CN113713747B - Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring - Google Patents
Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring Download PDFInfo
- Publication number
- CN113713747B CN113713747B CN202111055095.3A CN202111055095A CN113713747B CN 113713747 B CN113713747 B CN 113713747B CN 202111055095 A CN202111055095 A CN 202111055095A CN 113713747 B CN113713747 B CN 113713747B
- Authority
- CN
- China
- Prior art keywords
- pipe
- micro heat
- reaction
- cooling container
- baffle plate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
-
- 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
-
- 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
-
- 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
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- 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
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00099—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor the reactor being immersed in the heat exchange medium
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
- B01J2219/00792—One or more tube-shaped elements
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00822—Metal
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00837—Materials of construction comprising coatings other than catalytically active coatings
- B01J2219/00842—For protection channel surface, e.g. corrosion protection
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00867—Microreactors placed in series, on the same or on different supports
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
Abstract
The invention discloses a nitration micro heat pipe reaction device and a nitration micro heat pipe reaction method on a halogen-containing benzene ring, wherein the device comprises a first cooling container, a first-stage reactor, a second cooling container and a second-stage reactor; a first liquid inlet pipe and a first liquid outlet pipe are arranged on the first cooling container; the first-stage reactor comprises a first-stage reaction micro heat pipe and a first collector which are arranged in a first cooling container, one end of the first-stage reaction micro heat pipe is respectively externally connected with a sulfuric acid pipe and a nitric acid pipe, the other end of the first-stage reaction micro heat pipe is connected with the first collector, and the first collector is externally connected with an acid mixing pipe; a second liquid inlet pipe and a second liquid outlet pipe are arranged on the second cooling container; the secondary reactor comprises a secondary reaction micro heat pipe and a second collector which are arranged in a second cooling container, one end of the secondary reaction micro heat pipe is respectively externally connected with a chlorobenzene pipe and an acid mixing pipe, and the second collector is externally connected with a discharging pipe. The invention solves the problem that the existing nitration reactor has large volume, difficult heat dissipation and low heat dissipation efficiency to cause the reduction of the nitration yield.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a micro heat pipe reaction device and a method for nitration reaction on a halogen-containing benzene ring.
Background
The reaction process of introducing nitro group into organic matter molecule during nitration reaction is widely applied in the fields of sewage treatment, flue gas purification, organic matter synthesis and the like. The nitration reaction is mainly divided into two types, one type is the nitration reaction of aliphatic compounds, and the specific reaction process is realized through a free radical process; the other is aromatic compound, and the introduction of the nitro is completed through electrophilic substitution reaction. The halogenated nitrobenzene is an important fine chemical intermediate, and the preparation process needs to introduce nitro on a halogenated benzene ring. The nitration reaction on the halogen-containing benzene ring belongs to the nitration reaction of aromatic compounds, a large amount of heat is released in the reaction process, the released heat is concentrated, and the heat removal rate becomes a prominent problem for controlling the nitration reaction rate and the output of the halogenated nitrobenzene.
However, the existing preparation process of the halogenated nitrobenzene compounds is mostly finished in kettle type equipment such as enamel kettles, steel kettles, cast iron kettles or stainless steel kettles and the like, and has the defects of low reaction efficiency and slow heat release removal. Despite the use of jacket cooling and cooling coils, large amounts of heat generated by large-scale production are still difficult to remove quickly in a short time, which severely limits the nitration reaction rate.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a nitration micro heat pipe reaction device and a nitration micro heat pipe reaction method on a halogen-containing benzene ring, and aims to solve the problems of large volume, difficult heat dissipation and low heat dissipation efficiency of the existing nitration reactor, which cause the reduction of the nitration yield.
In one aspect, the invention provides a nitration micro heat pipe reaction device on a halogen-containing benzene ring, comprising,
the cooling device comprises a first cooling container, a second cooling container and a third cooling container, wherein the first cooling container is provided with a first liquid inlet pipe and a first liquid outlet pipe;
the primary reactor comprises a primary reaction micro heat pipe and a first collector which are arranged in the first cooling container, one end of the primary reaction micro heat pipe is respectively externally connected with a sulfuric acid pipe and a nitric acid pipe, the sulfuric acid pipe is provided with a sulfuric acid valve, the nitric acid pipe is provided with a nitric acid valve, the other end of the primary reaction micro heat pipe is connected to the first collector, and the first collector is externally connected with an acid mixing pipe;
a second cooling container, wherein a second liquid inlet pipe and a second liquid outlet pipe are arranged on the second cooling container, a second liquid inlet valve is arranged on the second liquid inlet pipe, and a second liquid outlet valve is arranged on the second liquid outlet pipe;
the secondary reactor comprises a secondary reaction micro heat pipe and a second collector which are arranged in the second cooling container, one end of the secondary reaction micro heat pipe is respectively connected with a chlorobenzene pipe and an acid mixing pipe externally, the chlorobenzene pipe is provided with a chlorobenzene valve, the acid mixing pipe is provided with an acid mixing valve externally, the second collector is connected with a discharge pipe externally, and the discharge pipe is provided with a discharge valve.
Further, install the sulphuric acid flowmeter on the sulphuric acid pipe, install the nitric acid flowmeter on the nitric acid pipe, install the mixed acid flowmeter on mixing the acid pipe, install the chlorobenzene flowmeter on the chlorobenzene pipe.
Furthermore, a first liquid level pipe is connected outside the first collector, and a first liquid level meter is installed at the tail end of the first liquid level pipe; the second collector is externally connected with a second liquid level pipe, and a second liquid level meter is installed at the tail end of the second liquid level pipe.
Furthermore, a first baffle plate a and a first baffle plate b are arranged inside the first cooling container, the first baffle plate a is arranged above the first-stage reactor, one end of the first baffle plate a is fixedly connected to the inner wall of one side end of the first cooling container, the other end of the first baffle plate a extends to one end of the first-stage reaction micro heat pipe connected with the sulfuric acid pipe and the nitric acid pipe, the first baffle plate b is arranged below the first-stage reactor, one end of the first baffle plate b is fixedly connected to the inner wall of the other side end of the first cooling container, the other end of the first baffle plate b extends to one end of the first-stage reaction micro heat pipe connected with the first collector, the first liquid inlet pipe is communicated with the first cooling container above the first baffle plate a, and the first liquid outlet pipe is communicated with the lower side of the first baffle plate a and is far away from the first cooling container on one side of the first baffle plate b.
Furthermore, a second baffle plate a and a second baffle plate b are arranged inside the second cooling container, the second baffle plate a is arranged above the secondary reactor, one end of the second baffle plate a is fixedly connected to the inner wall of one side end of the second cooling container, the other end of the second baffle plate a extends to one end of the secondary reaction micro heat pipe connected with the acid mixing pipe and the chlorobenzene pipe, the second baffle plate b is arranged below the secondary reactor, one end of the second baffle plate b is fixedly connected to the inner wall of the other side end of the second cooling container, the other end of the second baffle plate b extends to one end of the secondary reaction micro heat pipe connected with the second collector, the second liquid inlet pipe is communicated with the second cooling container above the second baffle plate a, and the second liquid outlet pipe is communicated with the second cooling container below the second baffle plate a and far away from one side of the second baffle plate b.
Furthermore, the first cooling container is close to first feed liquor pipe and installs first thermometer, the second cooling container is close to second feed liquor pipe installs the second thermometer.
Furthermore, the primary reaction micro heat pipe and the secondary reaction micro heat pipe extend in a snake shape.
Furthermore, the discharge pipe is in a snake shape extending in a way of turning back and forth up and down.
On the other hand, the invention provides a nitration micro heat pipe reaction method on a halogen-containing benzene ring, which adopts the nitration micro heat pipe reaction device on the halogen-containing benzene ring and comprises the following steps:
s1, opening a first liquid inlet valve and a first liquid outlet valve, and introducing circulating cooling liquid into a first cooling container;
s2, opening a sulfuric acid valve and a nitric acid valve, introducing concentrated sulfuric acid into the primary reaction micro heat pipe through a sulfuric acid pipe, simultaneously introducing concentrated nitric acid into the primary reaction micro heat pipe through a nitric acid pipe, mixing the concentrated sulfuric acid and the concentrated nitric acid in the primary reaction micro heat pipe to generate a mixed acid solution, and enabling the generated mixed acid solution to flow into and be collected in a first collector;
s3, opening a second liquid inlet pipe and a second liquid outlet pipe, and introducing circulating cooling liquid into a second cooling container;
s4, when the mixed acid solution collected in the first collector reaches a set liquid level height, opening the mixed acid valve and a chlorobenzene valve, introducing the mixed acid solution into the secondary reaction micro heat pipe through the mixed acid pipe, simultaneously introducing the chlorobenzene solution into the secondary reaction micro heat pipe through the chlorobenzene pipe, mixing the mixed acid solution and the chlorobenzene solution in the secondary reaction micro heat pipe to generate halogenated nitrobenzene, and enabling the generated halogenated nitrobenzene to flow into and be collected in a second collector;
and S5, when the halogenated nitrobenzene collected in the second collector reaches the set liquid level height, opening the discharge valve and continuously collecting the halogenated nitrobenzene.
The invention has the beneficial effects that: the application provides a nitration micro heat pipe reaction unit on halogenous benzene ring comprises two-stage reactor, the first order reaction micro heat pipe of one-stage reactor is used for realizing the mixed reaction of concentrated nitric acid and concentrated sulfuric acid, first collector is used for collecting the mixed acid solution that produces through the reaction of one-stage reaction micro heat pipe, in the reaction process, circulate to first cooling container and let in the coolant liquid, the surface of one-stage reaction micro heat pipe receives the coolant liquid to erode and can dispel the heat fast, the second order reaction micro heat pipe of two-stage reactor is used for realizing the nitration of chlorobenzene, the second collector is used for collecting the halogenated nitrobenzene that produces through the reaction of second order reaction micro heat pipe, in the reaction process, circulate to second cooling container and let in the coolant liquid, the surface of second order reaction micro heat pipe receives the coolant liquid to erode and can dispel the heat fast. Therefore, the mixed reaction of concentrated nitric acid and concentrated sulfuric acid is realized through the first-stage reaction micro-channel, and the nitration reaction of chlorobenzene is realized through the second-stage reaction micro-channel, so that the two-stage reaction is quickly radiated, the reaction process is continuous and uninterrupted, the reaction rate is higher, the preparation efficiency is improved, and the problem that the nitration reaction yield is reduced due to the large volume, the difficult heat radiation and the low heat radiation efficiency of the conventional nitration reactor is solved.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
In the drawing, 100-first cooling vessel; 110-a first liquid inlet pipe; 111-a first inlet valve; 120-a first outlet pipe; 121-a first liquid outlet valve; 130-first baffle a; 140-first baffle b; 150-a first thermometer; 200-a first stage reactor; 210-first order reaction micro heat pipe; 220-a first collector; 221-a first level tube; 222-a first liquid level meter; 230-sulfuric acid pipe; 231-sulfuric acid valve; 232-sulfuric acid flow meter; 240-nitric acid tube; 241-nitric acid valve; 242-nitric acid flow meter; 250-acid mixing pipe; 251-acid mixing valve; 252-mixed acid flow meter; 300-a second cooling vessel; 310-a second liquid inlet pipe; 311-a second liquid inlet valve; 320-a second liquid outlet pipe; 321-a second liquid outlet valve; 330-second baffle a; 340-second baffle b; 350-a second thermometer; 400-a secondary reactor; 410-secondary reaction micro heat pipe; 420-a second collector; 421-second liquid level tube; 422-a second level gauge; 430-chlorobenzene tube; a 431-chlorobenzene valve; 432-chlorobenzene flow meter; 440-a tapping pipe; 450-discharge valve.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
The embodiment of the invention provides a nitration micro heat pipe reaction device on a halogen-containing benzene ring, which comprises a first cooling container 100, a first-stage reactor 200, a second cooling container 300 and a second-stage reactor 400, as shown in fig. 1.
The first-stage reactor 200 comprises a first-stage reaction micro heat pipe 210 and a first collector 220 which are arranged in a first cooling container 100, one end of the first-stage reaction micro heat pipe 210 is externally connected with a sulfuric acid pipe 230 and a nitric acid pipe 240 respectively, a sulfuric acid valve 231 is arranged on the sulfuric acid pipe 230, a nitric acid valve 241 is arranged on the nitric acid pipe 240, the other end of the first-stage reaction micro heat pipe 210 is connected with the first collector 220, and the first collector 220 is externally connected with an acid mixing pipe 250.
A second liquid inlet pipe 310 and a second liquid outlet pipe 320 are arranged on the second cooling container 300, a second liquid inlet valve 311 is installed on the second liquid inlet pipe 310, and a second liquid outlet valve 321 is installed on the second liquid outlet pipe 320.
The secondary reactor 400 comprises a secondary reaction micro heat pipe 410 and a second collector 420 which are arranged in the second cooling container 300, one end of the secondary reaction micro heat pipe 410 is respectively externally connected with a chlorobenzene pipe 430 and an acid mixing pipe 250, the chlorobenzene pipe 430 is provided with a chlorobenzene valve 431, the acid mixing pipe 250 is provided with an acid mixing valve 251, the second collector 420 is externally connected with a discharge pipe 440, and the discharge pipe 440 is provided with a discharge valve 450.
The application provides a nitration reaction micro heat pipe reaction unit on halogenous benzene ring comprises two-stage reactor, the first order reaction micro heat pipe 210 of first order reactor 200 is used for realizing the mixed reaction of concentrated nitric acid and concentrated sulfuric acid, first collector 220 is used for collecting the mixed acid solution that produces through the reaction of first order reaction micro heat pipe 210, in the reaction process, let in the coolant liquid to first cooling container 100 circulation, the surface of first order reaction micro heat pipe 210 is washed away by the coolant liquid and can dispel the heat fast, the second order reaction micro heat pipe 410 of second order reactor 400 is used for realizing the nitration reaction of chlorobenzene, second collector 420 is used for collecting the halogeno nitrobenzene that produces through the reaction of second order reaction micro heat pipe 410, in the reaction process, in the coolant liquid is let in to second cooling container 300 circulation, the surface of second order reaction micro heat pipe 410 is washed away by the coolant liquid and can dispel the heat fast. Therefore, the mixed reaction of concentrated nitric acid and concentrated sulfuric acid is realized through the first-stage reaction micro-channel, and the nitration reaction of chlorobenzene is realized through the second-stage reaction micro-channel, so that the two-stage reaction is quickly radiated, the reaction process is continuous and uninterrupted, the reaction rate is higher, the preparation efficiency is improved, and the problem that the nitration reaction yield is reduced due to the large volume, the difficult heat radiation and the low heat radiation efficiency of the conventional nitration reactor is solved.
The cooling liquid circulated in the first cooling container 100 and the second cooling container 300 is preferably water which is clean, cheap and easily available.
In this embodiment, the first-stage reaction micro heat pipe 210, the sulfuric acid pipe 230, the nitric acid pipe 240, the mixed acid pipe 250, the chlorobenzene pipe 430, and the second-stage reaction micro heat pipe 410 are all metal pipes, a plurality of pipes can be arranged according to the output, the pipe length is determined according to the specific space design, the pipe inner diameter is 7-9 mm, the pipe thickness is 1mm, the pipe is coated with a SiO2 thin film, the coating thickness is 0.5mm, so as to avoid corrosion of acid-base solution, and the first-stage reaction micro heat pipe 210 and the second-stage reaction micro heat pipe 410 rapidly release heat generated by reaction by increasing the heat dissipation area.
In this embodiment, the first-stage reaction micro heat pipe 210 and the second-stage reaction micro heat pipe 410 extend in a serpentine shape, so that the paths of the mixed acid reaction and the nitration reaction of chlorobenzene can be increased in a limited space, and the reaction is ensured to be sufficient. The discharge pipe 440 is in a serpentine extension which is turned back and forth up and down, so that solid precipitates can be conveniently intercepted at a low-lying position of the discharge pipe 440 by means of inertia, and solid residues in reaction products can be effectively removed.
In this embodiment, the sulfuric acid flow meter 232 is installed on the sulfuric acid pipe 230, and the nitric acid flow meter 242 is installed on the nitric acid pipe 240, so that the sulfuric acid valve 231 and the nitric acid valve 241 can be adjusted by observing the sulfuric acid flow meter 232 and the nitric acid flow meter 242, and a proper ratio of concentrated nitric acid to concentrated sulfuric acid is formed. Similarly, the mixed acid flow meter 252 is installed on the mixed acid pipe 250, and the chlorobenzene flow meter 432 is installed on the chlorobenzene pipe 430, so that the mixed acid valve 251 and the chlorobenzene valve 431 are adjusted through the mixed acid flow meter 252 and the chlorobenzene flow meter 432 to ensure the introduction ratio of the mixed acid solution and the chlorobenzene solution. The sulfuric acid flow meter 232, the nitric acid flow meter 242, the mixed acid flow meter 252 and the chlorobenzene flow meter 432 are corrosion-resistant flow meters, such as corrosion-resistant turbine flow sensors.
In this embodiment, the first collector 220 is externally connected with a first liquid level pipe 221, and a first liquid level meter 222 is installed at the end of the first liquid level pipe 221, so that the liquid level height of the mixed acid solution in the first collector 220 can be observed through the first liquid level meter 222. Similarly, a second liquid level pipe 421 is connected outside the second collector 420, and a second liquid level meter 422 is installed at the end of the second liquid level pipe 421, so that the liquid level height of the halogenated nitrobenzene in the second collector 420 can be observed through the second liquid level meter 422.
In this embodiment, the first cooling container 100 is provided with the first thermometer 150 near the first liquid inlet pipe 110, so that the temperature of the cooling liquid in the first cooling container 100 can be observed by the first thermometer 150, and during the reaction process, the opening degrees of the first liquid inlet valve 111 and the first liquid outlet valve 121 can be adjusted by observing the first thermometer 150, so as to control the flow rate of the cooling liquid, and the reading of the first thermometer 150 can be maintained at about 15 ℃. Similarly, the second cooling container 300 is provided with a second thermometer 350 adjacent to the second inlet pipe 310, so that the temperature of the cooling liquid in the second cooling container 300 can be observed by the second thermometer 350.
In this embodiment, a first baffle plate a130 and a first baffle plate b140 are disposed inside the first cooling container 100, the first baffle plate a130 is disposed above the first-stage reactor 200, one end of the first baffle plate a130 is fixedly connected to an inner wall of one end of the first cooling container 100, the other end of the first baffle plate a130 extends to one end of the first-stage reaction micro heat pipe 210 connected to the sulfuric acid pipe 230 and the nitric acid pipe 240, the first baffle plate b140 is disposed below the first-stage reactor 200, one end of the first baffle plate b140 is fixedly connected to an inner wall of the other end of the first cooling container 100, the other end of the first baffle plate b140 extends to one end of the first-stage reaction micro heat pipe 210 connected to the first collector 220, the first liquid inlet pipe 110 is communicated with the first cooling container 100 above the first baffle plate a130, and the first liquid outlet pipe 120 is communicated with the first cooling container 100 below the first baffle plate a130, which is far away from the first baffle plate b 140. By arranging the first baffle plate a130 and the first baffle plate b140, the cooling liquid forms a bypass flow in the first cooling container 100, and the generated forced convection flow helps to take away heat of the first-stage reaction micro heat pipe 210 and the first collector 220, so that the quick release of reaction heat is facilitated, and the reaction efficiency of mixed acid is improved.
Similarly, a second baffle plate a330 and a second baffle plate b340 are disposed inside the second cooling container 300, the second baffle plate a330 is disposed above the secondary reactor 400, one end of the second baffle plate a330 is fixedly connected to an inner wall of one end of the second cooling container 300, the other end of the second baffle plate a330 extends to one end of the secondary reaction micro-heat pipe 410, which is connected to the acid mixing pipe 250 and the chlorobenzene pipe 430, the second baffle plate b340 is disposed below the secondary reactor 400, one end of the second baffle plate b340 is fixedly connected to an inner wall of the other end of the second cooling container 300, the other end of the second baffle plate b340 extends to one end of the secondary reaction micro-heat pipe 410, which is connected to the second collector 420, the second liquid inlet pipe 310 is communicated with the second cooling container 300 above the second baffle plate a330, and the second liquid outlet pipe 320 is communicated with the second cooling container 300 below the second baffle plate a330, which is far away from the second baffle plate b 340. Through the arrangement of the second baffle plate a330 and the second baffle plate b340, the cooling liquid forms a circumferential flow in the second cooling container 300, and the generated forced convection flow helps to take away heat of the second-stage reaction micro heat pipe 410 and the second collector 420, so that the reaction heat can be rapidly released, and the efficiency of the nitration reaction of chlorobenzene can be improved.
The baffle plate can be made of stainless steel, the thickness of the baffle plate is 8-10mm, and in order to reinforce the baffle plate and prevent the baffle plate from being washed and deformed by cooling liquid, reinforcing ribs can be welded with the inner walls of the first cooling container 100 and the second cooling container 300 below and above the baffle plate to play a supporting role.
The lower end plates of the first cooling container 100 and the second cooling container 300 can be connected by flanges, so that the installation and maintenance of the internal baffle plate, the micro heat pipe and the collector are facilitated.
The cooling liquid is preferably water which is clean, cheap and easy to obtain.
The embodiment of the invention also provides a nitration micro heat pipe reaction method on the halogen-containing benzene ring, which adopts the nitration micro heat pipe reaction device on the halogen-containing benzene ring and comprises the following steps:
step S1, opening a first liquid inlet valve 111 and a first liquid outlet valve 121, and introducing circulating cooling liquid into a first cooling container 100;
step S2, opening a sulfuric acid valve 231 and a nitric acid valve 241, introducing concentrated sulfuric acid into the primary reaction micro heat pipe 210 through a sulfuric acid pipe 230, simultaneously introducing concentrated nitric acid into the primary reaction micro heat pipe 210 through a nitric acid pipe 240, mixing the concentrated sulfuric acid and the concentrated nitric acid in the primary reaction micro heat pipe 210 to generate a mixed acid solution, enabling the generated mixed acid solution to flow into and be collected in a first collector 220, in the mixed acid reaction process, observing a first thermometer 150, controlling the flow rate of a cooling liquid by adjusting the opening degrees of a first liquid inlet valve 111 and a first liquid outlet valve 121, enabling the reading of the first thermometer 150 to be kept at about 15 ℃, and adjusting the sulfuric acid valve 231 and the nitric acid valve 241 by observing a sulfuric acid flow meter 232 and a nitric acid flow meter 242 to form a proper ratio of the concentrated nitric acid and the concentrated sulfuric acid.
S3, opening a second liquid inlet pipe 310 and a second liquid outlet pipe 320, and introducing circulating cooling liquid into a second cooling container 300;
step S4, when the mixed acid solution collected in the first collector 220 reaches a set liquid level height, opening the mixed acid valve 251 and the chlorobenzene valve 431, introducing the mixed acid solution into the secondary reaction micro heat pipe 410 through the mixed acid pipe 250, simultaneously introducing the chlorobenzene solution into the secondary reaction micro heat pipe 410 through the chlorobenzene pipe 430, mixing the mixed acid solution and the chlorobenzene solution in the secondary reaction micro heat pipe 410 to generate halogenated nitrobenzene (chloronitrobenzene and o-chloronitrobenzene), and flowing and collecting the generated halogenated nitrobenzene into the second collector 420;
and S5, when the halogenated nitrobenzene collected in the second collector 420 reaches the set liquid level height, opening the discharge valve 450 and continuously collecting the halogenated nitrobenzene.
The preparation of the halogenated nitrobenzene is carried out by adopting the embodiment of the invention, 2.7 parts of p-halogenated nitrobenzene is prepared by introducing 2.5 parts of concentrated nitric acid, 2.5 parts of concentrated sulfuric acid and 3 parts of chlorobenzene solution, the reaction rate is up to 90 percent, and the preparation efficiency is improved by 8 percent compared with that of the existing equipment.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (5)
1. A nitration micro heat pipe reaction method on a halogen-containing benzene ring is characterized in that the method adopts a nitration micro heat pipe reaction device on the halogen-containing benzene ring, and the nitration micro heat pipe reaction device on the halogen-containing benzene ring comprises:
the cooling device comprises a first cooling container, a second cooling container and a third cooling container, wherein the first cooling container is provided with a first liquid inlet pipe and a first liquid outlet pipe;
the primary reactor comprises a primary reaction micro heat pipe and a first collector which are arranged in the first cooling container, one end of the primary reaction micro heat pipe is respectively externally connected with a sulfuric acid pipe and a nitric acid pipe, the sulfuric acid pipe is provided with a sulfuric acid valve, the nitric acid pipe is provided with a nitric acid valve, the other end of the primary reaction micro heat pipe is connected to the first collector, and the first collector is externally connected with an acid mixing pipe;
a second cooling container, wherein a second liquid inlet pipe and a second liquid outlet pipe are arranged on the second cooling container, a second liquid inlet valve is arranged on the second liquid inlet pipe, and a second liquid outlet valve is arranged on the second liquid outlet pipe;
the secondary reactor comprises a secondary reaction micro heat pipe and a second collector which are arranged in the second cooling container, one end of the secondary reaction micro heat pipe is respectively externally connected with a chlorobenzene pipe and an acid mixing pipe, the chlorobenzene pipe is provided with a chlorobenzene valve, the acid mixing pipe is provided with an acid mixing valve, the second collector is externally connected with a discharge pipe, and the discharge pipe is provided with a discharge valve;
a first baffle plate a and a first baffle plate b are arranged in the first cooling container, the first baffle plate a is arranged above the first-stage reactor, one end of the first baffle plate a is fixedly connected to the inner wall of one side end of the first cooling container, the other end of the first baffle plate a extends to one end of the first-stage reaction micro heat pipe connected with the sulfuric acid pipe and the nitric acid pipe, the first baffle plate b is arranged below the first-stage reactor, one end of the first baffle plate b is fixedly connected to the inner wall of the other side end of the first cooling container, the other end of the first baffle plate b extends to one end of the first-stage reaction micro heat pipe connected with the first collector, the first liquid inlet pipe is communicated with the first cooling container above the first baffle plate a, and the first liquid outlet pipe is communicated with the first cooling container below the first baffle plate a and far away from one side of the first baffle plate b;
a second baffle plate a and a second baffle plate b are arranged in the second cooling container, the second baffle plate a is arranged above the secondary reactor, one end of the second baffle plate a is fixedly connected to the inner wall of one side end of the second cooling container, the other end of the second baffle plate a extends to one end of the second-stage reaction micro heat pipe connected with the acid mixing pipe and the chlorobenzene pipe, the second baffle plate b is arranged below the secondary reactor, one end of the second baffle plate b is fixedly connected to the inner wall of the other side end of the second cooling container, the other end of the second baffle plate b extends to one end of the second-stage reaction micro heat pipe connected with a second collector, the second liquid inlet pipe is communicated with the second cooling container above the second baffle plate a, and the second liquid outlet pipe is communicated with the second cooling container below the second baffle plate a and far away from one side of the second baffle plate b;
the first-stage reaction micro heat pipe and the second-stage reaction micro heat pipe extend in a snake shape,
the method comprises the following steps:
s1, opening a first liquid inlet valve and a first liquid outlet valve, and introducing circulating cooling liquid into a first cooling container;
s2, opening a sulfuric acid valve and a nitric acid valve, introducing concentrated sulfuric acid into the primary reaction micro heat pipe through a sulfuric acid pipe, simultaneously introducing concentrated nitric acid into the primary reaction micro heat pipe through a nitric acid pipe, mixing the concentrated sulfuric acid and the concentrated nitric acid in the primary reaction micro heat pipe to generate a mixed acid solution, and enabling the generated mixed acid solution to flow into and be collected in a first collector;
s3, opening a second liquid inlet pipe and a second liquid outlet pipe, and introducing circulating cooling liquid into a second cooling container;
s4, when the mixed acid solution collected in the first collector reaches a set liquid level height, opening the mixed acid valve and the chlorobenzene valve, introducing the mixed acid solution into the secondary reaction micro heat pipe through the mixed acid pipe, simultaneously introducing the chlorobenzene solution into the secondary reaction micro heat pipe through the chlorobenzene pipe, mixing the mixed acid solution and the chlorobenzene solution in the secondary reaction micro heat pipe to generate halogenated nitrobenzene, and enabling the generated halogenated nitrobenzene to flow into and be collected in the second collector;
and S5, when the halogenated nitrobenzene collected in the second collector reaches the set liquid level height, opening the discharge valve and continuously collecting the halogenated nitrobenzene.
2. The micro heat pipe reaction method of nitration reaction on a halogen-containing benzene ring according to claim 1, characterized in that: the device comprises a sulfuric acid pipe, a nitric acid flowmeter, a chlorobenzene flowmeter and a sulfuric acid flowmeter, wherein the sulfuric acid pipe is provided with the sulfuric acid flowmeter, the nitric acid pipe is provided with the nitric acid flowmeter, the mixed acid pipe is provided with the mixed acid flowmeter, and the chlorobenzene pipe is provided with the chlorobenzene flowmeter.
3. The micro heat pipe reaction method of nitration reaction on a halogen-containing benzene ring according to claim 1, characterized in that: the first collector is externally connected with a first liquid level pipe, and the tail end of the first liquid level pipe is provided with a first liquid level meter; the second collector is externally connected with a second liquid level pipe, and a second liquid level meter is installed at the tail end of the second liquid level pipe.
4. The micro heat pipe reaction method of nitration reaction on a halogen-containing benzene ring according to claim 1, characterized in that: the first cooling container is close to the first liquid inlet pipe and is provided with a first thermometer, and the second cooling container is close to the second liquid inlet pipe and is provided with a second thermometer.
5. The micro heat pipe reaction method for nitration reaction on a halogen-containing benzene ring according to claim 1, wherein: the discharge pipe is in snake-shaped extension which is folded back and forth up and down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111055095.3A CN113713747B (en) | 2021-09-09 | 2021-09-09 | Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111055095.3A CN113713747B (en) | 2021-09-09 | 2021-09-09 | Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113713747A CN113713747A (en) | 2021-11-30 |
| CN113713747B true CN113713747B (en) | 2023-04-07 |
Family
ID=78682956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111055095.3A Active CN113713747B (en) | 2021-09-09 | 2021-09-09 | Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113713747B (en) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613285B (en) * | 2008-06-25 | 2012-12-05 | 中国科学院大连化学物理研究所 | Synthetic method and special equipment for nitrobenzene |
| CN103834476A (en) * | 2012-11-26 | 2014-06-04 | 北京中天金谷粮油工程技术有限公司 | Fatty acid condenser for edible oil |
| CN102964255B (en) * | 2012-12-04 | 2013-12-25 | 山东力宝得化工股份有限公司 | Safe production method for alkyl nitrate |
| CN105330549A (en) * | 2015-11-20 | 2016-02-17 | 南京理工大学 | Method for preparing isooctyl nitrate in micro-channel reactor |
| CN107935857A (en) * | 2017-12-11 | 2018-04-20 | 中国科学院大连化学物理研究所 | A kind of production method of isooctyl ester nitrate |
| WO2020131258A1 (en) * | 2018-12-21 | 2020-06-25 | Sabic Global Technologies B.V. | Method for the manufacture of 4-nitro-n-(c1-8 alkyl)phthalimide |
| CN112661648A (en) * | 2020-12-30 | 2021-04-16 | 中海油天津化工研究设计院有限公司 | Process method for co-producing sulfur magnesium fertilizer by isooctyl nitrate |
| CN113105331A (en) * | 2021-04-09 | 2021-07-13 | 海南夸克科技有限公司 | Method for preparing 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane by using microchannel reactor |
-
2021
- 2021-09-09 CN CN202111055095.3A patent/CN113713747B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113713747A (en) | 2021-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2622297B1 (en) | Waste heat boiler | |
| CN113713747B (en) | Nitration micro-heat pipe reaction device and method on halogen-containing benzene ring | |
| CN210584968U (en) | Continuous forced mixing pipeline reactor | |
| CN207300003U (en) | A kind of pipe heat exchanger | |
| CN217410743U (en) | Vertical pipeline solution mixing reactor | |
| CN201239625Y (en) | Novel nitrator | |
| US3863712A (en) | Liquid heat exchange system | |
| CN215464455U (en) | Annular continuous nitration reaction device | |
| CN210357184U (en) | Coil pipe in synthetic kettle and synthetic kettle | |
| CN202048820U (en) | Special heat exchanger for blast furnace slag flushing water | |
| US4423770A (en) | Device for reducing thermal stresses on a heat exchanger | |
| CN201561658U (en) | Steam exhaustion and waste drainage device of heating furnace water cooling system | |
| CN215233316U (en) | Converter and sulfur-containing waste treatment system | |
| CN113750926B (en) | Reaction unit suitable for strong exothermic system | |
| CN214438289U (en) | Dilute sulfuric acid preparation device | |
| CN211601641U (en) | Novel propylene polymerization extrinsic cycle heat transfer device | |
| CN203880674U (en) | Shell-and-tube high-temperature waste heat steam boiler with small circulation ratio | |
| JP3910842B2 (en) | Double tube heat exchanger | |
| CN216879280U (en) | Barrel type reactor | |
| CN219454776U (en) | Novel rotatable vane high-flux heat exchanger | |
| CN212431916U (en) | Acid washing device of circulating gas heat exchanger | |
| CN214810707U (en) | Large-scale polymerization loop reactor | |
| CN209230320U (en) | A kind of thread helix winding bundled tube tubular heat exchanger easy to repair | |
| CN217635708U (en) | Flue gas desulfurization waste heat recovery system | |
| CN218981098U (en) | Temperature control structure of ultrafiltration concentration liquid exchange salting-out tank |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |