CN101239916A - Aniline post processing system and method - Google Patents
Aniline post processing system and method Download PDFInfo
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- CN101239916A CN101239916A CNA2008101025212A CN200810102521A CN101239916A CN 101239916 A CN101239916 A CN 101239916A CN A2008101025212 A CNA2008101025212 A CN A2008101025212A CN 200810102521 A CN200810102521 A CN 200810102521A CN 101239916 A CN101239916 A CN 101239916A
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- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 title claims abstract description 688
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000012805 post-processing Methods 0.000 title claims abstract description 12
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims abstract description 152
- 239000007788 liquid Substances 0.000 claims abstract description 116
- 239000001257 hydrogen Substances 0.000 claims abstract description 83
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 83
- 239000007789 gas Substances 0.000 claims abstract description 74
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000003054 catalyst Substances 0.000 claims abstract description 38
- 239000002351 wastewater Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 149
- 239000000428 dust Substances 0.000 claims description 59
- 238000011084 recovery Methods 0.000 claims description 39
- 230000018044 dehydration Effects 0.000 claims description 35
- 238000006297 dehydration reaction Methods 0.000 claims description 35
- 150000002431 hydrogen Chemical class 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 16
- 241000282326 Felis catus Species 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 230000006837 decompression Effects 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 10
- 230000007246 mechanism Effects 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 230000001174 ascending effect Effects 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 230000002265 prevention Effects 0.000 claims description 2
- 230000001131 transforming effect Effects 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 16
- 239000000843 powder Substances 0.000 abstract description 8
- 238000012545 processing Methods 0.000 abstract description 5
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract 2
- 238000005507 spraying Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 21
- 239000000047 product Substances 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 2
- -1 benzol amine Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 1
- 150000001448 anilines Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LQNUZADURLCDLV-IDEBNGHGSA-N nitrobenzene Chemical group [O-][N+](=O)[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 LQNUZADURLCDLV-IDEBNGHGSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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Abstract
Disclosed is a post-processing system and method of aniline, which relates to a device and method for processing catalyst powder after fluidized bed for hydrogenation preparing aniline from nitrobenzene, and reducing nitrobenzene content in aniline. In the invention, over-hot gas containing catalyst powder is directly fed into a device provided with an inclined barrier and a valve tray structure. Rising of catalyst powder is prevented by the inclined barrier, the valve tray structure and liquid spraying, the sparaying liquid at the bottome is discharged timely. The invention also proposes three methods for processing the gas induced from the device to respectively obtain eligible aniline (wherein nitrobenzene content is less than 0.5 mg/kg), eligible wastewater (wherein aniline content is less than 50 mg/kg) and eligible hydrogen (aniline is less than 0.1% and used for circulation). The device of the invention can effectively solve the default that, the catalyst powder is deposited in the cooled liquid thereby jamming a heat changer and increasing the process resistance), and realize long-period continuous operation.
Description
Technical field
The invention belongs to the chemical industry equipment field, the apparatus and method for of nitrobenzene function in the aniline is handled, reduced to particularly a kind of catalyst dust of realizing simultaneously.
Background technology
Aniline is the very important Chemicals of a class.Along with the widespread use of urethane in fields such as construction industry, automobile, electrical equipment and wrapping material, the output of the main raw material methyl vulcabond of urethane (be called for short MDI, got by the aniline preparation) improves rapidly, causes increasing considerably of aniline consumption.Aniline is mainly used in the production of MDI and rubber ingredients at present, also can be used for agricultural chemicals, pigment dyestuff and field of medicaments etc., and the annual requirement in the world is about about 4,000,000 tons.
The method of suitability for industrialized production aniline has three kinds, i.e. oil of mirbane liquid-phase hydrogenatin method, oil of mirbane gas phase hydrogenation method, phenol ammoniation process at present.The phenol ammoniation process depends on the source of phenol strongly, and oil of mirbane liquid-phase hydrogenatin method catalyst system therefor is platinum or palladium catalyst, and price is very expensive and because fine particles behind the liquid phase outflow reactor, reclaims difficulty.Directly influence the cost of whole Aniline Production.So most of producers all adopt oil of mirbane gas phase hydrogenation legal system to be equipped with aniline.Its primary process is that oil of mirbane and hydrogen are heated vaporization simultaneously, feeds fluidized-bed reactor, under the effect of metal load type catalyst (great majority are copper-based catalysts), generates aniline in the time of 240-320 ℃.After 190-240 ℃ reactant gases goes out fluidized-bed reactor, behind multi-stage heat exchanger condensation and aniline and water standing demix, obtain aniline crude product (room temperature).Carry out the fractionation of aniline and water then by extraneous heat supply, and the rectifying of aniline and oil of mirbane, highly purified aniline product obtained.
The intensity of the copper-based catalysts used of preparation aniline is not high, can form many particles less than 10 microns after the medium-term and long-term wearing and tearing of aniline fluidized-bed.This part particle has exceeded the trapping ability of cyclonic separator in the fluidized-bed, is taken in the interchanger by air-flow.When crude benzol amine was cooled off in multi-stage heat exchanger gradually, liquid material became sticky.Because the caliber of heat transfer tube is thin and the pipeline bending is many, catalyzer can deposit in interchanger gradually.The pipeline of interchanger is stopped up gradually, and the resistance of process increases gradually, makes that the mechanism of delivering gas and oil of mirbane etc. might heavy-duty service or overload, and power consumption rolls up.When serious, interchanger stops up substantially fully after 4-5 month, and the cleaning of must stopping influences ordinary production.Take not only time-consuming but also contaminate environment of cleaning interchanger apart.The way of this periodical operation, not environmental protection can seem uneconomical all the more, be unfavorable for process continuous operation and environment protection along with the maximization of aniline device.Simultaneously, the present method of cooling of technology is cooled aniline and oil of mirbane simultaneously and is present in the organic phase.If there is fluctuation in the fluidized-bed process of front, make then that the aniline of back is refining to be subjected to very big influence, be unfavorable for stable operation.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention proposes the overheated gas system that a kind of direct processing contains aniline, water, hydrogen, oil of mirbane and granules of catalyst, make to contain the fine grain hot gas flow of solid, and directly enter in the device of nitrobenzene in catalyst dust processing and the reduction aniline without interchanger.In this device, solid dust is watered by liquid and drenches back discharge at the bottom of tower.Utilize this technology can thoroughly solve aniline reaction device back interchanger, really realize continuous operation by the dust blocking problem.The disengaging zone is set simultaneously can reduces nitrobenzene in the gas that this device, increase the turndown ratio of follow-up system.
Technical scheme of the present invention is as follows:
1. an aniline post processing system (1) is characterized in that this system comprises:
(1). a catalyst dust is handled and the device (2) that reduces nitrobenzene in the aniline, and this device comprises:
(a) gas inlet (2a), this inlet (2a) links to each other with the barrel of device (2).
(b) circulating liquid outlet (2c) that is arranged on device (2) bottom.(2c) barrel with device (2) links to each other.
(c) the oblique baffle plate of multilayer district (3) that the prevention particle that is arranged on gas inlet (2a) top moves upward; The oblique baffle plate of multilayer district (3) links to each other with the barrel of device (2).
(d) float valve structural area (4) that is arranged on top, the oblique baffle plate of multilayer district (3).Float valve structural area (4) links to each other with the barrel of device (2).
(e) circulating liquid inlet (2d) that is arranged between the oblique baffle plate of multilayer district (3) and the float valve structural area (4).This inlet (2d) links to each other with the barrel of device (2).
(f) one is arranged on the gas of float valve structural area (4) top and the outlet (2e) of liquid mixture.This inlet (2e) links to each other with the barrel of device (2).
(g) phegma inlet (2f) that is arranged on float valve structural area (4) top.This inlet (2f) links to each other with the barrel of device (2).
(h) relief outlet that contains particulate liquid (2b) that is arranged on device (2) bottom, this outlet (2b) links to each other with device (2) barrel, and links to each other with subsider (5) by pipeline.
(2) subsiders (5) that are used to collect solid dust;
(3) one or more heat-exchanger rigs that link to each other with fluid pipeline (6,7);
(4) fixed beds (8) that are used for transforming fully oil of mirbane;
For the materials such as water, aniline and oil of mirbane in guaranteeing overheated gas noncondensing, make the catalyst dust caking or become mashed prod and be difficult for flowing, the gas temperature of the gas inlet (2a) of access to plant of the present invention (2) is 190-240 ℃, absolute pressure is 0.135-2MPa, gas composition is hydrogen (50%-75%), water (16%-32%), the material (0.05%-1%) of aniline (8%-16%) and oil of mirbane and other a small amount of nitrogenous elements.The concentration of solid particulate in gas is 40-10000mg/m
3
In order to guarantee the dust interception result in the oblique baffle plate of multilayer district (3), the present invention is pre-loaded into cold aniline liquid in device (2) bottom, and the overheated gas of access to plant (2) is fed in the cold aniline liquid earlier.The height of the aniline liquid of packing into is 0.5-2 a times of device (2) diameter.But upwards flow with the aniline liquid cooling of outer circulation simultaneously through the gas of multilayer oblique baffle plate district (3).In order to guarantee that liquid waters the effect of drenching dust, the height in the oblique baffle plate of the present invention's multilayer district (3) is set to 0.5-10 times of device (2) diameter.
For the gas (or gas-liquid mixture) of using device (2) does not contain dust, the present invention is provided with float valve structural area (4) in top, the oblique baffle plate of multilayer district (3), further stops dust.In order to guarantee that float valve stops the effect of dust, and make most oil of mirbane stay the bottom of this device (2), and do not enter subsequent separation system, this device with the height of float valve structural area be device (2) diameter 0.5-5 doubly.Simultaneously the inlet of circulation fluid (2d) is arranged on float valve structural area (4) below.
For preventing to be used for watering the nitrobenzene rising of the circulation aniline liquid that drenches catalyst dust, the present invention returns device (2) after subsider (5) clear liquid (nitrobenzene-containing and aniline) is transformed again in fixed bed (8).In order to guarantee that most of aniline can return device (2), the present invention is provided with certain gas-liquid separation space in fixed bed (8) top.In order to cut down the consumption of energy, the present invention emphasizes middle aniline of the interchanger (6,7) of outer circulation and saturation water heat exchange, produces 0.3-0.5MPa steam simultaneously, can be used for the tower bottoms body heating of Aniline Recovery Equipment in the postorder waste water.
In order to guarantee that most of oil of mirbane does not enter later separation workshop section, the present invention introduces the not liquid of nitrobenzene-containing by (2f), and simultaneously in order not increase the difficulty of later separation, this liquid is mixed solution or the purified petroleum benzin amine liquid or the pure water of aniline and water.The mixed solution of this aniline and water can be provided by aniline recovery workshop section or aniline dehydration workshop section in the follow-up waste water.In order to guarantee the separating effect of float valve structural area (4), simultaneously in order not roll up the later separation amount of liquid, the temperature of this liquid is 40-80 ℃.
Simultaneously, the present invention also provides a kind of processing catalyst dust and the method that purifies the aniline product that utilizes said system, and it is characterized in that: this method comprises the steps:
1) the oblique baffle plate of multilayer district (3), float valve structural area and each mouth of pipe (2a-2f) etc. that will install (2) link to each other one by one.Each mouth of pipe and interchanger (6,7), subsider (5) and the fixed bed equipment such as (8) that will install (2) link to each other with pipeline one by one, constitute complete aniline post processing system (2).
2) to installing the aniline (40 ℃) that (2) pour into certain liquid level.The overheated gas (190-240 ℃) that will contain aniline, water, oil of mirbane, hydrogen and catalysis thinner agent dust etc. then is by in inlet (2a) introducing device (2).Part is directly washed liquid by the dust of gas-entrained.The aniline fluid temperature raises gradually, when temperature is increased to 130-160 ℃, liquid is got through outlet (2c), enters interchanger (6,7).Temperature is reduced to 40-80 ℃ after the heat exchange, then from inlet (2d) return mechanism (2).This liquid flows downward naturally, contacts with the gas (hydrogen, water and aniline steam) that rises.Dust stopped by the float valve of the baffle plate in the oblique baffle plate of multilayer district (3) and float valve structural area (4), and watered pouring by liquid, in whereabouts return mechanism (2) the bottom liquid tagma.
3) introduce the not aniline of nitrobenzene-containing and the mixed solution of water by (2f), controlled temperature is at 40-80 ℃, with the gas (hydrogen that rises, water and aniline steam) contact and separate at float valve structural area (4), the ascending gas temperature becomes 100-120 ℃, wherein the content of oil of mirbane reduces 90%-99%, goes out device (2) by outlet (2e).
4) join by float valve structural area (4) nitrobenzene-containing liquid that flows downward and the circulation fluid of (2d) introducing, flow back into the bottom of device (2).Dust content is at 4-8g/l in the bottom liquid of control device (2).From the liquid extraction of tower bottom outlet (2b), enter (5) in the subsider the part dust-laden.
5) subsider (5) top clear liquid enters fixed bed (8) and hydrogen reaction.Oil of mirbane is converted into trace (0-10mg/kg), returns device (2), carry out the washing of dust by (2d).
6) fixed bed (8) top is entrained with minor amounts of aniline and water, and the gas of the hydrogen of trace oil of mirbane and device (2) outlet (2e) merges, and enters subsequent handling.
7) dust and heavier tar phase extraction bottom subsider (5) in due course are used for follow-up further recovery aniline.
Simultaneously, the gas that comes out at this system (1) and the different characteristics of gas composition of technology in the past, the invention allows for three kinds of gases that come out by system (1) and obtain qualified aniline (nitrobenzene is less than 0.5mg/kg), qualified waste water (aniline content is less than 50mg/kg) and the qualified hydrogen method (being different heat exchange and separation process) of (aniline is used for circulation less than 0.1%):
First method:
To be introduced into the interchanger refrigerating unit by the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) that outlet (2e) goes out device (2) and system (1), this gas cooling to 30-40 ℃, will be entered gas-liquid separator then, hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) feeds the aniline dehydration tower.Control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still, and then enter the aniline treating tower less than 500mg/kg, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.Control aniline recovery tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma.Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.The committed step of this flow process as shown in Figure 2.
Second method:
To go out aniline dehydration tower of gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) elder generation's feeding of device (2) and system (1) by outlet (2e), control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still less than 500mg/kg, and then enter the aniline treating tower, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.The a large amount of hydrogen G﹠Ws of cat head are cooled to 30-40 ℃ through interchanger, enter gas-liquid separator then, and hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) is introduced the aniline dehydration tower and is made phegma.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.Control aniline recovery tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma.Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.The committed step of this flow process as shown in Figure 3.
The third method:
To go out aniline dehydration tower of gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) elder generation's feeding of device (2) and system (1) by outlet (2e), control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still less than 500mg/kg, and then enter the aniline treating tower, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.The a large amount of hydrogen G﹠Ws of cat head directly enter the aniline recovery tower, and control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.Control aniline recovery tower top temperature is aniline working pressure under and the azeotropic temperature of water, aniline is passed through interchanger with the azeotrope of water and hydrogen be cooled to 30-40 ℃, enters gas-liquid separator then, and hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) is introduced the aniline dehydration tower and is made phegma.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower.The committed step of this flow process as shown in Figure 4.
The present invention compared with prior art has the following advantages and beneficial effect:
(1) catalyzer in the overheated gas of hydrogen, water, oil of mirbane, aniline and catalyst dust is watered pouring by liquid, and be continuously removed, heat-exchange equipment or separating device are stopped up, the time that can improve the device operate continuously greatly is (except that normal device overhaul is stopped work, but operate continuously is more than 5 years), help the high loading quiet run, prolong a year stream day, can improve the production cost of aniline output and reduction aniline.
(2) carry out the temperature control that device (2) bottom of nitrobenzene in the aniline was handled and reduced to catalyst dust among the present invention, and carry out lock out operation at this device, can make the most of oil of mirbane condensation in the gas, and shift out, and can in fixed bed, further oil of mirbane be converted into aniline from this bottom of device.Compared with prior art the content that oil of mirbane enters follow-up aniline refining plant can be reduced significantly, the aniline of MDI level can be guaranteed when catalyst activity is not high, still finally can access.Increase turndown ratio and the cycle that has prolonged catalyst regeneration, reduced running cost.
(3) hydrogen among the present invention does not contain dust through repeatedly contact washing with liquid, can omit the hydrogen trap (capture granules of catalyst) in original technology, reduces facility investment.
(4) interchanger among the present invention is a liquid liquid heat exchange structure, compare with the interchanger of the gas-liquid heat exchange mode of prior art, and the heat transfer coefficient height, heat interchanging area is few, can reduce facility investment and the consumption that reduces recirculated cooling water.
(5) Fig. 2 and flow process shown in Figure 3 can effectively be utilized aniline cooling in the overheated gas or the latent heat in aniline and the water cooling process respectively, the former external quantity of steam that is used for the device of aniline dewatering unit and waste water aniline recovery is reduced greatly, have energy-conservation characteristics.
Description of drawings
Fig. 1 aniline post processing system synoptic diagram.Among the figure: 1. total system; 2. catalyst dust is handled and the device that reduces nitrobenzene in the aniline; 3. install the oblique baffle plate of the multilayer district of (2); 4. install float valve structural area in (2); 5. subsider; 6,7 interchanger; 8. fixed bed; 2a, the import and export of a large amount of gases and small amount of liquid in the 2e device; 2b, 2c, 2d are rich in the import and export of aniline liquid.2f. the mixed solution intake of the aniline of nitrobenzene-containing and water not.
Fig. 2 catalyst dust is handled, oil of mirbane is removed, aniline dewaters, refining and recovery process synoptic diagram.
Fig. 3 catalyst dust is handled, oil of mirbane is removed, aniline dewaters, refining and recovery process synoptic diagram.
Fig. 4 catalyst dust is handled, oil of mirbane is removed, aniline dewaters, refining and recovery process synoptic diagram.
Embodiment
Further specify the present invention below in conjunction with embodiment.
The oblique baffle plate of barrel, multilayer district (3), float valve structural area (4) and each mouth of pipe (2a-2f) etc. that will install (2) link to each other one by one, constitute complete catalyst dust and handle and the device (2) that reduces nitrobenzene in the aniline.Wherein the height of the oblique baffle plate of multilayer district (3), float valve structural area (4) is respectively 1 times of device (2) diameter, 5 times.To install (2) bottom inlet (2a) links to each other with pipeline.Each mouth of pipe that will install (2) links to each other with pipeline one by one with interchanger (6,7) and subsider equipment such as (5), constitutes complete aniline post processing system (1).
To install the aniline (60 ℃) that at first pours into certain liquid level (assembly dia 0.5 times) at the bottom of (2) tower.With overheated gas (190 ℃, 0.2MPa (absolute pressure), the volume fraction of hydrogen, water and aniline is respectively 63%, 24%, 12%, other materials are 1%, catalyst powder dust concentration 120mg/m
3) by in inlet (2a) introducing device (2).When the aniline fluid temperature is increased to 140 ℃ gradually, liquid is introduced interchanger (6,7) (producing 0.32MPa steam in interchanger 6) through outlet (2c).Temperature is reduced to 60 ℃ by inlet (2d) backflow after the heat exchange.Dust is stopped by the float valve of the baffle plate in the oblique baffle plate of multilayer district (3) and float valve structural area (4), and is watered in pouring return mechanism (2) fluid zone by liquid.Dust content, enters (5) in the subsider from the liquid extraction of outlet (2b) with the part dust-laden at 5g/l in control device (2) liquid.Subsider (5) top clear liquid enters fixed bed, and (8, reaction conditions is: palladium catalyst, temperature are 80 ℃, and 2MPa) and hydrogen reaction, the nitrobenzene that transforms in the aniline liquid of back is 0.5mg/Kg.Return device (2) by inlet (2d), carry out the washing of dust.Dust and heavier tar phase extraction bottom subsider (5) in due course are used for follow-up further recovery aniline.
Introduce the not aniline of nitrobenzene-containing and the mixed solution of water by (2f), controlled temperature is at 40 ℃, with the gas (hydrogen that rises, water and aniline steam) contact and separate at float valve structural area (4), the ascending gas temperature becomes 100 ℃, wherein nitrobenzene reduces by 99%, goes out device (2) by outlet (2e).
To be introduced into interchanger refrigerating unit (Fig. 2 flow process) by the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) that outlet (2e) goes out device (2), this gas cooling to 30-40 ℃, will be entered gas-liquid separator then, hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) feeds the aniline dehydration tower.Control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still, and then enter the aniline treating tower less than 500mg/kg, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.Control aniline recovery tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma.Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.
Utilize this device and this method, except that normal device overhaul is stopped work, but this device operate continuously more than 5 years is saved 0.2 ton/ton of steam more than the aniline than prior art, is that the production cost of the aniline of computation of Period descends 50 yuan/ton more than the aniline with the year.
The oblique baffle plate of barrel, multilayer district (3), float valve structural area (4) and each mouth of pipe (2a-2f) etc. that will install (2) link to each other one by one, constitute complete catalyst dust and handle and the device (2) that reduces nitrobenzene in the aniline.Wherein the height of the oblique baffle plate of multilayer district (3), float valve structural area (4) is respectively 0.5 times of device (2) diameter, 5 times.To install (2) bottom inlet (2a) links to each other with pipeline.Each mouth of pipe that will install (2) links to each other with pipeline one by one with interchanger (6,7) and subsider equipment such as (5), constitutes complete aniline post processing system (1).
To install the aniline (40 ℃) that (2) bottom at first pours into certain liquid level (assembly dia 1 times).With overheated gas (200 ℃, 0.135MPa (absolute pressure), the volume fraction of hydrogen, water and aniline is respectively 72%, 18%, 9%, other materials are 1%, catalyst powder dust concentration 1200mg/m
3) by in inlet (2a) introducing device (2).When the aniline fluid temperature is increased to 130 ℃ gradually, liquid is introduced interchanger (6,7) (producing 0.3MPa steam in interchanger) through outlet (2c).Temperature is reduced to 40 ℃ by inlet (2d) backflow after the heat exchange.Dust is stopped by the float valve of the baffle plate in the oblique baffle plate of multilayer district (3) and float valve structural area (4), and is watered in pouring return mechanism (2) the bottom liquid tagma by liquid.Dust content, enters (5) in the subsider from the liquid extraction of outlet (2b) with the part dust-laden at 8g/l in control device (2) bottom liquid.Subsider (5) top clear liquid enters fixed bed, and (8, reaction conditions is: nickel catalyzator, temperature are 110 ℃, and 0.15MPa) and hydrogen reaction, the nitrobenzene that transforms in the aniline liquid of back is 5mg/Kg.Return device (2) by inlet (2d), carry out the washing of dust.Dust and heavier tar phase extraction bottom subsider (6) in due course are used for follow-up further recovery aniline.
Introduce the not aniline of nitrobenzene-containing and the mixed solution of water by (2f), controlled temperature is at 80 ℃, contacts and separates at float valve structural area (4) with the gas (hydrogen, water and aniline steam) that rises, and the ascending gas temperature becomes 114 ℃.Wherein nitrobenzene reduces by 95%, goes out device (2) by outlet (2e).
To go out gas (a large amount of hydrogen, water, an aniline and trace oil of mirbane) elder generation feeding aniline dehydration tower (Fig. 3 flow process) of device (2) by outlet (2e), control dehydration Tata still temperature and trim the top of column carry out separating of water and aniline, obtain the aniline product of water-content at the tower still less than 500mg/kg, and then enter the aniline treating tower, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.The a large amount of hydrogen G﹠Ws of cat head are cooled to 30-40 ℃ through interchanger, enter gas-liquid separator then, and hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) is introduced the aniline dehydration tower and is made phegma.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.Control aniline recovery tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma.Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.
Utilize this device and this method, except that normal device overhaul is stopped work, but this device operate continuously more than 5 years is saved 0.4 ton/ton of steam more than the aniline than prior art, is that the production cost of the aniline of computation of Period descends 70 yuan/ton more than the aniline with the year.
The oblique baffle plate of barrel, multilayer district (3), float valve structural area (4) and each mouth of pipe (2a-2f) etc. that will install (2) link to each other one by one, constitute complete catalyst dust and handle and the device (2) that reduces nitrobenzene in the aniline.Wherein the height of the oblique baffle plate of multilayer district (3), float valve structural area (4) is respectively 10 times of device (2) diameter, 5 times.To install (2) bottom inlet (2a) links to each other with pipeline.Each mouth of pipe that will install (2) links to each other with pipeline one by one with interchanger (6,7) and subsider equipment such as (5), constitutes complete aniline post processing system (1).
To install the aniline (40 ℃) that (2) bottom at first pours into certain liquid level (assembly dia 1.5 times).With overheated gas (240 ℃, 2MPa (absolute pressure), the volume fraction of hydrogen, water and aniline is respectively 51%, 32%, 16%, other materials are 1%, catalyst powder dust concentration 10000mg/m
3) by in inlet (2a) introducing device (2).When the aniline fluid temperature is increased to 160 ℃ gradually, liquid is introduced interchanger (6,7) (producing 0.5MPa steam in interchanger 6) through outlet (2c).Temperature is reduced to 80 ℃ by inlet (2d) backflow after the heat exchange.Dust is stopped by the float valve of the baffle plate in the oblique baffle plate of multilayer district (3) and float valve structural area (4), and is watered in pouring return mechanism (2) the bottom liquid tagma by liquid.Dust content, enters (5) in the subsider from the liquid extraction of tower bottom outlet (2b) with the part dust-laden at 4g/l in control device (2) bottom liquid.Subsider (5) top clear liquid enters fixed bed, and (8, reaction conditions is: copper catalyst, temperature are 150 ℃, and 0.3MPa) and hydrogen reaction, the nitrobenzene that transforms in the aniline liquid of back is 5mg/Kg.Return device (2) by inlet (2d), carry out the washing of dust.Dust and heavier tar phase extraction bottom subsider (5) in due course are used for follow-up further recovery aniline.
Introduce the not aniline of nitrobenzene-containing and the mixed solution of water by (2f), controlled temperature is at 80 ℃, with the gas (hydrogen that rises, water and aniline steam) contact and separate at float valve structural area (4), the ascending gas temperature becomes 120 ℃, wherein nitrobenzene reduces by 90%, goes out device (2) by outlet (2e).
To go out gas (a large amount of hydrogen, water, an aniline and trace oil of mirbane) elder generation feeding aniline dehydration tower (Fig. 4 flow process) of device (2) by outlet (2e), control dehydration Tata still temperature and trim the top of column carry out separating of water and aniline, obtain the aniline product of water-content at the tower still less than 500mg/kg, and then enter the aniline treating tower, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.A large amount of hydrogen G﹠Ws with the aniline dehydration column overhead directly feed the aniline recovery tower, and control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.The control tower top temperature is aniline working pressure under and the azeotropic temperature of water, aniline is passed through interchanger with the azeotrope of water and hydrogen be cooled to 30-40 ℃, enters gas-liquid separator then, and hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) is introduced the aniline dehydration tower and is made phegma.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower.
Utilize this device and this method, except that normal device overhaul is stopped work, but this device operate continuously more than 5 years is saved 0.55 ton/ton of steam more than the aniline than prior art, is that the production cost of the aniline of computation of Period descends 100 yuan/ton more than the aniline with the year.
Embodiment 4
The oblique baffle plate of barrel, multilayer district (3), float valve structural area (4) and each mouth of pipe (2a-2f) etc. that will install (2) link to each other one by one, constitute complete catalyst dust and handle and the device (2) that reduces nitrobenzene in the aniline.Wherein the height of the oblique baffle plate of multilayer district (3), float valve structural area (4) is respectively 0.5 times of device (2) diameter, 0.5 times.To install (2) bottom inlet (2a) links to each other with pipeline.Each mouth of pipe that will install (2) links to each other with pipeline one by one with interchanger (6,7) and subsider equipment such as (5), constitutes complete aniline post processing system (1).
To install the aniline (40 ℃) that (2) bottom at first pours into certain liquid level (assembly dia 2 times).With overheated gas (220 ℃, 0.15MPa (absolute pressure), the volume fraction of hydrogen, water and aniline is respectively 57.5%, 28%, 14%, other materials are 0.5%, catalyst powder dust concentration 40mg/m
3) by in inlet (2a) introducing device (2).When the aniline fluid temperature is increased to 145 ℃ gradually, liquid is introduced interchanger (6,7) (producing 0.35MPa steam in interchanger 6) through outlet (2c).Temperature is reduced to 80 ℃ by inlet (2d) backflow after the heat exchange.Dust is stopped by the float valve of the baffle plate in the oblique baffle plate of multilayer district (3) and float valve structural area (4), and is watered in pouring return mechanism (2) the bottom liquid tagma by liquid.Dust content, enters (5) in the subsider from the liquid extraction of outlet (2b) with the part dust-laden at 4g/l in control device (2) bottom liquid.Subsider (5) top clear liquid enters fixed bed, and (8, reaction conditions is: platinum catalyst, temperature are 80 ℃, and 1MPa) and hydrogen reaction, the nitrobenzene that transforms in the aniline liquid of back is 0mg/Kg.Return device (2) by inlet (2d), carry out the washing of dust.Dust and heavier tar phase extraction bottom subsider (5) in due course are used for follow-up further recovery aniline.
Introduce the not aniline of nitrobenzene-containing and the mixed solution of water by (2f), controlled temperature is at 60 ℃, with the gas (hydrogen that rises, water and aniline steam) contact and separate at float valve structural area (4), the ascending gas temperature becomes 105 ℃, wherein nitrobenzene reduces by 98%, goes out device (2) by outlet (2e).
To be introduced into interchanger refrigerating unit (Fig. 2 flow process) by the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) that outlet (2e) goes out device (2), this gas cooling to 30-40 ℃, will be entered gas-liquid separator then, hydrogen and liquid are separated.After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer.The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively.Independently aniline phase (containing less water and trace oil of mirbane) feeds the aniline dehydration tower.Control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still, and then enter the aniline treating tower less than 500mg/kg, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head.With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes.Control aniline recovery tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma.Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.
Utilize this device and this method, except that normal device overhaul is stopped work, but this device operate continuously more than 5 years is saved 0.2 ton/ton of steam more than the aniline than prior art, is that the production cost of the aniline of computation of Period descends 50 yuan/ton more than the aniline with the year.
Claims (10)
1. an aniline post processing system is characterized in that, this system comprises:
(1). a catalyst dust is handled and the device (2) that reduces nitrobenzene in the aniline, and this device comprises:
(a) gas inlet (2a), this inlet (2a) links to each other with the barrel of device (2);
(b) circulating liquid outlet (2c) that is arranged on device (2) bottom; (2c) barrel with device (2) links to each other;
(c) the oblique baffle plate of multilayer district (3) that the prevention particle that is arranged on gas inlet (2a) top moves upward; The oblique baffle plate of multilayer district (3) links to each other with the barrel of device (2);
(d) float valve structural area (4) that is arranged on top, the oblique baffle plate of multilayer district (3); Float valve structural area (4) links to each other with the barrel of device (2);
(e) circulating liquid inlet (2d) that is arranged between the oblique baffle plate of multilayer district (3) and the float valve structural area (4); This inlet (2d) links to each other with the barrel of device (2);
(f) one is arranged on the gas of float valve structural area (4) top and the outlet (2e) of liquid mixture; This inlet (2e) links to each other with the barrel of device (2);
(g) phegma inlet (2f) that is arranged on float valve structural area (4) top; This inlet (2f) links to each other with the barrel of device (2);
(h) relief outlet that contains particulate liquid (2b) that is arranged on device (2) bottom, this outlet (2b) links to each other with device (2) barrel, and links to each other with subsider (5) by pipeline;
(2) subsiders (5) that are used to collect solid dust;
(3) one or more heat-exchanger rigs that link to each other with fluid pipeline (6,7);
(4) fixed beds (8) that are used for transforming fully oil of mirbane.
2. system according to claim 1 is characterized in that, the height in the oblique baffle plate of multilayer district (3) be device (2) diameter 0.5-5 doubly.
3. system according to claim 1 is characterized in that, the height of float valve structural area (4) be device (2) diameter 0.5-5 doubly.
4. system according to claim 1, it is characterized in that, the gas temperature that enters gas inlet (2a) is 190-240 ℃, absolute pressure is 0.135-0.3MPa, gas composition is hydrogen (50%-75%), water (16%-32%), aniline (8%-16%), oil of mirbane and other impurity (0.05%-1% altogether); The concentration of solid particulate in gas is 40-10000mg/m
3
5. system according to claim 1 is characterized in that, the overheated gas of access to plant (2) bottom is cooled off by the aniline liquid of outer circulation; The aniline height that is pre-loaded into device (2) bottom is 0.5-2 a times of device (2) diameter; Aniline and saturation water heat exchange in the interchanger of outer circulation produce 0.3-0.5MPa steam, can be used for the tower bottoms body heating of aniline recovery tower in the follow-up waste water.
6. system according to claim 1 is characterized in that bigger gas-liquid separation space is arranged at the top of fixed bed (8), and catalyzer is that metal load type catalyst (copper, nickel, palladium or platinum etc.) service temperature is 80-150 ℃, and working pressure is 0.15-2MPa.
7. a method of utilizing system according to claim 1 to carry out the aniline aftertreatment is characterized in that this method comprises the steps:
1) the oblique baffle plate of barrel, multilayer district (3), float valve structural area and each mouth of pipe (2a-2f) etc. that will install (2) link to each other one by one; Each mouth of pipe and interchanger (6,7), subsider (5) and the fixed bed equipment such as (8) that will install (2) link to each other with pipeline one by one, constitute complete aniline post processing system (1);
2) to installing the aniline (40 ℃) that (2) pour into certain liquid level; The overheated gas (190-240 ℃) that will contain aniline, water, oil of mirbane, hydrogen and catalysis thinner agent dust etc. then is by in inlet (2a) introducing device (2); Part is directly washed liquid by the dust of gas-entrained; The aniline fluid temperature raises gradually, when temperature is increased to 130-160 ℃, liquid is got through outlet (2c), enters interchanger (6,7); Temperature is reduced to 40-80 ℃ after the heat exchange, then from inlet (2d) return mechanism (2); This liquid flows downward naturally, contacts with the gas (hydrogen, water and aniline steam) that rises; Dust stopped by the float valve of the baffle plate in the oblique baffle plate of multilayer district (3) and float valve structural area (4), and watered pouring by liquid, in whereabouts return mechanism (2) the bottom liquid tagma;
3) introduce the not aniline of nitrobenzene-containing and the mixed solution of water by (2f), controlled temperature is at 40-80 ℃, with the gas (hydrogen that rises, water and aniline steam) contact and separate at float valve structural area (4), the ascending gas temperature becomes 100-120 ℃, wherein the content of oil of mirbane reduces 90%-99%, goes out device (2) by outlet (2e);
4) join by float valve structural area (4) nitrobenzene-containing liquid that flows downward and the circulation fluid of (2d) introducing, flow back into the bottom of device (2); Dust content is at 4-8g/l in the bottom liquid of control device (2); From the liquid extraction of tower bottom outlet (2b), enter (5) in the subsider the part dust-laden;
5) subsider (5) top clear liquid enters fixed bed (8) and hydrogen reaction; Oil of mirbane is converted into trace (0-10mg/kg), returns device (2), carry out the washing of dust by (2d);
6) fixed bed (8) top is entrained with minor amounts of aniline and water, and the gas of the hydrogen of trace oil of mirbane and device (2) outlet (2e) merges, and enters subsequent handling;
7) dust and heavier tar phase extraction bottom subsider (5) in due course are used for follow-up further recovery aniline.
8. one kind is continued to handle the method that is gone out the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) of device (2) and system by outlet (2e), it is characterized in that this method comprises:
To be introduced into the interchanger refrigerating unit by the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) that outlet (2e) goes out device (2) and system (1), this gas cooling to 30-40 ℃, will be entered gas-liquid separator then, hydrogen and liquid are separated; After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer; The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively; Independently aniline phase (containing less water and trace oil of mirbane) feeds the aniline dehydration tower; Control dehydration Tata still and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still, and then enter the aniline treating tower less than 500mg/kg, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head; With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes; The control tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma; Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.
9. one kind is continued to handle the method that is gone out the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) of device (2) and system by outlet (2e), it is characterized in that this method comprises:
To go out aniline dehydration tower of gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) elder generation's feeding of device (2) and system (1) by outlet (2e), control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still less than 500mg/kg, and then enter the aniline treating tower, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head; The a large amount of hydrogen G﹠Ws of cat head are cooled to 30-40 ℃ through interchanger, enter gas-liquid separator then, and hydrogen and liquid are separated; After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer; The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively; Independently aniline phase (containing less water and trace oil of mirbane) is introduced the aniline dehydration tower and is made phegma; With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower, control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes; The control tower top temperature is the aniline under the working pressure and the azeotropic temperature of water, and layering after overcooling is returned the aniline recovery tower with the water in the quantizer and made phegma; Aniline in the quantizer is squeezed into aniline dehydration tower top mutually do phegma.
10. one kind is continued to handle the method that is gone out the gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) of device (2) and system (1) by outlet (2e), it is characterized in that this method comprises:
To go out aniline dehydration tower of gas (a large amount of hydrogen, water, aniline and trace oil of mirbane) elder generation's feeding of device (2) and system (1) by outlet (2e), control dehydration Tata still temperature and trim the top of column, carry out separating of water and aniline, obtain the aniline product of water-content at the tower still less than 500mg/kg, and then enter the aniline treating tower, under the situation of decompression, obtain the aniline product of nitrobenzene less than 0.5mg/kg at cat head; The a large amount of hydrogen G﹠Ws of cat head directly enter the aniline recovery tower, and control tower still temperature and trim the top of column obtain the water of aniline content less than 50mg/kg at the tower still, introduce the wastewater trough discharging, or are used for other purposes; The control tower top temperature is aniline working pressure under and the azeotropic temperature of water, aniline is passed through interchanger with the azeotrope of water and hydrogen be cooled to 30-40 ℃, enters gas-liquid separator then, and hydrogen and liquid are separated; After hydrogen goes out gas-liquid separator, contain the water and the aniline of denier,, return the recycle hydrogen system of aniline fluidized-bed through behind the strainer; The mixture of aniline and water enters (containing trace oil of mirbane) quantizer of aniline and water, obtains independently aniline phase and water respectively; Independently aniline phase (containing less water and trace oil of mirbane) is introduced the aniline dehydration tower and is made phegma; With in the quantizer independently water (containing minor amounts of aniline) feed the aniline recovery tower.
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| CNA2008101025212A CN101239916A (en) | 2008-03-24 | 2008-03-24 | Aniline post processing system and method |
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| CN102381984A (en) * | 2011-09-06 | 2012-03-21 | 江苏沿江化工资源开发研究院有限公司 | Method for hydrogen-water-aniline-tar separation with heat integration of continuous side discharging tower, rectification tower and recovery tower |
| CN104926663A (en) * | 2015-05-28 | 2015-09-23 | 国药集团化学试剂有限公司 | Preparation method for high-purity aniline containing trace nitrocompound |
| CN105418437A (en) * | 2014-09-09 | 2016-03-23 | 中国石油化工股份有限公司 | Aniline apparatus energy saving method |
| CN106595334A (en) * | 2016-12-08 | 2017-04-26 | 中山大学 | Water-saving fog-dissipation closed cooling tower with float valve structure |
| CN110092723A (en) * | 2018-01-31 | 2019-08-06 | 瑞典国际化工技术有限公司 | The method of aniline is continuously manufactured by by the catalytic hydrogenation of p-nitrophenyl |
| CN113019270A (en) * | 2021-03-25 | 2021-06-25 | 高洪东 | Liquid-phase nitrobenzene hydrogenation catalyst circulation process and device thereof |
| CN114057584A (en) * | 2020-08-06 | 2022-02-18 | 中石化南京化工研究院有限公司 | Method for reducing tar in aniline system |
| CN114149330A (en) * | 2021-12-06 | 2022-03-08 | 万华化学集团股份有限公司 | Energy-saving process for preparing aniline by nitrobenzene liquid-phase hydrogenation |
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2008
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| CN114057584A (en) * | 2020-08-06 | 2022-02-18 | 中石化南京化工研究院有限公司 | Method for reducing tar in aniline system |
| CN113019270A (en) * | 2021-03-25 | 2021-06-25 | 高洪东 | Liquid-phase nitrobenzene hydrogenation catalyst circulation process and device thereof |
| CN113019270B (en) * | 2021-03-25 | 2022-10-28 | 高洪东 | Liquid-phase nitrobenzene hydrogenation catalyst circulation process and device thereof |
| CN114149330A (en) * | 2021-12-06 | 2022-03-08 | 万华化学集团股份有限公司 | Energy-saving process for preparing aniline by nitrobenzene liquid-phase hydrogenation |
| CN114149330B (en) * | 2021-12-06 | 2023-10-17 | 万华化学集团股份有限公司 | Energy-saving process for preparing aniline by nitrobenzene liquid phase hydrogenation |
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