2,6- toluene di-tert-butyl phenol antioxidant alkylated reaction device and method
Technical field
The present invention relates to the device and method that a kind of tail gas recycle is recycled, more particularly to one kind 2,6- di-t-butyls are to first
The device and method of phenolic antioxidants alkylated reaction.
Background technology
2,6- toluene di-tert-butyl phenol antioxidant(Referred to as 2,6,4)It is one kind of alkyl phenol, is to make extensively both at home and abroad
Oil-soluble inhibitor, its oxidation resistance is stronger, and heat-resisting and stability is good, can be used as feed antioxidant, rubber
Processing stabilizer after age resistor and synthetic rubber etc..
At present, a kind of method of production 2,6- toluene di-tert-butyl phenols is:Using isobutene with paracresol as raw material, with right
Toluenesulfonic acid is catalyst, and reaction is alkylated under certain temperature and pressure, is obtained containing 2,6- di-t-butyls to toluene
The mixing liquid of phenol.Need to be passed through excessive isobutene in existing alkylation process, to ensure the complete reaction of paracresol,
Contain a large amount of unreacted isobutene gas and other hydrocarbon impurities gases, such gas in the tail gas produced after alkylated reaction
Outer it need to could be discharged into after charcoal absorption processing is up to standard into atmospheric environment.
Therefore, part raw material had both been caused during existing production 2,6- toluene di-tert-butyl phenols(Isobutene)Wave
Take, while also increasing the cost of waste gas pollution control and treatment, after especially production scale expands, problem above is even more serious so that 2,6-
The production cost increase of toluene di-tert-butyl phenol, seriously constrains the production-scale expansion of 2,6- toluene di-tert-butyl phenols.
The content of the invention
It is an object of the invention to provide a kind of 2,6- di-t-butyls pair that can be reduced production cost, mitigate environmental pollution
The device and method of cresols antioxidant alkylated reaction.
To achieve the above object, the technical solution adopted by the present invention is:
The equipment of one kind 2,6- toluene di-tert-butyl phenol antioxidant alkylated reactions, it is characterized in that, including it is multiple mutual
The reaction member of series winding, each reaction member includes being installed with heated at constant temperature agitator in reactor, reactor, reaction
Kettle is closed to be communicated with tail gas recycle entrance and gas outlet, and gas outlet is closed to be communicated with automatic switch, and reactor is also closed to be communicated with
Control on the tail gas recycle entrance and another reactor on the pressure inductor of automatic switch break-make, one of reactor
It is closed between automatic switch to be communicated with airtight connection on communicating pipe, communicating pipe and have unilaterally connected valve.
According to the equipment of described 2,6- toluene di-tert-butyl phenol antioxidant alkylated reactions, it is characterized in that, the equipment
Including three reaction members.
The method of one kind 2,6- toluene di-tert-butyl phenol antioxidant alkylated reactions, it is characterized in that, use above-mentioned 2,6-
The equipment that the tail gas recycle that toluene di-tert-butyl phenol antioxidant alkylated reaction is produced is recycled, step is as follows:
First the measured paracresol of standard meter and p-methyl benzenesulfonic acid are added in first reactor, it is closed after vacuumize and subtract
Pressure, is passed through the isobutene of vaporization;When reaction occurs malleation close in complete, reactor in first reactor and pressure continues
During rising, stopping is passed through isobutene;Second reactor and first reactor, the 3rd reactor and second reactor
Alkylated reaction time control is staggered half of reaction time, after first reactor reaction carries out half of reaction time, and second
Individual reactor proceeds by alkylated reaction, after second reactor reaction carries out half of reaction time, the 3rd reactor
Alkylated reaction is proceeded by, the like, circulation is carried out.
When the pressure in first reactor reaches 0.08~0.10 MPa, the pressure inductor control being attached thereto
Automatic switch is opened, and the on-condensible gas containing isobutene is flowed into by unilaterally connected valve and is in negative pressure state in first reactor
Second reactor, isobutene therein participates in reaction as the raw material of second reactor, the like.
When the gas pressure in first reactor drops to 0~0.001MPa, the pressure inductor control being attached thereto
The automatic switch of system is closed, and second reactor continues to react;The reaction of second reactor close to it is complete when, the 3rd is reacted
Kettle reaction proceeds to half of reaction time, the like.
To during the half-reaction cycle of the 3rd reactor after second reactor half-reaction cycle, first reactor
The alkylation liquid inside obtained completes cooling, exhaust and blowing, and completes the fill process of second of alkylated reaction, starts second
Alkylated reaction, the like.
The present invention provided with three reactors, first with second reactor, second with the 3rd reactor, the 3rd
Stagger successively half of reaction time with the alkylated reaction of first reactor, when the alkylated reaction in first reactor
Between reach after half of reaction time, the alkylated reaction in second reactor starts;When the pressure in first reactor reaches
During to 0.08~0.10MPa, the automatic switch for the pressure inductor control being attached thereto is opened, and is contained in first reactor
The on-condensible gases such as isobutene are entered in second reactor by the unidirectional connection valve being attached thereto to be participated in reacting;When first it is anti-
When answering the gas pressure in kettle to drop to 0~0.001MPa, the automatic switch for the pressure inductor control being attached thereto is closed;When
When pressure in second reactor reaches 0.08~0.10MPa, the automatic switch for the pressure inductor control being attached thereto is beaten
Open, the on-condensible gas such as isobutene contained in second reactor enters the 3rd reaction by the unidirectional connection valve being attached thereto
Reaction is participated in kettle;When the gas pressure in second reactor drops to 0~0.001MPa, the pressure sensitive being attached thereto
The automatic switch of device control is closed;Such circular response successively.
To during the half-reaction cycle of the 3rd reactor after second reactor half-reaction cycle, in the first reactor
Obtained alkylation liquid completes cooling, exhaust, blowing, and completes the fill process of second of alkylated reaction, starts second of alkane
Glycosylation reaction, the like.
The equipment as a production unit, staggers three reactors half successively between each two reactor during production
Reaction time, the alkylation tail gas produced after the completion of each reactor reaction will be therein different by the communicating pipe between two reactors
Butene recovery is recycled, to reach the purpose of reduction production cost.
Beneficial effects of the present invention are as follows:
By the recycling to tail gas in alkylation process, the discharge of alkylation tail gas can be greatly lowered
Amount, the isobutene tail gas of recovery can enter course of reaction as raw material, therefore save raw material, be controlled while also saving tail gas
The correlative charges of reason, so as to reduce production cost.
Compared with prior art, alkylated reaction cycle about 1.5h can be shortened using apparatus and method of the present invention, can
Accelerate material circulation, so as to increase economic efficiency.
Compared with prior art, often produce 1 ton of 2,6- toluene di-tert-butyl phenols antioxidant product can recycle it is different
About 0.023 ton of butylene, according to charcoal absorption tail gas, then can reduce about 0.05 ton of the usage amount of activated carbon, while reducing outer
0.0012 ton of the isobutene into atmospheric environment is discharged into, the pollution to environment is alleviated.
Brief description of the drawings
Fig. 1 is that arrow show the clear and coherent sequence of tail gas stream and reaction cycle in the structural representation of equipment of the present invention, figure
The direction of progress.
In accompanying drawing:
1st, tail gas recycle entrance;2nd, reactor;3rd, heated at constant temperature agitator;4th, pressure inductor;5th, gas outlet;6th, it is automatic
Switch;7th, unilaterally connected valve;8th, communicating pipe.
Embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings:
The equipment of one kind 2,6- toluene di-tert-butyl phenol antioxidant alkylated reactions, as shown in figure 1, including multiple mutual
The reaction member of series winding, each reaction member includes being installed with heated at constant temperature agitator 3 in reactor 2, reactor 2,
Reactor 2 is closed to be communicated with tail gas recycle entrance 1 and gas outlet 5, and gas outlet 5 is closed to be communicated with automatic switch 6, and reactor 2 is also
The closed pressure inductor 4 for being communicated with the control break-make of automatic switch 6, tail gas recycle entrance 1 on one of reactor 2 with it is another
It is closed between automatic switch 6 on one reactor 2 to be communicated with airtight connection on communicating pipe 8, communicating pipe 8 and have unilaterally connected valve 7.
In the present embodiment, the equipment includes three reaction members.
The method of one kind 2,6- toluene di-tert-butyl phenol antioxidant alkylated reactions, uses above-mentioned 2,6- di-t-butyls
The equipment that the tail gas recycle that p-cresol antioxidant alkylated reaction is produced is recycled, step is as follows:
First the measured paracresol of standard meter and p-methyl benzenesulfonic acid are added in first reactor, it is closed after vacuumize and subtract
Pressure, is passed through the isobutene of vaporization;When reaction occurs malleation close in complete, reactor in first reactor and pressure continues
During rising, stopping is passed through isobutene;Second reactor and first reactor, the 3rd reactor and second reactor
Alkylated reaction time control is staggered half of reaction time, after first reactor reaction carries out half of reaction time, and second
Individual reactor proceeds by alkylated reaction, after second reactor reaction carries out half of reaction time, the 3rd reactor
Alkylated reaction is proceeded by, the like, circulation is carried out.
When the pressure in first reactor reaches 0.08~0.10 MPa, the pressure inductor control being attached thereto
Automatic switch is opened, and the on-condensible gas containing isobutene is flowed into by unilaterally connected valve and is in negative pressure state in first reactor
Second reactor, isobutene therein participates in reaction as the raw material of second reactor, the like.
When the gas pressure in first reactor drops to 0~0.001MPa, the pressure inductor control being attached thereto
The automatic switch of system is closed, and second reactor continues to react;The reaction of second reactor close to it is complete when, the 3rd is reacted
Kettle reaction proceeds to half of reaction time, the like.
To during the half-reaction cycle of the 3rd reactor after second reactor half-reaction cycle, first reactor
The alkylation liquid inside obtained completes cooling, exhaust and blowing, and completes the fill process of second of alkylated reaction, starts second
Alkylated reaction, the like.
The present invention has three reactors in alkylated reaction process, regard three alkylated reaction kettles as a production
A communicating pipe passed through for isobutene, the throwing per two neighboring reactor are devised between unit, every two neighboring reactor
Material time control is staggered half of reaction time successively.
First the measured paracresol of standard meter and p-methyl benzenesulfonic acid are added in first reactor during production, it is closed after take out true
Sky decompression, is passed through the isobutene of vaporization.To accelerate reaction speed, the present invention is had single at present using the replacement of heated at constant temperature agitator
The agitator of one agitating function, to shorten the reaction time of alkylation.When the close complete, reactor of reaction in first reactor
Inside there is malleation and when pressure persistently rises, stopping is passed through isobutene.
The alkylated reaction time of second reactor and first reactor, the 3rd reactor and second reactor
Control is staggered half of reaction time, and reaction principle is constant.After first reactor reaction carries out half of reaction time, second
Reactor proceeds by alkylated reaction, and after second reactor reaction carries out half of reaction time, the 3rd reactor is opened
Beginning is alkylated reaction, the like, circulation is carried out.
When the pressure in first reactor reaches 0.08~0.10 MPa, the pressure inductor control being attached thereto
Automatic switch is opened, and the on-condensible gas containing isobutene is flowed into by unilaterally connected valve and is in negative pressure state in first reactor
Second reactor, isobutene therein participates in reaction as the raw material of second reactor, the like.
When the gas pressure in first reactor drops to 0~0.001MPa, the pressure inductor control being attached thereto
The automatic switch of system is closed, and second reactor continues to react;The reaction of second reactor close to it is complete when, the 3rd is reacted
Kettle reaction proceeds to half of reaction time, the like.To the 3rd reactor after second reactor half-reaction cycle
During the half-reaction cycle, the alkylation liquid obtained in first reactor completes cooling, exhaust and blowing, and completes the second alkylidene
Change the fill process of reaction, start second of alkylated reaction, the like.
When occurring malleation in second reactor and pressure persistently rises, stopping is passed through isobutene, when second reaction
When pressure in kettle reaches 0.08~0.10 MPa, the automatic switch for the pressure inductor control being attached thereto is opened, second
The on-condensible gas containing isobutene is flowed into just in alkylated reaction progress by the unilaterally connected valve being attached thereto in reactor
, the 3rd reactor in negative pressure state;When the gas pressure in second reactor drops to 0~0.001MPa,
The automatic switch for the pressure inductor control being attached thereto is closed, successively circular response, and connection dress is reclaimed by unidirectional isobutene
Put(Communicating pipe)It is recyclable and using the excess isobutylene gas being passed through in alkylation process, effective reduction alkylation tail gas
The discharge of middle isobutene.
In the present invention, the heated at constant temperature agitator in each reaction member is corresponded with reactor, three reactors
Between communicating pipe on be unilaterally connected valve, automatic switch is by pressure inductor control, and pressure inductor reactor is corresponded.
At a set temperature, heated at constant temperature agitator is heated to the reactant in reactor, is stirred simultaneously, accelerates material anti-
Speed is answered, after reaction stopping, heating and stirring operation synchronously stop.The alkylation tail gas produced in reactor passes through along connecting tube
Unilaterally connected valve unidirectionally flows out, into the tail gas recycle entrance for the next reactor being connected with the reactor.Pressure inductor
Sense the air pressure in reactor, when air pressure reaches the pressure value of setting, the automatic switch that pressure inductor control is attached thereto
Carry out break-make.Automatic switch is connected with pressure inductor, and open and-shut mode is controlled by the pressure change in reactor.Unilaterally connected
Valve was arranged on the communicating pipe between the tail gas recycle entrance of adjacent reaction kettle and gas outlet, the direction of its direction and exhaust gas flow
Unanimously, its effect is to ensure that direction flowing of the tail gas along setting.Communicating pipe be connect adjacent reaction kettle tail gas recycle entrance with
Gas outlet pipeline.
The present invention in alkylation process along with reacting kettle inner pressure change, by pressure inductor control from
The opening and closing of dynamic switch, passes through the unilaterally connected valve between three reactors, it is ensured that the flowing of the on-condensible gas containing isobutene by
Higher-pressure region flows to low-pressure area, makes the isobutene contained in alkylation tail gas as raw material and sequentially enters next reactor.This hair
The bright recycling to being alkylated tail gas can save material, and save the correlative charges for the treatment of tail gas, reduce production cost, together
When reduce pollution of the exhaust emissions to environment;And the present invention can shorten alkylated reaction cycle about 1.5h, can accelerate material
Circulation, so as to increase economic efficiency.