CN104098473A - Post-treatment method of aniline - Google Patents
Post-treatment method of aniline Download PDFInfo
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- CN104098473A CN104098473A CN201310118257.2A CN201310118257A CN104098473A CN 104098473 A CN104098473 A CN 104098473A CN 201310118257 A CN201310118257 A CN 201310118257A CN 104098473 A CN104098473 A CN 104098473A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to a post-treatment method of aniline in a fluidized bed gas phase hydrogenation for aniline production. The method is as below: the high temperature materials from a fluidized bed outlet is introduced into a scrubber from the middle lower part of the scrubber; the upper part of the scrubber is sprayed with the material, and the liquid material after spray is composed of aniline and a small amount of water; part of the liquid material is recovered and sent into a refining system, and the other part of the liquid material conducts heat exchange with bubbled soft water through a heat exchanger, wherein the heat is utilized for transferring a certain temperature to the upper part of the scrubber as spray material; the gas phase at the scrubber top comprises hydrogen, water vapor and part of aniline steam, and this part of the material conducts heat exchange with fresh hydrogen and is subjected to gas-liquid separation and aniline and water separation by a condenser; and the crude aniline as a spraying material enters into the upper part of the scrubber amine. The post-treatment method of aniline provided by the invention can effectively remove the catalyst particles in reduction material, improve system security and stability, and make full use of vaporization latent heat of aniline and water to achieve the purpose of saving energy.
Description
Technical field
The present invention relates to a kind of Chemicals production method, what be specifically related to is the post-treating method of product in oil of mirbane fluidized-bed gas phase hydrogenation aniline process processed.
Background technology
Aniline is a kind of important Organic chemical products, and Aniline Production great majority adopt By Catalytic Hydrogenation of Nitrobenzene method in the world at present, only has indivedual companies to adopt phenol ammonolysis process and iron powder reducing method.By Catalytic Hydrogenation of Nitrobenzene legal system aniline has gas phase hydrogenation method and By Liquid-phase Hydrogenation Process.Gas phase hydrogenation method is again because the reactor types difference adopting is divided into Fixed Bed Gas Phase shortening and two kinds of techniques of fluidized-bed gas phase hydrogenation.Domestic enterprise adopts fluidized-bed gas phase hydrogenation technique mostly, fluidized bed gas-phase catalytic hydrogenation is at 260 ℃～280 ℃, under 0.05～0.1 MPa condition, carry out, the selectivity of aniline is greater than 99%, this method heat transfer conditions is good, avoid local superheating, reduced the generation of side reaction, extended the work-ing life of catalyzer.
Existing apparatus fluidized-bed discharging (composition is mainly aniline, water and hydrogen, 210 ℃-240 ℃ of temperature), after new hydrogen heat exchange, then through two step condensations, realizes gas-liquid separation.Owing to preparing, the copper-based catalysts intensity that aniline uses is not high, in fluidized-bed, after long-term wearing and tearing, can form many particles that are less than 10 microns.This part particle has exceeded the trapping ability of cyclonic separator in fluidized-bed, by air-flow, is taken in interchanger.When crude benzol amine in multi-stage heat exchanger when cooling gradually; granules of catalyst can be combined by the tar in aniline; be bonded in exchanger tube wall; heat exchanger tube is stopped up gradually; resistance increases gradually; the mechanical means that makes delivering gas and oil of mirbane is heavy-duty service or overload likely, and current consumption increases.When serious, after 4-5 month, heat exchanger tube is stopped up substantially completely, the cleaning of must stopping, and impact is normally produced.Take that cleaning interchanger is both time-consuming a contaminate environment apart.In addition, high temperature reduction material is separated into aniline phase and water after cooling,, purification separated with aniline distillation tower through primary tower that crude benzol amine needs again, and treating process is a process heating up, and has caused the waste of cold energy and heat energy in this process.
Summary of the invention
The post-treating method that the object of this invention is to provide product in a kind of oil of mirbane fluidized-bed gas phase hydrogenation aniline process processed.
Main technical schemes of the present invention: aniline post-treating method, it is characterized in that: fluidized-bed is exported to high-temperature material, from washer middle and lower part, pass into washer, washer top sprays with material, it is aniline and a small amount of water that liquid phase material after spray forms, and wherein a part of extraction is entered refining system and refined, and another part carries out heat exchange through the soft water of interchanger and admission bag, utilize heat wherein, self heat exchange to certain temperature on washer top as spray material; Washer top gas phase consists of: hydrogen, water vapor and part aniline steam, after this part material and fresh hydrogen heat exchange, through condenser, carry out gas-liquid separation, the separation of aniline water, and crude benzol amine enters washer top, as spray material.
A kind of typical method of the present invention is: oil of mirbane generates aniline with hydrogen reaction in fluidized-bed, water, the mixture of hydrogen and a small amount of impurity is overflowed from fluidized-bed outlet, from bottom, (1a) enters washer (1), cold material sprays from washer top (1c) with (1d), washer outlet at bottom (1b) material enters refining system through liquid-solid separator (2) rear portion extraction, another part is the cold water heat exchange with admission bag through interchanger (8) outside washer, cooling itself is to certain temperature, from washer top (1d), return, as spray material, washer top exit (1e) material is through interchanger (6) and the hydrogen heat exchange of entering fluidized-bed, after condenser (7) condensation, enter gas-liquid separator (3) again and carry out gas-liquid separation, isolated liquid phase enters aniline water separator (4) again after aniline watercooler is cooling, the water admission stripper aniline recovery that aniline water separator (4) separates, aniline enters crude benzol amine tank mutually, from washer top (1c), enter washer again, as spray material.
Described washer is tower structure, inside establishes sieve plate, and washer bottom (1a) feeding temperature is 210 ℃-240 ℃, consists of hydrogen 6%-10%(wt), aniline 60%-70%(wt), water 20%-30%(wt) and a small amount of impurity and dust.
Described washer top (1c) and (1d) spray temperature of charge are 40 ℃-80 ℃, and outlet at bottom (1b) temperature of charge is 130 ℃-170 ℃.
Described washer top exit (1e) temperature of charge is 70 ℃-140 ℃, consist of aniline, water and hydrogen, through interchanger (6) and the recycle hydrogen heat exchange that enters fluidized-bed, utilize part heat, again through the laggard row gas-liquid separation of aniline water condenser condensation, liquid phase material after separation is cooled to 30 ℃-40 ℃ through aniline watercooler, enter aniline water separator, waste water after separation enters stripping tower aniline recovery, crude benzol amine enters crude benzol amine tundish, from washer (1c) entrance as spray material.
Described washer outlet at bottom liquid phase material after liquid-solid separator is removed dust wherein, through the soft water heat exchange of interchanger (8) and admission bag, cooling itself to 40 ℃-80 ℃.
Described liquid-solid separator (2) can adopt the forms such as gravity separator, cyclone separator, centrifuge separator.
The present invention adopts washer to wash fluidized-bed outlet high-temperature material, by baffle plate and spray, makes solid catalyst powder deposition in liquid phase material, then by liquid-solid separator, removes solid catalyst powder; By improving the temperature and the heat that utilizes washer bottom liquid phases material into refining system, make full use of the latent heat of vaporization of aniline in high temperature reduction material, reach energy-conservation object.
By method of the present invention, to aniline aftertreatment, can effectively remove the granules of catalyst in reducing material, improve security of system and stability, make full use of the latent heat of vaporization of aniline, water simultaneously, reach energy-conservation object.
Accompanying drawing explanation
Accompanying drawing 1 is the process flow sheet of former flow process, and accompanying drawing 2 is process flow sheets of the embodiment of the present invention.
In accompanying drawing 2,1-washer; 2-liquid-solid separator; 3-gas-liquid separator; 4-aniline water separator; 5-crude benzol amine tank; 6-hydrogen interchanger; 7-condenser; 8-interchanger; 9----transferpump; 10-aniline watercooler.
Embodiment
comparative example:
The former flow process of Aniline Unit: (temperature is 230 ℃ to the mixed gas generating after oil of mirbane and hydrogen reaction in fluidized-bed, consist of aniline 66.0%, water 25.5%, hydrogen 8.4%, granules of catalyst 2600ppm and a small amount of impurity) from bed top, overflow, through hydrogen interchanger and hydrogen heat exchange, through aniline condenser, realize gas-liquid separation again, condensate stream is through aniline water cooler, in aniline water separator, carry out aniline water separated, the crude benzol amine obtaining enters primary tower successively and rectifying tower is refined, and obtains finished product aniline; The water admission stripper aniline recovery obtaining, the steam 2.82t/t aniline that whole process consumes, easily stops up for the hydrogen interchanger of reducing material heat exchange, and cleaning in average every 5-6 month is once.Schema is shown in accompanying drawing 1.
following examples are shown in accompanying drawing 2.
embodiment 1
In liquid-solid separator (2), be filled with in advance the crude benzol amine of 50% liquid level, open Matter Transfer pump (9), (temperature is 220 ℃ from washer bottom (1a), to pass into fluidized-bed outlet reducing material, consist of aniline 66.0%, water 25.5%, hydrogen 8.5%, granules of catalyst 1250ppm and a small amount of impurity), regulate interchanger (8), making circulated sprinkling temperature of charge is 40 ℃, by under meter, regulate washer bottom liquid phases rate of discharge, controlling washer top exit material is 140 ℃, after the heat exchange of hydrogen interchanger, carry out again that cooling to realize gas-liquid separation separated with aniline water, water admission stripper aniline recovery after separation, crude benzol amine enters crude benzol amine tundish, as washing tower (1c) spray material, bottom temperature of charge is 162 ℃, and separated through inclined plate sedimentation formula liquid-solid separator, liquid phase consists of aniline 97%, water 3%(wt), a part is for washing tower top circulated sprinkling, and another part enters primary tower to be refined, and enters primary tower part and is controlled by washing tower tower top liquid level.
By this embodiment, fluidized-bed reducing material is carried out to aftertreatment, compare save 0.22 ton of/ton of aniline of steam with original flow process, in material, pressed powder content is below 5ppm, can not cause hydrogen interchanger to stop up.
embodiment 2
In liquid-solid separator (2), be filled with in advance the crude benzol amine of 50% liquid level, open Matter Transfer pump (9), (temperature is 230 ℃ from washer bottom (1a), to pass into fluidized-bed outlet reducing material, consist of aniline 64.9%, water 26.0%, hydrogen 9.0%, granules of catalyst 4000ppm and a small amount of impurity), regulate interchanger (8), making circulated sprinkling temperature of charge is 60 ℃, by under meter, regulate washer bottom liquid phases rate of discharge, controlling washer top exit material is 121 ℃, after the heat exchange of hydrogen interchanger, carry out again that cooling to realize gas-liquid separation separated with aniline water, water admission stripper aniline recovery after separation, crude benzol amine enters crude benzol amine tundish, as washing tower (1c) spray material, bottom temperature of charge is 152 ℃, and separated through rotary fluid solid separator, liquid phase consists of aniline 97.5%, water 2.5%(wt), a part is for washing tower top circulated sprinkling, and another part enters primary tower to be refined, and enters primary tower part and is controlled by washing tower tower top liquid level.
By this embodiment, fluidized-bed reducing material is carried out to aftertreatment, compare save 0.21 ton of/ton of aniline of steam with original flow process, in material, pressed powder content is below 5ppm, can not cause hydrogen interchanger to stop up.
embodiment 3
In liquid-solid separator (2), be filled with in advance the crude benzol amine of 50% liquid level, open Matter Transfer pump (9), (temperature is 240 ℃ from washer bottom (1a), to pass into fluidized-bed outlet reducing material, consist of aniline 65.4%, water 25%, hydrogen 8.5%, granules of catalyst 6500ppm and a small amount of impurity), regulate interchanger (8), making circulated sprinkling temperature of charge is 80 ℃, by under meter, regulate washer bottom liquid phases rate of discharge, controlling washer top exit material is 100 ℃, after the heat exchange of hydrogen interchanger, carry out again that cooling to realize gas-liquid separation separated with aniline water, water admission stripper aniline recovery after separation, crude benzol amine enters crude benzol amine tundish, as washing tower (1c) spray material, bottom temperature of charge is 143 ℃, and separated through centrifugate solid separator, liquid phase consists of aniline 96.5%, water 3.5%(wt), a part is for washing tower top circulated sprinkling, and another part enters primary tower to be refined, and enters primary tower part and is controlled by washing tower tower top liquid level.
By this embodiment, fluidized-bed reducing material is carried out to aftertreatment, compare save 0.23 ton of/ton of aniline of steam with original flow process, in material, pressed powder content is below 5ppm, can not cause hydrogen interchanger to stop up.
Claims (8)
1. an aniline post-treating method, it is characterized in that: fluidized-bed is exported to high-temperature material, from washer middle and lower part, pass into washer, washer top sprays with material, it is aniline and a small amount of water that liquid phase material after spray forms, and wherein a part of extraction is entered refining system and refined, and another part carries out heat exchange through the soft water of interchanger and admission bag, utilize heat wherein, self heat exchange to certain temperature on washer top as spray material; Washer top gas phase consists of: hydrogen, water vapor and part aniline steam, after this part material and fresh hydrogen heat exchange, through condenser, carry out gas-liquid separation, the separation of aniline water, and crude benzol amine enters washer top, as spray material.
2. aniline post-treating method as claimed in claim 1, it is characterized in that: oil of mirbane generates aniline with hydrogen reaction in fluidized-bed, water, the mixture of hydrogen and a small amount of impurity is overflowed from fluidized-bed outlet, from washer (1) bottom (1a), enter, cold aniline sprays from washer top (1c) with (1d), washer outlet at bottom (1b) material enters refining system through liquid-solid separator (2) rear portion, another part carries out heat exchange through interchanger (8) and the soft water of admission bag outside washer, cooling itself is to certain temperature, from washer top (1d), return, as spray material, washer top exit (1e) material enters gas-liquid separator (3) again through interchanger (6) and carries out gas-liquid separation after condenser (7) condensation, cooling through aniline watercooler again, enter aniline water separator (4), the water admission stripper aniline recovery that aniline water separator (4) separates, aniline enters crude benzol amine tank mutually, from washer top (1c), enter again, as spray material.
3. aniline post-treating method as claimed in claim 2, it is characterized in that washer is sieve-plate structure, at the bottom of tower, (1a) feeding temperature is 210 ℃-240 ℃, consists of hydrogen 6%-10%(wt), water 20%-30%(wt) and a small amount of impurity and dust aniline 60%-70%(wt).
4. aniline post-treating method as claimed in claim 2, it is characterized in that washer top (1c) and (1d) spray temperature of charge be 40 ℃-80 ℃, consist of aniline 90%-98%, water 2%-10%, and a small amount of impurity; Outlet at bottom (1b) temperature of charge is 130 ℃-170 ℃, consists of aniline 90-98%, water 2%-10%, and a small amount of impurity.
5. aniline post-treating method as claimed in claim 2, is characterized in that a washer outlet at bottom material part is as washer circulated sprinkling material, and another part enters primary tower.
6. aniline post-treating method as claimed in claim 2, it is characterized in that washer top exit (1e) temperature of charge is 70 ℃-140 ℃, consist of aniline, water and hydrogen, through interchanger (6) and the recycle hydrogen heat exchange that enters fluidized-bed, utilize part heat, after condenser condenses, enter again gas-liquid separator (3) and carry out gas-liquid separation, cooling through aniline watercooler again, enter aniline water separator (4), after separated, aniline enters crude benzol amine tank mutually, from washer top (1c), enter washer, as spray material, water admission stripper aniline recovery.
7. aniline post-treating method as claimed in claim 2, it is characterized in that washer bottom for the liquid-phase outlet material of circulated sprinkling through interchanger (8) and the soft water heat exchange of entering energy recovery drum, be soft water heating, cooling itself to 40 ℃-80 ℃.
8. aniline post-treating method as claimed in claim 2, is characterized in that liquid-solid separator (2) adopts gravity separator or cyclone separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310118257.2A CN104098473A (en) | 2013-04-08 | 2013-04-08 | Post-treatment method of aniline |
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| CN201310118257.2A CN104098473A (en) | 2013-04-08 | 2013-04-08 | Post-treatment method of aniline |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105627785A (en) * | 2016-03-29 | 2016-06-01 | 内蒙古乌海化工有限公司 | Method of recycling condensate water of PVC polymeric slurry steam stripping system |
| CN113877232A (en) * | 2020-07-02 | 2022-01-04 | 中国石油化工股份有限公司 | Method and system for treating aniline-containing gas |
| 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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| US5147421A (en) * | 1991-07-12 | 1992-09-15 | Calvert Environmental, Inc. | Wet scrubber particle discharge system and method of using the same |
| CN1600696A (en) * | 2004-10-12 | 2005-03-30 | 南化集团研究院 | Nitrobenzene extraction method for treating aniline wastewater |
| CN101518747A (en) * | 2008-04-16 | 2009-09-02 | 浙江争光实业股份有限公司 | Recycling system of chlorination mother solution and recycling method thereof |
| CN102744066A (en) * | 2012-05-08 | 2012-10-24 | 中国石油化工股份有限公司 | Nitrobenzene hydrogenation aniline preparation catalyst for fluidized bed |
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2013
- 2013-04-08 CN CN201310118257.2A patent/CN104098473A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1445639A (en) * | 1973-09-20 | 1976-08-11 | Rolls Royce | Gas turbine engine total energy system |
| US5147421A (en) * | 1991-07-12 | 1992-09-15 | Calvert Environmental, Inc. | Wet scrubber particle discharge system and method of using the same |
| CN1600696A (en) * | 2004-10-12 | 2005-03-30 | 南化集团研究院 | Nitrobenzene extraction method for treating aniline wastewater |
| CN101518747A (en) * | 2008-04-16 | 2009-09-02 | 浙江争光实业股份有限公司 | Recycling system of chlorination mother solution and recycling method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105627785A (en) * | 2016-03-29 | 2016-06-01 | 内蒙古乌海化工有限公司 | Method of recycling condensate water of PVC polymeric slurry steam stripping system |
| CN113877232A (en) * | 2020-07-02 | 2022-01-04 | 中国石油化工股份有限公司 | Method and system for treating aniline-containing gas |
| CN113877232B (en) * | 2020-07-02 | 2024-01-26 | 中国石油化工股份有限公司 | Treatment method and system for aniline-containing gas |
| 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 |
| 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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Application publication date: 20141015 |