CN107185264A - A kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery - Google Patents

A kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery Download PDF

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Publication number
CN107185264A
CN107185264A CN201710348180.6A CN201710348180A CN107185264A CN 107185264 A CN107185264 A CN 107185264A CN 201710348180 A CN201710348180 A CN 201710348180A CN 107185264 A CN107185264 A CN 107185264A
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China
Prior art keywords
steam
hot water
water
rectifying column
chlorobenzene
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Pending
Application number
CN201710348180.6A
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Chinese (zh)
Inventor
王奎
邵威
王兴俊
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ANHUI PROVINCE CHEMICAL INDUSTRY DESIGN INSTITUTE
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ANHUI PROVINCE CHEMICAL INDUSTRY DESIGN INSTITUTE
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Priority to CN201710348180.6A priority Critical patent/CN107185264A/en
Publication of CN107185264A publication Critical patent/CN107185264A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/007Energy recuperation; Heat pumps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Connection condenser at the top of the technique of the nitro-chlorobenzene rectifying column tower top waste heat recovery of the present invention, specially rectifying column, vapour phase paranitrochlorobenzene enters condenser, and condensation paranitrochlorobenzene is completed by the heat exchange using hot water as circulating cooling medium;The circulating hot water outlet pipe connection steam-water separation bag of condenser, hot water enters flash separation after steam-water separation bag, and the vapour phase of flash separation is outwards transferred out after steam-water separation wraps the demister in portion by regulating valve, completes flash separation;The liquid phase hot water of steam-water separation bag is connected by its underpart pipeline with hot water circulating pump, and the shell side of rectifying column tower top condenser is pumped to by hot water circuit, and hot water continues continuous recycle as circulating cooling medium;Fresh water is persistently supplemented by being connected to the pipeline of steam-water separation bag, forms the circulatory system.This technique can realize continuous operation, reclaim the preheating of nitro-chlorobenzene rectifying column tower top, and by-product low-pressure steam is avoided that heat-energy losses, saves electric energy again.

Description

A kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery
Technical field
The present invention is a kind of technique of heat energy utilization waste heat recovery, and in particular to a kind of nitro-chlorobenzene rectifying column tower top heat energy Utilize the process of waste heat recovery.
Background technology
Nitro-chlorobenzene is important chemical industry, medicine, pesticide intermediate, is widely used in:Dyestuff, medicine, the synthesis of agricultural chemicals. Nitro-chlorobenzene molecular formula C6-H4-Cl-N-O2.Molecular weight 157.56.Meet hyperpyrexia, naked light is flammable.Reacted with strong oxidizer.By Height thermal decomposition, produces poisonous nitrogen oxides and hydrogen chloride.It has three kinds of isomers:O-nitrochlorobenzene is yellow crystal.With hardship Almond.Relative density 1.305.32~33 DEG C of fusing point.245~246 DEG C of boiling point.127 DEG C of flash-point.It is water insoluble;It is dissolved in benzene, second Alcohol, ether.M-chloronitrobenzene pale yellow crystals.Relative density 1.534 (20/4 DEG C).46 DEG C of fusing point.236 DEG C of boiling point.Flash-point 127 ℃.It is water insoluble;It is dissolved in most organic solvents.The faint yellow monocline prismatic crystals of paranitrochlorobenzene.Relative density 1.520.Fusing point 82~84 DEG C.242 DEG C of boiling point.127 DEG C of flash-point (closed-cup).It is water insoluble;It is soluble in hot ethanol, ether, carbon disulfide etc. organic Solvent.
This process is the chemical reaction that nitro is introduced on aromatic hydrocarbons, i.e., produced to one nitro of introducing on the phenyl ring of chlorobenzene To, o-, m- nitro chlorobenzene.Technology theory:A set of nitrification installation by three pots of cascade reactions of a device (be annular nitrator, 1# nitrifications pot, 2# nitrifications pot, 3# nitrifications pot) the acid nitro-chlorobenzene mixture of generation, separated after alkali cleaning, washing and adjacent nitre is made Base chlorobenzene, paranitrochlorobenzene and m-chloronitrobenzene.Separation includes rectifying column separation and Crystallization Separation.Chemical equation:
In nitro-chlorobenzene rectifying separation, rectifying tower top temperature is higher, reaches 156~158 DEG C, and this is due in rectifying point From light component paranitrochlorobenzene vapour phase in tower in the inner-tower filling material section temperature that vapour phase is brought into after vapour-liquid membrane mass transfer.This part temperature The paranitrochlorobenzene vapour phase that up to 156~158 DEG C of degree needs condensation to become liquid phase, a part of rectifying column itself backflow, another portion Divide and enter later crystallization process, finished product paranitrochlorobenzene is produced by crystal refining.
Paranitrochlorobenzene is changed into liquid phase this phase transition process from vapour phase, releases substantial amounts of heat, and this partial heat need to be through overheat Transmission, which is taken out, could realize the phase transition process of paranitrochlorobenzene.Traditional process is cooled down using recirculated water, this portion Heat is divided to be taken away by recirculated water into circulating cooling water tower systems.This traditional process had not only wasted electric energy but also consumed Substantial amounts of water resource.
Traditional process technical disadvantages have:
1st, selection recirculated water, because paranitrochlorobenzene side and the water side temperature difference are larger, easily causes equipment as cooling medium Damage;
2nd, selection recirculated water, because paranitrochlorobenzene side and the water side temperature difference are larger, is caused to nitroxyl chloride as cooling medium Benzene crystallization causes blockage of condenser, causes production accident;
3rd, selection recirculated water is as cooling medium, and substantial amounts of heat is absorbed by recirculated water takes circulating cooling tower system to, makes Into heat-energy losses;
4th, selection recirculated water is as cooling medium, and substantial amounts of heat is absorbed by recirculated water takes circulating cooling tower system to, disappears Consuming electric power.
The content of the invention
Not enough present in existing conventional art in order to solve, the present invention provides a kind of nitro-chlorobenzene rectifying column tower top heat energy Using the process of waste heat recovery, steam is generated.The technique has both saved electric energy, turn avoid the accident in production and keeps away Exempt from heat-energy losses, and by-product low-pressure steam, use for nitro-chlorobenzene insulation.
In order to realize the purpose of the present invention, adopt the following technical scheme that:
A kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery, including nitro-chlorobenzene rectifying column tower top condenser Heat exchanging process, carbonated drink flash separation, fluid conveying and supplement fresh water process:
Specially:Light component paranitrochlorobenzene is heated in tower after rectifying column separates nitro-chlorobenzene is changed into vapour phase from liquid phase Connection condenser at the top of rectifying tower top, the rectifying column is risen to, vapour phase paranitrochlorobenzene enters the tube side of overhead condenser, shell side Using hot water as circulating cooling medium, complete to condense the heat of paranitrochlorobenzene by the heat exchange of overhead condenser tube side and shell side Exchange process;The circulating hot water outlet pipe connection steam-water separation bag of the condenser, hot water enters flash distillation point after steam-water separation bag From the vapour phase of flash separation outwards uses unit after steam-water separation wraps the demister in portion by Stress control regulating valve It is stable to transfer out, complete flash separation;The liquid phase hot water of the steam-water separation bag is followed by its underpart pipeline and hot water Ring pump is connected, and hot water enters hot water circulating pump intracavitary, and providing power by hot water circulating pump is delivered to nitro-chlorobenzene rectifying tower The shell side of condenser is pushed up, hot water continues continuous recycle as circulating cooling medium and completes fluid delivery process;The carbonated drink Fresh water is required supplementation with after the steam output of separation bag, fresh water passes through the pipeline for being connected to steam-water separation bag, adjusted by liquid level The stable input of section valve forms the circulatory system.
Wherein, the heat exchanging process of (1) nitro-chlorobenzene rectifying column tower top condenser:
Check whether nitro-chlorobenzene rectifying column tower top condenser system meter displaying device is normal, check steam-water separation Bao Yi Whether table display device is normal, checks that hot water circulating pump and instrument are displayed whether normally;Then steam-water separation bag moisturizing system is opened System opens hot water circulating pump imported valve to being intake in steam-water separation bag, starts hot water circulating pump, opens hot water circuit pump inlet Valve, by delivery to overhead condenser import, is back to steam-water separation bag through overhead condenser outlet, forms closed cycle system System.After rectifying column is working properly, tower top temperature reaches 156-158 DEG C, enters cold from tower reactor rising nitro-chlorobenzene vapour phase through tower top Condenser tube side, near 100-105 DEG C of 156-158 DEG C of nitro-chlorobenzene vapour phase, its heat is transmitted to the aqueous phase of condenser shell side, water from 132 DEG C rise to 135 DEG C and form steam water interface into steam-water separation bag.
(2) carbonated drink flash separation:135 DEG C of steam water interface enters steam-water separation bag, carbonated drink flash separation, steam On top, water is in bottom;In steam-water separation bag, top is flash separation space, and bottom is liquid phase region, Liquid level 40~ 65% is advisable.
(3) byproduct steam process:In process of production, the continuous flash separation of steam is produced, and this some vapor is exactly by-product Steam, the insulation of process equipment and process pipe that this steam can be used in nitro-chlorobenzene production;To make byproduct steam from vapour Water separation bag is conveyed from inside to outside, and design pressure table is wrapped in steam-water separation, and user is supplied to pressure regulation automatic stabilisation.
(4) fresh water process is supplemented:By process (1) as can be seen that nitro-chlorobenzene rectifying column tower top waste heat reclaiming process Circulating cooling system be a closed circuit circulatory system, the stable outside supply of byproduct steam, it is necessary to supplement fresh water, carbonated drink point The steam of how many unit mass is transferred out from bag, is accomplished by supplementing how many unit mass fresh by liquid level auto-adjustment control Water.
(5) fluid delivery process:This process is that the liquid hot water of steam-water separation bag bottom provides power by heat-exchanger pump, defeated Hot water is sent as circulating cooling medium and supplies nitro-chlorobenzene rectifying column tower top condenser, overhead condenser goes out steam water interface return Steam-water separation bag, forms recycling process.
Compared with prior art, the present invention has advantages below:
Invention provides a kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery, and this technique had both realized that serialization was grasped Make, reclaimed the preheating of nitro-chlorobenzene rectifying column tower top, by-product low-pressure steam avoids heat-energy losses, saves electric energy again.
Brief description of the drawings
Fig. 1 is system circulation schematic flow sheet of the invention;
In figure:1- rectifying columns, 2- condensers, 3- demisters, 4- steam-water separation bags, 5- hot water circulating pumps, 6- Stress controls Regulating valve, 7- Liquid level adjusting valves door.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention Premised on implemented, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to Following embodiments.
As shown in figure 1, the present embodiment provides a kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery, including: Heat exchanging process, carbonated drink flash separation, byproduct steam, fluid conveying and the supplement of nitro-chlorobenzene rectifying column tower top condenser Fresh water;Also include:Nitro-chlorobenzene rectifying column 1 is in the rectifying separation equipment for separating paranitrochlorobenzene and o-nitrochlorobenzene, tower Light component paranitrochlorobenzene is heated from liquid phase to be changed into vapour phase and rises to nitro-chlorobenzene rectifying column 1 pushing up, and this portion temperature is up to 156- 158 DEG C, technique needs condensation its gas phase is changed into liquid phase, could realize a part of rectifying separative element itself backflow and extraction, Another part enters later crystallization process, and finished product paranitrochlorobenzene is produced by crystal refining.Overhead condensation is designed in technique Device 2, vapour phase paranitrochlorobenzene enters the tube side of overhead condenser 2, and shell side is cold by tower top using hot water as circulating cooling medium The heat exchange of the tube side of condenser 2 and shell side, realizes the purpose of condensation paranitrochlorobenzene, temperature is also up to 156-158 DEG C to nitre The heat transfer of base chlorobenzene has given circulating cooling medium hot water.The circulating hot water outlet pipe connection steam-water separation of overhead condenser 2 Bag 4, hot water enters flash separation after steam-water separation bag 4, and vapour phase is on top, and liquid phase hot water is in bottom.The vapour phase warp of flash separation After the demister 3 for crossing the top of steam-water separation bag 4, outwards conveyed by Stress control regulating valve 6 using unit is stable, this part is steamed Vapour is the steam of waste heat recovery by-product.The liquid phase hot water of steam-water separation bag 4 is connected by its underpart pipeline with hot water circulating pump 5, Hot water enters the intracavitary of hot water circulating pump 5, and providing power by hot water circulating pump 5 is delivered to the overhead condensation of nitro-chlorobenzene rectifying column 1 The shell side of device 2, hot water continues continuous recycle as circulating cooling medium.Need to mend after the steam output of steam-water separation bag 4 Fresh water is filled, fresh water passes through the pipeline for being connected to steam-water separation bag 4, pass through the stable input of Liquid level adjusting valve door 7.
This technique can realize continuous operation, reclaim the preheating of nitro-chlorobenzene rectifying column tower top, by-product low-pressure steam, Heat-energy losses are avoided that again, save electric energy.
Above content is only citing made for the present invention and explanation, and affiliated those skilled in the art are to being retouched The specific embodiment stated is made various modifications or supplement or substituted using similar mode, without departing from the design of invention Or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.

Claims (1)

1. a kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery, including rectifying column (1) and condenser (2) are completed Carbonated drink flash separation and the fluid conveying of hot water circulating pump (5) that heat exchanging process, steam-water separation bag (4) are completed, it is special Levy and be, light component paranitrochlorobenzene is heated is changed into vapour phase from liquid phase and rises in tower after rectifying column (1) separates nitro-chlorobenzene Rectifying column (1) is pushed up, and connection condenser (2) at the top of the rectifying column (1), vapour phase paranitrochlorobenzene enters overhead condenser (2) Tube side, shell side completes condensation pair using hot water as circulating cooling medium by the heat exchange of overhead condenser (2) tube side and shell side The heat exchanging process of nitro-chlorobenzene;The circulating hot water outlet pipe connection steam-water separation bag (4) of the condenser (2), hot water enters Steam-water separation bag (4) flash separation afterwards, the vapour phase of flash separation passes through after the demister (3) on steam-water separation bag (4) top Stress control regulating valve (6) is outwards transferred out using unit is stable, completes flash separation;The steam-water separation bag (4) Liquid phase hot water be connected by its underpart pipeline with hot water circulating pump (5), hot water enter hot water circulating pump (5) intracavitary, pass through heat Water-circulating pump (5) provides the shell side that power is delivered to nitro-chlorobenzene rectifying column (1) overhead condenser (2), and hot water is cold as circulating But medium continues continuous recycling completion fluid delivery process;Required supplementation with after the steam output of the steam-water separation bag (4) Fresh water, fresh water passes through the pipeline for being connected to steam-water separation bag (4), is followed by the stable input formation of Liquid level adjusting valve door (7) Loop system.
CN201710348180.6A 2017-05-17 2017-05-17 A kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery Pending CN107185264A (en)

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CN201710348180.6A CN107185264A (en) 2017-05-17 2017-05-17 A kind of process of nitro-chlorobenzene rectifying column tower top waste heat recovery

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113244646A (en) * 2021-07-05 2021-08-13 山东彩客东奥化学有限公司 Rectifying tower is used in nitrobenzene production

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103449443A (en) * 2013-09-06 2013-12-18 上海森松环境技术工程有限公司 Heat energy recovery system and technology of water system of polycrystalline silicon reducing furnace
CN104406148A (en) * 2014-11-26 2015-03-11 大连福佳·大化石油化工有限公司 Power generation system capable of recovering waste heat of rectifying tower air cooler

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103449443A (en) * 2013-09-06 2013-12-18 上海森松环境技术工程有限公司 Heat energy recovery system and technology of water system of polycrystalline silicon reducing furnace
CN104406148A (en) * 2014-11-26 2015-03-11 大连福佳·大化石油化工有限公司 Power generation system capable of recovering waste heat of rectifying tower air cooler

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113244646A (en) * 2021-07-05 2021-08-13 山东彩客东奥化学有限公司 Rectifying tower is used in nitrobenzene production

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Application publication date: 20170922