CN105664801B - A kind of gas/liquid feed switched device and heavy organic matter pyrolysis installation - Google Patents
A kind of gas/liquid feed switched device and heavy organic matter pyrolysis installation Download PDFInfo
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- CN105664801B CN105664801B CN201610246204.2A CN201610246204A CN105664801B CN 105664801 B CN105664801 B CN 105664801B CN 201610246204 A CN201610246204 A CN 201610246204A CN 105664801 B CN105664801 B CN 105664801B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00132—Controlling the temperature using electric heating or cooling elements
- B01J2219/00135—Electric resistance heaters
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Abstract
The invention discloses a kind of gas/liquid feed switched device and heavy organic matter pyrolysis installations, the feeding device includes wet tank and one end is used to connect feeder, the other end is used to connect the inlet ductwork of materials equipment, inlet ductwork is equipped with the selector valve device at least four nozzles, two of them nozzle is separately connected the air inlet and liquid outlet of wet tank, and liquid outlet is equipped with the outlet tube for going deep into bottom inside wet tank；Selector valve device makes gas be directly entered materials equipment along inlet ductwork or gas is made to enter wet tank for its internal liquid along inlet ductwork indentation materials equipment for switching.The feeding device realizes that gas and liquid feedstock, equipment are more compact using same inlet ductwork；The driving device of liquid feedstock is eliminated, gas itself does not lose；Adjusting selector valve device can be realized the switching of gas/liquid charging, easy to operate, it is easy to accomplish automation control when materials equipment needs continuously or to be repeatedly alternately repeated charging.
Description
Technical field
The invention belongs to heavy organic matter pyrolytic technique fields, and in particular to a kind of gas/liquid feed switched device, together
When further relate to a kind of heavy organic matter pyrolysis installation using above-mentioned feeding device.
Background technique
Heavy organic matter is resource important on the earth, including coal, biomass, heavy oil, pitch and organic solid castoff
Deng.The main body of these heavy organic matters is organic macromolecule, the heterogeneous property with height, is insoluble in Conventional solvents under room temperature,
Basic utilization ways are to be converted into its macromolecular by thermal depolymerization and all kinds of isolation technics and prepare the small of various chemical products
Molecule intermediate, relevant technique research and development are related to skill elements, the relevant equipment such as pyrolysis, extraction heat, heat filter and fractionation and are related to
All kinds of autoclaves, extraction equipment and distilling apparatus.
The thermal decomposition product of heavy organic matter is gas-liquid-solid three-phase mixture, at the reaction temperatures viscosity it is low, it is easy to dissolve, extraction
Take and filter, but three-phase is mixing cured at normal temperature or semi-solid preparation together, it is difficult to the volatile component for separating, and generating, drop
It is distilled again under temperature to room temperature, each unit technology is performed separately, low efficiency and effect is poor.
In the prior art, CN204544144U discloses a kind of thermosol kettle with microporous filter, including thermosol kettle
Autoclave body, the cooling coil and steam-heating pipe being set in thermosol kettle autoclave body；It is provided with stirring shaft in the thermosol kettle autoclave body,
3 paddle slurries are provided on stirring shaft；The thermosol kettle autoclave body bottom increase has the micro porous filtration for filter activity charcoal
Device, microporous filter are matched with thermosol kettle inner wall of kettle.Microporous filter is arranged in thermosol kettle the device, uses
In filter activity charcoal, equipment investment is small, and occupied area is small, realizes the pyrolysis of organic matter to a certain extent.
But the pyrolysis and separation process due to heavy organic matter are more complicated, during which need or continuously or discontinuously or more
Gas or liquid are alternately injected in secondary repetition into reaction kettle, and gas is generally used for maintaining the pressure of reaction system or aeration mixed
It closes, liquid can be solvent, extractant, cleaning agent etc..
In the prior art, CN104877697A discloses a kind of equipment that disintegration produces tar waste solid-liquid ingredient, including
Extraction kettle, distillation still, material kettle, surge tank, solidification tar tank, tar light oil tank, extractant tank, No.1 condenser, No. two it is cold
The material outlet of condenser, vacuum pump and air compressor, the material pot is connected with the material inlet of extraction kettle by material pipeline,
The extractant outlet of the extractant tank is connected with the extractant entrance of extraction kettle by extractant supply line, the extraction kettle
Compressed air inlet is connected with air compressor by compressed air supply line.It can be seen that tradition from equipment disclosed above
Reaction kettle feeding device be all that material, gas and liquid are provided separately individual pipeline, cause materials equipment nozzle more, connect
Pipeline is more, not compact enough；Liquid feedstock needs special driving equipment, at high cost；As needed in reaction kettle continuous work repeatedly
It is alternately repeated gas, liquid feedstock, then the equipment and valve for needing to control and adjust are more, are not easy to realize that continuous and automatic is grasped
Make.
Summary of the invention
The object of the present invention is to provide a kind of gas/liquid feed switched device, liquid feedstock is not required to additional driving dress
It sets, easy switching, it is easy to accomplish continuous production.
A second object of the present invention is to provide a kind of heavy organic matter pyrolysis installations using above-mentioned feeding device.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
A kind of gas/liquid feed switched device, including wet tank and one end are for connecting feeder, the other end is used
In the inlet ductwork of connection materials equipment, the inlet ductwork is equipped with selector valve device, and the selector valve device has at least
Four nozzles, two of them nozzle are connected in inlet ductwork, and another two nozzle is separately connected the air inlet of wet tank and goes out
Liquid mouth, the liquid outlet are equipped with the outlet tube for going deep into bottom inside wet tank；Selector valve device for switch make gas along into
Mouth pipeline is directly entered materials equipment, or so that gas is entered wet tank and set its internal liquid along inlet ductwork indentation materials
It is standby.
Preferably, the selector valve device is four-way valve.The selector valve device can also be that other in this field can be real
The valve module of existing handoff functionality.
The wet tank, which is equipped with below liquidometer or wet tank, is equipped with weighing device, for monitor liquid into
Doses.
Along gas flow direction, gas flowmeter is equipped in the upstream of four-way valve in the inlet ductwork；The inlet tube
Road is additionally provided with pressure reducing valve and check valve in the upstream of gas flowmeter.
Gas/liquid feed switched device of the invention, setting has the switching of at least four nozzles in inlet ductwork
Valve gear, two of them nozzle are connected in inlet ductwork, so that the gas from feeder is entered materials along inlet ductwork and are set
It is standby；The another two nozzle of selector valve device is separately connected the air inlet and liquid outlet of wet tank, makes after switching from gas supply dress
The gas set enters wet tank, and the liquid indentation in wet tank is protruded into the outlet tube of bottom, is entered along inlet ductwork
Materials equipment.
Gas/liquid feed switched device of the invention, using same inlet ductwork can be realized gas and liquid into
Material does not need gas, liquid inlet conduit and import nozzle, equipment is respectively set more compact；It will be in wet tank using gas
Liquid be pressed into materials equipment, eliminate the driving device of liquid feedstock, and the pressure of only gas used herein, gas sheet
Body does not lose；Only adjusting selector valve device can be realized the switching of gas/liquid charging, when materials equipment needs are continuous or more
It is secondary when being alternately repeated charging, it is easy to operate, it is easy to accomplish automation control.
A kind of heavy organic matter pyrolysis installation should including pyrolytic reaction kettle and above-mentioned gas/liquid feed switched device
Inlet ductwork one end in feeding device is used to connect feeder, the other end is connected with the feed inlet of pyrolytic reaction kettle.
The autoclave body of the pyrolytic reaction kettle is lined with quartz lining.The quartz lining is quartz liner；Quartz lining is resistance to
Corrosion.
Fluid collection tube is connected on the autoclave body of the pyrolytic reaction kettle, bottom is protruded into one end of the fluid collection tube,
Fluid collection tube is equipped with the filter device for separation of solid and liquid.The effect of liquid pressure in kettle in hot lower kettle
Under, by fluid collection tube filter device filtering after from fluid collection tube be discharged pyrolytic reaction kettle, realize kettle in liquid with
The hot separation of solid；Solid matter is not easy to plug filter device since gravity is settled down to bottom, and filtering accuracy is high；It crosses
Filter device is detachably connected with separation of solid and liquid pipe, and when blocking only needs to change filter device.
The filter device is the filtering head that fluid collection tube is arranged in and protrudes into bottom one end end.The filtering head and solid
Liquid separating pipe is detachably connected, and is installed more convenient with replacement.The filtering head is metal material, high pressure resistant, corrosion-resistant.
The thermocouple sheath for placing thermocouple is equipped in pyrolytic reaction kettle autoclave body, autoclave body periphery is equipped with heating mantle.?
Thermocouple is inserted into thermocouple sheath, for measuring and controlling the temperature of material in autoclave body.
Pyrolytic reaction kettle autoclave body includes autoclave body ontology and kettle cover, and autoclave body ontology is detachably connected with kettle cover.Autoclave body ontology with
Kettle cover junction is sealed using open loop type, high pressure resistant and high temperature.Fluid collection tube and thermocouple sheath are connected on kettle cover；Kettle cover
On be additionally provided with material inlet and evacuation port, for the addition of material and the emptying of gas；Gaseous products under operating condition, that is, wave
Hair divides product, is discharged from autoclave body top.On the pipeline being connected with the nozzle being arranged on kettle cover, it is equipped with out at autoclave body
Close valve.The pressure gauge for measuring pressure in autoclave body is additionally provided on kettle cover.
Pyrolytic reaction kettle autoclave body is equipped with agitating device；There are three agitator arms for installation in the stirring slurry of agitating device, are suitble to
In the big autoclave body of ratio of height to diameter.Preferably, which is made of 2520 material of stainless steel.
The fluid collection tube is connected with liquid collection tank far from one end of pyrolytic reaction kettle autoclave body.Liquid collection tank is used for
Collect the product liquid after being separated by solid-liquid separation.
Gas vent is additionally provided on the pyrolytic reaction kettle, the gas vent connects condenser pipe, the condenser pipe
It has been sequentially connected in series first-stage condenser and secondary condenser.
The gas vent of pyrolytic reaction kettle is sequentially connected level-one, secondary condenser, the gas warp generated in pyrolytic reaction kettle
Gas vent sequentially enters condensed in two stages device and is condensed, and the temperature of condensed in two stages is stepless adjustable, can be obtained with different boilings
The fraction of point range；The pyrolysis installation realizes the gas-liquid separation at the reaction temperatures of heavy organic productions mixture, solid-liquid
The cold fractionation of the grade of separation and the collection of product liquid, gaseous product is collected, and integrated level is high, and occupied area is small, easy to use.
The end of the condenser pipe is connected with cold-trap.Detection branch is connected with before cold-trap on the condenser pipe,
The end of detection branch can connecting detection device, such as gas chromatograph, mass spectrograph or spectrometer, for real at reaction conditions
The on-line analysis of existing gaseous product.The detection branch is equipped with sampling valve.
The liquid outlet of the first-stage condenser and secondary condenser is connected separately with condensation collecting tank.Collecting tank is condensed to use
In collection gaseous product condensation portion.Subtracting on counterbalance valve, with inlet ductwork is equipped on condenser pipe after secondary condenser
The intermittent or continous way operation under the conditions of certain pressure may be implemented in pressure valve cooperation.The feeder being connect with inlet ductwork
High-pressure flow gas circuit can be formed, realizes that high pressure continuous flow moves the operation of reaction system.
Heavy organic matter pyrolysis installation of the invention, for coupling thermal depolymerization, extraction heat, thermosol filter, fractionation multiple technologies member
The complexes of element, wherein pyrolytic reaction kettle integrates the function of thermal depolymerization, extraction heat and thermosol filter, at the reaction temperatures
It carries out；Using gas/liquid feed switched device, make antipyretic reaction kettle more compact structure, easy switching, it is easy to accomplish continuously certainly
Dynamic production；Volatile matter product under reaction temperature is directly realized by multistage cooling fractionation with less equipment, does not need to drop to room temperature
It can directly be separated；The cold fraction for being separated into different temperature zones of the direct grade of volatile matter product, and adjusted by the cold temperature of grade
It obtains the fraction of different temperature zones and then carries out the regulation of each fractional composition.
The pyrolysis installation can be mixed to coal/pitch/biomass and by coal/pitch/biomass derived SOLID ORGANIC matter
Object carry out thermosol extraction, it is hot filter, depolymerize, grade is cold the couplings of multiple monotechnicses such as separates and operated, can carry out
It the production of heavy organic matter use aspects and is worked, is subtracted using the experimental study of thermodynamics, dynamics, the technique of related fields etc.
The workload of few relevant operation, improves efficiency.Device integrated level is high, have structure is simple, occupied area is small, temperature control is good,
The advantages that abundant, reproducible is reacted and separated, is suitble to promote the use of.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the gas/liquid feed switched device of embodiment 1；
Fig. 2 is the gas/liquid feed switched device switching state schematic diagram of Fig. 1；
Fig. 3 is the structural schematic diagram of the heavy organic matter pyrolysis installation of embodiment 2；
Fig. 4 is the structural schematic diagram of the pyrolytic reaction kettle in Fig. 3.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
Embodiment 1
The gas/liquid feed switched device of the present embodiment, as shown in Figure 1, including wet tank 34 and one end for connecting
Feeder, the other end are connect for connecting the inlet ductwork 40 of pyrolytic reaction kettle (materials equipment), is set in the inlet ductwork 40
There is four-way valve 33, two nozzles of the four-way valve 33 are connected on the inlet pipeline 40, and another two nozzle is separately connected liquid
The air inlet 34-1 and liquid outlet 34-2 of storage tank 34, liquid outlet 34-2 are equipped with the liquid out for going deep into bottom inside wet tank 34
Pipe 41；Four-way valve 33 makes gas be directly entered pyrolytic reaction kettle along inlet ductwork for switching, or gas is made to enter wet tank
Its internal liquid is pressed into pyrolytic reaction kettle along inlet ductwork by 34；It is equipped with weighing device 35 below the wet tank 34, is used for
Monitor the inlet amount of liquid；
Along gas flow direction, gas flowmeter 36, gas are equipped in the upstream of four-way valve 33 in the inlet ductwork 40
Flowmeter 36 is equipped with bypass, and bypass is equipped with the 5th switch valve 37；The gas piping 40 the upstream of gas flowmeter 36 also
Equipped with pressure reducing valve 39 and check valve 38.
Four-way valve 33 is arranged in the gas/liquid feed switched device of the present embodiment in inlet ductwork 40, four-way valve 33
Two nozzles are connected in inlet ductwork 40, so that the gas from feeder is entered pyrolytic reaction kettle along inlet ductwork 40, such as
It is gas feed shown in Fig. 1；The another two nozzle of four-way valve 33 is separately connected the air inlet 34-1 and liquid outlet of wet tank 34
34-2 adjusts (as shown in Figure 2) after four-way valve switches over, so that the gas from feeder is entered wet tank 34, by liquid
Liquid indentation in body storage tank 34 is protruded into the outlet tube 41 of bottom, is entered pyrolysis reactor along inlet ductwork 40, is completed liquid
Charging.
Gas/liquid feed switched device of the invention, using same inlet ductwork can be realized gas and liquid into
Material does not need gas, liquid inlet conduit and import nozzle, equipment is respectively set more compact；It will be in wet tank using gas
Liquid be pressed into materials equipment, eliminate the driving device of liquid feedstock, and the pressure of only gas used herein, gas sheet
Body does not lose；Only adjusting four-way valve can be realized the switching of gas/liquid charging, when materials equipment needs continuously or repeatedly to hand over
It is easy to operate, it is easy to accomplish automation control when for repeating to feed.
Embodiment 2
The heavy organic matter pyrolysis installation of the present embodiment, as shown in figure 3, including pyrolytic reaction kettle 1 and described in embodiment 1
Gas/liquid feed switched device, it is 40 one end of inlet ductwork connection feeder (gas bomb) in the feeding device, another
End is connected with the feed inlet 17 of pyrolytic reaction kettle 1；The intracorporal middle part of kettle of pyrolytic reaction kettle is protruded into one end of inlet ductwork 40
Hereinafter, being equipped with second switch valve 22 close to autoclave body outside pyrolytic reaction kettle autoclave body in inlet ductwork 40；
As shown in figure 4, the autoclave body of the pyrolytic reaction kettle 1 includes autoclave body ontology 1-1 and kettle cover 1-2, autoclave body ontology 1-1 with
Kettle cover 1-2 is detachably connected, i.e., fastens, realize with gasket 14 by 13 sets of U-shaped open loop on flange and using sealing screw 15
Open loop sealing；The feed inlet 17 of pyrolytic reaction kettle is arranged on kettle cover 1-2, is connected with fluid collection tube 2 on the kettle cover 1-2,
One end of the fluid collection tube 2 protrudes into bottom and is connected with the filtering head 3 for separation of solid and liquid, fluid collection tube 2 it is another
End stretches out autoclave body and is externally connected with liquid collection tank 23, for collecting the product liquid after being separated by solid-liquid separation；It is close on fluid collection tube 2
Autoclave body is equipped with first switch valve 19；The top of liquid collection tank 23 is equipped with relief valve 24；
The autoclave body ontology 1-1 is lined with quartz lining 4, form of the quartz lining 4 using quartz liner, high temperature resistant
And it is corrosion-resistant；The autoclave body periphery ontology 1-1 is equipped with heating mantle 5；It is equipped in the autoclave body of the pyrolytic reaction kettle 1 for placing thermocouple
Thermocouple sheath 7, thermocouple sheath 7 is mounted on kettle cover 1-2, for placing material in thermocouple measurement and control autoclave body
Temperature；
It is additionally provided with gas vent 18 and evacuation port 16 on the kettle cover 1-2, is equipped with third switch valve 21 at evacuation port 16；Gas
Body outlet 18 connects condenser pipe, and close autoclave body is equipped with the 4th switch valve 20 on condenser pipe；It is flowed on condenser pipe along gas
Direction has been sequentially connected in series first-stage condenser 25 and secondary condenser 26, is equipped with counterbalance valve 31 at the rear of secondary condenser 26, cold
The end of solidifying pipeline is for connecting glass cold-trap；On condenser pipe, detection branch is equipped between secondary condenser 26 and counterbalance valve 3
Road, detection branch are equipped with sampling valve 32, and the end of detection branch is used for connecting detection device, such as gas chromatograph, mass spectrograph
Or spectrometer etc., for realizing the on-line analysis of gaseous product at reaction conditions；
The liquid outlet of the first-stage condenser 25 and secondary condenser 26 is connected separately with the first condensation collecting tank 27,
Two condensation collecting tanks 28, for collecting gaseous product condensation portion；The pipeline that level-one, secondary condenser are connect with condensation collecting pipe
On be equipped with switch valve；First-stage condenser 25 and secondary condenser 26 are respectively equipped with the first temperature controller 29, the second temperature controller 30, and two
The temperature of grade condensation is electrodeless adjustable；
The autoclave body of pyrolytic reaction kettle is additionally provided with agitating device, and the agitating device includes motor 10, rotary shaft 8 and agitating shaft
6, the motor 10 is driven with rotary shaft 8 by belt 11, and agitating shaft 6 is located in autoclave body, is arranged at intervals with three agitator arms
9；Rotary shaft 8 and junction of the agitating shaft 6 outside autoclave body are equipped with for cooling cooling bath 12；
Also pyrolytic reaction kettle is made of 2520 material of stainless steel, and the filtering head is metal material；The pyrolytic reaction kettle, instead
Answer pressure in 0-10MPa, it is adjustable；Temperature is adjustable at -600 DEG C of room temperature, can process control；Autoclave body volume (quartz liner volume)
For 1L；The mixing speed of agitating device is 0-1000r/min, adjustable.
In the heavy organic matter pyrolysis installation of the present embodiment, the temperature of first-stage condenser is 200-500 DEG C of (maximum temperature
600℃)；The temperature of secondary condenser is 100-500 DEG C (600 DEG C of maximum temperature)；Solvent tank volume 1000ml, liquid collection tank
Tank volume 500ml is collected in volume 500ml, first-stage condenser volume 500ml, secondary condenser volume 500ml, the first condensation, the
Tank volume 500ml is collected in two condensations；Balance weighing range 0-5kg, precision 0.1g.
The heavy organic matter pyrolysis installation of the present embodiment, is further equipped with intelligent controlling device, turns to gas flow, stirring
Speed.The parameters such as autoclave body interior reaction temperature and condensed in two stages device temperature carry out real-time control, the spies such as high, easy to operate with accuracy
Point.
The heavy organic matter pyrolysis installation of the present embodiment, operating process when use are as follows:
(1) preparation:
I. four switch valves (first switch valve 19, second switch valve 22, the close to autoclave body gas circuit original state: are closed
Three switch valves 21, the 4th switch valve 20), pressure reducing valve 39 is unscrewed, closes the 5th switch valve 37 that gas flowmeter 36 bypasses, and will
The state of four-way valve 33 switches to gas circuit without solvent tank 34, is directly connected to the autoclave body of pyrolytic reaction kettle 1；Shut counterbalance valve
31, and sampling valve 32 is closed, first-stage condenser 25, secondary condenser 26 are simultaneously closed off respectively and on condensation collecting tank connecting line
Switch valve；
Ii. prepare reaction mass: adding reaction mass in the autoclave body ontology 1-1 of pyrolytic reaction kettle, including coal (pitch or its
His heavy organic matter), volume, catalyst etc., cover kettle cover 1-2, tighten sealing screw 15 and realize open loop sealing；
Iii. it inflates: opening feeder (steel cylinder), rotating pressure-decreasing valve 39 to feeder outlet pressure reaches requirement
Reaction pressure；The second switch valve 22 close to autoclave body is opened, until pressure reaches reaction pressure in autoclave body, closes second switch
Valve 22；In gas replenishment process, the inlet pressure of pyrolytic reaction kettle can also be increased, be conducive to gas in this way and enter kettle faster
In vivo；
(2) by taking the pyrolysis of the thermosol of coal as an example, control device is opened, control the stirring rate of agitating device, while heat is set
The temperature program(me) of solution reaction kettle, until reaching final reaction temperature；
(3) temperature of first-stage condenser 25 and secondary condenser 26 is set, condensation temperature is made to reach set temperature；
(4) condensation of gaseous product with separate: when setting thermosol/depolymerize/extraction time reach after, open and the 4th open
Valve 20 is closed, the gas evolution (10-100ml/min) that counterbalance valve 31 to back pressure valve outlet has certain flow is slowly rotated, gas produces
Object is condensed in condensed in two stages device；With the reduction of reaction pressure, counterbalance valve 31 is gradually unscrewed, guarantees exit gas flow
It is roughly the same；When reaction pressure drops to normal pressure, counterbalance valve 31 is unscrewed completely, after a period of time, closes the 4th switch valve 20；
(5) the condensed liquid of gaseous product is collected: open first-stage condenser 25 and secondary condenser 26 respectively with condensation
Tank connected switch valve is collected, the liquid distillate with different boiling range can be obtained, is opened described in closing after collecting completely
Close valve；The fraction product of arbitrary temp section within the scope of experimental temperature can be obtained by adjusting the temperature of condensed in two stages.
(6) collection of product liquid: before liquefied gas product, pyrolytic reaction kettle is first subjected to pressurising, which can
Plenum Process before reference reaction, i.e. opening second switch valve 22, are closed again after pressure in pyrolytic reaction kettle reaches certain pressure
Close second switch valve 22；First switch valve 19 is opened, in pyrolytic reaction kettle under the action of high pressure gas, liquid will pass through liquid
The filtering head 3 of 2 end of collecting pipe is pressed into liquid collection tank, leaves solid residue, rear to close first switch valve 19；To big
After partially liq enters liquid collection tank, the relief valve 24 opened in liquid collection tank carries out pressure release, is conducive to the taking-up of product；
(7) supplementing solvent: before supplementing solvent, needing to shed pressure in pyrolytic reaction kettle, guarantees safety operation, that is, beats
It opens after the third switch valve 21 above autoclave body carries out pressure release and shuts the third switch valve 21 again；Second opened in inlet ductwork opens
Valve 22 is closed, while the state of four-way valve 33 is switched into gas circuit and passes through solvent tank 34, it under pressure will be in solvent tank 34
Solvent is pressed into the autoclave body of pyrolytic reaction kettle 1, and the quantity of solvent of supplement is measured by balance 35；It is cut after to solvent make-up
The state of four-way valve 33 is changed to gas circuit without solvent tank 34；
(8) residue in solvent cleaning kettle: under the action of agitating device, further by the intracorporal solid residue of kettle
With it is remaining that product liquid is cleaned；
(9) collection step for repeating product liquid, product liquid is further collected, multiple solvent cleaning and liquid
After collection of products, solid residue can be cleaned up, and obtain product liquid as much as possible；For coal/pitch/biology
Matter and by coal/pitch/biomass derived SOLID ORGANIC matter mixture thermosol heat filter and thermal depolymerization, no ash content finally can be obtained
Or low-ash semicoke solution, it is solution under reaction temperature, sees after cooling and be further processed to obtain no ash content or low-ash
Semicoke.In last autoclave body residue is also undissolved ash content, minerals and a small amount of carbon residue under reaction temperature.
It is cold with glass after counterbalance valve 31 in the end of condenser pipe in the heavy organic matter pyrolysis installation of the present embodiment
Trap condenses to room temperature and collects remaining fraction.If you need to realize continuous flowing reaction process, pressure reducing valve 39 and counterbalance valve 31 are adjusted
To certain aperture, design gas flowmeter 36 is certain flow, and closes the 5th switch valve of gas flowmeter bypass；Such as
When reaction pressure will be set as 2MPa, 39 outlet pressure of pressure reducing valve is adjusted to more bigger than reaction pressure, such as 2.1MPa, adjusts back
Pressure valve 31 to reaction pressure remains unchanged and (does not increase and also do not reduce), while 36 registration of flowmeter keeps stablizing, and at this moment gas will
Continuous flowing is realized by pyrolytic reaction kettle.
The heavy organic matter pyrolysis installation of the present embodiment, for coupling thermal depolymerization, extraction heat, thermosol filter, fractionation multiple technologies
The complexes of element, wherein pyrolytic reaction kettle integrates the function of thermal depolymerization, extraction heat and thermosol filter, in reaction temperature
Lower progress；Using gas/liquid feed switched device, make antipyretic reaction kettle more compact structure, easy switching, it is easy to accomplish continuous
Automatic production；Volatile matter product under reaction temperature is directly realized by multistage cooling fractionation with less equipment, does not need to drop to often
Temperature can be separated directly；The cold fraction for being separated into different temperature zones of the direct grade of volatile matter product, and pass through the cold temperature tune of grade
Section obtains the fraction of different temperature zones and then carries out the regulation of each fractional composition.The pyrolysis installation can be to coal/pitch/biomass
And carry out that thermosol extractant is hot to be filtered, depolymerize, cold point of grade by coal/pitch/biomass derived SOLID ORGANIC matter mixture
From etc. the coupling of multiple monotechnicses operated, the production of heavy organic matter use aspects can be carried out and utilize related fields
The experimental study of thermodynamics, dynamics, technique etc. works, and reduces the workload of relevant operation, improves efficiency；It may be implemented one
Intermittent or continous way operation under the conditions of constant-pressure, feeder can form high-pressure flow gas circuit, realize that high pressure continuous flow is dynamic
The operation of reaction system, it is easy to use.Device integrated level is high, have structure is simple, occupied area is small, temperature control is good, reaction and
The advantages that abundant, reproducible is separated, is suitble to promote the use of.
The pyrolysis of heavy organic matter is carried out using heavy organic matter pyrolysis installation as described in example 2, specific as follows:
Experimental example 1: hot depolymerization, extraction and the filtering of coal
Gas rich coal crushing grinding is dried in vacuo more than for 24 hours, the heavy as experiment is organic at room temperature to 200 meshes are crossed
Matter raw material weighs heavy organic matter material 100g, mixes solvent 500g with quality proportioning for the washing oil of 1 ︰ 1 and a de- brilliant carbolineum
It is added in pyrolytic reaction kettle, temperature of reaction kettle is 500 DEG C, pressure 5MPa, reaction time 45min, carries out the cold temperature of grade of 2 tests
Degree is controlled as 350 DEG C, 150 DEG C and 250 DEG C, 100 DEG C, and according to the operating process of embodiment 2, experimental result deducts recycling
Solvent, it is as follows to calculate acquisition each section yield in conjunction with subtractive: semi-coke yield 57.34%, wherein dry basis ash content produces content
0.24%；Residual residue 14.2%, wherein carbon content 4.0%；Liquid product yield 24.89%, wherein 350 DEG C of >, 350-250
DEG C, the yield 5.10%, 5.31%, 4.30%, 5.54%, 4.64% of 250-150 DEG C, 150-100 DEG C, 100 DEG C or less fraction.
Experimental example 2: hot depolymerization, extraction and the filtering of pitch
Hard pitch crushing grinding is dried in vacuo more than for 24 hours, the heavy as experiment has at room temperature to 200 meshes are crossed
Machine matter raw material weighs heavy organic matter material 100g, mixes solvent with quality proportioning for the washing oil of 1 ︰ 1 and a de- brilliant carbolineum
500g is added in pyrolytic reaction kettle, and temperature of reaction kettle is 500 DEG C, pressure 5MPa, reaction time 45min, carries out the grade of 2 tests
Cold temperature is controlled as 400 DEG C, 200 DEG C and 350 DEG C, 150 DEG C, and according to the operating process of embodiment 2, experimental result is deducted back
The solvent of receipts, it is as follows to calculate acquisition each section yield in conjunction with subtractive: asphalitine yield 21.34%, wherein dry basis ash content production contain
Amount 0.10%；Residual residue 2.20%, wherein carbon content 4.0%；Liquid product yield 74.39%, wherein 400 DEG C of >, 400-
The yield 23.10% of 350 DEG C, 350-200 DEG C, 250-150 DEG C, 100 DEG C or less fractions, 27.31%, 14.30%, 4.54%,
5.14%.
Embodiment 3: hot depolymerization, extraction and the filtering of biomass
Soybean fiber residue after extracting soybean protein and polysaccharide, is air-dried, crushing grinding to 200 meshes excessively, room temperature
It more than lower vacuum drying for 24 hours, as the heavy organic matter material of experiment, weighs heavy organic matter material 50g, match with quality
Than the washing oil and de- brilliant carbolineum mixing solvent 500g for 1 ︰ 1, temperature of reaction kettle is 450 DEG C, pressure 5MPa, reaction time
45min, the cold temperature of grade for carrying out 2 tests is controlled as 350 DEG C, 150 DEG C and 250 DEG C, 100 DEG C, according to the behaviour of embodiment 2
Make process, experimental result deducts recovered solvent, and it is as follows to calculate acquisition each section yield in conjunction with subtractive: semi-coke yield
27.34%, wherein dry basis ash content produces content 0.10%；Residual residue 7.2%, wherein carbon content 6.0%；Liquid product yield
60.89%, wherein 350 DEG C, 350-250 DEG C, 250-150 DEG C, 150-100 DEG C, 100 DEG C of > or less the yields 11.10% of fraction,
15.31%, 14.30%, 15.54%, 4.64%.
In other embodiments of the invention, the selector valve device can also can realize identical cut for other in this field
Change the valve module of function.
Claims (7)
1. a kind of gas/liquid feed switched device, it is characterised in that: including wet tank and one end for connecting gas supply dress
It sets, the other end is filled for connecting the inlet ductwork of materials equipment, the inlet ductwork equipped with selector valve device, the switching valve
It is set to four-way valve；The selector valve device tool is there are four nozzle, and two of them nozzle is connected in inlet ductwork, another two nozzle
It is separately connected the air inlet and liquid outlet of wet tank, which is equipped with the outlet tube for going deep into bottom inside wet tank；
Selector valve device makes gas be directly entered materials equipment along inlet ductwork for switching, or so that gas is entered wet tank will be in it
Liquid indentation in portion's is protruded into the outlet tube of bottom, is pressed into materials equipment along inlet ductwork；
The wet tank, which is equipped with below liquidometer or wet tank, is equipped with weighing device, for monitoring the inlet amount of liquid；
Along gas flow direction, gas flowmeter is equipped in the upstream of four-way valve in the inlet ductwork；In the inlet ductwork
Pressure reducing valve and check valve are additionally provided in the upstream of gas flowmeter.
2. a kind of heavy organic matter pyrolysis installation, including pyrolytic reaction kettle, it is characterised in that: further include described in claim 1
Gas/liquid feed switched device, inlet ductwork one end in the feeding device is for connecting feeder, the other end and pyrolysis
The feed inlet of reaction kettle is connected.
3. heavy organic matter pyrolysis installation according to claim 2, it is characterised in that: in the autoclave body of the pyrolytic reaction kettle
It is lined with quartz lining.
4. heavy organic matter pyrolysis installation according to claim 2 or 3, it is characterised in that: the kettle of the pyrolytic reaction kettle
Fluid collection tube is connected on body, bottom is protruded into one end of the fluid collection tube, and fluid collection tube is equipped with for solid-liquid point
From filter device.
5. heavy organic matter pyrolysis installation according to claim 4, it is characterised in that: the fluid collection tube is far from pyrolysis
Autoclave body one end of reaction kettle is connected with liquid collection tank.
6. heavy organic matter pyrolysis installation according to claim 2, it is characterised in that: be additionally provided on the pyrolytic reaction kettle
Gas vent, the gas vent connect condenser pipe, and the condenser pipe has been sequentially connected in series first-stage condenser and B-grade condensation
Device.
7. heavy organic matter pyrolysis installation according to claim 6, it is characterised in that: the first-stage condenser and second level are cold
The liquid outlet of condenser is connected separately with condensation collecting tank.
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| CN106318422A (en) * | 2016-09-05 | 2017-01-11 | 神华集团有限责任公司 | Method and device for treating direct coal liquefaction residues |
| CN107694493B (en) * | 2017-09-20 | 2023-07-14 | 南京林业大学 | Multifunctional multiphase sectional reaction device and multiphase sectional reaction method |
| CN109529722B (en) * | 2018-12-20 | 2021-07-13 | 山东玉皇化工有限公司 | Method and device for continuously feeding low-boiling-point material to high-pressure device |
| CN113713718A (en) * | 2021-09-14 | 2021-11-30 | 山东理工大学 | Comprehensive platform for realizing high-pressure thermochemical multifunctional conversion research |
| CN115814704A (en) * | 2023-02-23 | 2023-03-21 | 北京西融新材料科技有限公司 | Reaction device and application thereof |
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| CN102226094B (en) * | 2011-05-16 | 2014-03-12 | 科威国际技术转移有限公司 | Method for preparing biomass fuel by pyrolysis liquefaction of biomass |
| CN102504855A (en) * | 2011-11-08 | 2012-06-20 | 河南中埠新能源有限公司 | Device for producing high-quality biological oil by rapidly pyrolyzing biomasses and waste plastics |
| CN202558933U (en) * | 2012-04-25 | 2012-11-28 | 北京工业大学 | Accurate control device for gas-liquid mixing feeding |
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| CN205700468U (en) * | 2016-04-19 | 2016-11-23 | 河南城建学院 | Gas/liquid feed switched device and heavy organic matter pyrolysis installation |
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