CN110478951A - A kind of technique and catalyst settler increasing catalyst sedimentation - Google Patents
A kind of technique and catalyst settler increasing catalyst sedimentation Download PDFInfo
- Publication number
- CN110478951A CN110478951A CN201910874150.8A CN201910874150A CN110478951A CN 110478951 A CN110478951 A CN 110478951A CN 201910874150 A CN201910874150 A CN 201910874150A CN 110478951 A CN110478951 A CN 110478951A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- autoclave body
- retention plate
- conveying pipeline
- sedimentation
- 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.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 77
- 238000004062 sedimentation Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 230000014759 maintenance of location Effects 0.000 claims abstract description 30
- 150000001412 amines Chemical class 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 230000010412 perfusion Effects 0.000 claims description 17
- 239000006228 supernatant Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 2
- WDCYWAQPCXBPJA-UHFFFAOYSA-N 1,3-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC([N+]([O-])=O)=C1 WDCYWAQPCXBPJA-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005235 decoking Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000007868 Raney catalyst Substances 0.000 description 1
- 229910000564 Raney nickel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004986 phenylenediamines Chemical class 0.000 description 1
- 239000001965 potato dextrose agar Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 210000000664 rectum Anatomy 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/24—Feed or discharge mechanisms for settling tanks
- B01D21/2405—Feed mechanisms for settling tanks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/24—Feed or discharge mechanisms for settling tanks
- B01D21/2444—Discharge mechanisms for the classified liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/24—Feed or discharge mechanisms for settling tanks
- B01D21/245—Discharge mechanisms for the sediments
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to catalyst sedimentation fields, provide a kind of technique and settler for increasing catalyst sedimentation, catalyst settler, including autoclave body and the conveying pipeline being through to inside autoclave body, retention plate is provided in the autoclave body, multiple through-holes are provided on the retention plate, the conveying pipeline is through retention plate；The technique for increasing catalyst sedimentation, including the catalyst in mixed amine liquid is carried out gravitational settling in settler；After catalyst and clear liquid separation in mixed amine liquid, clear liquid is conveyed into dealcoholysis tower；Catalyst is heavy to be delivered in catalyst circulation slot, is recycled.Settler and sedimentation process of the present invention can settle completely catalyst, effectivelying prevent catalyst to enter subsequent separation system influences separating effect, reduce the distillation system catalyst amount of bringing into, the increase for avoiding tar growing amount improves the yield of product, so that production line Load lifting, product energy consumption, material consumption reduce, catalyst after sedimentation can be recycled and be used, reduce catalyst consumption, reduce production cost.
Description
Technical field
The invention belongs to catalyst sedimentation fields, specifically, being related to a kind of technique and catalysis for increasing catalyst sedimentation
Agent settler.
Background technique
Currently, the technique in synthesis phenylenediamine is substantially in hydrogenation reactor, in certain pressure, temperature, nickel catalysis
Under the action of agent and methanol, mixing dinitrobenzene reacts generation mixing phenylenediamine (abbreviation PDA) reducing solution, unreacted with hydrogen
Complete mixing dinitrobenzene enters catalyst sedimentation system after entering protection reactor the reaction was continued, and reducing solution passes through catalyst
Water, methanol, PDA, tar and trace catalyst particle (referred to as mixing amine liquid) that reaction generates are mainly contained after sedimentation, it be from object
Product is separated in material, needs to be separated using a series of tower sequence.
In the actual production process, the process that Raney nickel particle stirs together with reaction mixture in autoclave
In it is gradually levigate, it is easy to the logistics after being reacted is taken away, and the price of catalyst is very high, this will increase production cost.
In the prior art generally using ceramic cross-flow membrane catalyst separation device, however its catalyst does not settle and causes in use
Partial catalyst finally takes mixed amine decoking tower reboiler, catalyst and tar mixing to by mixed amine liquid band to dealcoholysis tower, dehydrating tower
After be adhered on reboiler tubulation, reduce Matter Transfer latus rectum, mix amine decoking tower bottom siphon circulation amount it is small, evaporation capacity is inadequate,
The entire production line load reduction is caused, product energy consumption, material consumption increase.
Summary of the invention
For deficiency above-mentioned in the prior art, the purpose of the present invention is to provide a kind of techniques for increasing catalyst sedimentation
And catalyst settler, using this method and settler, catalyst can be effectively prevent, which to enter subsequent separation system, influences separation
Effect reduces the distillation system catalyst amount of bringing into, while can recycle catalyst and use, and reduces catalyst consumption, reduces production
Cost.
In order to achieve the above object, the solution that the present invention uses is:
A kind of catalyst settler, including autoclave body, autoclave body bottom top center be provided be through to it is defeated inside autoclave body
Expects pipe, the conveying pipeline top are provided with feed inlet, and the autoclave body top side is provided with supernatant outlet, sets in the autoclave body
It is equipped with retention plate, multiple through-holes are provided on the retention plate, the outer wall of the retention plate fits with inner wall of kettle, described defeated
Expects pipe is through retention plate, and the conveying pipeline fits with retention plate, and the autoclave body bottom is provided with discharge port.
Further, the autoclave body outer wall is provided with collet, is provided with steam inlet above the collet, under the collet
Side is provided with steam (vapor) outlet.
Further, the bottom of the conveying pipeline is in flare openings structure.
Further, the length of the conveying pipeline is the 1/3~1/2 of autoclave body depth.
Further, the retention plate is provided with 1~3, and the through-hole diameter retained on plate described from bottom to up is gradually
Reduce.
Further, the through-hole is uniformly distributed in a ring on retention plate.
Further, it is horizontally arranged with the first perfusion tube above the retention plate, first perfusion tube one end passes through the
Two perfusion tubes are communicated with supernatant outlet, and the bottom wall and side wall of first perfusion tube are provided with multiple inlets.
Further, exhaust outlet is additionally provided at the top of the conveying pipeline.
A kind of technique increasing catalyst sedimentation, comprising the following steps:
1) mixed amine liquid is entered inside autoclave body by the feed inlet of autoclave body, the catalyst in mixed amine liquid carries out weight in autoclave body
Power sedimentation；
2) after mixing catalyst and the clear liquid separation in amine liquid in step 1), clear liquid by the supernatant outlet at the top of autoclave body into
Enter in dealcoholysis tower；
3) catalyst deposit in step 2) after separation is delivered to by the discharge port of autoclave body bottom and is urged in settler bottom
In agent circulating slot, it is recycled.
The beneficial effects of the present invention are:
1. settler of the present invention and sedimentation process can settle completely catalyst, catalyst is effectively prevent to enter subsequent point
From systematic influence separating effect, reduces the distillation system catalyst amount of bringing into and improved so as to avoid the increase of tar growing amount
The yield of product, so that production line Load lifting, product energy consumption, material consumption are reduced.
It is used 2. settler of the present invention and sedimentation process can recycle the catalyst after sedimentation, reduces catalyst consumption, drop
Low production cost.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is the structural schematic diagram of present invention retention plate；
Fig. 3 is the side view of the first perfusion tube of the invention.
Icon: 1- supernatant outlet, 2- feed inlet, 3- exhaust outlet, the first perfusion tube of 4-, the spare mouth of 5-, 6- autoclave body, 7-
Retain plate, 8- thermometer mouth, 9- conveying pipeline, 10- collet, 11- steam inlet, 12- liquid level instrument mouth, 13- discharge port, 14- steaming
Vapor outlet, 15- manhole with vertical hanging cover, the second perfusion tube of 16-, 17- inlet, 18- through-hole.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being usually described and illustrated herein in the accompanying drawings is implemented
The component of example can be arranged and be designed with a variety of different configurations.
Therefore, the detailed description of the embodiment of the present invention provided in the accompanying drawings is not intended to limit below claimed
The scope of the present invention, but be merely representative of selected embodiment of the invention.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
It should also be noted that similar label and letter indicate similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined in a attached drawing, does not then need that it is further defined and explained in subsequent attached drawing.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, or be somebody's turn to do
Invention product using when the orientation or positional relationship usually put, be merely for convenience of description of the present invention and simplification of the description, without
It is that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore not
It can be interpreted as limitation of the present invention.
Term " first ", " second ", " third " etc. are only used for distinguishing description, are not understood to indicate or imply relatively heavy
The property wanted.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, term " setting ",
" installation ", " connected ", " connection " shall be understood in a broad sense, for example, it may be fixedly connected, may be a detachable connection or one
Connect to body；It can be directly connected, the connection inside two elements can also be can be indirectly connected through an intermediary.
For the ordinary skill in the art, the concrete meaning of above-mentioned term in the present invention can be understood with concrete condition.
Embodiment
A kind of catalyst settler, including autoclave body 6, the 6 bottom top center of autoclave body, which is provided with, to be through to inside autoclave body 6
Conveying pipeline 9, in order to enable mixed amine liquid with more smoothly flowing out, the circulation such as will not result in blockage because of pressure the reason of is unsmooth,
The bottom of conveying pipeline 9 is in flare openings structure, and the length of conveying pipeline 9 is the 1/3~1/2 of 6 depth of autoclave body, the conveying pipeline
9 tops are provided with feed inlet 2 and exhaust outlet 3, and 6 top side of autoclave body is provided with supernatant outlet 1, sets in the autoclave body 6
It is equipped with retention plate 7, is provided with multiple through-holes 18 on the retention plate 7, wherein through-hole 18 uniformly divides in a ring on retention plate 7
Cloth, retention plate 7 may be provided with 1~3, and 18 diameter of through-hole retained on plate 7 from bottom to up is gradually reduced；The retention plate 7
Outer wall fit with 6 inner wall of autoclave body, the conveying pipeline 9 through retention plate 7, and the conveying pipeline 9 with retain plate 7 fit；
The first perfusion tube 4 is horizontally arranged with above retention plate 7,4 one end of the first perfusion tube is communicated with supernatant by the second perfusion tube 16
Outlet 1, the bottom wall and side wall of the first perfusion tube 4 are provided with multiple inlets 17, so that supernatant enters the by inlet 17
In one perfusion tube 4, by 16 output valve supernatant outlet 1 of the second perfusion tube, 6 bottom of autoclave body is provided with discharge port 13,
Autoclave body 6 is discharged for catalyst.Wherein, 6 outer wall of autoclave body is provided with collet 10, and steam inlet 11, collet are provided with above collet 10
10 lower sections are provided with steam (vapor) outlet 14, steam are inputted into collet 10 by steam inlet 11, steam circulates in collet 10
Heat is provided for autoclave body 6, to facilitate the sedimentation of catalyst in mixed amine liquid, then steam is flowed from the steam (vapor) outlet 14 of bottom
Out, hot water can also be passed through in the present embodiment into collet 10 instead of steam.
Settler of the present invention is fed by feed inlet 2 when in use, by mixed amine liquid, is then entered in autoclave body 6 by conveying pipeline 9
Portion, because the density of catalyst is greater than the density of mixed amine liquid, catalyst can be in natural subsidence under self gravitation effect to 6 bottom of autoclave body
Portion, with increasing for mixed amine liquid, the supernatant liquid level after catalyst sedimentation is increased, when liquid level is increased at retention plate 7, if on
The small catalyst particles not settled completely are mixed in clear liquid, then can be trapped the interception of plate 7 can not pass through, and supernatant then may be used
Smoothly continue to rise by the through-hole 18 on retention plate 7, finally autoclave body 6 can be discharged in supernatant by supernatant outlet 1,
Then by the discharge port 13 of 6 bottom of autoclave body by catalyst recycling and reusing.
A kind of technique increasing catalyst sedimentation, comprising the following steps:
1) mixed amine liquid is entered inside autoclave body 6 by the feed inlet 2 of autoclave body 6, mix the catalyst in amine liquid in autoclave body 6 into
Row gravitational settling；
2) after mixing catalyst and the clear liquid separation in amine liquid in step 1), clear liquid passes through the supernatant outlet 1 at the top of autoclave body 6
Into in dealcoholysis tower；
3) catalyst deposit in step 2) after separation is delivered in 6 bottom of autoclave body by the discharge port 13 of 6 bottom of autoclave body
In catalyst circulation slot, it is recycled.
In one 10,000 tons/year of production system, by using settler provided in this embodiment and sedimentation process, In
Mixed amine liquid increases a settler before entering dealcoholysis tower, allows mixed amine liquid further progress gravity settling separation, and catalyst is separated
Out:
Catalyst consumption ring is than decline 0.31kg/t, and catalyst unit price is 127 yuan/kilogram, that is, producing 10000 tons of phenylenediamines per year can
To save catalyst cost are as follows: ten thousand yuan of 10000 × 0.31 × 127=39.4.
In conclusion settler provided by the invention and sedimentation process can reduce the distillation system catalyst amount of bringing into, simultaneously
Catalyst can be recycled and be used, reduce catalyst consumption, reduce production cost.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of catalyst settler, including autoclave body, which is characterized in that autoclave body bottom top center, which is provided with, is through to autoclave body
Internal conveying pipeline, the conveying pipeline top are provided with feed inlet, and the autoclave body top side is provided with supernatant outlet, described
It is provided with retention plate in autoclave body, multiple through-holes are provided on the retention plate, the outer wall of the retention plate is affixed with inner wall of kettle
It closes, the conveying pipeline is through retention plate, and the conveying pipeline fits with retention plate, and the autoclave body bottom is provided with discharge port.
2. catalyst settler according to claim 1, which is characterized in that the autoclave body outer wall is provided with collet, described
It is provided with steam inlet above collet, is provided with steam (vapor) outlet below the collet.
3. catalyst settler according to claim 1, which is characterized in that the bottom of the conveying pipeline is in flare openings
Structure.
4. catalyst settler according to claim 1, which is characterized in that the length of the conveying pipeline is autoclave body depth
1/3~1/2.
5. catalyst settler according to claim 1, which is characterized in that the retention plate is provided with 1~3, and from
Under it is supreme it is described retention plate on through-hole diameter be gradually reduced.
6. catalyst settler according to claim 1, which is characterized in that the through-hole is uniform in a ring on retention plate
Distribution.
7. catalyst settler according to claim 1, which is characterized in that be horizontally arranged with first above the retention plate
Perfusion tube, first perfusion tube one end are communicated with supernatant outlet, the bottom wall of first perfusion tube by the second perfusion tube
And side wall is provided with multiple inlets.
8. catalyst settler according to claim 1, which is characterized in that be additionally provided with exhaust at the top of the conveying pipeline
Mouthful.
9. increasing the technique of catalyst sedimentation using according to any one of claims 1 to 88 described in any item catalyst settlers, feature exists
In, comprising the following steps:
1) mixed amine liquid is entered inside autoclave body by the feed inlet of autoclave body, it is heavy that the catalyst in mixed amine liquid carries out gravity in autoclave body
Drop；
2) after mixing catalyst and the clear liquid separation in amine liquid in step 1), clear liquid is entered de- by the supernatant outlet at the top of autoclave body
In alcohol tower；
3) catalyst deposit in step 2) after separation is delivered to catalyst by the discharge port of autoclave body bottom and follows in autoclave body bottom
In annular groove, it is recycled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910874150.8A CN110478951A (en) | 2019-09-17 | 2019-09-17 | A kind of technique and catalyst settler increasing catalyst sedimentation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910874150.8A CN110478951A (en) | 2019-09-17 | 2019-09-17 | A kind of technique and catalyst settler increasing catalyst sedimentation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110478951A true CN110478951A (en) | 2019-11-22 |
Family
ID=68558356
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910874150.8A Pending CN110478951A (en) | 2019-09-17 | 2019-09-17 | A kind of technique and catalyst settler increasing catalyst sedimentation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110478951A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111054103A (en) * | 2020-01-08 | 2020-04-24 | 深圳市科拉达精细化工有限公司 | Settler for accelerating sedimentation of oil slurry catalyst particles |
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| CN101209403A (en) * | 2006-12-27 | 2008-07-02 | 中国石油化工股份有限公司 | Method and equipment for liquid-solid continuously separation for slurry state bed reactor |
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-
2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111054103A (en) * | 2020-01-08 | 2020-04-24 | 深圳市科拉达精细化工有限公司 | Settler for accelerating sedimentation of oil slurry catalyst particles |
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