CN114805086A - Process and system for producing diphenylamine by adopting aniline continuous condensation method - Google Patents
Process and system for producing diphenylamine by adopting aniline continuous condensation method Download PDFInfo
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- CN114805086A CN114805086A CN202210526011.8A CN202210526011A CN114805086A CN 114805086 A CN114805086 A CN 114805086A CN 202210526011 A CN202210526011 A CN 202210526011A CN 114805086 A CN114805086 A CN 114805086A
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- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 title claims abstract description 247
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 title claims abstract description 235
- 238000009833 condensation Methods 0.000 title claims abstract description 58
- 230000005494 condensation Effects 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 47
- 230000008569 process Effects 0.000 title claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 52
- 238000006482 condensation reaction Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 230000009471 action Effects 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000000746 purification Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims description 40
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 claims description 35
- 239000002912 waste gas Substances 0.000 claims description 31
- 238000003860 storage Methods 0.000 claims description 25
- 238000010521 absorption reaction Methods 0.000 claims description 18
- 230000009615 deamination Effects 0.000 claims description 16
- 238000006481 deamination reaction Methods 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- -1 alkyl aniline Chemical compound 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002910 solid waste Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- 238000004056 waste incineration Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims 1
- 230000000149 penetrating effect Effects 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000007806 chemical reaction intermediate Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 239000011797 cavity material Substances 0.000 description 6
- 230000002194 synthesizing effect Effects 0.000 description 4
- 239000000975 dye Substances 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229910017971 NH4BF4 Inorganic materials 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001944 continuous distillation Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- NYGZLYXAPMMJTE-UHFFFAOYSA-M metanil yellow Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC(N=NC=2C=CC(NC=3C=CC=CC=3)=CC=2)=C1 NYGZLYXAPMMJTE-UHFFFAOYSA-M 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/60—Preparation of compounds containing amino groups bound to a carbon skeleton by condensation or addition reactions, e.g. Mannich reaction, addition of ammonia or amines to alkenes or to alkynes or addition of compounds containing an active hydrogen atom to Schiff's bases, quinone imines, or aziranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/08—Preparation of ammonia from nitrogenous organic substances
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for producing diphenylamine by adopting an aniline continuous condensation method, which mainly comprises four production units of condensation reaction, ammonia separation and purification, aniline separation and diphenylamine purification, and comprises the following steps: s1, condensation reaction: the aniline raw material is subjected to heat exchange and temperature rise with the condensation reaction discharge material through a heat exchanger, enters a preheater, and is further heated and heated to the reaction temperature by using heat conduction oil; and (3) the preheated aniline enters a condensation reactor, and the aniline is subjected to condensation reaction under the action of a catalyst to generate diphenylamine and ammonia. The invention overcomes the defects of the prior art, has reasonable design, adopts aniline continuous condensation method to produce diphenylamine, and generates condensation reaction under certain temperature, pressure and catalyst action to produce diphenylamine; the reaction intermediate liquid is subjected to ammonia removal as a byproduct under low pressure, and unreacted aniline and the generated byproduct are rectified and separated from diphenylamine under the vacuum condition, so that the method has high social use value and application prospect.
Description
Technical Field
The invention relates to the technical field of diphenylamine, in particular to a process and a system for producing diphenylamine by adopting an aniline continuous condensation method.
Background
Diphenylamine is an important chemical intermediate, and is mainly used for synthesizing virus reagents, various antioxidants, medical reagents, fruit preservatives, photoelectric cavity materials and the like.
Diphenylamine is also a raw material of dye industry, and is condensed with nitrophenol to obtain a vulcanized new blue BBF dye for dyeing cotton-flax, adhesive fiber and cotton blended fabrics; besides, diphenylamine can also be used for producing dyes of acid golden yellow G, etc.
Diphenylamine itself has sterilizing and insecticidal properties and is used in the agricultural and pharmaceutical industries. The paper treated by diphenylamine can be used for coating fruits, so that the deterioration of the fruits can be inhibited, the preservation period can be prolonged and the like.
There are many methods for producing diphenylamine, but the technical route for synthesizing diphenylamine only by aniline has better industrial value; the traditional method for synthesizing diphenylamine from aniline uses halides such as aluminum trichloride, HCl, BF3 or NH4BF4 and the like as catalysts, and is synthesized in a kettle manner under the conditions of 1.6-2.0 MPa and 300-350 ℃, and the diphenylamine product is obtained by salting out, neutralizing, distilling and crystallizing a crude product. The method adopts intermittent operation, generates a large amount of waste acid, alkaline residue and the like in the process, has serious corrosion pollution and severe working conditions, and has high aniline unit consumption and high production cost in the production process.
Therefore, the inventor aims to provide a process and a system for producing diphenylamine by adopting an aniline continuous condensation method, which take the experience of abundant design development and actual manufacturing of related industries for years, research and improvement are carried out aiming at the existing structure and deficiency, and the aim of achieving more practical value is fulfilled.
Disclosure of Invention
In order to solve the problems mentioned in the background art, the invention provides a process and a system for producing diphenylamine by adopting an aniline continuous condensation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for producing diphenylamine by adopting an aniline continuous condensation method comprises the following steps:
s1, condensation reaction:
the aniline raw material is subjected to heat exchange and temperature rise with the condensation reaction discharge material through a heat exchanger, enters a preheater, and is further heated and heated to the reaction temperature by using heat conduction oil; the preheated aniline enters a condensation reactor, and the aniline is subjected to condensation reaction under the action of a catalyst to generate diphenylamine and ammonia;
the condensation reactor is a fixed bed reactor, the temperature is controlled at 340-360 ℃, the pressure is controlled at 2.0MPa, the catalyst is aluminum oxide, the catalyst needs to be replaced periodically, and the generated waste catalyst is entrusted with qualified unit treatment;
s2, ammonia separation and purification:
the condensation reaction discharge material in the step S1 is sent into a gas-liquid separator after being subjected to heat exchange and temperature reduction with raw material aniline through a heat exchanger, the condensation reaction discharge material enters the gas-liquid separator to separate ammonia gas from a liquid phase, and a crude diphenylamine solution from which the ammonia gas is separated enters a deamination tower;
the deammoniation tower is vacuumized by a liquid ring vacuum pump and rectified under the pressure of-0.05 MPa to further remove a small amount of ammonia and water remained in the crude diphenylamine solution, and a water phase generated after the condensation of a material from the top of the deammoniation tower is used as wastewater to be sent to a sewage treatment station in a factory for pretreatment;
ammonia gas containing a small amount of organic matters separated from the top of the gas-liquid separator and the deamination tower is condensed and separated to obtain ammonia gas with higher content, and the ammonia gas is prepared into liquid ammonia by a liquid ammonia preparation system and is sent to a liquid ammonia tank area for storage;
s3, aniline separation:
the discharge of the deamination tower enters an aniline front tower, the aniline front tower is rectified under the pressure of-0.05 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump, and a distillate containing 2-methylpyridine and a small amount of aniline at the tower top enters a 2-methylpyridine rectifying tower after being condensed;
the bottom kettle liquid of the aniline front tower enters an aniline tower, the 2-picoline rectifying tower is rectified under normal pressure, and the bottom aniline kettle liquid of the 2-picoline rectifying tower also enters the aniline tower;
discharging materials from the bottoms of the aniline front tower and the 2-methylpyridine rectifying tower into an aniline tower, then utilizing a liquid ring vacuum pump to vacuumize and rectify the materials under the pressure of-0.08 MPa, and condensing aniline discharged from the top of the tower and returning the aniline to a condensation reactor for reuse;
feeding the bottom discharge of the aniline tower into a light component tower, performing vacuum distillation by using a liquid ring vacuum pump under the pressure of-0.09 MPa, and respectively conveying the alkyl aniline mixture discharged from the top of the light component tower to a solid waste incineration device for use after condensation and transfer in a middle tank;
s4, diphenylamine purification:
discharging the bottom of the light component tower into a diphenylamine tower, performing rectification under the pressure of-0.09 MPa by using a liquid ring vacuum pump for vacuumizing, and condensing diphenylamine discharged from the tower top and then conveying the diphenylamine to a diphenylamine storage tank in a tank area for storage; the discharged material at the bottom of the diphenylamine tower enters a diphenylamine recovery tower, the diphenylamine is further recovered by rectification under the pressure of-0.09 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump, the diphenylamine discharged from the tower top is sent to a diphenylamine storage tank in a tank area for storage after being condensed, and the residual alkyl diphenylamine mixture in the tower is treated as solid waste.
The process adopts aniline continuous condensation method to produce diphenylamine; aniline is subjected to condensation reaction under certain temperature and pressure and the action of a catalyst to generate diphenylamine. Removing by-product ammonia from the reaction intermediate liquid under low pressure, and rectifying and separating unreacted aniline and generated by-product and diphenylamine under vacuum condition.
Chemical equation of main reaction:
side chemical reaction formula:
a system for producing diphenylamine by adopting an aniline continuous condensation method comprises a condensation reactor, a gas-liquid separator, a deamination tower, an aniline front tower, a rectification tower, an aniline tower, a light component tower, a diphenylamine tower and a diphenylamine recovery tower, wherein the bottom of the condensation reactor is connected with a heat exchanger through a pipeline, the heat exchanger is communicated with a preheater, and a discharge hole of the preheater is connected with a feed inlet of the condensation reactor;
the heat exchanger, the gas-liquid separator, the deamination tower and the aniline front tower are sequentially connected through a pipeline, distillate containing picoline and a small amount of aniline at the top of the aniline front tower enters the rectification tower after being condensed, aniline kettle liquid at the bottoms of the aniline front tower and the rectification tower enters the aniline tower, the discharge of the aniline tower enters the light component tower, the discharge of the light component tower at the bottom of the light component tower enters the diphenylamine tower, and the discharge of the diphenylamine tower at the bottom of the diphenylamine tower enters the diphenylamine recovery tower for further rectification and recovery.
Preferably, a reboiler is arranged at the tower bottom of the diphenylamine recovery tower, diphenylamine discharged from the tower top of the diphenylamine recovery tower is condensed and then sent to a diphenylamine storage tank for storage, ammonia gas byproduct of the diphenylamine recovery tower is cooled and separated through a condensation buffer tank, the ammonia gas is changed into liquid ammonia gas after passing through an ice maker, and then the liquid ammonia gas is compressed and condensed by a compressor and then sent to a liquid ammonia tank for storage;
and a pipeline between the condensation buffer tank and the ice maker is communicated with a recovery processing pipeline, and one end of the recovery processing pipeline is connected with a waste gas treatment tank.
Preferably, the middle of the top of the waste gas treatment tank is communicated with an absorption tower, a plurality of layers of adsorption fillers are arranged in the absorption tower, and the recovery treatment pipeline penetrates through the bottom of the waste gas treatment tank and is provided with a spray head at the inward extending end.
Preferably, a U-shaped baffle plate is arranged on the inner wall of the waste gas treatment tank and positioned outside the spray head, the opening of the U-shaped baffle plate is downward, and two sides of the bottom of the U-shaped baffle plate are respectively and horizontally connected with a transverse plate;
a plurality of groups of first buffer plates are symmetrically arranged on two side walls of the U-shaped baffle plate, and the first buffer plates are inclined upwards by a certain angle;
the bottom of horizontal board is provided with a plurality of groups second buffer board, and the second buffer board inclines certain angle setting towards the recovery processing pipeline.
Preferably, the upper end both sides of exhaust-gas treatment jar are provided with the rotation main shaft respectively perpendicularly, and the lateral wall that rotates the main shaft is provided with the stirring wheel respectively, the outer wall that the roof that rotates the main shaft and run through the exhaust-gas treatment jar upwards extends the end has cup jointed first gear, and one side meshing of first gear is connected with the second gear, and the bottom of second gear is connected with the motor through the pivot.
Preferably, the inner wall of the rotating main shaft is provided with a cavity which is communicated up and down, the upper end of the rotating main shaft is inserted with a circulating pipeline, the bottom of one rotating main shaft extends to the inner bottom of the waste gas treatment tank, and a screw pump is arranged on a pipeline of the circulating pipeline.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the fixed bed continuous synthesis process with aniline as a raw material, a crude product is recovered by continuous distillation, unreacted aniline returns to a reaction system for recycling, and crude diphenylamine is distilled by a diphenylamine tower and a diphenylamine recovery tower to obtain diphenylamine;
2. the process for continuously synthesizing diphenylamine overcomes the defects of serious corrosion pollution, high energy consumption, high aniline unit consumption and the like of an intermittent method, greatly improves the labor environment, can realize continuous large-scale production, and is a novel process which is competitively developed by various countries at present;
3. in the invention, the by-product ammonia is removed from the reaction intermediate liquid under low pressure, and unreacted aniline and the generated by-product and diphenylamine are rectified and separated under the vacuum condition;
4. the waste gas treatment tank is arranged, so that the residual waste gas can be effectively absorbed and treated, and the waste gas is absorbed and filtered by the absorption tower and then is discharged at high altitude, so that the environment is not polluted, and the environment is more environment-friendly.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a schematic diagram of the system of the present invention;
FIG. 3 is a schematic view of the connection structure of a diphenylamine recovery column according to the invention;
FIG. 4 is a schematic view of the construction of an exhaust treatment canister according to the present invention;
in the figure: the device comprises a condensation reactor 1, a heat exchanger 101, a preheater 102, a gas-liquid separator 2, a deamination tower 3, an aniline front tower 4, a rectifying tower 5, an aniline tower 6, a light component tower 7, a diphenylamine tower 8, a diphenylamine recovery tower 9, a waste gas treatment tank 91, an absorption tower 92, a circulating pipeline 93, a screw pump 94, a rotating main shaft 95, a stirring wheel 96, a first gear 97, a second gear 98 and a motor 99;
the system comprises a reboiler 901, a diphenylamine storage tank 902, a condensation buffer tank 903, an ice maker 904, a compressor 905, a liquid ammonia tank 906, a recovery processing pipeline 907, a spray head 908, a U-shaped baffle 909, a transverse plate 910, a first buffer plate 911 and a second buffer plate 912.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all, embodiments of the present invention. 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
Referring to fig. 1, a process for producing diphenylamine by using an aniline continuous condensation method comprises the following steps:
s1, condensation reaction:
the aniline raw material is subjected to heat exchange and temperature rise with the condensation reaction discharge material through a heat exchanger, enters a preheater, and is further heated and heated to the reaction temperature by using heat conduction oil; the preheated aniline enters a condensation reactor, and the aniline is subjected to condensation reaction under the action of a catalyst to generate diphenylamine and ammonia;
the condensation reactor is a fixed bed reactor, the temperature is controlled at 340-;
s2, ammonia separation and purification:
the condensation reaction discharge material in the step S1 is sent into a gas-liquid separator after being subjected to heat exchange and temperature reduction with raw material aniline through a heat exchanger, the condensation reaction discharge material enters the gas-liquid separator to separate ammonia gas from a liquid phase, and a crude diphenylamine solution from which the ammonia gas is separated enters a deamination tower;
the deammoniation tower is vacuumized by a liquid ring vacuum pump and rectified under the pressure of-0.05 MPa to further remove a small amount of ammonia and water remained in the crude diphenylamine solution, and a water phase generated after the condensation of a material from the top of the deammoniation tower is used as wastewater to be sent to a sewage treatment station in a factory for pretreatment;
ammonia gas containing a small amount of organic matters separated from the top of the gas-liquid separator and the deamination tower is condensed and separated to obtain ammonia gas with higher content, and the ammonia gas is prepared into liquid ammonia by a liquid ammonia preparation system and is sent to a liquid ammonia tank area for storage;
s3, aniline separation:
the discharge of the deamination tower enters an aniline front tower, the aniline front tower is rectified under the pressure of-0.05 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump, and a distillate containing 2-methylpyridine and a small amount of aniline at the tower top enters a 2-methylpyridine rectifying tower after being condensed;
the bottom kettle liquid of the aniline front tower enters an aniline tower, the 2-picoline rectifying tower is rectified under normal pressure, and the bottom aniline kettle liquid of the 2-picoline rectifying tower also enters the aniline tower;
discharging materials from the bottoms of the aniline front tower and the 2-methylpyridine rectifying tower, feeding the materials into an aniline tower, and then rectifying the materials under the pressure of-0.08 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump, and condensing aniline discharged from the top of the tower and returning the aniline to a condensation reactor for reuse;
feeding the bottom discharge of the aniline tower into a light component tower, performing vacuum distillation by using a liquid ring vacuum pump under the pressure of-0.09 MPa, and respectively sending the alkyl aniline mixture discharged from the top of the light component tower to a solid waste incineration device for use after condensation and transfer in an intermediate tank;
s4, diphenylamine purification:
discharging the bottom of the light component tower into a diphenylamine tower, performing rectification under the pressure of-0.09 MPa by using a liquid ring vacuum pump for vacuumizing, and condensing diphenylamine discharged from the tower top and then conveying the diphenylamine to a diphenylamine storage tank in a tank area for storage; the discharged material at the bottom of the diphenylamine tower enters a diphenylamine recovery tower, the diphenylamine is further recovered by rectification under the pressure of-0.09 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump, the diphenylamine discharged from the tower top is sent to a diphenylamine storage tank in a tank area for storage after being condensed, and the residual alkyl diphenylamine mixture in the tower is treated as solid waste.
Referring to fig. 2-4, a system for producing diphenylamine by adopting an aniline continuous condensation method comprises a condensation reactor 1, a gas-liquid separator 2, a deamination tower 3, an aniline front tower 4, a rectification tower 5, an aniline tower 6, a light component tower 7, a diphenylamine tower 8 and a diphenylamine recovery tower 9, wherein the bottom of the condensation reactor 1 is connected with a heat exchanger 101 through a pipeline, the heat exchanger 101 is communicated with a preheater 102, and a discharge hole of the preheater 102 is connected with a feed inlet of the condensation reactor 1;
the heat exchanger 101, the gas-liquid separator 2, the deamination tower 3 and the aniline front tower 4 are sequentially connected through a pipeline, distillate containing 2-methylpyridine and a small amount of aniline at the tower top of the aniline front tower 4 enters the rectification tower 5 after being condensed, aniline kettle liquid at the tower bottoms of the aniline front tower 4 and the rectification tower 5 enters the aniline tower 6, the discharge of the aniline tower 6 enters the light component tower 7, the discharge of the tower bottom of the light component tower 7 enters the diphenylamine tower 8, and the discharge of the tower bottom of the diphenylamine tower 8 enters the diphenylamine recovery tower 9 for further rectification and recovery.
A reboiler 901 is arranged at the bottom of the diphenylamine recovery tower 9, diphenylamine discharged from the top of the diphenylamine recovery tower 9 is condensed and then sent to a diphenylamine storage tank 902 for storage, the byproduct ammonia gas of the diphenylamine recovery tower 9 is cooled and separated through a condensation buffer tank 903, and the ammonia gas is compressed and condensed through an ice maker 904 to become liquid ammonia gas, and then sent to a liquid ammonia tank 906 for storage;
a pipeline between the condensation buffer tank 903 and the ice maker 904 is communicated with a recovery processing pipeline 907, one end of the recovery processing pipeline 907 is connected with the waste gas treatment tank 91, the middle of the top of the waste gas treatment tank 91 is communicated with an absorption tower 92, a plurality of layers of adsorption fillers are arranged in the absorption tower 92, and the adsorption fillers are activated carbon which can effectively adsorb impurities in the waste gas;
the recovery processing pipeline 907 penetrates through the bottom of the waste gas treatment tank 91 and is provided with a spray head 908 at the inward extending end, a U-shaped baffle plate 909 is arranged on the inner wall of the waste gas treatment tank 91 and positioned outside the spray head 908, the opening of the U-shaped baffle plate 909 is arranged downwards, and two sides of the bottom are respectively and horizontally connected with a transverse plate 910;
a plurality of groups of first buffer plates 911 are symmetrically arranged on two side walls of the U-shaped baffle 909, and the first buffer plates 911 are arranged by inclining upwards by 30-60 degrees; the bottom of the transverse plate 910 is provided with a plurality of groups of second buffer plates 912, and the second buffer plates 912 are inclined towards the recovery processing pipeline 907 by 30-60 degrees, so that the retention time of waste gas in water can be effectively prolonged, and the ammonia gas processing effect is further improved;
under the combined action of the first buffer plate 911 and the second buffer plate 912, the flow velocity of water is reduced, so that the absorption time of water on ammonia gas is effectively prolonged, and the effect of waste gas treatment is improved;
two sides of the upper end of the waste gas treatment tank 91 are respectively and vertically provided with a rotating main shaft 95, the side walls of the rotating main shafts 95 are respectively provided with a stirring wheel 96, the rotating main shafts 95 penetrate through the outer wall of the upward extending end of the top wall of the waste gas treatment tank 91 and are sleeved with a first gear 97, one side of the first gear 97 is meshed and connected with a second gear 98, and the bottom of the second gear 98 is connected with a motor 99 through a rotating shaft;
the motor 99 drives the second gear 98 to rotate through the rotating shaft, and the second gear 98 drives the first gear 97 to rotate, so that the rotating main shaft 95 and the stirring wheel 96 are driven to rotate, the liquid in the waste gas treatment tank 91 is mixed and stirred, and the absorption and dissolution of waste gas are accelerated;
the inner wall of the rotating main shaft 95 is provided with a cavity which is communicated up and down, the upper end of the rotating main shaft 95 is inserted with a circulating pipeline 93, the bottom of one rotating main shaft 95 extends to the inner bottom of the waste gas treatment tank 91, a screw pump 94 is arranged on the pipeline of the circulating pipeline 93, the screw pump 94 adopts a 3G three-screw pump, is a screw type displacement pump, mainly utilizes the principle of screw meshing, depends on the mutual meshing of the rotating screws in a pump sleeve, seals the conveyed medium in the meshing cavity, and continuously pushes the medium to a discharge port at a constant speed along the axial direction of the screws, so as to provide stable pressure for the system; selecting a 3G three-screw pump of 100 multiplied by 2-46 model number of Beijing eight-side pump industry machinery Limited liability company;
under the action of the screw pump 94, the absorption liquid enters the circulating pipeline 93 through a cavity in the rotating main shaft 95 and then enters the waste gas treatment tank 91 through a cavity in the other rotating main shaft 95 in a circulating manner, and the absorption liquid is filtered by the filter element arranged on the pipeline of the circulating pipeline 93, so that the absorption effect of the absorption liquid is improved, and the waste gas treatment capacity is further improved;
diphenylamine from the top of the diphenylamine recovery tower 9 is condensed and then sent to a diphenylamine storage tank 902 for storage, and the remaining alkyl diphenylamine mixture in the tower is treated as solid waste; the by-product ammonia gas of the diphenylamine recovery tower 9 contains partial impurities, is filtered by a filter screen in the condensation buffer tank 903 and then is cooled and separated to obtain ammonia gas with higher gaseous content, and then the ammonia gas is changed into liquid ammonia gas after passing through the ice maker 904, and is compressed and condensed by the compressor 905 and then is sent to the liquid ammonia tank 906 for storage. A small amount of unabsorbed ammonia waste gas is sent into the waste gas treatment tank 91 through a recovery treatment pipeline 907 for absorption treatment; at this time, the residual exhaust gas enters the exhaust gas treatment tank 91 under the action of the air pump on the pipeline of the recovery treatment pipeline 907, and is sprayed out to the exhaust gas treatment tank 91 through the spray head 908, at this time, water with a certain liquid level is injected into the exhaust gas treatment tank 91, the tail gas generated after further treatment is absorbed and filtered by the absorption tower 92 and then is discharged in high altitude, and the absorption liquid generated in the exhaust gas treatment tank 91 is periodically sent to the water absorption tank for use without being discharged outside.
Diphenylamine material balance table
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
In the present invention, unless otherwise expressly stated or limited, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; they may be mechanically coupled, directly coupled, or indirectly coupled through intervening agents, both internally and/or in any other manner known to those skilled in the art. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The control mode of the invention is automatically controlled by the controller, the control circuit of the controller can be realized by simple programming of a person skilled in the art, the supply of the power supply also belongs to the common knowledge in the field, and the invention is mainly used for protecting mechanical devices, so the control mode and the circuit connection are not explained in detail in the invention.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A process for producing diphenylamine by adopting an aniline continuous condensation method is characterized by comprising the following steps of:
s1, condensation reaction:
the aniline raw material is subjected to heat exchange and temperature rise with the condensation reaction discharge material through a heat exchanger, enters a preheater, and is further heated and heated to the reaction temperature by using heat conduction oil; the preheated aniline enters a condensation reactor, and the aniline is subjected to condensation reaction under the action of a catalyst to generate diphenylamine and ammonia;
s2, ammonia separation and purification:
the condensation reaction discharge material in the step S1 is sent into a gas-liquid separator after being subjected to heat exchange and temperature reduction with raw material aniline through a heat exchanger, the condensation reaction discharge material enters the gas-liquid separator to separate ammonia gas from a liquid phase, and a crude diphenylamine solution from which the ammonia gas is separated enters a deamination tower;
s3, aniline separation:
the discharge of the deamination tower enters an aniline front tower, the aniline front tower is rectified under the pressure of-0.05 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump, and a distillate containing 2-methylpyridine and a small amount of aniline at the tower top enters a 2-methylpyridine rectifying tower after being condensed;
the bottom kettle liquid of the aniline front tower enters an aniline tower, the 2-picoline rectifying tower is rectified under normal pressure, and the bottom aniline kettle liquid of the 2-picoline rectifying tower also enters the aniline tower;
feeding the bottom discharge of the aniline tower into a light component tower, performing vacuum distillation by using a liquid ring vacuum pump under the pressure of-0.09 MPa, and respectively sending the alkyl aniline mixture discharged from the top of the light component tower to a solid waste incineration device for use after condensation and transfer in an intermediate tank;
s4, diphenylamine purification:
discharging the bottom of the light component tower into a diphenylamine tower, performing rectification under the pressure of-0.09 MPa by using a liquid ring vacuum pump for vacuumizing, and condensing diphenylamine discharged from the tower top and then conveying the diphenylamine to a diphenylamine storage tank in a tank area for storage; the discharge at the bottom of the diphenylamine tower enters a diphenylamine recovery tower, and the diphenylamine is further recovered by rectification under the pressure of-0.09 MPa by utilizing the vacuum pumping of a liquid ring vacuum pump.
2. The process for producing diphenylamine by using the continuous condensation method of aniline as claimed in claim 1, wherein the condensation reactor in the step S1 is a fixed bed reactor, the temperature is controlled at 340-360 ℃, and the pressure is controlled at 2.0 MPa.
3. The process for producing diphenylamine by the continuous condensation method of aniline according to claim 1, wherein the deamination tower in step S2 is further refined under a pressure of-0.05 MPa by using a liquid ring vacuum pump for evacuation in a liquid ring vacuum pump, a small amount of residual ammonia and water in the crude diphenylamine solution are further removed, and a water phase produced by condensation of a material from the top of the deamination tower is sent to a sewage treatment station in a factory for pretreatment.
4. The process for producing diphenylamine by using the continuous condensation method of aniline as claimed in claim 1, wherein in step S3, after the bottoms of the aniline front tower and the 2-methylpyridine rectification tower enter the aniline tower, the aniline is rectified under the pressure of-0.08 MPa by using the vacuum pumping of a liquid ring vacuum pump, and the aniline coming out of the tower top is condensed and then returned to the condensation reactor for reuse.
5. A system for producing diphenylamine by adopting an aniline continuous condensation method, which adopts the process for producing diphenylamine by adopting an aniline continuous condensation method according to any one of claims 1 to 4, and is characterized by comprising a condensation reactor (1), a gas-liquid separator (2), a deamination tower (3), an aniline front tower (4), a rectification tower (5), an aniline tower (6), a light component tower (7), a diphenylamine tower (8) and a diphenylamine recovery tower (9), wherein the bottom of the condensation reactor (1) is connected with a heat exchanger (101) through a pipeline, the heat exchanger (101) is communicated with a preheater (102), and a discharge hole of the preheater (102) is connected with a feed inlet of the condensation reactor (1);
the heat exchanger (101), vapour and liquid separator (2), deaminizing tower (3), preceding tower (4) of aniline connect gradually through the pipeline, the distillate that tower (4) top of the tower contained 2-methylpyridine, a small amount of aniline gets into rectifying column (5) after the condensation before the aniline, aniline tower bottom aniline kettle liquid gets into aniline tower (6) before tower (4) and rectifying column (5) of the aniline tower bottom, and the ejection of compact of aniline tower (6) gets into light component tower (7), and the ejection of compact of the light component tower (7) tower bottom gets into diphenylamine tower (8), and the ejection of compact of the diphenylamine tower bottom gets into diphenylamine recovery tower (9) and further retrieves.
6. The system for producing diphenylamine by adopting the aniline continuous condensation method according to claim 5, wherein a reboiler (901) is arranged at the bottom of the diphenylamine recovery tower (9), diphenylamine discharged from the top of the diphenylamine recovery tower (9) is condensed and then sent to a diphenylamine storage tank (902) for storage, ammonia gas by-produced by the diphenylamine recovery tower (9) is cooled and separated through a condensation buffer tank (903), and the ammonia gas is changed into liquid ammonia gas through an ice maker (904), then compressed and condensed through a compressor (905), and then sent to a liquid ammonia tank (906) for storage;
and a pipeline between the condensation buffer tank (903) and the ice maker (904) is communicated with a recovery processing pipeline (907), and one end of the recovery processing pipeline (907) is connected with an exhaust gas processing tank (91).
7. The system for producing diphenylamine by using the continuous condensation method of aniline according to claim 6, wherein the middle of the top of the waste gas treatment tank (91) is communicated with an absorption tower (92), a plurality of layers of adsorption packing are arranged in the absorption tower (92), and the inward extending end of the recovery treatment pipeline (907) penetrating through the bottom of the waste gas treatment tank (91) is provided with a spray head (908).
8. The system for producing diphenylamine by using the continuous condensation method of aniline according to claim 6, wherein a U-shaped baffle plate (909) is arranged on the inner wall of the waste gas treatment tank (91) and outside the spray head (908), the U-shaped baffle plate (909) is downward opened, and two sides of the bottom of the U-shaped baffle plate are horizontally connected with transverse plates (910) respectively;
a plurality of groups of first buffer plates (911) are symmetrically arranged on two side walls of the U-shaped baffle plate (909), and the first buffer plates (911) are arranged in an upward inclined mode at a certain angle;
the bottom of the transverse plate (910) is provided with a plurality of groups of second buffer plates (912), and the second buffer plates (912) are inclined at a certain angle towards the recovery processing pipeline (907).
9. The system for producing diphenylamine by using the aniline continuous condensation method according to claim 5, wherein two sides of the upper end of the waste gas treatment tank (91) are respectively and vertically provided with a rotating main shaft (95), the side walls of the rotating main shafts (95) are respectively provided with a stirring wheel (96), the rotating main shafts (95) penetrate through the outer wall of the upward extending end of the top wall of the waste gas treatment tank (91) and are sleeved with first gears (97), one side of the first gears (97) is engaged with second gears (98), and the bottoms of the second gears (98) are connected with a motor (99) through rotating shafts.
10. The system for producing diphenylamine by using the continuous condensation method of aniline according to claim 9, wherein a cavity is formed in the inner wall of the rotating main shaft (95) and is communicated with the cavity up and down, a circulating pipeline (93) is inserted into the upper end of the rotating main shaft (95), the bottom of one rotating main shaft (95) extends towards the inner bottom of the waste gas treatment tank (91), and a screw pump (94) is installed on the pipeline of the circulating pipeline (93).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2692149Y (en) * | 2004-04-08 | 2005-04-13 | 曹宏生 | Diphenyl amine prodcuction and ammonia recorery device |
| CN1629132A (en) * | 2004-09-03 | 2005-06-22 | 南京工业大学 | Method for preparing diphenylamine by aniline liquid phase condensation and denitrification coupling |
| CN104478738A (en) * | 2014-11-19 | 2015-04-01 | 南通新邦化工科技有限公司 | Reaction method for continuously synthesizing diphenylamine from aniline |
| CN217774097U (en) * | 2022-05-16 | 2022-11-11 | 杰超橡塑南通有限公司 | Production system for continuously synthesizing diphenylamine by using aniline as raw material |
-
2022
- 2022-05-16 CN CN202210526011.8A patent/CN114805086A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2692149Y (en) * | 2004-04-08 | 2005-04-13 | 曹宏生 | Diphenyl amine prodcuction and ammonia recorery device |
| CN1629132A (en) * | 2004-09-03 | 2005-06-22 | 南京工业大学 | Method for preparing diphenylamine by aniline liquid phase condensation and denitrification coupling |
| CN104478738A (en) * | 2014-11-19 | 2015-04-01 | 南通新邦化工科技有限公司 | Reaction method for continuously synthesizing diphenylamine from aniline |
| CN217774097U (en) * | 2022-05-16 | 2022-11-11 | 杰超橡塑南通有限公司 | Production system for continuously synthesizing diphenylamine by using aniline as raw material |
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