar compound preferably is selected from the petroleum that boiling point is higher than 140 DEG C
Fraction, wherein the aromatic hydrocarbon of the mainly carbon atom containing at least nine, such as the isomers of trimethylbenzene, the isomers of durol, uncle
The isomers of butyl benzene, the isomers of methyl naphthalene and dimethylnaphthalene.Non-polar compound preferably is selected from saturated alcohols, preferably contains 7
To the saturated alcohols of 11 carbon atoms, such as diisobutyl carbinol (DIBC), 3,5,5- trimethyl hexanols, iso-heptanol；Carboxylate, such as methyl
Cyclohexyl, heptyl acetate, butyl benzoate and cognac oil；Phosphate, such as trioctyl phosphate, tricresyl phosphate -2- ethyl butyl ester, phosphorus
Sour three -2- ethylhexyls and tricresyl phosphate-n-octyl；Quaternary urea, such as four-normal-butyl ureas.Alkane in hydride, that is, working solution
Base anthraquinone hydrogenation generates obtained solution after corresponding alkyl hydrogen anthraquinone.
Oxidation reaction apparatus provided by the utility model be used for process for prepairng hydrogen peroxide by anthraquinone, the hydride can first with
PH adjusting agent mixing, is adjusted to subacidity for pH value, enters back into reactor, to avoid oxidation reaction hydrogen peroxide generated
It decomposes.The pH adjusting agent can be any known organic acid or inorganic acid solution, preferably phosphoric acid.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, in order to meet oxidation reaction institute
Reaction temperature is needed, the hydride can enter back into reactor after heat exchanger is heated or cooled.The heat exchanger can be this
The heat exchanger of any known form in field.
Oxidation reaction apparatus provided by the utility model is used for process for prepairng hydrogen peroxide by anthraquinone, to the subsequent of the oxidation solution
Processing step does not do any restrictions, can be conventional treatment known in the art, such as extracts oxidation solution with the pure water containing phosphoric acid
In hydrogen peroxide, obtain that there is certain density hydrogenperoxide steam generator.
Illustrate oxidation reaction apparatus provided by the utility model with reference to the accompanying drawings, but the utility model not therefore and by
To any restrictions.
Attached drawing 1 is the oxidation reaction apparatus schematic diagram of the utility model.As shown in Fig. 1, oxidation reaction apparatus, including according to
Reactor 1, exhaust gas cooler 2, gas-liquid separator 3 and the supercharging equipment 4 of secondary connection；Wherein hydride is arranged in the reactor
Entrance 11, oxygen-containing gas entrance 18 and oxidation solution outlet 19, offgas outlet 14, the tail gas is arranged in the reactor head
The entrance of 14 connection exhaust gas cooler 2 of outlet, the outlet gas-liquid separator 3 of the exhaust gas cooler, the gas-liquid
Separator is equipped with the gas-liquid separator offgas outlet 17 of condensate outlet 16 and top, and the gas-liquid separator offgas outlet 17 connects
Lead to the entrance of supercharging equipment 4, the oxygen-containing gas entrance 18 of reactor described in the outlet of the supercharging equipment.
The hydrogenated liquid entrance 11 of hydride, oxygen-containing gas enter reactor 1 through oxygen-containing gas entrance 18, in reactor 1
It carries out oxidation reaction and obtains oxidation solution and tail gas containing hydrogen peroxide.Oxidation solution is through 19 discharge reactor of oxidation solution outlet, tail
Gas enters gas-liquid separator 3 after offgas outlet 14 enters the cooling of exhaust gas cooler 2, separates lime set and is discharged through condensate outlet 16,
Tail gas after cooling enters through gas-liquid separator offgas outlet 17 is recycled back to reactor 1 after the compression of supercharging equipment 4.Wherein, contain
Carrier of oxygen is the mixture of oxygen rich gas and nitrogen.The rate of oxygen is consumed according to oxidation reaction, continuously to before Returning reactor
Tail gas in through oxygen pipeline 12 fill into oxygen rich gas or pure oxygen.Consumed according to the dissolution of nitrogen, through the interval of nitrogen pipeline 13 or
Continuously nitrogen is filled into the tail gas before Returning reactor.It, can according to accumulation situation of the inert gas in circulation mixed gas
Through a small amount of interval emptying end gas of tail gas drain 20.
Next the embodiments of the present invention are provided, but the utility model is not by its any restriction.In example, indicate to contain
The percentage for the amount of having, is such as weight percentage without special marking.
Embodiment 1
Reactor size is Φ 500mm × 24000mm, and built-in structured packing, reactor is two sections, is equipped between two sections cold
But device and knockout drum.Hydride 4.8m from hydrogenation process3/ h is cooled to 45 DEG C, and injects 85% phosphoric acid
After acid content is adjusted to 5mg/l by solution, into reactor.In reactor, hydride and 23.3Nm3/ h oxygen rich gas (oxygen
Volumetric concentration is 95%) to react to obtain the oxidation solution containing hydrogen peroxide.Oxidizing reaction temperature is 45 DEG C~55 DEG C, reaction
Device top pressure is 0.45MPa.The oxidation efficiency of gained oxidation solution is 7g/l.The oxidized tail gas of reactor head is cold through cooler
But to 40 DEG C, and after knockout drum withdrawal liquid, Returning reactor after compressor adherence pressure to 0.55MPa is entered back into.
The amount of nitrogen is 132Nm in recycled offgas3/ h, the volumetric concentration for controlling oxygen in mixed gas is 15%.After oxidation solution enters
Continuous extraction process carries out separation and obtains 27.5% hydrogenperoxide steam generator.
The hydride is that ethyl hydrazine, tetrahydro ethyl hydrazine, ethyl anthrahydroquinone, tetrahydro ethyl anthrahydroquinone, tricresyl phosphate are pungent
The mixture of ester and heavy aromatics.The concentration of general anthraquinone is 130~140g/l, and the volume ratio of heavy aromatics and trioctyl phosphate is 75:
25.Wherein, general anthraquinone refers to the summation of ethyl hydrazine, tetrahydro ethyl hydrazine, ethyl anthrahydroquinone and tetrahydro ethyl anthrahydroquinone, ethyl anthracene
Quinhydrones and tetrahydro ethyl anthrahydroquinone account for 45 weight % of general anthraquinone.
The oxidation solution be ethyl hydrazine, tetrahydro ethyl hydrazine, trioctyl phosphate and heavy aromatics mixture.General anthraquinone
Concentration is 130~140g/l, and the volume ratio of heavy aromatics and trioctyl phosphate is 75:25.Wherein, general anthraquinone refers to ethyl hydrazine, four
The summation of hydrogen ethyl hydrazine.
The oxidation efficiency is the amount containing hydrogen peroxide in unit bulk oxidation liquid.Measurement method are as follows: 5mL is taken to aoxidize
Liquid is in separatory funnel；It is extracted reaction solution 4~5 times with pure water, about 20mL water every time；20mL is added to gained extract liquor
1+4H2SO4Solution (H2SO4Volume ratio with water is 1:4)；The KMnO of concentration 0.1mol/L is used into extract liquor4Standard solution
It is titrated to blush, 30s colour-fast is terminal.Then oxidation efficiency (gH2O2/ L)=concentration of standard solution (0.1mol/L) × mark
Quasi- liquor capacity (mL) × 34.01/5.
Embodiment 2
Hydride 4.8m3/ h and 27.5Nm3(oxygen volumetric concentration is 80% to/h oxygen rich gas, and nitrogen volumetric concentration is
20%) it reacts.The amount of nitrogen is 82.8Nm in recycled offgas3/ h, the volumetric concentration for controlling oxygen in mixed gas is 21%.Instead
Answering device top pressure is 0.3MPa, and compressor adherence pressure to 0.4MPa, other reaction process and condition are the same as embodiment 1.Tail gas
Outer discharge capacity is 22Nm3/h.The oxidation efficiency of gained oxidation solution is 7g/l.Oxidation solution enters subsequent extraction process and carries out separation acquisition
27.5% hydrogenperoxide steam generator.
Embodiment 3
Hydride 4.8m3/ h and 44Nm3(oxygen volumetric concentration 50%, nitrogen volumetric concentration are 50%) anti-to/h oxygen rich gas
It answers.The amount of nitrogen is 125Nm in recycled offgas3/ h, the volumetric concentration for controlling oxygen in mixed gas is 15%.Reaction process and
Condition is the same as embodiment 1.The outer discharge capacity of tail gas is 22Nm3/h.The oxidation efficiency of gained oxidation solution is 7g/l.Oxidation solution enters subsequent extraction
It takes process to carry out separation and obtains 27.5% hydrogenperoxide steam generator.
Embodiment 4
Hydride 4.8m3/ h and 22Nm3/ h oxygen rich gas (oxygen volumetric concentration 99.9%) reaction.Nitrogen in recycled offgas
Amount be 253Nm3/ h, the volumetric concentration for controlling oxygen in mixed gas is 8%.Reactor head pressure is 0.8MPa, compression
Machine adherence pressure is to 0.9MPa, other reaction process and condition are the same as embodiment 1.The oxidation efficiency of gained oxidation solution is 7g/l.Oxygen
Change liquid and carries out separation 27.5% hydrogenperoxide steam generator of acquisition into subsequent extraction process.
Comparative example 1
Hydride 4.8m3/ h and 131Nm3/ h air reaction.Reaction process and condition are the same as embodiment 1.The oxygen of gained oxidation solution
Change efficiency is 7g/l.Oxidation solution enters subsequent extraction process and carries out separation 27.5% hydrogenperoxide steam generator of acquisition.Reactor head
Oxidized tail gas be cooled to 12 DEG C through two-stage cooler, then be cooled to -3 DEG C through turbo-expander, recycled in knockout drum
Part organic solvent heavy aromatics is finally vented after the processing of carbon fiber adsorption system.Exhaust emissions amount is 109Nm3/h.Heavy aromatics
Concentration of emission is 80mg/m3。
Although the utility model is described and illustrated by reference to specific embodiment, the technology of this field
Personnel will recognize that the utility model is suitable for different versions, they do not need to be explained herein.Therefore, it is
The true scope of determining the utility model, it should uniquely refer to the attached claims.
Claims (10)
1. a kind of oxidation reaction apparatus, which is characterized in that including reactor (1), the exhaust gas cooler (2), gas-liquid being sequentially communicated
Separator (3) and supercharging equipment (4)；Wherein reactor setting hydride entrance (11), oxygen-containing gas entrance (18) and
Oxidation solution exports (19), and offgas outlet (14) are arranged in the reactor head, and it is cold that the offgas outlet (14) is connected to tail gas
But the entrance of device (2), the outlet gas-liquid separator (3) of the exhaust gas cooler, the gas-liquid separator are equipped with solidifying
Liquid exports the gas-liquid separator offgas outlet (17) of (16) and top, and the gas-liquid separator offgas outlet (17) is connected to pressurization
The entrance of equipment (4), the oxygen-containing gas entrance (18) of reactor described in the outlet of the supercharging equipment.
2. oxidation reaction apparatus described in accordance with the claim 1, which is characterized in that the tail gas of the gas-liquid separator (3) goes out
Mouth is also connected to tail gas drain (20) through valve.
3. oxidation reaction apparatus according to claim 1 or 2, which is characterized in that before the supercharging equipment (4) or be pressurized
Oxygen-containing gas is also set up after equipment (4) makes up line (12).
4. oxidation reaction apparatus according to claim 1 or 2, which is characterized in that hydride entrance (11) setting
In the bottom of the reactor, the oxidation solution outlet (19) is set to the top.
5. oxidation reaction apparatus according to claim 1 or 2, which is characterized in that hydride entrance (11) setting
In the top of the reactor, the oxidation solution outlet (19) is set to the bottom of the reactor.
6. oxidation reaction apparatus according to claim 1 or 2, which is characterized in that the exhaust gas cooler (2) is located at institute
The inside for the reactor stated, as the heat transfer zone of the reactor head, the offgas outlet (14) of reactor head with it is described
Gas-liquid separator (3) connection.
7. oxidation reaction apparatus according to claim 6, which is characterized in that the heat transfer zone of the reactor is described
The 2-15% of reactor.
8. oxidation reaction apparatus according to claim 7, which is characterized in that the heat transfer zone of the reactor is described
The 5-10% of the height of reactor.
9. oxidation reaction apparatus according to claim 6, which is characterized in that the heat transfer zone of the inside reactor is anti-
The form of setting coil pipe or U-tube in device shell is answered, wherein heat transferring medium walks tube side, and reaction end gas goes out through tail gas upwards through shell side
Mouth discharge.
10. oxidation reaction apparatus according to claim 6, which is characterized in that the gas-liquid separator (3) also is located at institute
The inside for the reactor stated.
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| CN201821203299.0U CN209143699U (en) | 2018-07-27 | 2018-07-27 | A kind of oxidation reaction apparatus |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137864A (en) * | 2020-01-02 | 2020-05-12 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137864A (en) * | 2020-01-02 | 2020-05-12 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
| CN111137864B (en) * | 2020-01-02 | 2024-04-05 | 黎明化工研究设计院有限责任公司 | Oxidation tower for preparing hydrogen peroxide by anthraquinone process |
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