CN113694858B - Continuous nitration reaction device and method for benzene ring nitration - Google Patents
Continuous nitration reaction device and method for benzene ring nitration Download PDFInfo
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- CN113694858B CN113694858B CN202010455702.4A CN202010455702A CN113694858B CN 113694858 B CN113694858 B CN 113694858B CN 202010455702 A CN202010455702 A CN 202010455702A CN 113694858 B CN113694858 B CN 113694858B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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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
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
Abstract
The invention discloses a continuous nitration reaction device and a continuous nitration reaction method for benzene ring nitration. The invention realizes continuous nitration production, has large device operation flexibility, can be stably operated in a wider output range, has high production efficiency, good product quality, less byproducts, low energy consumption and raw material consumption, and safe and reliable production process.
Description
Technical Field
The invention relates to a continuous nitration reaction device and a continuous nitration reaction method for benzene ring nitration, belonging to the field of nitration production processes.
Background
The reaction for introducing nitro group into aromatic ring is called nitration reaction, nitration is electrophilic substitution, nitration reaction is strong exothermic reaction, its reaction heat is 142KJ/mol, and at the same time of reaction, the sulfuric acid in mixed acid is diluted by the water produced by reaction, and also produces dilution heat (about 7% -10% of reaction heat). If the reaction temperature is continuously increased, side reaction is caused, nitric acid is largely decomposed, and nitrophenol byproducts are increased, which are main reasons for accidents in nitrobenzene production. Meanwhile, the nitration reaction is non-homogeneous reaction, the reaction is carried out at the acid layer and the interface of the acid layer and the organic layer, and the nitration speed is controlled by interphase mass transfer and chemical kinetics, so that the reaction can be stably carried out. Therefore, the safe operation of the nitration reaction can be ensured only by controlling the reaction temperature to be proper and the stirring effect to be good.
In China, manufacturers for producing mixed dinitrobenzene by using nitrobenzene as a raw material through mixed acid nitration adopt intermittent operation in the production process. As is well known, intermittent operation in the production process has the defects of small production capacity, poor stability of the production process, poor operation environment, high labor intensity and the like. Therefore, the development of a new continuous nitration process and the improvement of the yield and the quality of the dinitrobenzene are the necessary way for the forward development of the dinitrobenzene industry in China.
The existing nitration reactor is generally a reaction kettle with strong stirring, and a cooling coil is arranged in the nitration reactor to lead out reaction heat. The nitration reactors are generally operated in series, the retention time of the materials in the reactors is about 15-30 min, after the reaction is finished, the reaction products continuously enter a separator from the nitration reactors and are divided into an organic phase and an acid phase, and the organic phase is the part of washing and purifying the mixed dinitrobenzene. And the acid phase is diluted sulfuric acid, and a waste acid concentration part is removed or the acid phase is directly used as a sewage treatment station for acid-containing wastewater. As shown in fig. 1, the disadvantages of this process design are:
1. when the kettle type nitration reactor is used for taking heat in the formation process of nitration reaction, the heat transfer is mainly carried out through a kettle outer jacket, a heat transfer coil needs to be arranged in the kettle to increase the heat transfer area when the heat transfer of the jacket can not meet the requirement, the heat transfer coil is additionally arranged to enable the stirring diameter to be forcibly reduced, the mixing effect is weakened, the heat transfer coefficient is reduced, and the overall heat transfer effect of the kettle type nitration reactor is poor.
2. When the kettle type nitration reactor is used for intermittent reaction, dropwise feeding is generally adopted, local overheating and uneven concentration distribution in the kettle can occur at the feeding part, so that the product quality is low and the production capacity is limited.
3. When the kettle type nitration reactor is used for the continuous nitration reaction process, a plurality of kettles are required to be connected in series, the retention time of materials in the kettles is uneven, non-nitrated compounds and over-nitrated compounds are not easy to control in the production process, and the production process is complex. Meanwhile, if the material in the reactor is too much, once the reaction explodes, the destructiveness is extremely high.
The continuous nitration reactor process adopts a mixed acid nitration process, and the mixed acid nitration method has the advantages that: the nitration capability is strong, the reaction speed is high, and the nitration yield is high; the specific heat capacity of the sulfuric acid is large, the heat emitted in the nitration reaction can be absorbed, the heat transfer efficiency is high, and the nitration reaction can be carried out stably; the product has high purity and is not easy to generate side reactions such as oxidation and the like. However, in the conventional nitration process, the main disadvantages of the above processes are that in order to control the reaction temperature, the nitration time is long, the concentrated sulfuric acid in the mixed acid is diluted with the nitration reaction, the post-nitration capability in the reaction is weakened, the number of byproducts is increased, and the cooling area required for the nitration equipment is enough.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a continuous nitration reaction device and a method for benzene ring nitration, which realize continuous nitration production, have large device operation flexibility, can be stably operated in a wider yield range, and have high production efficiency, good product quality, less by-products, low energy consumption and raw material consumption, and safe and reliable production process.
In order to achieve the purpose, the invention adopts the following technical means:
the invention provides a continuous nitration reaction device for benzene ring nitration, which comprises: nitrify the head tank, mix sour blending tank, nitrify the charge pump, mix sour charge pump, continuous nitration reactor, two crude nitre product knockout drums, wherein:
an outlet of the nitration raw material tank is connected with an inlet of the continuous nitration reactor through the nitration feed pump, an outlet of the mixed acid preparation tank is connected with an inlet of the continuous nitration reactor through the mixed acid feed pump, and outlets of the continuous nitration reactor are respectively connected with inlets of the two crude nitrate product separation tanks;
the continuous nitration reactor integrates the functions of flowing, mixing, reacting and heat exchanging;
and the two crude nitrate product separation tanks are crude nitrate product separation tanks integrating stirring, cooling, suction filtration, water washing and alkali washing functions.
Preferably, the continuous nitrification reactor comprises:
a cooling structure comprising perforated plates integrally interconnected and having a jacket structure;
a cylindrical reactor having a plurality of reaction chambers therein, each of the reaction chambers being separated by a respective one of the perforated sheets;
the stirrer comprises a stirring rod, a plurality of stirring blades and a stirring motor, the stirring rod is inserted into the center of the cylindrical reactor, and each stirring blade is positioned in each reaction chamber;
more preferably, each reaction chamber further has a feed inlet at an upper portion thereof.
More preferably, the reaction chamber, the perforated plate, stirring vane are all five, and the first trompil quantity of perforated plate to the third the trompil quantity of perforated plate increases in proper order, and the third the trompil quantity of perforated plate to the fifth the trompil quantity of perforated plate is the same, and each the aperture ratio of perforated plate equals only the difference of aperture size.
Preferably, the two crude nitrate product separation tanks comprise:
a tank body;
a crude saltpeter product feed port, which is located obliquely above the tank body;
the water or alkali feeding port is positioned above the tank body in an inclined manner;
the stirrer comprises a stirring rod, a plurality of stirring blades and a stirring motor, the stirring rod is inserted into the center of the tank body, the plurality of stirring blades are positioned in the center of the tank body, and the stirring motor is positioned above the tank body;
the jacket pipe is wound on the side face of the tank body and is filled with circulating chilled water;
the suction filtration structure comprises a filter plate and a plurality of suction filtration ports, the filter plate is positioned at the bottom of the tank body, and the plurality of suction filtration ports are positioned obliquely below the tank body;
and the discharge port is positioned below the tank body.
The invention also provides a method for carrying out continuous nitration reaction of benzene ring nitration by using the device, which comprises the following steps: firstly, fully mixing excessive raw materials to be nitrified and a solvent in a nitrifying raw material tank, pumping the mixture to a continuous nitrification reactor through a nitrifying feed pump, simultaneously fully mixing concentrated sulfuric acid and concentrated nitric acid in a mixed acid preparation tank to form mixed acid, and pumping the mixed acid to the continuous nitrification reactor through a mixed acid feed pump; after all the materials enter the continuous nitration reactor, flowing, mixing, reacting and exchanging heat simultaneously; after the nitrified mixture flows out of the continuous nitration reactor, the nitrified mixture enters a crude nitrate product separation tank, a solvent mixed in the nitrified mixture is pumped out in a vacuum suction filtration mode, then water is added for washing, sulfuric acid in the nitrified mixture is washed out, vacuum is started after full stirring, waste acid is pumped out, alkaline water is added for alkaline washing after the water washing is finished, the residual sulfuric acid in the nitrified mixture is further washed out, vacuum is started after full stirring, neutralized wastewater is pumped out, a nitrified product is obtained, and the nitrified product is discharged through a discharge port.
Preferably, the waste acid and the waste water are pumped out to a waste water station for further treatment.
Compared with the prior art, the invention has the beneficial effects that:
1. the nitration reaction has strong heat release, and the produced water can dilute the reaction medium and release heat, and simultaneously, the water can reduce the catalytic action of the concentrated sulfuric acid. In the kettle type reaction in the prior art, the problems of high local concentration, high reaction rate and incapability of timely dispersing heat can be caused due to weak stirring dispersing capacity, and the generation of byproducts can be promoted by the local overheating. The continuous nitration reactor of the invention solves the problems of local overheating and insufficient stirring, realizes the simultaneous flow, mixing, reaction and heat exchange of materials, and strengthens mass transfer and heat transfer.
2. The invention can also inject or supplement mixed acid at the inlet or different parts of the nitration reactor, the reaction is always carried out under higher mixed acid concentration, the reaction speed and the reaction speed distribution can be adjusted, the reaction process is stable, and the production process is safe and reliable.
3. The crude nitrate product separating tank integrates the functions of stirring, cooling, suction filtration, water washing and alkali washing, has high operation elasticity, and has a cooling function by the jacketed pipe.
4. Compared with the traditional tubular continuous nitration (pipeline type, no stirring) process and kettle type nitration process in the prior art, the continuous nitration production process can improve the yield of the crude product by about 6 percent and reduce the by-products by about 6 percent for the reaction of preparing 2,4-dinitrotoluene from toluene. If the dinitro substance is a byproduct in the nitration reaction, the increase of the dinitro substance content inevitably increases material loss and environmental pollution, and increases the possibility of explosion (the dinitro substance has explosion danger in distillation at higher concentration).
5. In general, the invention realizes continuous nitration production, has large device operation flexibility, can stably operate in a wider yield range, and has high production efficiency, good product quality, less byproducts, low energy consumption and raw material consumption, and safe and reliable production process.
Drawings
FIG. 1 is a flow diagram of a prior art nitration process;
FIG. 2 is a flow diagram of the nitration reaction process of the present invention;
FIG. 3 is a schematic view of the structure of a continuous nitrification reactor of the present invention;
FIG. 4 is a schematic structural view of a continuous nitrification reactor having a feed supplement port in an embodiment of the present invention;
FIG. 5 is a schematic cross-sectional view of a first screen panel in accordance with an embodiment of the present invention;
FIG. 6 is a schematic cross-sectional view of a second perforated plate in accordance with an embodiment of the present invention;
FIG. 7 is a schematic cross-sectional view of third through fifth perforated decks in accordance with an embodiment of the present invention;
FIG. 8 is a schematic diagram of the structure of the crude nitrate product separation tank of the present invention.
Wherein the symbols in fig. 1 are illustrated as follows:
1-acid mixer
2-nitration reactor
3-separator
4-extraction kettle
5-separator
6-waste acid concentrating device
7-alkali washing and water washing device
The symbols in fig. 2 are illustrated as follows:
1-nitrifying raw material tank
2-mixed acid preparation tank
3-nitration feeding pump
4-mixed acid feeding pump
5-continuous nitration reactor
6-separating tank for crude nitrate product
7-crude nitre product separating tank
The symbols in fig. 3 are illustrated as follows:
a-sieve plate
B-sieve plate
C-mesh plate
The symbols in fig. 4 are illustrated as follows:
a-sieve plate
B-sieve plate
C-sieve plate
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and substitutions are intended to be within the scope of the invention.
Referring to FIG. 2, FIG. 2 is a flow chart of the nitration process of the present invention. Firstly, after fully mixing excessive raw materials to be nitrified and a solvent in a nitrifying raw material tank 1, pumping the mixture to a continuous nitrification reactor 5 through a nitrifying feed pump 3, meanwhile, fully mixing concentrated sulfuric acid and concentrated nitric acid in a mixed acid preparation tank 2 to form mixed acid, and pumping the mixed acid to the continuous nitrification reactor 5 through a mixed acid feed pump 4; after all the materials enter the continuous nitration reactor 5, the materials are fully mixed and reacted in the flowing process under the forced stirring of the continuous nitration reactor 5, and fully exchange heat with the circulating cooling water under the covering of a jacket of a cooling structure and in the process of passing through a sieve plate; after the nitrified mixture flows out of the continuous nitration reactor 5, the nitrified mixture enters a crude nitrate product separation tank 6 and a crude nitrate product separation tank 7, a solvent mixed in the nitrified mixture is pumped out in a vacuum suction filtration mode, then water is added for washing, sulfuric acid in the nitrified mixture is washed out, vacuum is started after full stirring, waste acid is pumped out, alkaline water is added for alkaline washing after the water washing is finished, residual sulfuric acid in the nitrified mixture is further washed out, vacuum is started after full stirring, neutralized wastewater is pumped out, the nitrified product is obtained, and the nitrified product is discharged through a discharge port.
In one embodiment of the invention, the spent acid and the wastewater are pumped to a wastewater plant for further treatment.
Referring to FIG. 3, FIG. 3 is a schematic structural diagram of the continuous nitrification reactor of the present invention. The continuous nitrification reactor comprises: a cooling structure comprising perforated plates integrally interconnected and having a jacket structure; a cylindrical reactor having a plurality of reaction chambers therein, each of the reaction chambers being separated by a respective one of the perforated sheets; the agitator, including puddler, a plurality of stirring vane and agitator motor, the puddler inserts cylindrical reactor center, each stirring vane is located each in the reaction chamber.
In an embodiment of the present invention, each of the reaction chambers further has a feed inlet at the upper part, as shown in fig. 4, so that mixed acid can be injected or supplemented at any time to adjust the reaction rate and the reaction rate distribution.
In an embodiment of the present invention, the reaction chamber, the mesh plates, and the stirring blades are all five, the number of openings of the first mesh plate is 10/square meter, the number of openings of the second mesh plate is 20/square meter, the number of openings of the third to fifth mesh plates is 45/square meter, and the total opening ratio is 20%, as shown in fig. 5 to 7.
Referring to fig. 8, fig. 8 is a schematic structural diagram of two crude nitrate product separation tanks according to the present invention. Two of the crude nitrate product separation tanks include: a tank body; a crude saltpeter product feed inlet, which is located obliquely above the tank body; the water or alkali feeding port is positioned above the tank body in an inclined manner; the stirrer comprises a stirring rod, a plurality of stirring blades and a stirring motor, the stirring rod is inserted into the center of the tank body, the plurality of stirring blades are positioned in the center of the tank body, and the stirring motor is positioned above the tank body; the jacket pipe is wound on the side face of the tank body and is filled with circulating chilled water; the suction filtration structure comprises a filter plate and a plurality of suction filtration ports, the filter plate is positioned at the bottom of the tank body, and the plurality of suction filtration ports are positioned obliquely below the tank body; and the discharge port is positioned below the tank body.
Referring to Table 1, table 1 shows the yields of the nitrated crude products and the ratios of by-products, all by weight, under the conventional process shown in FIG. 1 and under the examples of the present invention. It can be seen that the apparatus and process of the present invention represent a significant advance over the prior art, with an increase in crude product yield of about 6% and a reduction in by-products of extremely high value for practical industrial production.
TABLE 1
Claims (5)
1. A continuous nitration reaction apparatus for nitration of benzene rings, comprising: nitrify the head tank, mix sour blending tank, nitrify the charge pump, mix sour charge pump, continuous nitration reactor, two crude nitre product knockout drums, wherein:
an outlet of the nitration raw material tank is connected with an inlet of the continuous nitration reactor through the nitration feed pump, an outlet of the mixed acid preparation tank is connected with an inlet of the continuous nitration reactor through the mixed acid feed pump, and outlets of the continuous nitration reactor are respectively connected with inlets of the two crude nitrate product separation tanks;
the continuous nitration reactor integrates the functions of flowing, mixing, reacting and heat exchanging;
the two crude nitrate product separation tanks are crude nitrate product separation tanks integrating stirring, cooling, suction filtration, water washing and alkali washing functions;
the continuous nitrification reactor comprises:
a cooling structure comprising perforated plates integrally interconnected and having a jacket structure;
a cylindrical reactor having a plurality of reaction chambers therein, each of the reaction chambers being separated by a respective one of the perforated sheets;
the stirrer comprises a stirring rod, a plurality of stirring blades and a stirring motor, the stirring rod is inserted into the center of the cylindrical reactor, and each stirring blade is positioned in each reaction chamber;
the reaction chamber the orifice plate stirring vane is five, first the trompil quantity of orifice plate is to the third the trompil quantity of orifice plate increases in proper order, and the third the trompil quantity of orifice plate is to the fifth the trompil quantity of orifice plate is the same, each the percent opening of orifice plate equals the difference of pore size.
2. The apparatus of claim 1, wherein each of said reaction chambers further comprises a charging port at an upper portion thereof.
3. The apparatus of claim 1, wherein the two crude nitrate product separation tanks comprise:
a tank body;
a crude saltpeter product feed inlet, which is located obliquely above the tank body;
the water or alkali feeding port is positioned above the tank body in an inclined manner;
the stirrer comprises a stirring rod, a plurality of stirring blades and a stirring motor, the stirring rod is inserted into the center of the tank body, the plurality of stirring blades are positioned in the center of the tank body, and the stirring motor is positioned above the tank body;
the jacket pipe is wound on the side face of the tank body and is filled with circulating chilled water;
the suction filtration structure comprises a filter plate and a plurality of suction filtration ports, the filter plate is positioned at the bottom of the tank body, and the plurality of suction filtration ports are positioned obliquely below the tank body;
and the discharge port is positioned below the tank body.
4. A method for continuous nitration of benzene rings using the apparatus of any one of claims 1 to 3, comprising the steps of: firstly, fully mixing excessive raw materials to be nitrified and a solvent in a nitrifying raw material tank, pumping the mixture to a continuous nitrification reactor through a nitrifying feed pump, simultaneously fully mixing concentrated sulfuric acid and concentrated nitric acid in a mixed acid preparation tank to form mixed acid, and pumping the mixed acid to the continuous nitrification reactor through a mixed acid feed pump; after all the materials enter the continuous nitration reactor, flowing, mixing, reacting and exchanging heat simultaneously; after the nitrified mixture flows out of the continuous nitration reactor, the nitrified mixture enters a crude nitrate product separation tank, a solvent mixed in the nitrified mixture is pumped out in a vacuum suction filtration mode, then water is added for washing, sulfuric acid in the nitrified mixture is washed out, vacuum is started after full stirring, waste acid is pumped out, alkaline water is added for alkaline washing after the water washing is finished, residual sulfuric acid in the nitrified mixture is further washed out, vacuum is started after full stirring, neutralized wastewater is pumped out, a nitrified product is obtained, and the nitrified product is discharged through a discharge port.
5. A method according to claim 4, characterised in that the spent acid and the waste water are pumped out to a waste water station for further treatment.
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