CN104084206B - Aromatic amine hydrogenation catalyst recycling method - Google Patents
Aromatic amine hydrogenation catalyst recycling method Download PDFInfo
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- CN104084206B CN104084206B CN201410265355.3A CN201410265355A CN104084206B CN 104084206 B CN104084206 B CN 104084206B CN 201410265355 A CN201410265355 A CN 201410265355A CN 104084206 B CN104084206 B CN 104084206B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 113
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 35
- 150000004982 aromatic amines Chemical class 0.000 title claims abstract description 22
- 238000004064 recycling Methods 0.000 title abstract description 4
- 239000012528 membrane Substances 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000004062 sedimentation Methods 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract 3
- 238000007599 discharging Methods 0.000 claims description 25
- 239000012530 fluid Substances 0.000 claims description 20
- 230000000149 penetrating effect Effects 0.000 claims description 20
- 238000005374 membrane filtration Methods 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- -1 aromatic nitro compound Chemical class 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 238000009903 catalytic hydrogenation reaction Methods 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 23
- 239000002699 waste material Substances 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 6
- 239000006228 supernatant Substances 0.000 abstract 3
- 239000000463 material Substances 0.000 abstract 2
- 238000012545 processing Methods 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- VOZKAJLKRJDJLL-UHFFFAOYSA-N 2,4-diaminotoluene Chemical compound CC1=CC=C(N)C=C1N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- NTBYINQTYWZXLH-UHFFFAOYSA-N 1,2-dichloro-4-nitrobenzene Chemical class [O-][N+](=O)C1=CC=C(Cl)C(Cl)=C1 NTBYINQTYWZXLH-UHFFFAOYSA-N 0.000 description 1
- WDCYWAQPCXBPJA-UHFFFAOYSA-N 1,3-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC([N+]([O-])=O)=C1 WDCYWAQPCXBPJA-UHFFFAOYSA-N 0.000 description 1
- PLAZTCDQAHEYBI-UHFFFAOYSA-N 2-nitrotoluene Chemical compound CC1=CC=CC=C1[N+]([O-])=O PLAZTCDQAHEYBI-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- LZVRUDMTJCUUNP-UHFFFAOYSA-N [N+](=O)([O-])C1=C(OC)C=CC(C1)(N)C(C)=O Chemical compound [N+](=O)([O-])C1=C(OC)C=CC(C1)(N)C(C)=O LZVRUDMTJCUUNP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to an aromatic amine hydrogenation catalyst recycling method. The method comprises the following steps: (1) membrane-filtering and sedimentation separation are carried out, wherein hydrogenation feed liquid from a hydrogenation reaction kettle is delivered into a first-stage membrane filter; through membrane filtering separation, a permeated liquid discharged material enters a subsequent process, and concentrated liquid is subjected to sedimentation separation in a first-stage sedimentation tank; according to detected activity effect, a catalyst separated from the bottom of the first-stage sedimentation tank is delivered back to the hydrogenation reaction kettle and is reused, or is recovered as a waste catalyst; a supernatant is discharged into a next-stage membrane filter; the above membrane-filtering and sedimentation separation operations are repeated, and a supernatant from the final N-stage sedimentation tank is discharged into a last-stage membrane filter, wherein N is no less than 2; and (2) last-stage membrane filtering separation is carried out, wherein the supernatant from the N-stage sedimentation tank enters the last-stage membrane filter; after membrane filtering separation, a permeated liquid discharged material enters a subsequent process, and concentrated liquid is delivered back into the N-stage sedimentation tank; and the catalyst is separated from the bottom.
Description
(1) technical field
The present invention relates to the recoverying and utilizing method of a kind of hydrogenation catalyst, be that aromatic amine hydrogenation is urged in particular
The method that the on-line continuous separation and recovery of agent utilizes.
(2) background technology
Aromatic amine compounds is particularly important Organic Ingredients, is widely used in dyestuff, medicine, chemurgy
The production fields such as product.Most aromatic amine compounds are to be prepared by reduction by virtue nitro compound,
Hydrogenating reduction method becomes the most industrial with the advantage such as its technique cleaning, reduction efficiency height, good product quality
The main stream approach of reduction nitro.
During hydrogenating reduction, it usually needs use catalyst and promote the carrying out of reaction.In hydrogenation reaction mistake
Cheng Zhong, catalyst is crushed during being stirred vigorously together with reaction mixture in reactor, and particle diameter is relatively
Little catalyst is easily brought into subsequent handling by logistics, causes resultant metal content overproof and equipment fault.
Patent CN02112764.6, a kind of method disclosing inorganic membrane filtration separating catalyst, it uses and adds
Hydrogen generates Matter Transfer and iterates through inorganic filter film, and liquid-phase product is collected through after fenestra, solid-phase catalyst
The method staying reactor recycling.But this technique interval is carried out, and affects production efficiency, concurrently separates
Catalyst fully recovering, fail to separate the catalyst inactivated, to follow-up hydrogenation reaction impact.
Patent CN200710163811.3, describe a kind of toluenediamine hydrogenation catalyst is continuously separated circulation
Method and equipment thereof, it uses a kind of inclined plate separator to be continuously separated and recycle urging in crude tolu ne diamine
Agent, feeding catalyst concentration 0.5-3.0wt%, after this device separates, in clear liquid, catalyst concn controls
200-600ppm。
Patent CN201210026615.2, discloses the recycling of a kind of toluenediamine hydrogenation catalyst microgranule
Method and device, it uses the micro-swirl concentrator of settling tank gravitational settling, one-level and the micro-cyclone clarificator of one-level
Processing, in the case of imported catalyst content is not more than 5wt%, device outlet catalyst content is not more than
0.05wt%.In existing commercial production, though method that aromatic amine hydrogenation catalyst be continuously separated recovery is had been disclosed,
But catalyst content is higher in the feed liquid after Fen Liing, unfavorable to following process process and product quality；Tradition adds
Hydrogen technique is relatively big due to the loss of catalyst, need to supplement and add normally entering of new catalyst holding hydrogenation reaction
OK, integral membrane be recovered by filtration technology to reclaim catalyst do not carry out difference utilize.Therefore, in the urgent need to opening
Send out efficient on-line continuous a kind of and separate and recover the method utilizing catalyst.
(3) summary of the invention
Present invention aim at providing a kind of efficient on-line continuous separation and recovery to utilize aromatic amine hydrogenation catalyst
Method, do not distinguish separation and recovery and separate solving in existing commercial production aromatic amine hydrogenation dead catalyst
The higher problem affecting following process of catalyst content in the feed liquid obtained.
For realizing the object of the invention, the technical scheme used is as follows:
The recoverying and utilizing method of a kind of aromatic amine hydrogenation catalyst, comprises the following steps:
(1) membrane filtration-settlement separate: the hydrogenation feed liquid coming from hydrogenation reaction kettle continuously enters one-level membrane filtration
Device, is separated by membrane filtration, and penetrating fluid discharging enters subsequent handling (i.e. the postprocessing working procedures of aromatic amine product),
Concentrated solution enters one-level subsider and carries out settlement separate, and the catalyst separated bottom one-level subsider returns
Hydrogenation reaction kettle is continuing with or reclaims as dead catalyst, and upper clear supernate discharging is to next stage film mistake
Filter, repeats above-mentioned membrane filtration-settlement separate operation, and the upper clear supernate discharging of last N level subsider is to final stage
Film filter, wherein N >=bis-；Described hydrogenation reaction kettle carries out aromatic nitro compound catalytic hydrogenation system
The reaction of standby aromatic amine；
(2) final stage membrane filtration separates: the upper clear supernate coming from N level subsider enters final stage film filter,
Being separated by membrane filtration, penetrating fluid discharging enters subsequent handling, and concentrated solution backs into N level subsider, from
Bottom separating catalyst, generally as waste catalyst recovery.
Further, described aromatic amine hydrogenation catalyst is nickeliferous, palladium, platinum, rhodium or iridium isoreactivity component
Granule or fine catalyst.
Further, the described hydrogenation feed liquid coming from hydrogenation reaction kettle before carrying out membrane filtration-settlement separate,
First carry out settlement separate: make to continuously enter subsider from the hydrogenation feed liquid of hydrogenation reaction kettle and carry out settlement separate,
The isolated catalyst concentration slurry in bottom returns hydrogenation reaction kettle and is continuing with, after upper clear supernate discharging enters
Continuous one-level film filter.
Further, described settlement separate may be used without multistage operations, preferably 2～3 grades sedimentations, i.e. subsider
The discharging of upper clear supernate elder generation carry out settlement separate to next subsider, after what is settlement separate last
The upper clear supernate of individual subsider enters back into one-level membrane separator.
Further, described membrane filtration-settlement separate 2-6 level that preferably employs operates (i.e. N is selected from two～six), more
Preferably employ 2-3 level operation (i.e. N is two or three).
Further, the catalyst concn that the penetrating fluid of entrance subsequent handling contains is less than 40ppm.
In the present invention, described film filter can use the inorganic of pottery, metal or other composite composition
Film, the average pore size of film is at 1nm～1um, and filtered version can use cross-flow or and the mode that flows.General raw material
Enter film filter and be divided into both sides: seepage side and circulation side.The clean liquid (penetrating fluid) of seepage side enters follow-up
Manufacturing procedure, the dope (concentrated solution) of circulation side enters subsider.
Compared with prior art, advantage of the invention is that and separated, continuously by continuous feed, continuous sedimentation
Membrane filtration-settlement separate, solve catalyst in catalytic hydrogenation commercial production continuous ON-LINE SEPARATION reclaim ask
Topic, membrane filtration pattern is collaborative with gravitational settling mode to be optimized so that the separation efficiency of hydrogenation liquid catalyst obtains
Bigger lifting, significantly reduces the amount of feed liquid entrained catalyst, makes catalyst obtain difference simultaneously and reclaims.
(4) accompanying drawing explanation
Fig. 1 is the schematic diagram of a kind of embodiment of present invention process flow process.
(5) detailed description of the invention
With specific embodiment, technical scheme is described further below, but the protection model of the present invention
Enclose and be not limited to this:
Embodiment 1
2-nitro-4-acetyl-anisidine, methanol, nickel aluminum powder catalyst and hydrogen enter by a certain percentage and add
Hydrogen reactor carries out hydrogenation reaction, and wherein nickel aluminum powder catalyst content is 3.5%, and catalyst particle size is at 100-500
Mesh.2-amino-4-acetyl-anisidine hydrogenation the feed liquid that hydrogenation produces, enters subsider and carries out settlement separate.
Bottom subsider, isolated catalyst pulp returns hydrogenation system use, and upper clear supernate catalyst concn is about
0.20%, it is pumped to subsequent film defecator.Subsequent film defecator uses titanium metal film, and film average pore size is big
Little for 50nm.
After settlement separate upper clear supernate enters the separation of one-level film filter, the penetrating fluid catalyst content obtained
For 20ppm, discharging is to subsequent processing；The dope catalyst content obtained is 6000ppm, enters one-level and sinks
Fall groove carries out settlement separate.Bottom subsider, isolated catalyst slurry returns hydrogenation still use, and top is clear
Secondary membrane device delivered to by liquid pump.
After the upper clear supernate entrance secondary membrane device separation that one-level is settlement separate, the penetrating fluid catalyst obtained
Content is 20ppm, and direct discharging is to subsequent processing；The dope catalyst content obtained is 6000ppm, enters
Enter secondary settling tank and carry out settlement separate.Bottom subsider, isolated catalyst pulp is as waste catalyst
Being recycled by manufacturer, upper clear supernate is pumped to three grades of film filters.
After two grades of settlement separate upper clear supernate enter three grades of film filters separation, the penetrating fluid catalyst obtained
Content is 20ppm, and direct discharging is to subsequent processing；The dope obtained backs into secondary settling tank.
Embodiment 2
Mix dinitrobenzene, methanol, nickel aluminum powder catalyst and hydrogen enter hydrogenation reaction kettle by a certain percentage to be carried out
Reaction, wherein nickel aluminum powder catalyst content is 5.1%, and catalyst particle size is at 100-500 mesh.Hydrogenation produces
Mixed diamidogen hydrogenation feed liquid, enters subsider and carries out settlement separate.Isolated catalyst pulp bottom subsider
Return hydrogenation system uses, and upper clear supernate catalyst concn is about 0.31%, is pumped to subsequent film defecator.
Subsequent film defecator uses ceramic membrane, and film mean pore size is 45nm.
After settlement separate upper clear supernate enters the separation of one-level film filter, the penetrating fluid catalyst content obtained
For 27ppm, discharging is to subsequent processing；The dope catalyst content obtained is 9000ppm, enters one-level and sinks
Fall groove carries out settlement separate.Isolated catalyst bottom subsider, its hydrogen-absorption speed is theoretical less than 50% to be inhaled
Hydrogen speed, it is impossible to return and be continuing with, recycled by manufacturer as dead catalyst；Upper clear supernate pump
Deliver to secondary membrane device.
After the upper clear supernate entrance secondary membrane device separation that one-level is settlement separate, the penetrating fluid catalyst obtained
Content is 27ppm, and direct discharging is to subsequent processing；The dope catalyst content obtained is 9000ppm, enters
Enter secondary settling tank and carry out settlement separate.Bottom subsider, isolated catalyst pulp is as waste catalyst
Being recycled by manufacturer, upper clear supernate is pumped to three grades of film filters.
After two grades of settlement separate upper clear supernate enter three grades of film filters separation, the penetrating fluid catalyst obtained
Content is 27ppm, and direct discharging is to subsequent processing；The dope catalyst content obtained is 13500ppm, enters
Enter three grades of subsiders and carry out settlement separate.Bottom subsider, isolated catalyst pulp is as waste catalyst
Being recycled by manufacturer, upper clear supernate is pumped to level Four film filter.
After three grades of settlement separate upper clear supernate enter the separation of level Four film filter, the penetrating fluid catalyst obtained
Content is 27ppm, and direct discharging is to subsequent processing；The dope obtained backs into three grades of subsiders.
Embodiment 3
Methylnitrobenzene, methanol, nickel aluminum powder catalyst and hydrogen enter hydrogenation reaction kettle reaction according to a certain percentage,
Wherein nickel aluminum powder catalyst content is 4.5%, and catalyst particle size is at 100-500 mesh.The methylbenzene that reaction obtains
Amine hydrogenation feed liquid, enters subsider and carries out settlement separate.Bottom subsider, isolated catalyst pulp returns
Hydrogenation system uses, and upper clear supernate catalyst concn is about 0.27%, is pumped to subsequent film defecator.Follow-up
Film filter uses titanium-aluminium alloy metal film, and film mean pore size is 100nm.
After settlement separate upper clear supernate enters the separation of one-level film filter, the penetrating fluid catalyst content obtained
For 25ppm, discharging is to subsequent processing；The dope catalyst content obtained is 8000ppm, enters one-level and sinks
Fall groove carries out settlement separate.Bottom subsider, isolated catalyst slurry returns hydrogenation still use, and top is clear
Secondary membrane device delivered to by liquid pump.
After the upper clear supernate entrance secondary membrane device separation that one-level is settlement separate, the penetrating fluid catalyst obtained
Content is 25ppm, and direct discharging is to subsequent processing；The dope catalyst content obtained is 8000ppm, enters
Enter secondary settling tank and carry out settlement separate.Bottom subsider, isolated catalyst pulp is as waste catalyst
Being recycled by manufacturer, upper clear supernate is pumped to three grades of film filters.
After two grades of settlement separate upper clear supernate enter three grades of film filters separation, the penetrating fluid catalyst obtained
Content is 25ppm, and direct discharging is to subsequent processing；The dope obtained backs into secondary settling tank.
Embodiment 4
3,4-dichloronitrobenzenes, methanol, nickel aluminum powder catalyst and hydrogen enter hydrogenation reaction kettle and react, its
Middle nickel aluminum powder catalyst content is 0.71%, and catalyst particle size is at 100-500 mesh.3,4 dichloros that reaction obtains
Aniline hydrogenation feed liquid, enters one-level film filter and separates, and the penetrating fluid catalyst content obtained is 35ppm,
Discharging is to subsequent processing；The dope catalyst content obtained is 15000ppm, enters one-level subsider and sinks
Fall separates.Bottom subsider, isolated catalyst slurry returns hydrogenation still use, and upper clear supernate is pumped to two
Level film filter.
After the upper clear supernate entrance secondary membrane device separation that one-level is settlement separate, the penetrating fluid catalyst obtained
Content is 35ppm, and direct discharging is to subsequent processing；The dope catalyst content obtained is 15000ppm, enters
Enter secondary settling tank and carry out settlement separate.Bottom subsider, isolated catalyst pulp is as waste catalyst
Being recycled by manufacturer, upper clear supernate is pumped to three grades of film filters.Subsequent film defecator uses pottery
Porcelain film, film mean pore size is 200nm.
After two grades of settlement separate upper clear supernate enter three grades of film filters separation, the penetrating fluid catalyst obtained
Content is 35ppm, and direct discharging is to subsequent processing；The dope obtained backs into secondary settling tank.
Claims (9)
1. a recoverying and utilizing method for aromatic amine hydrogenation catalyst, comprises the following steps:
(1) membrane filtration-settlement separate: the hydrogenation feed liquid from hydrogenation reaction kettle enters one-level film filter, logical
Crossing membrane filtration to separate, penetrating fluid discharging enters subsequent handling, and concentrated solution enters one-level subsider and carries out sedimentation point
From, the catalyst separated bottom one-level subsider, according to the active effect of detection, returns hydrogenation reaction kettle
It is continuing with or reclaims as dead catalyst, upper clear supernate discharging to next stage film filter, repeats
Above-mentioned membrane filtration-settlement separate operation, the upper clear supernate discharging of last N level subsider to final stage film filter,
Wherein N >=bis-；Described hydrogenation reaction kettle carries out aromatic nitro compound catalytic hydrogenation and prepares the anti-of aromatic amine
Should；
(2) final stage membrane filtration separates: the upper clear supernate coming from N level subsider enters final stage film filter,
Being separated by membrane filtration, penetrating fluid discharging enters subsequent handling, and concentrated solution backs into N level subsider, from
Bottom separating catalyst.
2. the recoverying and utilizing method of aromatic amine hydrogenation catalyst as claimed in claim 1, it is characterised in that:
The described hydrogenation feed liquid coming from hydrogenation reaction kettle, before carrying out membrane filtration-settlement separate, first settles
Separating: make to continuously enter subsider from the hydrogenation feed liquid of hydrogenation reaction kettle and carry out settlement separate, bottom separates
The catalyst concentration slurry gone out returns hydrogenation reaction kettle and is continuing with, and upper clear supernate discharging enters follow-up one-level
Film filter.
3. the recoverying and utilizing method of aromatic amine hydrogenation catalyst as claimed in claim 2, it is characterised in that:
Described settlement separate employing Multistage settling operation, the upper clear supernate elder generation discharging of subsider is to next subsider
Carrying out settlement separate, after Multistage settling separates, the upper clear supernate of last subsider enters back into one-level film
Separator.
4. the recoverying and utilizing method of aromatic amine hydrogenation catalyst as claimed in claim 3, it is characterised in that:
Described settlement separate employing 2～3 grades of settling operation.
5. the recoverying and utilizing method of the aromatic amine hydrogenation catalyst as described in one of Claims 1 to 4, its feature
Be: described aromatic amine hydrogenation catalyst be nickeliferous, palladium, platinum, rhodium or the granule of iridium active component or
Fine catalyst.
6. the recoverying and utilizing method of the aromatic amine hydrogenation catalyst as described in one of Claims 1 to 4, its feature
It is: the catalyst concn that the penetrating fluid of entrance subsequent handling contains is less than 40ppm.
7. the recoverying and utilizing method of the aromatic amine hydrogenation catalyst as described in one of Claims 1 to 4, its feature
Being: in step (1), N is selected from two～six.
8. the recoverying and utilizing method of aromatic amine hydrogenation catalyst as claimed in claim 7, it is characterised in that:
In step (2), N is two or three.
9. the recoverying and utilizing method of the aromatic amine hydrogenation catalyst as described in one of Claims 1 to 4, its feature
It is: described film filter uses the inoranic membrane that pottery or metal are constituted, and the average pore size of film exists
1nm～1 μm.
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| CN114308141A (en) * | 2021-12-15 | 2022-04-12 | 安徽华尔泰化工股份有限公司 | Separation process and separation system for phenylenediamine hydrogenation reduction liquid catalyst |
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| CN103846008A (en) * | 2012-12-04 | 2014-06-11 | 厦门市天泉鑫膜科技股份有限公司 | Device for continuously concentrating and separating substance by membrane and separation method |
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Inventor after: He Xubin Inventor after: Wang Xinwu Inventor after: Yang Risheng Inventor after: Yuan Wenbing Inventor after: Ruan Liangfeng Inventor after: Zhu Jingxin Inventor after: Tao Jianguo Inventor after: Meng Ming Inventor before: He Xubin Inventor before: Wang Xinwu Inventor before: Yang Risheng Inventor before: Yuan Wenbing Inventor before: Ruan Liangfeng Inventor before: Zhu Jingxin Inventor before: Tao Jianguo Inventor before: Meng Ming |
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