CN107551958B - The switching method of reactor for epoxidation reaction - Google Patents
The switching method of reactor for epoxidation reaction Download PDFInfo
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- CN107551958B CN107551958B CN201710981371.6A CN201710981371A CN107551958B CN 107551958 B CN107551958 B CN 107551958B CN 201710981371 A CN201710981371 A CN 201710981371A CN 107551958 B CN107551958 B CN 107551958B
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Abstract
The present invention relates to a kind of switching method of reactor for epoxidation reaction, mainly solve the problems, such as that operation element amount is big in the prior art, security reliability is poor.The present invention by using a kind of reactor for epoxidation reaction switching method, reactor is carried out to the automatic switchover of nominal situation and regeneration regime, retain original interlock, without manual hand manipulation, the technical solution that nominal situation and regeneration regime switching time were reduced to 0.1 second from 80~120 seconds preferably solves the above problem, can be used in the automatic switchover of propylene oxide unit reactor.
Description
Technical field
The present invention relates to a kind of switching methods of reactor for epoxidation reaction.
Background technique
In the process unit production process of peroxide passivation production propylene oxide, epoxidation heat-producing chemical reaction occurs,
The heat needs of reaction are withdrawn, to guarantee that chemical reactor can continuous, steady, reliably and securely be run.It is in the prior art
A kind of mixed aerosol device cooling protection system of entrained-flow reactor of CN200910259974.0, discloses the system by 12
Subsystem composition, can effective protection equipment, improve the utilization of capacity of entrained-flow reactor, the safety of support personnel and equipment.
CN201620097954.3 is suitable for the serialization security reaction device that rate of heat release is fast and thermal discharge is big, and it is anti-to disclose a kind of safety
Device is answered, which can improve working environment, and safe and reliable.CN201310683291.4 prepares propylene oxide
Method discloses propylene and is mixed into each of the process unit containing n tandem reactor with hydrogen peroxide raw material and reacts
Device can isolate the reactor after one of reactor catalyst inactivation from process unit, carry out catalyst regeneration behaviour
The technical solution of work.
In the prior art, CN200910259974.0 and CN201620097954.3 is disclosed only in normal operating operating condition
The method of lower safety operation, due to only considering the defencive function under normal operating operating condition, once reactor enters regenerative operation work
Condition needs for reactor to be switched out from process flow, is transferred to manual mode, could complete the regenerative operation of reactor.
Although CN201310683291.4 discloses the method for normal operating operating condition switching regenerative operation operating condition, but this method needs greatly
Valve combination is measured, construction investment is high, and is still manual switching.So needing to react when prior art reactor regenerates
The interlocking of device is switched to bypass, and reactor lacks interlock protection at this time, or needs artificial to arrive part valve imperative operation
"ON" or off position, operation element amount are big, it is also possible to the dangerous situation of human operational error occur.The prior art as a result,
There is a problem of that construction investment is high, operation element amount is big, security reliability is poor.
Summary of the invention
The technical problem to be solved by the present invention is to the problem that operation element amount is big, security reliability is poor in the prior art,
A kind of new switching method of reactor for epoxidation reaction is provided, it is small with operation element amount, security reliability is good
Advantage.
To solve the above problems, The technical solution adopted by the invention is as follows: a kind of reactor for epoxidation reaction
Switching method, two kinds of operation modes of design " bringing normally into operation " and " regeneration is run ", two different operation modes can be in auto-controlling apparatus
One key switching is realized on the active station or auxiliary operation platform of table；Under " bringing normally into operation " mode, calandria type fixed bed reactor
Interlock protection function operate normally, can satisfy completely protection process equipment requirement；And when switching to " regeneration operation ", it should
Reactor enters special regeneration regime interlock protection state, and interlock original at this time includes following several mapping modes:
(1) calandria type fixed bed reactor and its protection of the temperature runaway of outlet still have, but the setting value for interlocking temperature changes automatically
Protection value when to regenerate；(2) the low-pressure protection of cooling cooling water still has, and surpasses caused by preventing cooling cooling water from stopping transport
It is warm dangerous；(3) when regenerating, the process stream of reactor stops charging, and feed rate protection will be no longer valid by auto by pass,
Reactor maloperation is fed when regeneration is run in order to prevent simultaneously, and process stream charging/discharging valve goalkeeper forces to close by interlock system
It closes；(4) reactor design entrance to outlet regeneration by-pass line, under " regeneration operation " operation mode, by by-pass line valve
It automatically opens, when guaranteeing reactor regenerative operation, main flow still " bringing normally into operation "；(5) when reactor regenerates, all meetings are indirectly
The signal of triggering other position interlockings of main flow movement is all bypassed and invalidation；(6) scram of process other parts
Signal will not influence the regenerative operation of reactor.
In above-mentioned technical proposal, it is preferable that epoxidation reaction is that peroxide passivation prepares propylene oxide, propylene oxide unit column
The reaction temperature of tubular fixed-bed reactor " bringing normally into operation " operation mode be 10~100 DEG C, reaction pressure be 1.0~
5.0MPaG, 0.2~9.0h of propylene weight air speed-1；The regeneration temperature of " regeneration operation " operation mode is 200~260 DEG C, regeneration
Pressure is 0.4~2.0MPaG.
In above-mentioned technical proposal, it is preferable that " bringing normally into operation " operation mode: propylene feedstocks and hydrogen peroxide raw material (11) pass through
Feed rate measures the material (12) that FT1 and feed rate control valve FV1 is constant flow rate and enters calandria type fixed bed reaction
Device R1 pipe side, under the action of catalyst, material (12) carry out epoxidation reaction, generate propylene oxide material (13) and pass through reactor effluent stream
Adjustable valve door FV2 is that the material (14) of constant flow rate is sent out, and reactor R1 bypass valve UV1 is closed, and reaction temperature is by anti-
The temperature on device R1 is answered to measure the measurement that TT1 carries out temperature；The heat that epoxidation reaction is released is removed by cooling cooling water, is pressurized
Cooling cooling water (24) enter calandria type fixed bed reactor R1 shell-side, absorbing reaction heat simultaneously is partially vaporizated into vapour-liquid two-phase flow
(21) drum D1 is entered, vapor-liquid separation is carried out in drum D1, is sent outside from the top drum D1 outflow steam (22)；From drum D1
It is cooling cooling water (24) that cooling cooling water (23) are flowed out by forced circulation pump P1 pressurization in lower part, the pressure of cooling cooling water by
The measurement of pressure measurement PT1 progress pressure.
In above-mentioned technical proposal, it is preferable that " regeneration operation " operation mode: reactor R1 feed rate control valve FV1
It closes, reactor R1 discharging flow control valve FV2 is closed, and reactor R1 bypass valve UV1 is opened.
In above-mentioned technical proposal, it is preferable that catalyst is TS-1 type titanium-silicon molecular sieve catalyst, and titanium silicon ratio is SiO2: TiO2
=10~200.
Switching method using the present invention for the reactor of epoxidation reaction designs " bringing normally into operation " and " regeneration is run "
Two kinds of operation modes, in two kinds of mutual handoff procedures of operation mode, the interlock protection function of " bringing normally into operation " reactor is normal
Operation meets the requirement of protection process equipment；" regeneration operation " reactor is retaining necessary interlock, without additional artificial
Manual operation requires, and reactor is cut out automatically from main flow, entire process flow still bringing normally into operation；Two kinds of operation moulds
The switching time of formula was reduced to 0.1 second from 80~120 seconds；Construction investment is thus reduced, reduces operation element amount, improve
Security reliability achieves preferable technical effect, achieves preferable technical effect.
Detailed description of the invention
Fig. 1 is the process flow diagram of " bringing normally into operation " operation mode；
Fig. 2 is the process flow diagram of " regeneration operation " operation mode.
Fig. 1, in 2,11 propylene and hydrogen peroxide raw material, 12 propylene and hydrogen peroxide raw material, 13 propylene oxide materials, 14 epoxies third
Alkane material, 21 vapour-liquid two-phase cooling cooling waters, 22 steam, 23 cooling cooling waters, 24 cooling cooling waters, R1 are calandria type fixed bed anti-
Answer device, D1 drum, P1 forced circulation pump, the measurement of FT1 feed rate, the measurement of TT1 reaction temperature, the survey of PT1 cooling cooling water pressure
Amount, FV1 feed rate control valve, FV2 discharging flow control valve, UV1 bypass valve.
" bringing normally into operation " operation mode: propylene feedstocks and hydrogen peroxide raw material 11 are by feed rate measurement FT1 and feeding flow
Adjustable valve door FV1 is that the material 12 of constant flow rate enters calandria type fixed bed reactor R1 pipe side, under the action of catalyst, object
Material 12 carries out epoxidation reaction, generates material of the propylene oxide material 13 by discharging flow control valve FV2 for constant flow rate
14 send out, and reactor R1 bypass valve UV1 is closed, and reaction temperature carries out temperature by the temperature measurement TT1 on reactor R1
Measurement.The heat that epoxidation reaction is released is removed by cooling cooling water, and the cooling cooling water 24 of pressurization enters calandria type fixed bed
Reactor R1 shell-side, absorbing reaction heat are simultaneously partially vaporizated into vapour-liquid two-phase flow 21 and enter drum D1, and vapour is carried out in drum D1
Liquid separation, from the top drum D1, outflow steam 22 is sent outside；From the lower part drum D1, outflow cooling cooling water 23 passes through forced circulation pump
P1 pressurization is cooling cooling water 24, and the pressure of cooling cooling water is carried out the measurement of pressure by pressure measurement PT1.
" regeneration operation " operation mode: reactor R1 feed rate control valve FV1 is closed, reactor R1 discharging flow tune
It saves valve FV2 to close, reactor R1 bypass valve UV1 is opened.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
[comparative example 1]
Prior art production scale is the process unit that 100,000 tons/year of peroxide passivations produce propylene oxide, " bringing normally into operation "
In " regeneration is run " mutual handoff procedure of operation mode, using manual hand manipulation, a large amount of valve combinations, handoff procedure are needed
The time 80 seconds are spent, construction investment is high, operation element amount is big, security reliability is poor.
[embodiment 1]
Switching method of the present invention for the reactor of epoxidation reaction, as shown in Figure 1 and Figure 2.Production scale is 100,000
The process unit of ton/year peroxide passivation production propylene oxide, " bringing normally into operation " operation mode: propylene feedstocks and hydrogen peroxide raw material 11
Enter by the material 12 that feed rate measurement FT1 and feed rate control valve FV1 is constant flow rate calandria type fixed bed anti-
Device R1 pipe side is answered, under the action of catalyst, material 12 carries out epoxidation reaction, generates propylene oxide material 13 and passes through discharging flow
Control valve FV2 is that the material 14 of constant flow rate is sent out, and reactor R1 bypass valve UV1 is closed, and reaction temperature is by reactor
Temperature measurement TT1 on R1 carries out the measurement of temperature.The heat that epoxidation reaction is released is removed by cooling cooling water, and pressurization is removed
Hot cooling water 24 enters calandria type fixed bed reactor R1 shell-side, and absorbing reaction heat is simultaneously partially vaporizated into the entrance of vapour-liquid two-phase flow 21
To drum D1, vapor-liquid separation is carried out in drum D1, outflow steam 22 is sent outside from the top drum D1；From the lower part drum D1, outflow is removed
Hot cooling water 23 is cooling cooling water 24 by forced circulation pump P1 pressurization, the pressure of cooling cooling water by pressure measurement PT1 into
The measurement of row pressure.The reaction temperature of reactor is 70 DEG C, reaction pressure 4.0MPaG, propylene weight air speed 6.0h-1, catalysis
Agent is TS-1 type titanium-silicon molecular sieve catalyst, and titanium silicon ratio is SiO2: TiO2=55." regeneration operation " operation mode: reactor R1 into
Expect that flow control valve FV1 is closed, reactor R1 discharging flow control valve FV2 is closed, and reactor R1 bypass valve UV1 is beaten
It opens.The regeneration temperature of reactor is 220 DEG C, regeneration pressure 0.8MPaG.
The method automatically switched as a result, using the present invention, " bringing normally into operation " are mutually switched with " regeneration is run " operation mode
In the process, a large amount of valve combinations are not needed, handoff procedure spends the time 0.1 second, and construction investment is low, operation element amount is small, safety
Good reliability.The selectivity of propylene oxide reaches 97.0% or more, and product propylene purity reaches 99.95% or more.
[comparative example 2]
Prior art production scale is the process unit that 200,000 tons/year of peroxide passivations produce propylene oxide, " bringing normally into operation "
In " regeneration is run " mutual handoff procedure of operation mode, using manual hand manipulation, a large amount of valve combinations, handoff procedure are needed
The time 100 seconds are spent, construction investment is high, operation element amount is big, security reliability is poor.
[embodiment 2]
With [embodiment 1], only production scale is changed to 200,000 tons/year, the method automatically switched using the present invention, " normal
Put into operation " with " regeneration is run " mutual handoff procedure of operation mode, a large amount of valve combinations are not needed, handoff procedure spends the time
0.1 second, construction investment was low, operation element amount is small, security reliability is good.The selectivity of propylene oxide reaches 97.0% or more, ring
Ethylene Oxide product purity reaches 99.95% or more.
[comparative example 3]
Prior art production scale is the process unit that 300,000 tons/year of peroxide passivations produce propylene oxide, " bringing normally into operation "
In " regeneration is run " mutual handoff procedure of operation mode, using manual hand manipulation, a large amount of valve combinations, handoff procedure are needed
The time 120 seconds are spent, construction investment is high, operation element amount is big, security reliability is poor.
[embodiment 3]
With [embodiment 1], only production scale is changed to 300,000 tons/year, the method automatically switched using the present invention, " normal
Put into operation " with " regeneration is run " mutual handoff procedure of operation mode, a large amount of valve combinations are not needed, handoff procedure spends the time
0.1 second, construction investment was low, operation element amount is small, security reliability is good.The selectivity of propylene oxide reaches 97.0% or more, ring
Ethylene Oxide product purity reaches 99.95% or more.
[embodiment 4]
With [embodiment 1], only process operation parameter changes, " bringing normally into operation " operation mode: the reaction temperature of reactor
It is 10 DEG C, reaction pressure 1.0MPaG, propylene weight air speed 0.2h-1, catalyst is TS-1 type titanium-silicon molecular sieve catalyst, titanium
Silicon ratio is SiO2: TiO2=10." regeneration operation " operation mode: regeneration temperature is 200 DEG C, regeneration pressure 0.4MPaG.Using
The method that the present invention automatically switches, " bringing normally into operation " do not need a large amount of with " regeneration is run " mutual handoff procedure of operation mode
Valve combination, handoff procedure spend the time 0.1 second, and construction investment is low, operation element amount is small, security reliability is good.Propylene oxide
Selectivity reach 97.0% or more, product propylene purity reaches 99.95% or more.
[embodiment 5]
With [embodiment 1], only process operation parameter changes, " bringing normally into operation " operation mode: the reaction temperature of reactor
It is 100 DEG C, reaction pressure 5.0MPaG, propylene weight air speed 9.0h-1, catalyst is TS-1 type titanium-silicon molecular sieve catalyst, titanium
Silicon ratio is SiO2: TiO2=200." regeneration operation " operation mode: regeneration temperature is 260 DEG C, regeneration pressure 2.0MPaG.Using
The method that the present invention automatically switches, " bringing normally into operation " do not need a large amount of with " regeneration is run " mutual handoff procedure of operation mode
Valve combination, handoff procedure spend the time 0.1 second, and construction investment is low, operation element amount is small, security reliability is good.Propylene oxide
Selectivity reach 97.0% or more, product propylene purity reaches 99.95% or more.
Claims (5)
1. a kind of switching method of the reactor for epoxidation reaction, two kinds of operations of setting " bringing normally into operation " and " regeneration is run "
Mode, two different operation modes can realize one key switching on the active station or auxiliary operation platform of automatic instrument(s)；" just
Often put into operation " under mode, the interlock protection function of calandria type fixed bed reactor operates normally, and can satisfy protection technique completely and sets
Standby requirement；And when switching to " regeneration operation ", which enters special regeneration regime interlock protection state, originally at this time
Interlock include following several mapping modes: (1) calandria type fixed bed reactor and its temperature runaway of outlet protection still deposits
, but the setting value for interlocking temperature is automatically changed to protection value when regenerating；(2) low-pressure of cooling cooling water is protected still
In the presence of overtemperature caused by preventing cooling cooling water from stopping transport is dangerous；(3) process stream of reactor stops charging, charging when regenerating
Traffic protection will be no longer valid by auto by pass, while regenerate reactor maloperation when running in order to prevent and feeding, process stream
Charging/discharging valve goalkeeper is forcibly closed by interlock system；(4) regeneration by-pass line of the setting reactor inlet to outlet, " regeneration
By-pass line valve is automatically opened under operation " operation mode, guarantees that main flow is still " normal to throw when reactor regenerative operation
Fortune "；(5) when reactor regenerates, all signals that can trigger other position interlockings of main flow movement indirectly, which are all bypassed, to be had no
Effectization；(6) fault stop signal of process other parts will not influence the regenerative operation of reactor.
2. the switching method for the reactor of epoxidation reaction according to claim 1, it is characterised in that epoxidation reaction
Propylene oxide, the reaction of propylene oxide unit calandria type fixed bed reactor " bringing normally into operation " operation mode are prepared for peroxide passivation
Temperature is 10~100 DEG C, and reaction pressure is 1.0~5.0MPaG, 0.2~9.0h of propylene weight air speed-1；" regeneration operation " operation
The regeneration temperature of mode is 200~260 DEG C, and regeneration pressure is 0.4~2.0MPaG.
3. the switching method of the reactor according to claim 1 or claim 2 for epoxidation reaction, it is characterised in that " normal to throw
Fortune " operation mode: propylene feedstocks and hydrogen peroxide raw material (11) are by feed rate measurement (FT1) and feed rate control valve
(FV1) enter calandria type fixed bed reactor (R1) pipe side, under the action of catalyst, material for the material (12) of constant flow rate
(12) epoxidation reaction is carried out, generating propylene oxide material (13) by discharging flow control valve (FV2) is constant flow rate
Material (14) is sent out, and reactor (R1) bypass valve (UV1) is closed, and reaction temperature is measured by the temperature on reactor (R1)
(TT1) measurement of temperature is carried out；The heat that epoxidation reaction is released is removed by cooling cooling water, the cooling cooling water (24) of pressurization
Into calandria type fixed bed reactor (R1) shell-side, absorbing reaction heat is simultaneously partially vaporizated into vapour-liquid two-phase flow (21) and enters drum
(D1), vapor-liquid separation is carried out in drum (D1), is sent outside from the drum top (D1) outflow steam (22)；It is flowed from the drum lower part (D1)
Cooling cooling water (23) is cooling cooling water (24) by forced circulation pump (P1) pressurization out, and the pressure of cooling cooling water is by pressure
Measure the measurement that (PT1) carries out pressure.
4. the switching method for the reactor of epoxidation reaction according to claim 1, it is characterised in that " regeneration operation "
Operation mode: reactor (R1) feed rate control valve (FV1) is closed, reactor (R1) discharging flow control valve (FV2)
It closes, reactor (R1) bypass valve (UV1) is opened.
5. the switching method for the reactor of epoxidation reaction according to claim 3, it is characterised in that catalyst TS-
1 type titanium-silicon molecular sieve catalyst, titanium silicon ratio are SiO2: TiO2=10~200.
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| CN109289721B (en) * | 2018-10-12 | 2021-07-16 | 胜帮科技股份有限公司 | Device and method for quickly taking away reaction heat in preparation of propylene oxide by HPPO method |
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