CN107266320B - Process method for comprehensive energy consumption recovery in nitrochlorobenzene rectification separation - Google Patents
Process method for comprehensive energy consumption recovery in nitrochlorobenzene rectification separation Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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Abstract
The comprehensive energy consumption recovery process in the rectification separation of nitrochlorobenzene comprises two parts, wherein the first part is the heat recovery of a tower top condenser, the second part is the heat recovery of condensed water of a rectifying tower kettle reboiler, and the first part specifically comprises the following steps: the rectifying tower and the tower top condenser complete the operation of a heat exchange unit, the steam-water bag at the tower top completes the flash evaporation separation of steam and water and the operation of a fluid conveying unit completed by a hot water circulating pump; the second part is specifically as follows: condensed water in a reboiler of the rectifying tower enters a primary steam drum through a first steam trap to complete flash separation, and byproduct steam is conveyed outwards; liquid-phase hot water in the primary steam drum enters the secondary steam drum through the second liquid level regulating valve to complete decompression flash evaporation, and byproduct steam is conveyed outwards; and the condensed water at the lower part of the secondary steam pocket enters a hot water collecting tank through a second steam trap, and the hot water in the hot water collecting tank is supplied to the steam pocket on the top of the tower for water supplement through a hot water supplementing pump. The process realizes energy consumption comprehensive recovery of byproduct steam, avoids heat energy loss, saves electric energy and protects the environment.
Description
Technical Field
The invention relates to a comprehensive energy consumption recovery process in nitrochlorobenzene rectification separation, in particular to nitrochlorobenzene rectification overhead condenser heat recovery and tower kettle reboiler condensate water heat recovery.
Background
Nitrochlorobenzene is an important intermediate for chemical industry, medicine, pesticide and dye, and is widely applied to: synthesis of dyes, medicines, pesticides and dyes. Molecular formula of nitrochlorobenzene C6-H4-Cl-N-O2. Molecular weight 157.56. It can be burnt by high heat and open fire. Reacts with strong oxidants. Decomposed by high heat to generate toxic nitrogen oxides and hydrogen chloride.
Nitrochlorobenzene has three isomers:
o-nitrochlorobenzene, O-chlororonidazene;
p-nitrochlorobenzene, P-chlororonidazene;
m-nitrochlorobenzene, M-Chloronitrobenzene.
The o-nitrochlorobenzene is yellow crystals. Has bitter almond flavor. The relative density was 1.305. The melting point is 32-33 ℃. The boiling point is 245-246 ℃. Flash point 127 ℃. Is insoluble in water; dissolving in benzene, ethanol, and diethyl ether.
P-nitrochlorobenzene is a light yellow monoclinic prismatic crystal. The relative density was 1.520. The melting point is 82-84 ℃. The boiling point was 242 ℃. Flash point 127 deg.C (closed cup). Is insoluble in water; is easy to dissolve in organic solvents such as hot ethanol, ether, carbon disulfide, etc.
M-nitrochlorobenzene is pale yellow crystal. The relative density was 1.534(20/4 ℃ C.). Melting point 46 ℃. Boiling point 236 ℃. Flash point 127 ℃. Is insoluble in water; is soluble in most organic solvents.
The process is a chemical reaction of introducing nitro group to arene, i.e. introducing a nitro group to benzene ring of chlorobenzene to prepare o-, p-and m-nitrochlorobenzene. The technological theory is that a set of nitration device generates an acidic nitrochlorobenzene mixture through one-device three-pot series reaction (namely an annular nitrator, a 1# nitrator, a 2# nitrator and a 3# nitrator), and the acidic nitrochlorobenzene mixture is separated into o-nitrochlorobenzene, p-nitrochlorobenzene and m-nitrochlorobenzene after alkaline washing and water washing. The separation comprises rectifying tower separation and crystallization separation.
The chemical reaction formula is as follows:
in the rectification separation process, the vapor phase of the light component p-nitrochlorobenzene in the tower rises to the top of the rectification tower after mass transfer through a vapor film and a liquid film at a packing section in the tower, the temperature of the vapor phase p-nitrochlorobenzene is up to 157 +/-2 ℃, the process needs to condense the vapor phase p-nitrochlorobenzene into a liquid phase, one part of the rectification tower is subjected to self reflux, the other part enters a subsequent crystallization process, and the finished product p-nitrochlorobenzene is produced through crystallization and refining. The phase change process of the p-nitrochlorobenzene from the vapor phase to the liquid phase releases a large amount of heat, and the heat is taken out by adopting heat transfer, so that the phase change process of the p-nitrochlorobenzene from the vapor phase to the liquid phase is realized. The traditional process method is to cool by adopting circulating water at 25-32 ℃, and the part of heat enters a circulating cooling water tower system, thereby wasting electric energy and consuming a large amount of water resources.
The nitrochlorobenzene rectifying reboiler heat source steam is condensed after heat exchange, the temperature of the condensed water reaches 183 +/-2 ℃, the heat is large, and the condensed water is recovered by a technical process, so that the nitrochlorobenzene rectifying reboiler heat source steam can be used as a heating heat source for production and can also be used as heat preservation steam.
The traditional process has many technical defects:
1. the waste heat at the top of the rectifying tower is not recovered, and the method also has the following defects:
1) circulating water is selected as a cooling medium, and the temperature difference between the p-nitrochlorobenzene oil side and the water side is large, so that the tower top condenser is prone to cracking and damage; but also causes the blockage of the condenser tube array caused by the crystallization of the p-nitrochlorobenzene, thereby causing production accidents.
2) Circulating water is selected as a cooling medium, and the circulating water absorbs heat to be brought to a circulating cooling tower system, so that heat energy loss is caused, the packing of the cooling tower is damaged, and electric energy is consumed.
2. The waste heat of the condensed water of the reboiler of the rectifying tower is not recovered, and the following defects are also provided:
1) condensate water in a reboiler at the bottom of the rectifying tower is not recovered, so that water resources are greatly wasted;
2) the condensed water of the reboiler at the rectifying tower is discharged into a ditch or sewer, which pollutes the environment and damages an underground drainage pipe network.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a process method for comprehensively recovering energy consumption in the rectification separation of nitrochlorobenzene, and a byproduct of steam is generated. The process saves electric energy, avoids accidents in production and avoids heat loss, and also produces low-pressure steam for production and heat preservation of nitrochlorobenzene, thereby protecting the environment.
In order to realize the purpose of the invention, the following technical scheme is adopted:
a process method for recovering comprehensive energy consumption in rectification separation of nitrochlorobenzene comprises two parts, wherein the first part is used for recovering heat of a condenser at the top of a tower, and the second part is used for recovering heat of condensed water of a reboiler at the bottom of a rectification tower;
the first part is specifically as follows: vapor-phase nitrochlorobenzene at the top of the rectifying tower enters a tube pass of a condenser at the top of the rectifying tower, hot water is taken as a circulating cooling medium by a shell pass, and the heat exchange process of condensing the nitrochlorobenzene is completed through the heat exchange between the tube pass and the shell pass of the condenser at the top of the rectifying tower; a circulating hot water outlet pipe of the tower top condenser is connected with a tower top steam-water drum, hot water enters the tower top steam-water drum after heat absorption and is subjected to flash separation, and a vapor phase, namely byproduct steam is stably conveyed out to an external use unit through a first steam outlet pressure regulating valve through a pipeline at the upper part of the tower top steam-water drum to finish the outward conveying process of the byproduct steam; liquid-phase hot water of the tower top steam-water drum is connected with a hot water circulating pump through a pipeline at the lower part of the hot water circulating pump, power is provided by the hot water circulating pump to be conveyed to a shell pass of a condenser at the tower top of the nitrochlorobenzene rectifying tower, and hot water is continuously recycled as a circulating cooling medium to finish a fluid conveying process; the steam of the tower top steam-water drum is output outwards and needs external water supplement, and the external water is stably input into the tower top steam-water drum through a first liquid level regulating valve by a hot water supplement pump through a pipeline connected with the tower top steam-water drum to form a circulating system;
the second part is specifically as follows: condensed water of a reboiler of the rectifying tower kettle enters a primary steam drum through a first steam trap through pipeline connection, the condensed water enters the primary steam drum to complete flash separation, and a vapor phase of the flash separation, namely byproduct steam, is conveyed outwards through a second steam outlet pressure regulating valve after passing through a demister on the upper part of the vapor phase, so that the outward conveying process of the byproduct steam is realized; liquid phase hot water in the primary steam pocket is connected through a pipeline at the lower part of the primary steam pocket, the liquid phase hot water is stably regulated through a second liquid level regulating valve to enter the secondary steam pocket, the hot water enters the secondary steam pocket and then is subjected to reduced pressure flash evaporation, and a vapor phase of the reduced pressure flash evaporation, namely the byproduct steam is conveyed outwards through a third steam outlet pressure regulating valve at the upper part of the vapor phase, so that the outward conveying process of the byproduct steam is realized; the condensed water at the lower part of the secondary steam pocket enters a hot water collecting tank through a second steam trap and a pipeline, and the hot water in the hot water collecting tank is supplied to the steam pocket on the top of the tower for water supplement through a hot water supplementing pump.
Compared with the prior art, the invention has the following advantages:
the invention provides a process method for comprehensive energy consumption recovery in nitrochlorobenzene rectification separation, which not only realizes continuous operation, but also recovers the preheating of the top of a nitrochlorobenzene rectification tower and the heat of condensed water of a reboiler at the tower bottom, and produces low-pressure steam as a byproduct, thereby avoiding heat energy loss, saving water resources and electric energy, realizing the recycling of heat energy and protecting the environment.
Drawings
FIG. 1 is a schematic diagram of a system cycle of the present invention;
in the figure: 1-a rectifying tower, 2-a tower top condenser, 3-a tower top steam pocket, 4-a hot water circulating pump, 5-a hot water replenishing pump, 6-a hot water collecting tank, 7-a rectifying tower kettle reboiler, 8-a first-stage steam pocket, 9-a demister, 10-a second-stage steam pocket, 11-a first liquid level regulating valve, 12-a first steam outlet pressure regulating valve, 13-a first steam trap, 14-a second steam outlet pressure regulating valve, 15-a second liquid level regulating valve, 16-a third steam outlet pressure regulating valve and 17-a second steam trap.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
A process for recovering the comprehensive energy consumption in rectifying separation of nitrochlorobenzene includes such steps as recovering the heat from tower top condenser 2 and the condensed water from tower bottom reboiler 7,
the first part is specifically as follows: vapor-phase nitrochlorobenzene at the top of the rectifying tower 1 enters a tube pass of a condenser 2 at the top of the tower, hot water is taken as a circulating cooling medium by a shell pass, and the heat exchange process of condensing the nitrochlorobenzene is completed through the heat exchange between the tube pass and the shell pass of the condenser 2 at the top of the tower; a circulating hot water outlet pipe of the tower top condenser 2 is connected with a tower top steam-water drum 3, hot water enters the tower top steam-water drum 3 after heat absorption and is subjected to flash evaporation separation, and a vapor phase, namely byproduct steam is stably conveyed out to an external use unit through a first steam outlet pressure regulating valve 12 through a pipeline at the upper part of the tower top steam-water drum 3, so that the outward conveying process of the byproduct steam is completed; the liquid phase hot water of the tower top steam-water drum 3 is connected with a hot water circulating pump 4 through a pipeline at the lower part of the hot water circulating pump 4, the hot water is provided with power through the hot water circulating pump 4 and is conveyed to the shell pass of the tower top condenser 2 of the nitrochlorobenzene rectifying tower 1, and the hot water is continuously and circularly used as a circulating cooling medium to finish the fluid conveying process; the steam of the tower top steam-water drum 3 needs external water supplement after being output outwards, and the external water is stably input into the tower top steam-water drum 3 through a first liquid level regulating valve 11 by a hot water supplementing pump 5 through a pipeline connected to the tower top steam-water drum 3 to form a circulating system;
wherein, (1) the heat exchange process of the condenser at the top of the nitrochlorobenzene rectifying tower:
checking whether instrument display facilities of a system of the rectifying tower 1 and the tower top condenser 2 are normal or not, checking whether instrument display facilities of a tower top steam-water drum 3 are normal or not, and checking whether a hot water circulating pump 4 and instrument display are normal or not; and then, a hot water replenishing pump 5 is opened to feed water into the tower top steam water drum 3, an inlet valve of a hot water circulating pump 4 is opened, hot water is conveyed to an inlet of a tower top condenser 2 and returns to the tower top steam water drum 3 through an outlet of the tower top condenser 2, and a closed circulation system is formed. After the rectifying tower 1 works normally, the temperature of the top of the tower reaches 157 +/-2 ℃, nitrochlorobenzene vapor phase ascends from a tower kettle and enters a condenser 2 tube side at the top of a cooling tower through the top of the tower, the temperature of the nitrochlorobenzene vapor phase is about 100 ℃ from 157 +/-2 ℃, the heat of the nitrochlorobenzene vapor phase is transferred to a water phase at the shell side of the condenser 2 at the top of the tower, and water is heated from 133 ℃ to 135 ℃ to form a steam-water mixture which enters a steam-water drum 3 at the.
(2) Steam-water flash separation process: steam-water mixture at 135 ℃ enters a tower top steam-water drum 3, steam and water are subjected to flash separation, steam is arranged at the upper part, and water is arranged at the lower part; in the tower top steam water drum 3, the upper part is a flash separation space, the lower part is a liquid phase area, and the liquid level is preferably controlled to be about 50 percent.
(3) And (3) byproduct steam process: in the production process, steam is continuously generated by flash separation, the steam is byproduct steam, and the steam can be used for heat preservation of process equipment and process pipelines in nitrochlorobenzene production; in order to convey the byproduct steam from the tower top steam-water drum 3 to the outside, a pressure gauge is designed on the tower top steam-water drum 3, and the pressure is adjusted to automatically and stably supply the byproduct steam to users.
(4) And (3) supplementing external water: according to the process (1), the circulating cooling system of the waste heat recovery process at the top of the nitrochlorobenzene rectifying tower 1 is a closed circulating system, the byproduct steam is stably supplied outwards, so that external water needs to be supplemented, and the amount of steam in unit mass conveyed by the steam-water drum 3 at the top of the nitrochlorobenzene rectifying tower is automatically regulated and controlled by the first liquid level regulating valve 11 so that the amount of external water in unit mass needs to be supplemented.
(5) And (3) fluid conveying process: the process is that liquid phase hot water at the lower part of the tower top steam water drum 3 is powered by a hot water circulating pump 4, the hot water is conveyed to serve as a circulating cooling medium to be supplied to a tower top condenser 2, and a steam and water mixture discharged from the tower top condenser 2 returns to the tower top steam water drum 3 to form a recycling process.
The second part is specifically as follows: condensed water of a reboiler 7 of the rectifying tower kettle enters a primary steam drum 8 through a first steam trap 13 through pipeline connection, the condensed water enters the primary steam drum 8 to complete flash separation, and a vapor phase of the flash separation, namely byproduct steam passes through a demister 9 at the upper part of the vapor phase and is conveyed outwards through a second steam outlet pressure regulating valve 14, so that the outward conveying process of the byproduct steam is realized; liquid phase hot water in the primary steam drum 8 is connected through a pipeline at the lower part of the primary steam drum and stably regulated by a second liquid level regulating valve 15 to enter a secondary steam drum 10, the hot water enters the secondary steam drum 10 to complete decompression flash evaporation, and a vapor phase of the decompression flash evaporation, namely, byproduct steam is conveyed outwards through a third steam outlet pressure regulating valve 16 at the upper part of the vapor phase, so that the outward conveying process of the byproduct steam is realized; the condensed water at the lower part of the secondary steam pocket 10 enters the hot water collecting tank 6 through the second steam trap 17 through pipeline connection, and the hot water in the hot water collecting tank 6 is supplied to the steam pocket 3 at the top of the tower for water supplement through the hot water supplementing pump 5.
Wherein, (1) steam-water flash separation and byproduct steam conveying process: condensed water at 183 +/-2 ℃ enters a primary steam drum 8, steam and water are subjected to flash evaporation separation, steam is arranged at the upper part, and water is arranged at the lower part; in the first-stage steam drum 8, the upper part is a flash separation space, the lower part is a liquid phase area, and the liquid level is preferably controlled at 50%. The steam is generated by continuous flash separation, the part of the steam is byproduct steam of 0.6MPa, and the steam can be used as a heat source for the production of nitrochlorobenzene in the later process; in order to convey the byproduct steam from the primary steam drum 8 to the outside, a pressure gauge is arranged on the primary steam drum 8 and is automatically and stably supplied to users by pressure regulation.
(2) And (3) a reduced pressure flash process: the hot water in the liquid phase region at the lower part of the first-stage steam pocket 8 enters the second-stage steam pocket 10 through the stable regulation of a second liquid level regulating valve 15. The secondary steam pocket 10 is controlled at 0.2MPa, hot water enters the secondary steam pocket 10 for decompression flash evaporation, steam generated by flash evaporation is regulated, stabilized and conveyed outwards through a third steam outlet pressure regulating valve 16 at the upper part of the secondary steam pocket 10, the steam is a 0.2MPa by-product steam, and the steam can be used as heat preservation of nitrochlorobenzene process equipment and pipelines; in order to convey the byproduct steam from the inside of the secondary steam pocket 10 to the outside, a pressure gauge is designed on the secondary steam pocket 10 and is automatically and stably supplied to users by pressure regulation.
(3) And (3) condensate recovery process: some hot water is remained after the second-stage steam drum 10 is subjected to flash evaporation, the process adopts a second steam trap 17 to convey outwards, the hot water collecting tank 6 is designed in the part of hot water process, and the collected hot water can be supplied to the first part of overhead steam drum 3 for water supplement.
The process can realize continuous operation, namely, the waste heat of the condenser at the top of the nitrochlorobenzene rectifying tower is recovered, and the waste heat of the reboiler at the bottom of the nitrochlorobenzene rectifying tower is also recovered, so that the comprehensive recovery of the byproduct low-pressure steam by energy consumption is realized, the heat energy loss is avoided, the electric energy is saved, and the environment is protected.
Claims (1)
1. The utility model provides a process method of comprehensive energy consumption recovery in nitrochlorobenzene rectification separation, includes two parts, and the first part is top of the tower condenser (2) heat recovery, and the second part is the heat recovery of rectifying column cauldron reboiler (7) comdenstion water, its characterized in that:
the first part is specifically as follows: vapor-phase nitrochlorobenzene at the top of the rectifying tower (1) enters a tube pass of a condenser (2) at the top of the tower, hot water is taken as a circulating cooling medium by a shell pass, and the heat exchange process of condensing the nitrochlorobenzene is completed through the heat exchange between the tube pass and the shell pass of the condenser (2) at the top of the tower; a circulating hot water outlet pipe of the tower top condenser (2) is connected with a tower top steam water drum (3), hot water enters the tower top steam water drum (3) after heat absorption and is subjected to flash separation, and a vapor phase, namely byproduct steam passes through a pipeline at the upper part of the tower top steam water drum (3) and is stably conveyed out to an external use unit through a first steam outlet pressure regulating valve (12), so that the outward conveying process of the byproduct steam is completed; liquid-phase hot water of the tower top steam-water drum (3) is connected with a hot water circulating pump (4) through a pipeline at the lower part of the hot water circulating pump, power is provided by the hot water circulating pump (4) to be conveyed to the shell side of a condenser (2) at the tower top of the nitrochlorobenzene rectifying tower (1), and hot water is continuously recycled as a circulating cooling medium to finish the fluid conveying process; the steam of the tower top steam-water drum (3) is output outwards and needs external water supplement, and the external water is stably input into the tower top steam-water drum (3) through a first liquid level regulating valve (11) by a hot water supplement pump (5) through a pipeline connected to the tower top steam-water drum (3) to form a circulating system;
the second part is specifically as follows: condensed water of a reboiler (7) at the bottom of the rectifying tower enters a primary steam drum (8) through a first steam trap (13) through pipeline connection, the condensed water enters the primary steam drum (8) to complete flash separation, and a vapor phase of the flash separation, namely byproduct steam, is conveyed outwards through a second steam outlet pressure regulating valve (14) after passing through a demister (9) at the upper part of the vapor phase, so that the outward conveying process of the byproduct steam is realized; liquid phase hot water in the primary steam pocket (8) is connected through a pipeline at the lower part of the primary steam pocket, the liquid phase hot water is stably regulated through a second liquid level regulating valve (15) and enters the secondary steam pocket (10), the hot water completes decompression flash evaporation after entering the secondary steam pocket (10), a vapor phase of the decompression flash evaporation, namely, byproduct steam is conveyed outwards through a third steam outlet pressure regulating valve (16) at the upper part of the vapor phase, and the outward conveying process of the byproduct steam is realized; the condensed water at the lower part of the secondary steam pocket (10) enters a hot water collecting tank (6) through a second steam trap (17) through pipeline connection, and the hot water of the hot water collecting tank (6) is supplied to the steam pocket (3) at the top of the tower for water supplement through a hot water supplementing pump (5).
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