CN107537407A - The method that adipic dinitrile hydrogenation reaction system and the system treatment reactor severe block - Google Patents
The method that adipic dinitrile hydrogenation reaction system and the system treatment reactor severe block Download PDFInfo
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- CN107537407A CN107537407A CN201710894317.8A CN201710894317A CN107537407A CN 107537407 A CN107537407 A CN 107537407A CN 201710894317 A CN201710894317 A CN 201710894317A CN 107537407 A CN107537407 A CN 107537407A
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- reactor
- recurrent canal
- feed pump
- catalyst
- hydrogenation reaction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The method that adipic dinitrile hydrogenation reaction system and the system treatment reactor severe block, the system adds additional additional line A and additional line B on the basis of existing production system, so that by the opening and closing of hand valve, connection of the reactor feed pump for connecting line between platform, reactor sampling jar and recurrent canal three can be realized when processing returns to blockage；Methods described is used as pressure source by the use of the ethanol being continuously fed in recurrent canal, pressure is formed in the recurrent canal of blocking, after certain time is continuously fed to, the rapid hand valve B that opens makes the pressure in recurrent canal be come down in torrents downwards in a flash, rush at tamper, after repeated multiple times, catalyst particle severe being blocked in recurrent canal washes away, and realizes the conducting of recurrent canal.System and method for of the present invention, realize and under not parking state, solve the problem that reactor recurrent canal severe blocks in adipic dinitrile hydrogenation reaction production, maintain the progress of continuous production, reduce cost indirectly, improve production efficiency.
Description
Technical field
The present invention relates to adipic dinitrile hydrogenation to react production hexamethylene diamine technical field, specifically adipic dinitrile hydrogenation reaction system
The method that system and the system treatment reactor severe block.
Background technology
Present adipic dinitrile hydrogenation reactor recurrent canal often occurs because catalyst flowing does not cause the phenomenon of blocking freely, to oneself
The daily operating of dintrile hydrogenation reaction brings very big pressure.The main reason for reactor plugs is that catalyst grain size diminishes, glued
Degree is big, mobile performance is deteriorated, in decanter caused by catalyst wall built-up, accumulation.Once reactor blocks, processing not in time will
Seriously affect the daily operating of adipic dinitrile hydrogenation reaction, and the accident such as flush of hydrogen gas tower flooding.Adipic dinitrile hydrogenation reactor
Characteristic：Hydrogen is inflammable and explosive, pressure is high, catalyst is easy naturally, oxygen can not be run into, and the recurrent canal in reactor is once stifled
Plug, because pipeline is elongated, it is impossible to be diluted using existing equipment, handle adipic dinitrile hydrogenation reactor recurrent canal degree now and block
Method it is fairly simple, severe block when only stop reaction, processing duration of congestion length, most of catalyst buildup is in decanter
It is interior, the normal operation of adipic dinitrile hydrogenation reaction is have impact on, causes during duration of congestion the hexamethylene diamine of adipic dinitrile hydrogenation reaction generation miscellaneous
Matter raises.
The content of the invention
In order to solve the problems, such as that recurrent canal severe blocks in reactor in adipic dinitrile hydrogenation course of reaction, the invention discloses
A kind of adipic dinitrile hydrogenation reaction system, the reaction system compared with prior art, add additional line A and additional line B so that
Can solve the problems, such as the blocking of recurrent canal severe using the system in the case of not parking reaction；
In order to solve the problems, such as that recurrent canal severe blocks in reactor in adipic dinitrile hydrogenation course of reaction, the invention discloses also public affairs
Opened a kind of method that treatment reactor severe blocks, this method using the adipic dinitrile hydrogenation reaction system in the present invention for support,
The problem of recurrent canal severe blocks is can effectively solve the problem that, and it is simple to operate, effect is good.
Therefore, the technical scheme that the present invention is taken regarding to the issue above is：Adipic dinitrile hydrogenation reaction system, the system
Including hydrogen reactor head tank, reactor feed pump and reactor feed pump for platform, reactor, reactor sampling jar, catalyst
Blowdown vessel and catalyst detergent tank, wherein, decanter is provided with the reactor, decanter bottom is connected with recurrent canal, institute
State reactor feed pump and reactor feed pump for platform it is parallel with one another after one end be connected with hydrogen reactor head tank, the other end and instead
Device is answered to connect, the decanter side is connected by connecting line with catalyst emission tank, and catalyst emission pot bottom passes through company
Adapter road connects with catalyst detergent tank, and the catalyst detergent tank is connected to hydrogen reactor head tank by connecting line and sentenced
The bad use that follows of catalyst is realized, is connected at the top of the reactor sampling jar by connecting line with recurrent canal；In the system
Ethanol feed pump is additionally provided with, ethanol charging pump discharge is connected to reactor feed pump entering for platform by an additional line A
At mouthful, and reactor feed pump is additionally provided with additional line between the exit of platform and reactor sampling jar bottom outlet
B。
In the present invention, the reactor feed pump on the connecting line between the outlet of platform and reactor for being provided with hand valve
A。
In the present invention, the reactor sampling jar bottom outlet end is provided with sampling valve.
In the present invention, the hand valve B for connecting recurrent canal and reactor is provided between the recurrent canal and reactor.
In the present invention, sampling root is provided with the connecting line at the top of the reactor sampling jar between recurrent canal
Valve.
The method blocked using adipic dinitrile hydrogenation reaction system treatment reactor severe, is comprised the following steps：
1）Hand valve A and sampling valve are first shut off, sampling root valve is opened, by reactor feed pump for platform, reactor sampling jar
Connecting line connection between recurrent canal three；
2）Ethanol feed pump and reactor feed pump are opened for platform, and control reactor feed pump for platform with 30-60% load,
2.7-4.2MPa outlet pressure, it is sent into ethanol as the reacted device sampling jar of dilution in recurrent canal and decanter；
3）Hand valve B is opened, 5-10min is rinsed between recurrent canal and reactor with use ethanol as dilution, is then shut off hand
Valve B, ethanol is continuously fed into recurrent canal and decanter, to be formed by the ethanol constantly poured in recurrent canal and decanter
Pressure；
4）It is rapid to open hand valve B after ethanol is continuously fed to continue 3-5min, while decanter is increased to catalyst detergent tank
Catalyst emission amount；
5）Repeat step 3）With step 4）Operation 5-7 times, when tube wall temperature to be returned is gone up to 70 DEG C or so by 40-50 DEG C,
Then reactor has led to.
As preferable, the step 5）In, when tube wall temperature recovery to be returned is to 70 DEG C or so, taken by reactor
The catalyst that the sampling of sample tank is remained in recurrent canal, if catalyst particle size is not less than 600mm, reactor has led to；If catalyst
Particle diameter is less than 600mm, repeat step 3）With step 4）Operation to catalyst particle size is not less than 600mm.
In the present invention, step 1 is being carried out）To step 5）In operating process, reactor feed pump handles opening always,
To ensure being normally carried out for adipic dinitrile hydrogenation reaction.
Compared with prior art, the invention has the advantages that：
System of the present invention, compared with prior art, according to produced on-site situation, it adds additional additional line A and attached
Add pipeline B, by the opening and closing of hand valve, can realize that reactor feed pump takes for platform, reactor when processing returns to blockage
The connection of connecting line between sample tank and recurrent canal three, solve blocking for ethanol " flushing " recurrent canal and hardware condition is provided.
In addition, in the present invention, the blocking of reactor is substantially concentrated mainly on the part led on recurrent canal in reactor
Pipeline, because the catalyst to diminish that attenuates after reaction is flowed into reactor by recurrent canal, tiny catalyst is easy to returning
Blocked at the bottom conduit of return pipe.
For such case, in the method for the invention, the recurrent canal of alcohol flushing blocking, now ethanol conduct are first passed through
Dilution is present, and the catalyst in recurrent canal blocked to severe plays diluting effect, after secondly closing hand valve B, using continuing
The ethanol being sent into recurrent canal forms pressure as pressure source in the recurrent canal of blocking, fast after certain time is continuously fed to
Speed, which opens hand valve B, makes the pressure in recurrent canal be come down in torrents downwards in a flash, rushes at tamper, after repeated multiple times, severe is blocked up
The catalyst particle filled in recurrent canal washes away, and realizes the conducting of recurrent canal, and in above process, reactor feed pump institute
Pipeline all the time in normal reaction production status, it is achieved thereby that not stopping in adipic dinitrile hydrogenation reacts production hexamethylene diamine
Under car state, solve the problem that reactor recurrent canal severe blocks, maintain the progress of continuous production, reduce cost indirectly,
Improve production efficiency.
Brief description of the drawings
Fig. 1 is the process chart of system of the present invention；
Marked in figure：1st, hydrogen reactor head tank, 2, reactor feed pump, 3, reactor feed pump for platform, 301, hand valve A, 4,
Reactor, 401, decanter, 402, recurrent canal, 403, hand valve B, 5, reactor sampling jar, 501, sampling valve, 502, sampling root
Valve, 6, catalyst emission tank, 7, catalyst detergent tank, 8, ethanol feed pump, 9, additional line A, 10, additional line B.
Embodiment
The present invention is elaborated with reference to specific embodiment, the present embodiment premised on technical solution of the present invention,
Give detailed embodiment and specific operating process.
As shown in figure 1, The present invention gives adipic dinitrile hydrogenation reaction system, the system include hydrogen reactor head tank 1,
Reactor feed pump 2 and reactor feed pump are for platform 3, reactor 4, reactor sampling jar 5, catalyst emission tank 6 and catalyst
Washing tank 7, wherein, decanter 401 is provided with the reactor 4, the bottom of decanter 401 is connected with recurrent canal 402, described anti-
Answer device feed pump 2 and reactor feed pump for platform 3 it is parallel with one another after one end be connected with hydrogen reactor head tank 1, the other end with instead
Device 4 is answered to connect, the side of decanter 401 is connected by connecting line with catalyst emission tank 6, the bottom of catalyst emission tank 6
Connected by connecting line with catalyst detergent tank 7, the catalyst detergent tank 7 is connected to hydrogen reactor by connecting line and entered
Batch can 1 sentences the bad use that follows for realizing catalyst, and the top of reactor sampling jar 5 is connected by connecting line and recurrent canal 402
It is logical；Ethanol feed pump 8 is additionally provided with the system, the ethanol feed pump 8 outlet is connected to reaction by an additional line A9
Device feed pump is for the porch of platform 3, and reactor feed pump is for exit and the bottom outlet of reactor sampling jar 5 of platform 3
Between be additionally provided with additional line B10.
Above for the present invention basic embodiment, can more than on the basis of further improved, optimized or limited.
Such as, in the present invention, the reactor feed pump on the connecting line between the outlet of platform 3 and reactor 4 for setting
There is hand valve A301.
In the present invention, the bottom outlet end of reactor sampling jar 5 is provided with sampling valve 501.
In the present invention, it is provided between the recurrent canal 402 and reactor 4 for connecting recurrent canal 402 and reactor 4
Hand valve B403.
In the present invention, state and sampling root is provided with the connecting line between the top of reactor sampling jar 5 and recurrent canal 402
Valve 502.
The different embodiments using above-mentioned adipic dinitrile hydrogenation reaction system treatment reactor severe obstruction method are given below：
Embodiment 1
The method blocked using adipic dinitrile hydrogenation reaction system treatment reactor severe, is comprised the following steps：
1）It is first shut off hand valve A301 and sampling valve 501, opens sampling root valve 502, by reactor feed pump for platform 3, anti-
The connecting line between device sampling jar 5 and the three of recurrent canal 402 is answered to connect；
2）Ethanol feed pump 8 and reactor feed pump are opened for platform 3, and control reactor feed pump for platform 3 with 30% load,
2.7MPa outlet pressure, it is sent into ethanol as the reacted device sampling jar 5 of dilution in recurrent canal 402 and decanter 401；
3）Hand valve B403 is opened, rinses 5min, Ran Houguan between recurrent canal 402 and reactor 4 with use ethanol as dilution
Close hand valve B403, ethanol be continuously fed into recurrent canal 402 and decanter 401, with by the ethanol constantly poured in recurrent canal
402 and decanter 401 in form pressure；
4）It is rapid to open hand valve B403 after ethanol is continuously fed to continue 3min, while decanter 401 is increased to catalyst detergent
The catalyst emission amount of tank 7；
5）Repeat step 3 and step 4 operate 5 times, when the tube wall temperature of pipe 402 to be returned is gone up to 70 DEG C or so by 40-50 DEG C, then
Reactor 4 has led to.
In the step 5, when the tube wall temperature of pipe 402 to be returned is gone up to 70 DEG C or so, sampled by reactor sampling jar 5
The catalyst remained in recurrent canal 402, if catalyst particle size is not less than 600mm, reactor 4 has led to；If catalyst particle size
Less than 600mm, repeat step 3 and step 4 operate to catalyst particle size and are not less than 600mm.
Carry out step 1 into step 5 operating process, reactor feed pump 2 handles opening always, with guarantee oneself two
Hydrogenation of nitriles reaction is normally carried out.
Embodiment 2
The method blocked using adipic dinitrile hydrogenation reaction system treatment reactor severe, is comprised the following steps：
1）It is first shut off hand valve A301 and sampling valve 501, opens sampling root valve 502, by reactor feed pump for platform 3, anti-
The connecting line between device sampling jar 5 and the three of recurrent canal 402 is answered to connect；
2）Ethanol feed pump 8 and reactor feed pump are opened for platform 3, and control reactor feed pump for platform 3 with 60% load,
4.2MPa outlet pressure, it is sent into ethanol as the reacted device sampling jar 5 of dilution in recurrent canal 402 and decanter 401；
3）Hand valve B403 is opened, rinses 10min, Ran Houguan between recurrent canal 402 and reactor 4 with use ethanol as dilution
Close hand valve B403, ethanol be continuously fed into recurrent canal 402 and decanter 401, with by the ethanol constantly poured in recurrent canal
402 and decanter 401 in form pressure；
4）It is rapid to open hand valve B403 after ethanol is continuously fed to continue 5min, while decanter 401 is increased to catalyst detergent
The catalyst emission amount of tank 7；
5）Repeat step 3 and step 4 operate 7 times, when the tube wall temperature of pipe 402 to be returned is gone up to 70 DEG C or so by 40-50 DEG C, then
Reactor 4 has led to.
In the step 5, when the tube wall temperature of pipe 402 to be returned is gone up to 70 DEG C or so, sampled by reactor sampling jar 5
The catalyst remained in recurrent canal 402, if catalyst particle size is not less than 600mm, reactor 4 has led to；If catalyst particle size
Less than 600mm, repeat step 3 and step 4 operate to catalyst particle size and are not less than 600mm.
Carry out step 1 into step 5 operating process, reactor feed pump 2 handles opening always, with guarantee oneself two
Hydrogenation of nitriles reaction is normally carried out.
Embodiment 3
The method blocked using adipic dinitrile hydrogenation reaction system treatment reactor severe, is comprised the following steps：
1）It is first shut off hand valve A301 and sampling valve 501, opens sampling root valve 502, by reactor feed pump for platform 3, anti-
The connecting line between device sampling jar 5 and the three of recurrent canal 402 is answered to connect；
2）Ethanol feed pump 8 and reactor feed pump are opened for platform 3, and control reactor feed pump for platform 3 with 45% load,
3.5MPa outlet pressure, it is sent into ethanol as the reacted device sampling jar 5 of dilution in recurrent canal 402 and decanter 401；
3）Hand valve B403 is opened, rinses 8min, Ran Houguan between recurrent canal 402 and reactor 4 with use ethanol as dilution
Close hand valve B403, ethanol be continuously fed into recurrent canal 402 and decanter 401, with by the ethanol constantly poured in recurrent canal
402 and decanter 401 in form pressure；
4）It is rapid to open hand valve B403 after ethanol is continuously fed to continue 4min, while decanter 401 is increased to catalyst detergent
The catalyst emission amount of tank 7；
5）Repeat step 3 and step 4 operate 6 times, when the tube wall temperature of pipe 402 to be returned is gone up to 70 DEG C or so by 40-50 DEG C, then
Reactor 4 has led to.
In the step 5, when the tube wall temperature of pipe 402 to be returned is gone up to 70 DEG C or so, sampled by reactor sampling jar 5
The catalyst remained in recurrent canal 402, if catalyst particle size is not less than 600mm, reactor 4 has led to；If catalyst particle size
Less than 600mm, repeat step 3 and step 4 operate to catalyst particle size and are not less than 600mm.
Carry out step 1 into step 5 operating process, reactor feed pump 2 handles opening always, with guarantee oneself two
Hydrogenation of nitriles reaction is normally carried out.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is described as above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when a little change or modification made using technology contents described above
It is the equivalent embodiment of equivalent variations, as long as being the technical spirit according to the present invention without departing from technical solution of the present invention content
Any simple modification, equivalent change and modification made to above example, in the range of still falling within technical solution of the present invention.
Claims (8)
1. adipic dinitrile hydrogenation reaction system, it is characterised in that：The system includes hydrogen reactor head tank（1）, reactor feed
Pump（2）With reactor feed pump for platform（3）, reactor（4）, reactor sampling jar（5）, catalyst emission tank（6）And catalyst
Washing tank（7）, wherein, the reactor（4）Inside it is provided with decanter（401）, decanter（401）Bottom is connected with recurrent canal
（402）, the reactor feed pump（2）With reactor feed pump for platform（3）One end and hydrogen reactor head tank after parallel with one another
（1）Connection, the other end and reactor（4）Connection, the decanter（401）Side passes through connecting line and catalyst emission tank
（6）Connection, catalyst emission tank（6）Bottom passes through connecting line and catalyst detergent tank（7）Connection, the catalyst detergent tank
（7）Hydrogen reactor head tank is connected to by connecting line（1）Sentence the bad use that follows for realizing catalyst, the reactor sampling
Tank（5）Top passes through connecting line and recurrent canal（402）Connection；Ethanol feed pump is additionally provided with the system（8）, the ethanol
Feed pump（8）Outlet passes through an additional line A（9）Reactor feed pump is connected to for platform（3）Porch, and reactor feed
Pump is for platform（3）Exit and reactor sampling jar（5）Additional line B is additionally provided between bottom outlet（10）.
2. adipic dinitrile hydrogenation reaction system as claimed in claim 1, it is characterised in that：The reactor feed pump is for platform（3）
Outlet and reactor（4）Between connecting line on be provided with hand valve A（301）.
3. adipic dinitrile hydrogenation reaction system as claimed in claim 1, it is characterised in that：The reactor sampling jar（5）Bottom
Discharging end of line is provided with sampling valve（501）.
4. adipic dinitrile hydrogenation reaction system as claimed in claim 1, it is characterised in that：The recurrent canal（402）With reactor
（4）Between be provided with for connecting recurrent canal（402）And reactor（4）Hand valve B（403）.
5. adipic dinitrile hydrogenation reaction system as claimed in claim 1, it is characterised in that：The reactor sampling jar（5）Top
With recurrent canal（402）Between connecting line on be provided with sampling root valve（502）.
6. the method blocked using any adipic dinitrile hydrogenation reaction system treatment reactor severes of claim 1-5, it is special
Sign is, comprises the following steps：
1）It is first shut off hand valve A（301）And sampling valve（501）, open sampling root valve（502）, reactor feed pump is standby
Platform（3）, reactor sampling jar（5）And recurrent canal（402）Connecting line connection between three；
2）Open ethanol feed pump（8）With reactor feed pump for platform（3）, and reactor feed pump is controlled for platform（3）With 30-
60% load, 2.7-4.2MPa outlet pressure, using ethanol as the reacted device sampling jar of dilution（5）It is sent into recurrent canal
（402）And decanter（401）In；
3）Open hand valve B（403）, with use ethanol as dilution in recurrent canal（402）With reactor（4）Between rinse 5-
10min, it is then shut off hand valve B（403）, to recurrent canal（402）And decanter（401）In be continuously fed to ethanol, with by continuous
The ethanol poured in is in recurrent canal（402）And decanter（401）Middle formation pressure；
4）It is rapid to open hand valve B after ethanol is continuously fed to continue 3-5min（403）, while increase decanter（401）To catalysis
Agent washing tank（7）Catalyst emission amount；
5）Repeat step 3）With step 4）Operation 5-7 times, pipe to be returned（402）Tube wall temperature is gone up to 70 DEG C of left sides by 40-50 DEG C
When right, then reactor（4）Lead to.
7. the method blocked as claimed in claim 6 using adipic dinitrile hydrogenation reaction system treatment reactor severe, its feature
It is：The step 5）In, pipe to be returned（402）When tube wall temperature is gone up to 70 DEG C or so, pass through reactor sampling jar（5）Take
Sample remains in recurrent canal（402）Interior catalyst, if catalyst particle size is not less than 600mm, reactor（4）Lead to；If catalysis
Agent particle diameter is less than 600mm, repeat step 3）With step 4）Operation to catalyst particle size is not less than 600mm.
8. the method blocked as claimed in claim 6 using adipic dinitrile hydrogenation reaction system treatment reactor severe, its feature
It is：Carrying out step 1）To step 5）In operating process, reactor feed pump（2）Handle opening always, with guarantee oneself
Dintrile hydrogenation reaction is normally carried out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710894317.8A CN107537407B (en) | 2017-09-28 | 2017-09-28 | Adiponitrile hydrogenation reaction system and method for treating reactor heavy blockage by using same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710894317.8A CN107537407B (en) | 2017-09-28 | 2017-09-28 | Adiponitrile hydrogenation reaction system and method for treating reactor heavy blockage by using same |
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| Publication Number | Publication Date |
|---|---|
| CN107537407A true CN107537407A (en) | 2018-01-05 |
| CN107537407B CN107537407B (en) | 2020-09-22 |
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| CN201710894317.8A Active CN107537407B (en) | 2017-09-28 | 2017-09-28 | Adiponitrile hydrogenation reaction system and method for treating reactor heavy blockage by using same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109438256A (en) * | 2018-11-13 | 2019-03-08 | 中国化学赛鼎宁波工程有限公司 | A kind of production method and production system of hexamethylene diamine |
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| WO2003002246A1 (en) * | 2001-06-25 | 2003-01-09 | Institut Francais Du Petrole | Device and method for optimising the circulation of a suspension in a plant comprising a three-phase reactor |
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| CN107537407B (en) | 2020-09-22 |
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