CN112337409B - Production system of hexamethylenediamine - Google Patents
Production system of hexamethylenediamine Download PDFInfo
- Publication number
- CN112337409B CN112337409B CN202011338623.1A CN202011338623A CN112337409B CN 112337409 B CN112337409 B CN 112337409B CN 202011338623 A CN202011338623 A CN 202011338623A CN 112337409 B CN112337409 B CN 112337409B
- Authority
- CN
- China
- Prior art keywords
- hydrogenation reactor
- gas
- heat exchange
- hydrogenation
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 120
- 239000007788 liquid Substances 0.000 claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001257 hydrogen Substances 0.000 claims abstract description 32
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000007791 liquid phase Substances 0.000 claims abstract description 21
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012071 phase Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011229 interlayer Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 6
- 230000005587 bubbling Effects 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 20
- 239000003054 catalyst Substances 0.000 abstract description 13
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- -1 hydrogenation ware Chemical compound 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910000564 Raney nickel Inorganic materials 0.000 description 4
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000003889 chemical engineering Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009469 supplementation Effects 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910020637 Co-Cu Inorganic materials 0.000 description 1
- 101100425816 Dictyostelium discoideum top2mt gene Proteins 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- RYTYSMSQNNBZDP-UHFFFAOYSA-N cobalt copper Chemical compound [Co].[Cu] RYTYSMSQNNBZDP-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011796 hollow space material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 101150082896 topA gene Proteins 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
- B01J8/0278—Feeding reactive fluids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/44—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers
- C07C209/48—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of nitriles
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a production system of hexamethylenediamine, including hydrogenation ware, the gas-liquid separator, hydrogenation ware's quantity is two at least, hydrogenation ware is gas-liquid-solid three-phase fixed bed reactor, each hydrogenation ware's lateral wall is equipped with the heat transfer intermediate layer respectively, the sky is equipped with heat exchange coil respectively, each hydrogenation ware's top links to each other with adiponitrile source through first inlet pipe respectively, set up first valve respectively on each first inlet pipe, the bottom links to each other with the hydrogen source through the second inlet pipe respectively, set up the second valve respectively on each second inlet pipe, the lateral wall that is located high-order hydrogenation ware links to each other with the liquid phase material source through the third inlet pipe, and link to each other with the lateral wall that is located low-order hydrogenation ware through the overflow pipe, gas-liquid separator sets up at the top that corresponds hydrogenation ware. The invention has simple structure and convenient operation, can effectively reduce the mechanical loss of the catalyst, is convenient for enterprises to control the reaction temperature, and is beneficial to producing high-quality hexamethylenediamine products.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a production system of hexamethylenediamine.
Background
Chemical enterprises often utilize adiponitrile and hydrogen as raw materials to synthesize hexamethylenediamine in a curing bed reactor.
The existing production method of hexamethylenediamine mainly comprises the steps of carrying out reaction on adiponitrile hydrogenation in the presence of a skeletal nickel catalyst, wherein the reaction comprises a high-pressure method and a low-pressure method:
the high-pressure method adopts a cobalt-copper catalyst, the reaction temperature is 100-135 ℃ and the pressure is 60MPa, the reaction is carried out in a three-phase fluidized bed reactor, the solvent adopts liquid ammonia, and the equation is as follows:
NC(CH 2 ) 4 CN+4H 2 →Co-Cu H 2 N(CH 2 ) 6 NH 2
the selectivity of hexamethylenediamine is about 90-95%.
The low pressure process adopts adiponitrile and hydrogen as material, skeleton nickel as catalyst, sodium hydroxide solution as promoter, ethanol as diluent, and at 73-79 deg.c and pressure of about 2.2MPa, hexamethylenediamine is produced
NC(CH 2 ) 4 CN+4H 2 →Ni H 2 N(CH 2 ) 6 NH 2
The conversion of hexamethylenediamine is close to 100%.
The reaction condition for synthesizing hexamethylenediamine by a low-pressure method is mild, and the conversion rate is high, so that the hexamethylenediamine is generally adopted by chemical enterprises. However, in the currently used reactor, the catalyst installed in the reactor is damaged to generate floating problems due to mechanical loss, and the heat generated by the reaction is not easy to discharge, so that the reactor is unfavorable for enterprises to control the reaction temperature, and the requirement of producing high-quality hexamethylenediamine is difficult to meet.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a production system of hexamethylenediamine, which has the advantages of simple structure, convenient operation, capability of effectively reducing the mechanical loss of a catalyst, convenience for enterprises to control the reaction temperature and contribution to producing high-quality hexamethylenediamine products.
The technical scheme of the invention is as follows: the utility model provides a production system of hexamethylenediamine, including hydrogenation ware, gas-liquid separator, hydrogenation ware, gas-liquid separator's quantity is the same, and gas-liquid separator, hydrogenation ware's quantity is two at least, hydrogenation ware is gas-liquid-solid three-phase fixed bed reactor, each hydrogenation ware's lateral wall is equipped with the heat transfer intermediate layer respectively, each hydrogenation ware's sky is equipped with heat exchange coil respectively, each hydrogenation ware's top links to each other with adiponitrile source through first inlet pipe respectively, set up first valve on each first inlet pipe respectively, each hydrogenation ware's bottom links to each other with the hydrogen source through the second inlet pipe respectively, set up the second valve on each second inlet pipe respectively, hydrogenation ware's lateral wall that is located the high position links to each other with the liquid phase material source through the overflow pipe with hydrogenation ware's that is located the low position lateral wall that is located, utilize liquid level difference to overflow liquid phase material to the hydrogenation ware of low position, the lateral wall that is located the hydrogenation ware sets up the overflow mouth, form the material export, gas-liquid separator sets up at the top that corresponds hydrogenation ware, is used for with unreacted hydrogen that will separate.
And the heat exchange medium inlets of the heat exchange interlayer and the heat exchange coil are connected in parallel and are connected with the outlet of the medium circulating pump, and the heat exchange medium outlets of the heat exchange interlayer and the heat exchange coil are connected in parallel and are connected with the inlet of the medium circulating pump through the heat exchanger.
The downstream end of the first feeding pipe is positioned at the top of the hollow space of the hydrogenation reactor, a plurality of feeding ports are arranged, and the feeding ports are uniformly distributed along the circumference of the hydrogenation reactor.
The number of the feed inlets is three or four.
And a gas phase outlet of the gas-liquid separator supplies gas to a hydrogen source through a dealcoholization device and a compressor.
The shell of the hydrogenation reactor is formed by connecting an upper cylindrical section and a lower inverted conical section, and the second feeding pipe is connected with the lower part of the inverted conical section.
The technical scheme has the following beneficial effects:
1. the production system of hexamethylenediamine comprises a hydrogenation reactor and gas-liquid separators, wherein the number of the hydrogenation reactor and the number of the gas-liquid separators are the same, and the number of the gas-liquid separators and the number of the hydrogenation reactor are at least two, the hydrogenation reactor is used for synthesizing hexamethylenediamine, the gas-liquid separators are used for separating unreacted hydrogen and liquid-phase materials, the liquid-phase materials are trapped in the hydrogenation reactor, and the gas-phase materials are discharged and reused as gas-phase raw materials after dealcoholization and pressurization. The hydrogenation reactor is a gas-liquid-solid three-phase fixed bed reactor, and obviously a nickel catalyst is arranged. The side walls of the hydrogenation reactors are respectively provided with a heat exchange interlayer, and the inner spaces of the hydrogenation reactors are respectively provided with a heat exchange coil for fully exchanging heat with the hydrogenation reactors, so that enterprises can conveniently adjust the reaction temperature in the hydrogenation reactors, and the quality of the hexamethylenediamine obtained by synthesis can be controlled. The top of each hydrogenation reactor is connected with an adiponitrile source through a first feeding pipe, first valves are respectively arranged on each first feeding pipe, and the adiponitrile addition of each hydrogenation reactor can be controlled by controlling the opening of each first valve. The bottom of each hydrogenation reactor is connected with a hydrogen source through a second feeding pipe, a second valve is respectively arranged on each second feeding pipe, the hydrogen adding amount of each hydrogenation reactor can be controlled by controlling the opening of each second valve, and hydrogen enters from the bottom of the hydrogenation reactor in a bubbling mode and can be fully adsorbed by a catalyst in the hydrogenation reactor to fully contact with liquid phase materials for reaction, so that the utilization rate and the reaction efficiency of the catalyst are ensured, upward acting force is provided for the catalyst, and the catalyst is prevented from settling. The side wall of the hydrogenation reactor positioned at the high position is connected with a liquid phase material source through a third feeding pipe and is a mixed liquid of ethanol solution and sodium hydroxide. The side wall of the hydrogenation reactor at the high position is connected with the side wall of the hydrogenation reactor at the low position through an overflow pipe, liquid phase materials overflow to the hydrogenation reactor at the low position by utilizing liquid level difference, namely, the hydrogenation reactor at the high position firstly carries out the reaction of adiponitrile and hydrogen to synthesize a liquid phase material containing hexamethylenediamine, the liquid phase material containing hexamethylenediamine enters the hydrogenation reactor at the low position through overflow, unreacted adiponitrile further reacts with the hydrogen added by bubbling, and the adiponitrile adding amount of the hydrogenation reactor at the low position is adjusted by adjusting a first valve at the top of the hydrogenation reactor at the low position, so that the utilization rate of adiponitrile can be effectively improved, and the energy consumption of the reaction is effectively reduced. The side wall of the hydrogenation reactor at the low position is provided with an overflow port to form a material outlet, and finally the reacted liquid phase material is discharged through the overflow port for further processing. The gas-liquid separator is arranged at the top of the corresponding hydrogenation reactor and is used for separating out unreacted hydrogen, and liquid-phase materials are reserved in the hydrogenation reactor, so that the separated hydrogen can be used for recycling.
2. The downstream end of first inlet pipe is located the hollow top of hydrogenation ware, sets up a plurality of feed inlets, and a plurality of feed inlets are along hydrogenation ware's circumference evenly distributed, and the adiponitrile flow of single feed inlet is little, can effectively reduce the velocity of flow of liquid phase, effectively reduces the too big catalyst mechanical loss that leads to because of the impact force of catalyst, and these feed inlets evenly distributed, still can accelerate liquid phase material intensive mixing, guarantee simultaneously that the reaction is even in the hydrogenation ware, the heat production is even, makes the heat can be shifted out in time.
3. The shell of the hydrogenation reactor is formed by connecting the cylinder section at the upper part and the inverted cone section at the lower part, and the second feeding pipe is connected with the lower part of the inverted cone section, so that the added hydrogen can be effectively ensured to be uniformly distributed in the inner space of the hydrogenation reactor, and the reaction in the inner space of the reactor can be ensured to be uniformly carried out.
Further description is provided below with reference to the drawings and detailed description.
Drawings
FIG. 1 is a schematic diagram of the connection of the present invention.
In the drawing, 1 is a hydrogenation reactor, 1a is a cylindrical section, 1b is an inverted conical section, 2 is a gas-liquid separator, 3 is a heat exchange interlayer, 4 is a heat exchange coil, 5 is an overflow pipe, 6 is a medium circulating pump, 7 is a heat exchanger, 11 is a first feeding pipe, 12 is a second feeding pipe, 13 is a third feeding pipe, a is a first valve, and b is a second valve.
Detailed Description
In the invention, devices and equipment with specific structures are not marked, devices or equipment with general chemical engineering fields are generally adopted, and specific installation and connection modes are not marked, and are generally installed and connected in the chemical engineering fields or according to the guidance of manufacturers.
Example 1
Referring to fig. 1, the hexamethylenediamine production system comprises a hydrogenation reactor 1 and a gas-liquid separator 2, wherein the number of the hydrogenation reactor 1 and the number of the gas-liquid separator 2 are the same, and the number of the gas-liquid separator 2 and the number of the hydrogenation reactor 1 are at least two. The hydrogenation reactors 1 are gas-liquid-solid three-phase fixed bed reactors, specifically, the shell of each hydrogenation reactor is formed by connecting an upper cylindrical section 1a and a lower inverted conical section 1b to form a whole, and specifically, the top of each cylindrical section is a curved surface part protruding upwards. The side walls of each hydrogenation reactor 1 are respectively provided with a heat exchange interlayer 3, the inner space of each hydrogenation reactor 1 is respectively provided with a heat exchange coil 4, in the embodiment, the heat exchange interlayer 3 and the heat exchange medium inlet of the heat exchange coil 4 are connected in parallel and are connected with the outlet of the medium circulating pump 6, and the heat exchange interlayer 3 and the heat exchange medium outlet of the heat exchange coil 4 are connected in parallel and are connected with the inlet of the medium circulating pump 6 through the heat exchanger 7. The top of each hydrogenation reactor 1 is connected with an adiponitrile source through a first feeding pipe 11, a first valve a is respectively arranged on each first feeding pipe 11, in this embodiment, the downstream end of each first feeding pipe 11 is located at the hollow top of the hydrogenation reactor 1, a plurality of feeding ports are arranged, the feeding ports are uniformly distributed along the circumference of the hydrogenation reactor 1, and preferably, the number of the feeding ports is three or four. The bottom of each hydrogenation reactor 1 is connected to a hydrogen source through a second feed pipe 12, and a second valve b is disposed on each second feed pipe 12, and in this embodiment, the second feed pipe 12 is connected to the lower portion of the inverted conical section 1 b. The left side wall of the first hydrogenation reactor is connected with a liquid phase material source through a third feeding pipe 13, the liquid phase material source is ethanol solution mixed sodium hydroxide, the right side wall of the first hydrogenation reactor is connected with the left side wall of the second hydrogenation reactor through an overflow pipe 5, the right side wall of the second hydrogenation reactor is connected with the left side wall of the third hydrogenation reactor through an overflow pipe, an overflow port is formed in the right side wall of the third hydrogenation reactor, a material outlet is formed, obviously, the two overflow pipes are all obliquely extended, and the liquid phase material overflows to the low-order hydrogenation reactor by utilizing the liquid level difference. The gas-liquid separator 2 is arranged at the top of the corresponding hydrogenation reactor 1 and is used for separating out unreacted hydrogen, and specifically, a gas phase outlet of the gas-liquid separator 2 supplies gas to a hydrogen source through a dealcoholization device and a compressor.
Example two
The Raney nickel catalyst charged into each hydrogenation reactor had an average particle size of 40. Mu.m. The prepared ethanol solution and sodium hydroxide mixed solution sequentially flow through three hydrogenation reactors connected in series, and the temperature of each hydrogenation reactor is controlled at 73, 75 and 77 ℃ respectively. The adiponitrile is added into a first hydrogenation reactor, a second hydrogenation reactor and a third hydrogenation reactor from the top, and the total addition amount is controlled to be about 4.5m 3 And/h. And after the mixed liquid enters the first hydrogenation reactor, the mixed liquid overflows to the second hydrogenation reactor and the third hydrogenation reactor in sequence by utilizing the liquid level difference. The adiponitrile reacts with hydrogen gas to form an exothermic reaction, and closed circulation heat exchange is performed by using a heat exchange interlayer, a heat exchange coil, a medium circulation pump and a heat exchanger. The recycle hydrogen from each hydrogenation reactor was bubbled through the bottom of the reactor, with the hydrogen addition from each hydrogenation reactor being about 1300Nm 3 And/h, after the added hydrogen is adsorbed by the catalyst and fully contacted and reacted with the liquid phase material, the excessive part is separated by a gas-liquid separator and then discharged from the top of the hydrogenation reactor. The discharged circulating hydrogen is recycled to the bottom of each hydrogenation reactor after dealcoholization, compressor compression and fresh hydrogen supplementation.
The experiment of the applicant proves that the unit consumption of the Raney nickel catalyst used for producing each ton of products can be reduced by about 20 percent.
Example III
The Raney nickel catalyst charged into each hydrogenation reactor had an average particle size of 60. Mu.m. The prepared ethanol solution and sodium hydroxide mixed solution sequentially flow through three hydrogenation reactors connected in series, and the temperature of each hydrogenation reactor is controlled at 74, 76 and 78 ℃ respectively. Addition of adiponitrile from the topA hydrogenation reactor, a second hydrogenation reactor and a third hydrogenation reactor, the total addition amount is controlled to be about 6m 3 And/h. And after the mixed liquid enters the first hydrogenation reactor, the mixed liquid overflows to the second hydrogenation reactor and the third hydrogenation reactor in sequence by utilizing the liquid level difference. The adiponitrile reacts with hydrogen gas to form an exothermic reaction, and closed circulation heat exchange is performed by using a heat exchange interlayer, a heat exchange coil, a medium circulation pump and a heat exchanger. The recycle hydrogen from each hydrogenation reactor was bubbled through the bottom of the reactor, with the hydrogen addition to each hydrogenation reactor being about 1700Nm 3 And/h, after the added hydrogen is adsorbed by the catalyst and fully contacted and reacted with the liquid phase material, the excessive part is separated by a gas-liquid separator and then discharged from the top of the hydrogenation reactor. The discharged circulating hydrogen is recycled to the bottom of each reactor after dealcoholization, compressor compression and fresh hydrogen supplementation.
The experiment of the applicant proves that the unit consumption of the Raney nickel catalyst used for producing each ton of products can be reduced by about 20 percent.
Claims (4)
1. A hexamethylenediamine production system, characterized in that: comprises a hydrogenation reactor (1) and a gas-liquid separator (2), wherein the number of the hydrogenation reactor (1) and the number of the gas-liquid separator (2) are the same, the number of the gas-liquid separator (2) and the number of the hydrogenation reactor (1) are at least two,
the hydrogenation reactor (1) is a gas-liquid-solid three-phase fixed bed reactor, the shell of the hydrogenation reactor (1) is formed by connecting an upper cylindrical section (1 a) and a lower inverted conical section (1 b), the side wall of each hydrogenation reactor (1) is respectively provided with a heat exchange interlayer (3), the inner space of each hydrogenation reactor (1) is respectively provided with a heat exchange coil (4),
the top of each hydrogenation reactor (1) is connected with an adiponitrile source through a first feed pipe (11), a first valve (a) is respectively arranged on each first feed pipe (11), the downstream end of each first feed pipe (11) is positioned at the hollow top of the hydrogenation reactor (1), a plurality of feed inlets are arranged, the feed inlets are uniformly distributed along the circumference of the hydrogenation reactor (1),
the bottom of each hydrogenation reactor (1) is connected with a hydrogen source through a second feeding pipe (12), a second valve (b) is respectively arranged on each second feeding pipe (12), the second feeding pipe (12) is connected with the lower part of the inverted conical section (1 b), hydrogen enters from the bottom of the hydrogenation reactor in a bubbling mode,
the side wall of the hydrogenation reactor positioned at the high position is connected with a liquid phase material source through a third feeding pipe (13) and is a mixed liquid of ethanol solution and sodium hydroxide, the side wall of the hydrogenation reactor positioned at the high position is connected with the side wall of the hydrogenation reactor positioned at the low position through an overflow pipe (5), the liquid phase material overflows to the hydrogenation reactor positioned at the low position by utilizing the liquid level difference, the side wall of the hydrogenation reactor positioned at the low position is provided with an overflow port to form a material outlet,
the gas-liquid separator (2) is arranged at the top of the corresponding hydrogenation reactor (1) and is used for separating out unreacted hydrogen.
2. The hexamethylenediamine production system according to claim 1, wherein: the heat exchange medium inlets of the heat exchange interlayer (3) and the heat exchange coil (4) are connected in parallel and connected with the outlet of the medium circulating pump (6), and the heat exchange medium outlets of the heat exchange interlayer (3) and the heat exchange coil (4) are connected in parallel and connected with the inlet of the medium circulating pump (6) through the heat exchanger (7).
3. The hexamethylenediamine production system according to claim 1, wherein: the number of the feed inlets is three or four.
4. The hexamethylenediamine production system according to claim 1, wherein: and a gas phase outlet of the gas-liquid separator (2) supplies gas to a hydrogen source through a dealcoholization device and a compressor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011338623.1A CN112337409B (en) | 2020-11-25 | 2020-11-25 | Production system of hexamethylenediamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011338623.1A CN112337409B (en) | 2020-11-25 | 2020-11-25 | Production system of hexamethylenediamine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112337409A CN112337409A (en) | 2021-02-09 |
| CN112337409B true CN112337409B (en) | 2024-02-06 |
Family
ID=74365684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011338623.1A Active CN112337409B (en) | 2020-11-25 | 2020-11-25 | Production system of hexamethylenediamine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112337409B (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337894A (en) * | 2008-08-08 | 2009-01-07 | 德纳（南京）化工有限公司 | Process for preparation of meta-benzene dimethanamine by continuous hydrogenation reaction in stirring vessel |
| CN101890323A (en) * | 2009-05-22 | 2010-11-24 | 山西侨友化工股份有限公司 | Reactor for preparing succinyl oxide by maleic anhydride hydrogenation |
| CN102211002A (en) * | 2010-04-12 | 2011-10-12 | 中科合成油技术有限公司 | Hot oil circulating and cold quenching fixed bed Fischer-Tropsch synthesis reactor and application thereof |
| CN202506390U (en) * | 2012-03-29 | 2012-10-31 | 中国天辰工程有限公司 | Reactor for producing hexanediamine through adiponitrile hydrogenation |
| WO2014099610A1 (en) * | 2012-12-18 | 2014-06-26 | Invista Technologies S.À R.L. | Integrated process for diamine production |
| WO2016040661A1 (en) * | 2014-09-12 | 2016-03-17 | Invista North America S.A R.L. | Catalyst handling method and hydrogenation process |
| CN105555752A (en) * | 2013-09-13 | 2016-05-04 | 因温斯特技术公司 | Hydrogenation of dinitriles for the preparation of diamines |
| CN105582854A (en) * | 2014-10-21 | 2016-05-18 | 中国石油化工股份有限公司 | Fixed bed hydrogenation reactor and application method thereof |
| CN106810455A (en) * | 2016-12-27 | 2017-06-09 | 河南神马尼龙化工有限责任公司 | A kind of production method of high-quality essence hexamethylene diamine |
| CN108084035A (en) * | 2017-12-11 | 2018-05-29 | 大连理工大学 | A kind of method of adiponitrile direct hydrogenation preparing hexanediamine under the conditions of alkali-free |
| CN108654522A (en) * | 2018-06-08 | 2018-10-16 | 南京敦先化工科技有限公司 | A kind of coil jacket formula axial flow reactor |
| CN210434480U (en) * | 2019-07-07 | 2020-05-01 | 宿迁项王机械设备有限公司 | High-efficient hydrogenation unit of production hexamethylene diamine piperidine |
| CN111686645A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Micro-interface reinforced wax oil hydrogenation reaction system and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2921922B1 (en) * | 2007-10-04 | 2009-12-04 | Rhodia Operations | PROCESS FOR THE PRODUCTION OF AMINES BY HYDROGENATION OF NITRILIC COMPOUNDS |
-
2020
- 2020-11-25 CN CN202011338623.1A patent/CN112337409B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337894A (en) * | 2008-08-08 | 2009-01-07 | 德纳（南京）化工有限公司 | Process for preparation of meta-benzene dimethanamine by continuous hydrogenation reaction in stirring vessel |
| CN101890323A (en) * | 2009-05-22 | 2010-11-24 | 山西侨友化工股份有限公司 | Reactor for preparing succinyl oxide by maleic anhydride hydrogenation |
| CN102211002A (en) * | 2010-04-12 | 2011-10-12 | 中科合成油技术有限公司 | Hot oil circulating and cold quenching fixed bed Fischer-Tropsch synthesis reactor and application thereof |
| CN202506390U (en) * | 2012-03-29 | 2012-10-31 | 中国天辰工程有限公司 | Reactor for producing hexanediamine through adiponitrile hydrogenation |
| WO2014099610A1 (en) * | 2012-12-18 | 2014-06-26 | Invista Technologies S.À R.L. | Integrated process for diamine production |
| CN105555752A (en) * | 2013-09-13 | 2016-05-04 | 因温斯特技术公司 | Hydrogenation of dinitriles for the preparation of diamines |
| WO2016040661A1 (en) * | 2014-09-12 | 2016-03-17 | Invista North America S.A R.L. | Catalyst handling method and hydrogenation process |
| CN105582854A (en) * | 2014-10-21 | 2016-05-18 | 中国石油化工股份有限公司 | Fixed bed hydrogenation reactor and application method thereof |
| CN106810455A (en) * | 2016-12-27 | 2017-06-09 | 河南神马尼龙化工有限责任公司 | A kind of production method of high-quality essence hexamethylene diamine |
| CN108084035A (en) * | 2017-12-11 | 2018-05-29 | 大连理工大学 | A kind of method of adiponitrile direct hydrogenation preparing hexanediamine under the conditions of alkali-free |
| CN108654522A (en) * | 2018-06-08 | 2018-10-16 | 南京敦先化工科技有限公司 | A kind of coil jacket formula axial flow reactor |
| CN111686645A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Micro-interface reinforced wax oil hydrogenation reaction system and method |
| CN210434480U (en) * | 2019-07-07 | 2020-05-01 | 宿迁项王机械设备有限公司 | High-efficient hydrogenation unit of production hexamethylene diamine piperidine |
Non-Patent Citations (1)
| Title |
|---|
| 郭永学.气液固催化反应器.《制药设备与车间设计 第3版》.中国医药科技出版社,2019,第105-106页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112337409A (en) | 2021-02-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104945283A (en) | Method for preparing isocyanate monomer | |
| CN109400443B (en) | Device and method for preparing ethylene glycol through dimethyl oxalate hydrogenation | |
| CN101735182B (en) | Process for continuously producing succinic anhydride through hydrogenation of maleic anhydride | |
| CN103360265A (en) | Method for continuous hydrogenation of dinitrobenzene and recycling of reaction heat thereof | |
| CN112337409B (en) | Production system of hexamethylenediamine | |
| CN108499491A (en) | A kind of hexamethylene diamine synthesis reaction system | |
| CN108484565B (en) | System for producing carbonic ester and method for producing carbonic ester by using system | |
| CN112321438B (en) | Synthesis method of hexamethylenediamine | |
| CN111732496B (en) | System for producing 3, 5-trimethylcyclohexanol by hydrogenation of isophorone and application method thereof | |
| CN204097374U (en) | A kind of cyclohexanone oxamidinating reaction and tripping device | |
| CN216063152U (en) | 1, 4-butanediol grading hydrogenation system | |
| CN210683692U (en) | Slurry bed reaction device for preventing catalyst from settling | |
| CN218608084U (en) | Suspension bed reactor for producing succinic anhydride | |
| CN111892479B (en) | Method and device for improving primary conversion rate of methanol in chloromethane synthesis | |
| CN108033872B (en) | Method and equipment for clean and environment-friendly production of 1,1',2, 3-tetrachloropropene | |
| CN113248389A (en) | Production system and method of 1, 2-cyclohexanediamine | |
| CN115894409B (en) | Succinic anhydride production method adopting serial hydrogenation of suspension bed and fixed bed | |
| CN110172029A (en) | A kind of method of continuous synthesis 2-amino-2-methyl-1-propanol | |
| CN218710089U (en) | Device for producing tetramethyl piperidone through continuous catalytic synthesis | |
| CN208430098U (en) | A kind of catalyst regeneration system producing TW component | |
| CN215087001U (en) | Gas-liquid-solid three-phase continuous reaction device | |
| CN103756716A (en) | Biomass-oil catalytic hydrogenation reaction device and catalytic hydrogenation method thereof | |
| CN203602530U (en) | Device for producing toluene diisocynate by virtue of phosgenation reaction | |
| CN215464394U (en) | Production device of chalcone compound catalyzed by diethyl methylphosphonite | |
| CN213232063U (en) | Methanol synthesis system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |