CN114539063A - Method for producing nitrochlorobenzene by vacuum concentration method - Google Patents
Method for producing nitrochlorobenzene by vacuum concentration method Download PDFInfo
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- CN114539063A CN114539063A CN202210128857.6A CN202210128857A CN114539063A CN 114539063 A CN114539063 A CN 114539063A CN 202210128857 A CN202210128857 A CN 202210128857A CN 114539063 A CN114539063 A CN 114539063A
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- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 200
- 239000007791 liquid phase Substances 0.000 claims abstract description 136
- 239000002253 acid Substances 0.000 claims abstract description 102
- 238000000926 separation method Methods 0.000 claims abstract description 102
- 230000003647 oxidation Effects 0.000 claims abstract description 45
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 45
- 238000010025 steaming Methods 0.000 claims abstract description 39
- 238000006396 nitration reaction Methods 0.000 claims abstract description 35
- 238000003860 storage Methods 0.000 claims abstract description 34
- 239000012071 phase Substances 0.000 claims abstract description 29
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000007670 refining Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims description 57
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 23
- 238000001704 evaporation Methods 0.000 abstract description 3
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 229910001868 water Inorganic materials 0.000 description 11
- 238000004821 distillation Methods 0.000 description 10
- 239000002699 waste material Substances 0.000 description 7
- KMAQZIILEGKYQZ-UHFFFAOYSA-N 1-chloro-3-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC(Cl)=C1 KMAQZIILEGKYQZ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000802 nitrating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
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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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for producing nitrochlorobenzene by a vacuum concentration method, and relates to the technical field of nitrochlorobenzene production. The method comprises the following steps: (1) conveying the mixed solution I into an acid steaming device for concentration, inputting the generated mixed steam I into a condenser, and inputting the liquid phase I into a liquid separation tank II; (2) layering the liquid phase I in a liquid separation tank II, feeding the upper liquid phase II into a nitrochlorobenzene refining process, and feeding the lower liquid phase II into a mixed acid storage tank; (3) after the mixed steam I is condensed, the liquid phase II is input into a liquid separation tank I, and the gas phase I is input into a chemical tower; (4) and layering a liquid phase II in the liquid separation tank I, feeding the lower liquid phase I into high-purity chlorobenzene, and feeding the upper liquid phase I into an oxidation tower. This application utilizes evaporating the sour ware to handle the mixed liquid that produces nitrochlorobenzene, and the sulphuric acid solution recycle that the mixed liquid obtained after evaporating sour ware concentration continues to participate in nitration, realizes the recycle of spent acid, reduces the waste water treatment degree of difficulty.
Description
Technical Field
The invention relates to the technical field of nitrochlorobenzene production, in particular to a method for producing nitrochlorobenzene by a vacuum concentration method.
Background
The nitrochlorobenzene comprises p-nitrochlorobenzene, o-nitrochlorobenzene and m-nitrochlorobenzene, and the nitrochlorobenzene is an important intermediate in the industries of dyes, medicines, spices and the like. The existing commonly used preparation method of nitrochlorobenzene is to use chlorobenzene as raw material, nitric acid as nitrating agent and sulfuric acid as catalyst, one hydrogen atom in chlorobenzene molecule is replaced by nitro group in nitric acid molecule in the course of nitro reaction to obtain nitrochlorobenzene, and by-product water is also produced in the course of nitro reaction.
In the existing nitrochlorobenzene production process, nitration reaction is generally carried out under the condition of continuous low temperature (50-60 ℃), and a reaction device adopts a stirred tank reactor to operate in series. However, the production process has the defects of low production efficiency, long reaction time, high operation risk and the like. Sulfuric acid only plays a role in catalysis and dehydration in the nitration reaction, and a large amount of by-product water is generated in the nitration reaction process, so that the mass fraction of sulfuric acid in waste acid is reduced to 72-75%. As shown in fig. 1, the mixture after nitration is separated into mixed liquor of waste acid and nitrochlorobenzene by sedimentation, but the separated waste acid also contains a small amount of nitric acid and nitration products, and high-concentration sulfuric acid used as a catalyst is difficult to circulate, so that the consumption of sulfuric acid is high, a large amount of acidic waste liquid is difficult to treat, the production cost is high, and the subsequent water treatment difficulty is high.
Disclosure of Invention
The invention aims to provide a method for producing nitrochlorobenzene by a vacuum concentration method, which solves the following technical problems:
solves the problem that the catalyst is difficult to recycle in the prior nitrochlorobenzene production process.
The purpose of the invention can be realized by the following technical scheme:
a method for producing nitrochlorobenzene by a vacuum concentration method comprises the following steps:
(1) conveying mixed liquor I generated by a nitration reactor into an acid steaming device, conveying mixed steam I generated by acid steaming of the acid steaming device into a condenser for condensation, and conveying liquid phase I obtained after acid steaming of the acid steaming device into a liquid separation tank II;
(2) standing and layering the liquid phase I in a liquid separation tank II to obtain an upper liquid phase II and a lower liquid phase II, allowing the upper liquid phase II to enter a nitrochlorobenzene refining process, and conveying the lower liquid phase II to a mixed acid storage tank for storage;
(3) condensing the mixed steam I through a condenser to obtain a liquid phase II and a gas phase I, conveying the liquid phase II to a liquid separation tank I, and conveying the gas phase I to an oxidation tower;
(4) and standing and layering the liquid phase II in the liquid separation tank I to obtain an upper liquid phase I and a lower liquid phase I, wherein the lower liquid phase I is chlorobenzene with the concentration of more than 99.0%, and conveying the upper liquid phase I to an oxidation tower.
As a further scheme of the invention: the acid steaming device is pumped to the vacuum degree of 8.5-13.5KPa by a vacuum unit, an air inlet pipe of the vacuum unit is communicated with the acid steaming device, and an air outlet pipe of the vacuum unit is connected with an air inlet of a condenser.
As a further scheme of the invention: the temperature in the acid evaporator is 150-180 ℃.
As a further scheme of the invention: the gas outlet of the condenser is provided with a discharge pipe, a gas-liquid separation valve is arranged on the discharge pipe, a liquid outlet pipe is arranged at a liquid outlet of the gas-liquid separation valve, a gas outlet pipe is arranged at a gas outlet of the gas-liquid separation valve, a liquid phase II is conveyed to a liquid separation tank I through the liquid outlet pipe, and a gas phase I is conveyed to the oxidation tower through the gas outlet pipe.
As a further scheme of the invention: and an air pump is arranged on the outer wall of the oxidation tower and used for delivering oxygen into the oxidation tower, and the gas phase I, the oxygen in the oxidation tower and the upper liquid phase I react to obtain a nitric acid solution.
As a further scheme of the invention: the bottom of the liquid separation tank I is communicated with a liquid discharge pipe, a 2# liquid separation valve is arranged on the liquid discharge pipe, a liquid discharge port of the 2# liquid separation valve is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, the lower liquid phase I is conveyed into the nitration reactor through the lower liquid discharge pipe, and the upper liquid phase I is conveyed into the oxidation tower through the upper liquid discharge pipe.
As a further scheme of the invention: and the bottom of the liquid separation tank II is communicated with a discharge pipe, a 1# liquid separation valve is arranged on the discharge pipe, a liquid discharge port of the 1# liquid separation valve is provided with an upper discharge pipe and a lower discharge pipe, the lower liquid phase II is conveyed to a mixed acid storage tank through the lower discharge pipe for storage, and the upper liquid phase II is conveyed to a nitrochlorobenzene refining process through the upper discharge pipe.
As a further scheme of the invention: the bottom of the mixed acid storage tank is communicated with a 5# pump, and the 5# pump conveys the mixed acid in the mixed acid storage tank to the nitration reactor.
The invention has the beneficial effects that:
(1) this application will evaporate through vacuum unit and take out into the low pressure state in the sour ware to adjustment vacuum and evaporate sour ware temperature, the water that will nitrify in the reaction process and the moisture part that contains in the raw materials is evaporated and is got rid of, makes a large amount of mass fractions be 72% -75% waste sulfuric acid concentration in the waste liquid, realizes spent acid recycle, the spent acid of retrieving can satisfy the needs of nitrochlorobenzene production, the greatly reduced waste liquid treatment degree of difficulty reduces the manufacturing cost of nitrochlorobenzene.
(2) This application utilizes the mixed liquid of evaporating the sour ware to preparation nitrochlorobenzene in-process production to evaporate the acid concentration, makes nitric acid, nitric oxide, chlorobenzene and partial water gasification in the mixed liquid to take away partial heat in the gasification, make mixed liquid cool off fast, effectively avoid the emergence of side effect, gaseous phase through condenser condensation and liquid-liquid separation, the chlorobenzene that does not participate in nitration preparation nitrochlorobenzene in the mixed liquid is retrieved and is recycled.
(3) During this application carries the oxidation jar with insoluble nitric oxide that obtains after the condenser condensation, during the aqueous phase that obtains after separating with the chlorobenzene liquid carries the oxidation jar, and carry oxygen in to the oxidation jar through the air pump, nitric oxide and oxygen and water mixed oxidation preparation obtain nitric acid solution, and the nitric acid solution that obtains is treated the back and is regarded as nitrochlorobenzene's nitration raw materials recycle, reduces nitrochlorobenzene's manufacturing cost, reduces industrial waste gas's the processing degree of difficulty.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a flow diagram of a prior art nitrochlorobenzene separation process;
FIG. 2 is a flow chart of nitrochlorobenzene production by vacuum concentration according to the present invention.
FIG. 3 is a flow chart of the present invention for producing nitrochlorobenzene by vacuum concentration.
In the figure: 1. a nitration reactor; 2. an acid steaming device; 3. a condenser; 4. a liquid separation tank II; 5. a mixed acid storage tank; 6. a liquid separation tank I; 7. an oxidation tower; 8. a vacuum unit; 101. a pump # 1; 201. a # 2 pump; 301. a gas-liquid separation valve; 401. a # 3 pump; 402. 4# pump; 403. a No. 1 liquid separating valve; 501. a No. 5 pump; 601. a No. 6 pump; 602. 7# pump; 603. a No. 2 liquid separating valve; 701. an air pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Please refer to fig. 2-3:
the invention relates to a method for producing nitrochlorobenzene by a vacuum concentration method, which comprises the following steps:
(1) the mixed liquid I generated by the nitration reactor 1 is pumped into an acid steaming device 2 through a No. 1 pump 101, the acid steaming device 2 is pumped to the vacuum degree of 8.5KPa by a vacuum unit 8, the temperature in the acid steaming device 2 is 150 ℃, a No. 2 pump 201 is arranged at the bottom of the acid steaming device 2, an air inlet pipe of the vacuum unit 8 is communicated with the acid steaming device 2, and an air outlet pipe of the vacuum unit 8 is connected with an air inlet of a condenser 3. Mixed steam I generated by acid distillation in the acid distiller 2 is conveyed to the condenser 3 through the vacuum unit 8 for condensation, and liquid phase I obtained by acid distillation in the acid distiller 2 is conveyed to the liquid separation tank II 4 through a No. 2 pump 201;
(2) the bottom of a liquid separation tank II 4 is communicated with a discharge pipe, a 1# liquid separation valve 403 is arranged on the discharge pipe, a liquid discharge port of the 1# liquid separation valve 403 is provided with an upper discharge pipe and a lower discharge pipe, a 3# pump 401 is arranged on the upper discharge pipe, a 4# pump 402 is arranged on the lower discharge pipe, a liquid phase I is placed in the liquid separation tank II for standing and layering to obtain an upper liquid phase II and a lower liquid phase II, the lower liquid phase II is a sulfuric acid solution with the mass fraction of 83.23%, the lower liquid phase II is pumped into a mixed acid storage tank 5 for storage through the 4# pump 402, the bottom of the mixed acid storage tank 5 is communicated with a 5# pump 501, the 5# pump 501 conveys mixed acid in the mixed acid storage tank 5 to a nitration reactor 1 for preparing nitrochlorobenzene by carrying out nitration reaction, the upper liquid phase II is nitrochlorobenzene mixed liquid, the upper liquid phase II is pumped into a nitrochlorobenzene refining process through the 3# pump 401 for continuously refining and separating the nitrochlorobenzene, m-nitrochlorobenzene and o-nitrochlorobenzene.
(3) A discharge pipe is arranged at the gas outlet of the condenser 3, a gas-liquid separation valve 301 is arranged on the discharge pipe, a liquid outlet of the gas-liquid separation valve 301 is provided with a liquid outlet pipe, a gas outlet pipe is arranged at the gas outlet of the gas-liquid separation valve 301, mixed steam I is condensed by the condenser 3 to obtain a liquid phase II and a gas phase I, the liquid phase II is conveyed into a liquid separation tank I6 through the liquid outlet pipe, the gas phase I contains water-insoluble nitric oxide, and the gas phase I is conveyed into the oxidation tower 7 through the gas outlet pipe;
(4) the bottom of the liquid separation tank I6 is communicated with a liquid discharge pipe, a 2# liquid separation valve 603 is arranged on the liquid discharge pipe, a liquid discharge port of the 2# liquid separation valve 603 is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, a 7# pump 602 is arranged on the upper liquid discharge pipe, a 6# pump 601 is arranged on the lower liquid discharge pipe, a liquid phase II is placed in the liquid separation tank I for standing and layering to obtain an upper liquid phase I and a lower liquid phase I, the lower liquid phase I is chlorobenzene with the mass fraction of 99.5%, the lower liquid phase I is pumped into a nitration reactor through the 6# pump 601, the upper liquid phase I is water with the mass fraction of 99.3%, and the upper liquid phase I is pumped into an oxidation tower 7 through the 7# pump 602. An air pump 701 is arranged on the outer wall of the oxidation tower 7, the air pump 701 conveys oxygen into the oxidation tower 7, and the gas phase I, the oxygen in the oxidation tower 7 and the upper liquid phase I react to obtain nitric acid solution.
Example 2
Please refer to fig. 2-3:
the invention relates to a method for producing nitrochlorobenzene by a vacuum concentration method, which comprises the following steps:
(1) the mixed liquid I generated by the nitration reactor 1 is pumped into an acid steaming device 2 through a No. 1 pump 101, the acid steaming device 2 is pumped to the vacuum degree of 9.5KPa by a vacuum unit 8, the temperature in the acid steaming device 2 is 155 ℃, a No. 2 pump 201 is arranged at the bottom of the acid steaming device 2, an air inlet pipe of the vacuum unit 8 is communicated with the acid steaming device 2, and an air outlet pipe of the vacuum unit 8 is connected with an air inlet of a condenser 3. Mixed steam I generated by acid distillation in the acid distiller 2 is conveyed to the condenser 3 through the vacuum unit 8 for condensation, and liquid phase I obtained by acid distillation in the acid distiller 2 is conveyed to the liquid separation tank II 4 through a No. 2 pump 201;
(2) the bottom of a liquid separation tank II 4 is communicated with a discharge pipe, a 1# liquid separation valve 403 is arranged on the discharge pipe, a liquid discharge port of the 1# liquid separation valve 403 is provided with an upper discharge pipe and a lower discharge pipe, a 3# pump 401 is arranged on the upper discharge pipe, a 4# pump 402 is arranged on the lower discharge pipe, a liquid phase I is placed in the liquid separation tank II for standing and layering to obtain an upper liquid phase II and a lower liquid phase II, the lower liquid phase II is a sulfuric acid solution with the mass fraction of 85.14%, the lower liquid phase II is pumped into a mixed acid storage tank 5 for storage through the 4# pump 402, the bottom of the mixed acid storage tank 5 is communicated with a 5# pump 501, the 5# pump 501 conveys mixed acid in the mixed acid storage tank 5 to a nitration reactor 1 for preparing nitrochlorobenzene by carrying out nitration reaction, the upper liquid phase II is nitrochlorobenzene mixed liquid, the upper liquid phase II is pumped into a nitrochlorobenzene refining process through the 3# pump 401 for continuously refining and separating the nitrochlorobenzene, m-nitrochlorobenzene and o-nitrochlorobenzene.
(3) A discharge pipe is arranged at the gas outlet of the condenser 3, a gas-liquid separation valve 301 is arranged on the discharge pipe, a liquid outlet of the gas-liquid separation valve 301 is provided with a liquid outlet pipe, a gas outlet pipe is arranged at the gas outlet of the gas-liquid separation valve 301, mixed steam I is condensed by the condenser 3 to obtain a liquid phase II and a gas phase I, the liquid phase II is conveyed into a liquid separation tank I6 through the liquid outlet pipe, the gas phase I contains water-insoluble nitric oxide, and the gas phase I is conveyed into the oxidation tower 7 through the gas outlet pipe;
(4) the bottom of the liquid separation tank I6 is communicated with a liquid discharge pipe, a 2# liquid separation valve 603 is arranged on the liquid discharge pipe, a liquid discharge port of the 2# liquid separation valve 603 is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, a 7# pump 602 is arranged on the upper liquid discharge pipe, a 6# pump 601 is arranged on the lower liquid discharge pipe, a liquid phase II is placed in the liquid separation tank I for standing and layering to obtain an upper liquid phase I and a lower liquid phase I, the lower liquid phase I is chlorobenzene with the mass fraction of 99.4%, the lower liquid phase I is pumped into a nitration reactor through the 6# pump 601, the upper liquid phase I is water with the mass fraction of 99.1%, and the upper liquid phase I is pumped into an oxidation tower 7 through the 7# pump 602. An air pump 701 is arranged on the outer wall of the oxidation tower 7, the air pump 701 conveys oxygen into the oxidation tower 7, and the gas phase I, the oxygen in the oxidation tower 7 and the upper liquid phase I react to obtain nitric acid solution.
Example 3
Please refer to fig. 2-3:
the invention relates to a method for producing nitrochlorobenzene by a vacuum concentration method, which comprises the following steps:
(1) the mixed liquid I generated by the nitration reactor 1 is pumped into an acid steaming device 2 through a No. 1 pump 101, the acid steaming device 2 is pumped to the vacuum degree of 10KPa through a vacuum unit 8, the temperature in the acid steaming device 2 is 165 ℃, a No. 2 pump 201 is arranged at the bottom of the acid steaming device 2, an air inlet pipe of the vacuum unit 8 is communicated with the acid steaming device 2, and an air outlet pipe of the vacuum unit 8 is connected with an air inlet of a condenser 3. Mixed steam I generated by acid distillation in the acid distiller 2 is conveyed to the condenser 3 through the vacuum unit 8 for condensation, and liquid phase I obtained by acid distillation in the acid distiller 2 is conveyed to the liquid separation tank II 4 through a No. 2 pump 201;
(2) a discharge pipe is communicated with the bottom of the liquid separation tank II 4, a 1# liquid separation valve 403 is arranged on the discharge pipe, an upper discharge pipe and a lower discharge pipe are arranged on a liquid discharge port of the 1# liquid separation valve 403, a 3# pump 401 is arranged on the upper discharge pipe, a 4# pump 402 is arranged on the lower discharge pipe, a liquid phase I is placed in the liquid separation tank II for standing and layering to obtain an upper liquid phase II and a lower liquid phase II, the lower liquid phase II is a sulfuric acid solution with the mass fraction of 87.75%, the lower liquid phase II is pumped into a mixed acid storage tank 5 for storage through the 4# pump 402, a 5# pump 501 is communicated with the bottom of the mixed acid storage tank 5, the 5# pump 501 conveys the mixed acid in the mixed acid storage tank 5 to a nitration reactor 1 for preparing nitrochlorobenzene by carrying out nitration reaction, the upper liquid phase II is a nitrochlorobenzene mixed liquid, the upper liquid phase II is pumped into a nitrochlorobenzene refining process through the 3# pump 401 for continuously refining and separating the nitrochlorobenzene, m-nitrochlorobenzene and o-nitrochlorobenzene.
(3) A discharge pipe is arranged at the gas outlet of the condenser 3, a gas-liquid separation valve 301 is arranged on the discharge pipe, a liquid outlet of the gas-liquid separation valve 301 is provided with a liquid outlet pipe, a gas outlet pipe is arranged at the gas outlet of the gas-liquid separation valve 301, mixed steam I is condensed by the condenser 3 to obtain a liquid phase II and a gas phase I, the liquid phase II is conveyed into a liquid separation tank I6 through the liquid outlet pipe, the gas phase I contains water-insoluble nitric oxide, and the gas phase I is conveyed into the oxidation tower 7 through the gas outlet pipe;
(4) the bottom of the liquid separation tank I6 is communicated with a liquid discharge pipe, a 2# liquid separation valve 603 is arranged on the liquid discharge pipe, a liquid discharge port of the 2# liquid separation valve 603 is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, a 7# pump 602 is arranged on the upper liquid discharge pipe, a 6# pump 601 is arranged on the lower liquid discharge pipe, a liquid phase II is placed in the liquid separation tank I for standing and layering to obtain an upper liquid phase I and a lower liquid phase I, the lower liquid phase I is chlorobenzene with the mass fraction of 99.8%, the lower liquid phase I is pumped into a nitration reactor through the 6# pump 601, the upper liquid phase I is water with the mass fraction of 99.6%, and the upper liquid phase I is pumped into an oxidation tower 7 through the 7# pump 602. An air pump 701 is arranged on the outer wall of the oxidation tower 7, the air pump 701 conveys oxygen into the oxidation tower 7, and the gas phase I, the oxygen in the oxidation tower 7 and the upper liquid phase I react to obtain nitric acid solution.
Example 4
Please refer to fig. 2-3:
the invention relates to a method for producing nitrochlorobenzene by a vacuum concentration method, which comprises the following steps:
(1) the mixed liquid I generated by the nitration reactor 1 is pumped into an acid steaming device 2 through a No. 1 pump 101, the acid steaming device 2 is pumped to the vacuum degree of 11.5KPa by a vacuum unit 8, the temperature in the acid steaming device 2 is 170 ℃, a No. 2 pump 201 is arranged at the bottom of the acid steaming device 2, an air inlet pipe of the vacuum unit 8 is communicated with the acid steaming device 2, and an air outlet pipe of the vacuum unit 8 is connected with an air inlet of a condenser 3. Mixed steam I generated by acid distillation in the acid distiller 2 is conveyed to the condenser 3 through the vacuum unit 8 for condensation, and liquid phase I obtained by acid distillation in the acid distiller 2 is conveyed to the liquid separation tank II 4 through a No. 2 pump 201;
(2) a discharge pipe is communicated with the bottom of the liquid separation tank II 4, a 1# liquid separation valve 403 is arranged on the discharge pipe, an upper discharge pipe and a lower discharge pipe are arranged on a liquid discharge port of the 1# liquid separation valve 403, a 3# pump 401 is arranged on the upper discharge pipe, a 4# pump 402 is arranged on the lower discharge pipe, a liquid phase I is placed in the liquid separation tank II for standing and layering to obtain an upper liquid phase II and a lower liquid phase II, the lower liquid phase II is a sulfuric acid solution with the mass fraction of 87.75%, the lower liquid phase II is pumped into a mixed acid storage tank 5 for storage through the 4# pump 402, a 5# pump 501 is communicated with the bottom of the mixed acid storage tank 5, the 5# pump 501 conveys the mixed acid in the mixed acid storage tank 5 to a nitration reactor 1 for preparing nitrochlorobenzene by carrying out nitration reaction, the upper liquid phase II is a nitrochlorobenzene mixed liquid, the upper liquid phase II is pumped into a nitrochlorobenzene refining process through the 3# pump 401 for continuously refining and separating the nitrochlorobenzene, m-nitrochlorobenzene and o-nitrochlorobenzene.
(3) A discharge pipe is arranged at the gas outlet of the condenser 3, a gas-liquid separation valve 301 is arranged on the discharge pipe, a liquid outlet of the gas-liquid separation valve 301 is provided with a liquid outlet pipe, a gas outlet pipe is arranged at the gas outlet of the gas-liquid separation valve 301, mixed steam I is condensed by the condenser 3 to obtain a liquid phase II and a gas phase I, the liquid phase II is conveyed into a liquid separation tank I6 through the liquid outlet pipe, the gas phase I contains water-insoluble nitric oxide, and the gas phase I is conveyed into the oxidation tower 7 through the gas outlet pipe;
(4) the bottom of the liquid separation tank I6 is communicated with a liquid discharge pipe, a 2# liquid separation valve 603 is arranged on the liquid discharge pipe, a liquid discharge port of the 2# liquid separation valve 603 is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, a 7# pump 602 is arranged on the upper liquid discharge pipe, a 6# pump 601 is arranged on the lower liquid discharge pipe, a liquid phase II is placed in the liquid separation tank I for standing and layering to obtain an upper liquid phase I and a lower liquid phase I, the lower liquid phase I is chlorobenzene with the mass fraction of 99.3%, the lower liquid phase I is pumped into a nitration reactor through the 6# pump 601, the upper liquid phase I is water with the mass fraction of 99.5%, and the upper liquid phase I is pumped into an oxidation tower 7 through the 7# pump 602. An air pump 701 is arranged on the outer wall of the oxidation tower 7, the air pump 701 conveys oxygen into the oxidation tower 7, and the gas phase I, the oxygen in the oxidation tower 7 and the upper liquid phase I react to obtain nitric acid solution.
Example 5
Please refer to fig. 2-3:
the invention relates to a method for producing nitrochlorobenzene by a vacuum concentration method, which comprises the following steps:
(1) the mixed liquid I generated by the nitration reactor 1 is pumped into an acid steaming device 2 through a No. 1 pump 101, the acid steaming device 2 is pumped to the vacuum degree of 13.5KPa by a vacuum unit 8, the temperature in the acid steaming device 2 is 180 ℃, a No. 2 pump 201 is arranged at the bottom of the acid steaming device 2, an air inlet pipe of the vacuum unit 8 is communicated with the acid steaming device 2, and an air outlet pipe of the vacuum unit 8 is connected with an air inlet of a condenser 3. Mixed steam I generated by acid distillation in the acid distiller 2 is conveyed to the condenser 3 through the vacuum unit 8 for condensation, and liquid phase I obtained by acid distillation in the acid distiller 2 is conveyed to the liquid separation tank II 4 through a No. 2 pump 201;
(2) the bottom of a liquid separation tank II 4 is communicated with a discharge pipe, a 1# liquid separation valve 403 is arranged on the discharge pipe, a liquid discharge port of the 1# liquid separation valve 403 is provided with an upper discharge pipe and a lower discharge pipe, a 3# pump 401 is arranged on the upper discharge pipe, a 4# pump 402 is arranged on the lower discharge pipe, a liquid phase I is placed in the liquid separation tank II for standing and layering to obtain an upper liquid phase II and a lower liquid phase II, the lower liquid phase II is a sulfuric acid solution with the mass fraction of 81.89%, the lower liquid phase II is pumped into a mixed acid storage tank 5 for storage through the 4# pump 402, the bottom of the mixed acid storage tank 5 is communicated with a 5# pump 501, the 5# pump 501 conveys mixed acid in the mixed acid storage tank 5 to a nitration reactor 1 for preparing nitrochlorobenzene by carrying out nitration reaction, the upper liquid phase II is nitrochlorobenzene mixed liquid, the upper liquid phase II is pumped into a nitrochlorobenzene refining process through the 3# pump 401 for continuously refining and separating the nitrochlorobenzene, m-nitrochlorobenzene and o-nitrochlorobenzene.
(3) A discharge pipe is arranged at the gas outlet of the condenser 3, a gas-liquid separation valve 301 is arranged on the discharge pipe, a liquid outlet of the gas-liquid separation valve 301 is provided with a liquid outlet pipe, a gas outlet pipe is arranged at the gas outlet of the gas-liquid separation valve 301, mixed steam I is condensed by the condenser 3 to obtain a liquid phase II and a gas phase I, the liquid phase II is conveyed into a liquid separation tank I6 through the liquid outlet pipe, the gas phase I contains water-insoluble nitric oxide, and the gas phase I is conveyed into the oxidation tower 7 through the gas outlet pipe;
(4) the bottom of the liquid separation tank I6 is communicated with a liquid discharge pipe, a 2# liquid separation valve 603 is arranged on the liquid discharge pipe, a liquid discharge port of the 2# liquid separation valve 603 is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, a 7# pump 602 is arranged on the upper liquid discharge pipe, a 6# pump 601 is arranged on the lower liquid discharge pipe, a liquid phase II is placed in the liquid separation tank I for standing and layering to obtain an upper liquid phase I and a lower liquid phase I, the lower liquid phase I is chlorobenzene with the mass fraction of 99.1%, the lower liquid phase I is pumped into a nitration reactor through the 6# pump 601, the upper liquid phase I is water with the mass fraction of 99.0%, and the upper liquid phase I is pumped into an oxidation tower 7 through the 7# pump 602. An air pump 701 is arranged on the outer wall of the oxidation tower 7, oxygen is conveyed into the oxidation tower 7 through the air pump 701, and the nitric acid solution is obtained through reaction of the gas phase I, the oxygen in the oxidation tower 7 and the upper liquid phase I.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "left", "right", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation and a specific orientation configuration and operation, and thus, should not be construed as limiting the present invention. Furthermore, "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be directly connected or indirectly connected through an intermediate member, or they may be connected through two or more elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (8)
1. The method for producing nitrochlorobenzene by using a vacuum concentration method is characterized by comprising the following steps of:
(1) conveying mixed liquor I generated by a nitration reactor into an acid steaming device, conveying mixed steam I generated by acid steaming of the acid steaming device into a condenser for condensation, and conveying liquid phase I obtained after acid steaming of the acid steaming device into a liquid separation tank II;
(2) standing and layering the liquid phase I in a liquid separation tank II to obtain an upper liquid phase II and a lower liquid phase II, allowing the upper liquid phase II to enter a nitrochlorobenzene refining process, and conveying the lower liquid phase II to a mixed acid storage tank for storage;
(3) condensing the mixed steam I through a condenser to obtain a liquid phase II and a gas phase I, conveying the liquid phase II to a liquid separation tank I, and conveying the gas phase I to an oxidation tower;
(4) and standing and layering the liquid phase II in the liquid separation tank I to obtain an upper liquid phase I and a lower liquid phase I, wherein the lower liquid phase I is chlorobenzene with the concentration of more than 99.0%, and conveying the upper liquid phase I to an oxidation tower.
2. The method for producing nitrochlorobenzene according to claim 1, wherein the acid still is pumped by a vacuum unit to a vacuum degree of 8.5-13.5KPa, an air inlet pipe of the vacuum unit is communicated with the acid still, and an air outlet pipe of the vacuum unit is connected with an air inlet of a condenser.
3. The method for producing nitrochlorobenzene according to claim 2, wherein the internal temperature of the acid still is 150-180 ℃.
4. The method for producing nitrochlorobenzene according to claim 1, wherein a discharge pipe is arranged at a gas outlet of the condenser, a gas-liquid separation valve is arranged on the discharge pipe, a liquid outlet of the gas-liquid separation valve is provided with a liquid outlet pipe, a gas outlet pipe is arranged at a gas outlet of the gas-liquid separation valve, the liquid phase II is conveyed to the liquid separation tank I through the liquid outlet pipe, and the gas phase I is conveyed to the oxidation tower through the gas outlet pipe.
5. The method for producing nitrochlorobenzene by vacuum concentration according to claim 1, wherein an air pump is arranged on the outer wall of the oxidation tower and used for delivering oxygen into the oxidation tower, and the gas phase I, the oxygen in the oxidation tower and the upper liquid phase I react to obtain the nitric acid solution.
6. The method for producing nitrochlorobenzene by vacuum concentration according to claim 1, wherein a liquid discharge pipe is communicated with the bottom of the liquid separation tank I, a No. 2 liquid separation valve is arranged on the liquid discharge pipe, a liquid discharge port of the No. 2 liquid separation valve is provided with an upper liquid discharge pipe and a lower liquid discharge pipe, the lower liquid phase I is conveyed to the nitration reactor through the lower liquid discharge pipe, and the upper liquid phase I is conveyed to the oxidation tower through the upper liquid discharge pipe.
7. The method for producing nitrochlorobenzene by using a vacuum concentration method as claimed in claim 1, wherein a discharge pipe is communicated with the bottom of the liquid separation tank II, a No. 1 liquid separation valve is arranged on the discharge pipe, a liquid discharge port of the No. 1 liquid separation valve is provided with an upper discharge pipe and a lower discharge pipe, the lower liquid phase II is conveyed to the mixed acid storage tank through the lower discharge pipe for storage, and the upper liquid phase II is conveyed to the nitrochlorobenzene refining process through the upper discharge pipe.
8. The method for producing nitrochlorobenzene by using a vacuum concentration method according to claim 1, wherein a No. 5 pump is communicated with the bottom of the mixed acid storage tank, and the No. 5 pump conveys the mixed acid in the mixed acid storage tank to the nitration reactor.
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| CN202210128857.6A CN114539063A (en) | 2022-02-11 | 2022-02-11 | Method for producing nitrochlorobenzene by vacuum concentration method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607909A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The quick cooling and the waste acid recycling process of material behind the chlorobenzene thermal insulation nitration |
| CN101607910A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The removing process of the oxynitride that produces in the chlorobenzene thermal insulation nitration process |
| CN109096116A (en) * | 2018-09-11 | 2018-12-28 | 安徽东至广信农化有限公司 | A method of nitro-chlorobenzene is prepared using vacuum concentration process |
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- 2022-02-11 CN CN202210128857.6A patent/CN114539063A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607909A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The quick cooling and the waste acid recycling process of material behind the chlorobenzene thermal insulation nitration |
| CN101607910A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The removing process of the oxynitride that produces in the chlorobenzene thermal insulation nitration process |
| CN109096116A (en) * | 2018-09-11 | 2018-12-28 | 安徽东至广信农化有限公司 | A method of nitro-chlorobenzene is prepared using vacuum concentration process |
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Application publication date: 20220527 |