CN107973763A - A kind of process units and method for preparing 2- methylfurans - Google Patents
A kind of process units and method for preparing 2- methylfurans Download PDFInfo
- Publication number
- CN107973763A CN107973763A CN201711379256.8A CN201711379256A CN107973763A CN 107973763 A CN107973763 A CN 107973763A CN 201711379256 A CN201711379256 A CN 201711379256A CN 107973763 A CN107973763 A CN 107973763A
- Authority
- CN
- China
- Prior art keywords
- temperature
- regulating valve
- steam
- controller
- furfural
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VQKFNUFAXTZWDK-UHFFFAOYSA-N 2-Methylfuran Chemical class CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000008569 process Effects 0.000 title claims abstract description 21
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims abstract description 178
- 239000012043 crude product Substances 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 60
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000004821 distillation Methods 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 239000007791 liquid phase Substances 0.000 claims abstract description 43
- 239000000047 product Substances 0.000 claims abstract description 25
- 239000007792 gaseous phase Substances 0.000 claims abstract description 20
- 230000008676 import Effects 0.000 claims abstract description 17
- 230000001105 regulatory effect Effects 0.000 claims description 140
- 239000003054 catalyst Substances 0.000 claims description 102
- 239000007789 gas Substances 0.000 claims description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 69
- 239000012071 phase Substances 0.000 claims description 65
- 238000012546 transfer Methods 0.000 claims description 44
- 238000012856 packing Methods 0.000 claims description 30
- 229920006395 saturated elastomer Polymers 0.000 claims description 29
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 24
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 24
- 229910052794 bromium Inorganic materials 0.000 claims description 24
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 22
- 238000009835 boiling Methods 0.000 claims description 21
- 238000012544 monitoring process Methods 0.000 claims description 20
- 230000002708 enhancing effect Effects 0.000 claims description 19
- 238000002309 gasification Methods 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 230000020169 heat generation Effects 0.000 claims description 5
- 150000001299 aldehydes Chemical class 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 150000002240 furans Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- -1 hydrogen gas holder Chemical class 0.000 abstract 1
- 230000008859 change Effects 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000006392 deoxygenation reaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000010025 steaming Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/36—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0011—Heating features
- B01D1/0041—Use of fluids
- B01D1/0047—Use of fluids in a closed circuit
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0207—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly horizontal
- B01J8/0214—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly horizontal in a cylindrical annular shaped bed
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to a kind of process units and method for preparing 2 methylfurans;Including hydrogen gas holder, hydrogen gas holder is connected with the material inlet of radial reactor, liquid phase furfural measuring tank is connected with the material inlet of radial reactor, the material outlet of radial reactor passes sequentially through the first medium tube bank of the first feed preheater, cooler tube side, 2 methylfuran crude product storage tanks, feed pump, the tube bank of first feed preheater second medium is connected with the middle and lower part import of first rectifying column, gaseous phase outlet at the top of first rectifying column is restrained by the 3rd medium of the first feed preheater to be connected with the input end of pans, the second outlet end of pans is connected by the second feed preheater shell side with the import of Second distillation column middle and upper part, gaseous phase outlet at the top of Second distillation column is connected by the tube side of the second feed preheater tube side and condenser with finished product storage tank;Have the advantages that to reduce bed resistance, improve reaction efficiency, remove bed reacting replacing heat, reduce diffusional resistance.
Description
Technical field
The invention belongs to 2- methylfuran production technical fields, and in particular to a kind of process units for preparing 2- methylfurans
And method.
Background technology
Existing market is prepared in the process units of 2- methylfurans, and furfural material is needed with conduction oil or steam before reaction
Heating and gasifying, and the 2- methylfuran crude products produced after reacting need primary cycle water cooling and two level bromine cold water to condense, two
The charging of rectifying column needs to be heated to initial temperature with conduction oil or steam, and the gas phase that rectifying column comes out needs primary cycle water
Cooling and the condensation of two level bromine cold water, heating consume substantial amounts of heat, and cooling or condensation consume substantial amounts of cold.Due to adding hot and cold
Different equipment is but set, and number of devices is more, and device is integrally invested greatly.In addition, the reactor of 2- methylfurans is all axial
Adiabatic reactor, during reaction, fluid flows through catalyst bed from top to bottom vertically, and bed is with the external world without heat exchange.It is axial anti-
Answer device big there are bed resistance, catalyst granules is big, and diffusional resistance is big, and temperature drop variable gradient is big, and the later stage there is also catalyst
Bed skewness, react unbalanced, local overheating, sintering of catalyst, reduce catalyst service life, influence product quality and
The problems such as yield.
The content of the invention
The defects of it is an object of the invention to overcome in the prior art and provide a kind of simple in structure, design rationally, can
Efficiently use heat source and low-temperature receiver carries out the heat exchange of folder point, so as to reduce steam consumption, circulation water consumption, reduce number of devices, reduce
Plant investment at the same using radial reactor can reduce bed resistance, improve reaction efficiency, in time remove bed reaction change
The process units and method that prepare 2- methylfurans hot, reduce diffusional resistance and bed is substantially at temperature constant state.
The object of the present invention is achieved like this:Including hydrogen gas holder, liquid phase furfural measuring tank, finished product storage tank and feed pipe
Net, the hydrogen gas holder are connected by hydrogen gas compressor and hydrogen gas buffer with the material inlet of radial reactor, liquid phase furfural
Measuring tank is connected by furfural evaporator with the material inlet of radial reactor, and the material outlet of radial reactor passes sequentially through
The first medium tube bank of one feed preheater, cooler tube side, 2- methylfuran crude products storage tank, feed pump, the first feeding preheating
The tube bank of device second medium is connected with the middle and lower part import of first rectifying column, and first rectifying column outlet at bottom is collected with high-boiling components respectively
The bottoms material entrance of tank and the first reboiler tube side is connected, the top gas phase outlet of the first reboiler tube side and first rectifying column
Lower inlet be connected, the gaseous phase outlet at the top of first rectifying column pass through the 3rd medium of the first feed preheater tube bank and pans
Input end be connected, the first exit end of pans is connected with the middle and upper part import of first rectifying column, the second outlet of pans
End is connected by the second feed preheater shell side with the import of Second distillation column middle and upper part, and Second distillation column outlet at bottom is respectively with giving up
The bottoms material entrance of liquid collecting tank and the second reboiler tube side is connected, the top gas phase outlet and second of the second reboiler tube side
The lower inlet of rectifying column is connected, and the gaseous phase outlet at the top of Second distillation column passes through the second feed preheater tube side and condenser
Tube side is connected with finished product storage tank;The radial reactor includes housing, and housing ecto-entad has annular outer barrel room, catalyst successively
Bed and inner cylinder room, are equipped with narrow meshed annular outer tube wall between annular outer barrel room and catalyst bed, catalyst bed it is interior
Portion is equipped with some heat exchange pipelines, and narrow meshed annular inner tube wall, the top of housing are equipped between catalyst bed and inner cylinder room
Equipped with material inlet and steam (vapor) outlet, material inlet is connected with the top of annular outer barrel room, and steam (vapor) outlet passes through drum and heat exchange
The top of pipeline is connected;The bottom of housing is equipped with material outlet, bottom admission port and catalyst discharge port, and bottom admission port passes through
Hydroecium is connected with the bottom of heat exchange pipeline, and material outlet is connected with the bottom of inner cylinder room, catalyst discharge port and catalyst bed
The bottom of layer is connected;The water supply network is connected by pipeline with bottom admission port, and steam (vapor) outlet is by the first regulating valve with steaming
Steam pipe net is connected, and steam pipe network is connected by pipeline with the second regulating valve, the 3rd regulating valve and the 4th regulating valve respectively, and second adjusts
Section valve is connected by the steam pipe coil in furfural evaporator with steam condensate accumulator tank, and the 3rd regulating valve passes through the first reboiler
Shell side is connected with steam condensate accumulator tank, and the 4th regulating valve is connected by the shell side of the second reboiler with steam condensate accumulator tank;
The shell side import of the cooler is connected by the 5th regulating valve with lithium bromide come grid, the shell-side outlet and bromination of cooler
Lithium return pipe net is connected;The shell side import of the condenser is connected by the 6th regulating valve with lithium bromide come grid, condenser
Shell-side outlet be connected with lithium bromide return pipe net;Pressure is installed on pipeline between the steam (vapor) outlet and the first regulating valve
Table, furfural evaporator top are provided with the first thermometer table, the pipeline between cooler tube side and 2- methylfuran crude product storage tanks
On second temperature meter table is installed, first rectifying column tower reactor is provided with the 3rd thermometer table, between condenser and finished product storage tank
4th thermometer table is installed, Second distillation column tower reactor is provided with the 5th thermometer table on pipeline;The pressure gauge, the first temperature
Count table, second temperature meter table, the 3rd thermometer table, the 4th thermometer table and the 5th thermometer the table input terminal with controller respectively
It is connected, the output terminal of controller is adjusted with the first regulating valve, the second regulating valve, the 3rd regulating valve, the 4th regulating valve, the 5th respectively
Valve, the 6th regulating valve are connected.
Preferably, for the furfural evaporator to be vertically arranged, the lower part of furfural evaporator inner cylinder is equipped with steam pipe coil, inner cylinder
Top to be hollow.
Preferably, the surface of the annular outer tube wall and annular inner tube wall is evenly distributed with aperture.
Preferably, the heat exchange pipeline is vertically distributed in catalyst bed.
Preferably, the heat exchange pipeline is annularly distributed in catalyst bed.
Preferably, 2~4 vertical thermocouples are provided with the catalyst bed, vertical thermocouple is annularly distributed in
In catalyst bed;Multiple temperature measuring points are vertically evenly equipped with vertical thermocouple.
Preferably, the internal upper part of the first rectifying column is equipped with the first dumped packing layer, and the internal upper part of Second distillation column is set
There is the second dumped packing layer.
Preferably, first feed preheater is wound tube heat exchanger.
A kind of method for the process units for preparing 2- methylfurans, this method comprises the following steps:
Step 1:The hydrogen come from hydrogen gas holder, 25~35 DEG C of temperature, pressure 2Kpa, are pressurized to through hydrogen gas compressor
70~100 DEG C, pressure enters in annular outer barrel room after being 0.05~0.1Mpa through hydrogen gas buffer, material inlet;Liquid phase furfural
25~35 DEG C of furfurals of temperature that measuring tank comes enter furfural evaporator by gravity, in furfural evaporator inner cylinder steam pipe coil
The steam heat-exchanging of 0.9~1.1MPa, temperature rise to 160~175 DEG C of furfural gasifications, and gas phase furfural enters outside annular through material inlet
Cylinder is indoor;
Step 2:Entered and urged by the aperture by annular outer tube wall after hydrogen and the annular outer barrel room of gas phase furfural entrance
In agent bed, in Cu-series catalyst presence, gas phase furfural and hydrogen reaction generation gas phase 2- methylfurans are above-mentioned to react
Substantial amounts of reaction heat is discharged in journey, reaction heat exchanges heat with heat exchange pipeline, the deaerated water in heat exchange pipeline is absorbed heat life
Into saturated vapor;The Cu-series catalyst is CuO- silicon oxide catalysts, CuO- aluminium oxide catalysts or CuO- sial are compound
One of oxide catalyst;
Step 3:Gas phase 2- methylfurans enter in inner cylinder room through the aperture on annular inner tube wall, pass through through material outlet
First tube bank of the first feed preheater, cooler tube side enter 2- methylfurans crude product after temperature is reduced to 10~15 DEG C and store up
Groove;
Step 4:2- methylfuran crude products in 2- methylfuran crude product storage tanks are pressurized to 0.2~0.3MPa through feed pump
Afterwards, by the media for heat exchange of the first tube bank and the 3rd tube bank in the second tube bank of the first feed preheater and the first feed preheater extremely
Enter after 100~105 DEG C in first rectifying column tower reactor, enter into the 2- methylfuran crude products overflow in first rectifying column tower reactor
In first reboiler tube side, its in the first reboiler with gasifying after the steam heat-exchanging of shell side, the 2- methylfuran crude products of gasification
Ascend into first rectifying column, by the first dumped packing layer, the heavy constituent in the 2- methylfuran crude products of gasification is separated
Get off, fall into first rectifying column tower reactor, the light component in the 2- methylfuran crude products of gasification is by the first dumped packing layer by
Gaseous phase outlet at the top of one rectifying column enters heat exchange in the tube bank of the 3rd medium of the first feed preheater, and the light component after heat exchange becomes
Liquid phase enters in pans;High-boiling components in the first rectifying column tower reactor are periodically discharged into high-boiling components collecting tank;
Step 5:Into the liquid phase light component part in pans first is back to by first rectifying column centre inlet
In rectifying column, another part liquid phase light component is entered in Second distillation column tower reactor by the second feed preheater shell side, and liquid phase is light
Component overflow enters in the second reboiler tube side, and with gasifying after the steam heat-exchanging of shell side, gas phase light component enters Second distillation column
Interior, by the second dumped packing layer, in gas phase light component, high boiling substance, which is separated, falls into Second distillation column tower reactor, gas phase
2- methylfurans enter the second feed preheater tube side by the second dumped packing layer by the gaseous phase outlet at the top of Second distillation column
Exchange heat, become liquid phase 2- methylfurans after heat exchange, by the tube side of condenser with enter after bromine cold water further heat exchange into
In product storage tank;The waste water of the Second distillation column tower reactor is periodically discharged into waste collection tank;
Step 6:Deaerated water in water supply network is entered in heat exchange pipeline by bottom admission port and hydroecium, into heat exchange
Deaerated water in pipeline takes away the reaction heat in catalyst bed, and generates saturated vapor, and saturated vapor is by drum, steam (vapor) outlet
Enter with the first regulating valve in steam pipe network, the saturated vapor in steam pipe network respectively enters furfural evaporator, the first reboiler
Used with heated material in the second reboiler, the steam condensate produced after use returns to the recycling of steam condensate accumulator tank;Institute
It is 0.5MPa to state the deoxygenation water pressure in water supply network, and temperature is 105 DEG C;The saturated vapour pressure is 0.9~1.1MPa, temperature
Spend for 175~184 DEG C;
Step 7:Temperature measuring point on vertical thermocouple monitors the temperature of catalyst bed in real time, makes reaction bed temperature
For 175~184 DEG C;Temperature and steam pressure in catalyst bed are direct ratio;When the temperature of temperature measuring point detection is higher than 184 DEG C
Steam pressure raises, and the pressure of pressure gauge detection is more than 1.1MPa, and pressure signal is fed back to controller by pressure gauge at this time, control
Signal is transmitted to the first regulating valve, the increase of the first control valve opening by device, and the quantity of steam for being sent to steam pipe network increases, radial reactor
Interior heat transfer increase, recovers untill 175~184 DEG C until reaction bed temperature;When the temperature of temperature measuring point detection is less than 175 DEG C
When steam pressure reduce, pressure gauge detection pressure be less than 0.9MPa, pressure signal is fed back to controller by pressure gauge at this time, control
Signal is transmitted to the first regulating valve by device processed, and the first control valve opening reduces, and the quantity of steam for being sent to steam pipe network is reduced, and is radially reacted
Heat transfer reduces in device, recovers until reaction bed temperature untill 175~184 DEG C;
Step 8:The first thermometer table monitors gas phase furfural temperature at 160~175 DEG C at the top of furfural evaporator, works as temperature
During less than 160 DEG C, the first thermometer table transmits a signal to controller, and signal is transmitted to the second regulating valve by controller, and second adjusts
Valve opening increase is saved, is sent to the quantity of steam increase of steam pipe coil in furfural evaporator, heat transfer enhancing, until the first thermometer table temperature
Degree recovers untill 160~175 DEG C;Conversely, when temperature is higher than 175 DEG C, the first thermometer table transmits a signal to controller,
Signal is transmitted to the second regulating valve by controller, and the second control valve opening reduces, and is sent to the steam of steam pipe coil in furfural evaporator
Amount is reduced, and heat transfer weakens, and recovers until the first thermometer table temperature untill 160~175 DEG C;
Step 9:2- first in second temperature meter table monitoring pipeline between cooler tube side and 2- methylfuran crude product storage tanks
The temperature of base furans crude product is between 10~15 DEG C, and when temperature is less than 10 DEG C, second temperature meter table transmits a signal to control
Signal is transmitted to the 5th regulating valve by device, controller, and the 5th control valve opening reduces, and the bromine cool water quantity for being sent to cooler is reduced, and is passed
Heat weakens, and recovers until second temperature meter table temperature untill 10~15 DEG C;Conversely, when temperature is higher than 15 DEG C, second temperature
Meter table transmits a signal to controller, and signal is transmitted to the 5th regulating valve by controller, and the increase of the 5th control valve opening, is sent to cooling
The bromine cool water quantity increase of device, heat transfer enhancing, recovers untill 10~15 DEG C until second temperature meter table temperature;
Step 10:The bottom temperature of 3rd thermometer table monitoring first rectifying column is between 105~110 DEG C, when temperature is low
When 105 DEG C, the 3rd thermometer table transmits a signal to controller, and signal is transmitted to the 3rd regulating valve by controller, and the 3rd is adjusted
Valve opening increases, and is sent to the quantity of steam increase of the first reboiler, heat transfer enhancing, until the 3rd thermometer table temperature is recovered to 105
Untill~110 DEG C;When temperature is higher than 110 DEG C, the 3rd thermometer table transmits a signal to controller, and signal is transmitted to by controller
3rd regulating valve, the 3rd control valve opening reduce, and the quantity of steam for being sent to the first reboiler is reduced, and heat transfer weakens, until the 3rd temperature
Degree meter table temperature is recovered untill 105~110 DEG C;
Step 11:The bottom temperature of 5th thermometer table monitoring Second distillation column is between 80~85 DEG C, when temperature is low
When 80 DEG C, the 5th thermometer table transmits a signal to controller, and signal is transmitted to the 4th regulating valve, the 4th regulating valve by controller
Aperture increases, and is sent to the quantity of steam increase of the second reboiler, heat transfer enhancing, until the 5th thermometer table temperature recover to 105~
Untill 110 DEG C;Conversely, when temperature is higher than 85 DEG C, the 5th thermometer table transmits a signal to controller, and controller passes signal
To the 4th regulating valve, the 4th control valve opening reduces, and the quantity of steam for being sent to the second reboiler is reduced, and heat transfer weakens, until the 5th
Thermometer table temperature is recovered untill 105~110 DEG C;
Step 12:The temperature of 2- methylfurans in 4th thermometer table of condenser tube side and finished product storage tank monitoring pipeline
Between 10~15 DEG C, when temperature is less than 10 DEG C, the 4th thermometer table transmits a signal to controller, and controller passes signal
To the 6th regulating valve, the 6th control valve opening reduces, and the bromine cool water quantity for being sent to cooler is reduced, and heat transfer weakens, until the 4th temperature
Degree meter table temperature is recovered untill 10~15 DEG C;Conversely, when temperature is higher than 15 DEG C, the 4th thermometer table transmits a signal to control
Signal is transmitted to the 6th regulating valve by device processed, controller, and the increase of the 6th control valve opening, is sent to the bromine cool water quantity enhancing of condenser,
Heat transfer enhancing, recovers untill 10~15 DEG C until the 4th thermometer table temperature.
According to a kind of process units and method for preparing 2- methylfurans made of such scheme, gas raw material passes through radially
Catalyst bed in reactor walks radial flow path, substantially reduces gas flow, increases connecing for gas raw material and catalyst
Sectional area is touched, reactor resistance is greatly reduced compared to traditional reactor, reduces energy consumption, improve reaction rate;While by
Portion sets annular outer tube wall and annular inner tube wall in the inner, can effectively prevent in material bias current or material gas phase to gather etc. existing
As ensure that the uniformity that material mixes in reactor, ensure that reaction effect, improve the conversion ratio of furfural, reduce
Consumption;Heat exchange pipeline is set in catalyst bed at the same time, in time can be removed material reaction liberated heat, ensures that bed temperature is permanent
It is fixed, prevent material overtemperature in reactor from polymerisation coking occurs, avoid consumption rise and stop production to overhaul, reduce inspection
Accomplish this and personnel labor intensity;Simultaneous reactions liberated heat is absorbed by deaerated water, and while energy consumption is reduced, by-product steams
Vapour, has achieveed the purpose that energy saving;With resistance is small, reaction rate is fast, is less prone to failure, stable reaction, byproduct steam it is excellent
Point.
Brief description of the drawings
Fig. 1 is the structure diagram of the present invention.
Fig. 2 is the structure diagram of furfural evaporator in the present invention.
Fig. 3 is the structure diagram of radial reactor in the present invention.
Fig. 4 is the control planning schematic diagram of the present invention.
Embodiment
In order to which the technical features, objects and effects of the present invention are more clearly understood, now control illustrates this hair
Bright embodiment, in the various figures identical label represent identical component.To make simplified form, in each figure only schematically
Ground is indicated with inventing relevant part, they do not represent its practical structures as product.
As shown in Figure 1,2,3, 4, the present invention includes hydrogen gas holder 1, liquid phase furfural measuring tank 4, finished product storage tank 20 and supplies water
Pipe network 21, the hydrogen gas holder 1 are connected by hydrogen gas compressor 2 and hydrogen gas buffer 3 with the material inlet 6 of radial reactor,
Liquid phase furfural measuring tank 4 is connected by furfural evaporator 5 with the material inlet 6 of radial reactor, and the material of radial reactor goes out
Mouthfuls 10 first medium tube banks for passing sequentially through the first feed preheater 11,12 tube side of cooler, 2- methylfuran crude products storage tank 13,
Feed pump 14, the tube bank of 11 second medium of the first feed preheater are connected with the middle and lower part import of first rectifying column 15, the first rectifying
Bottoms material entrance of 15 outlet at bottom of tower respectively with 34 and first reboiler of high-boiling components collecting tank, 29 tube side is connected, and first boils again
The top gas phase outlet of 29 tube side of device is connected with the lower inlet of first rectifying column 15, the gaseous phase outlet at the top of first rectifying column 15
Restrained by the 3rd medium of the first feed preheater 11 and be connected with the input end of pans 16, the first exit end of pans 16 and
The middle and upper part import of first rectifying column 15 is connected, and the second outlet end of pans 16 passes through 17 shell side of the second feed preheater and
Two rectifying columns, 18 middle and upper part import is connected, 18 outlet at bottom of Second distillation column respectively with 35 and second reboiler 30 of waste collection tank
The bottoms material entrance of tube side is connected, the top gas phase outlet of 30 tube side of the second reboiler and the lower inlet of Second distillation column 18
It is connected, the gaseous phase outlet at the top of Second distillation column 18 passes through 17 tube side of the second feed preheater and the tube side and finished product of condenser 19
Storage tank 20 is connected;The radial reactor includes housing 48, and 48 ecto-entad of housing has annular outer barrel room 7, catalyst bed successively
Floor 8 and inner cylinder room 9, are equipped with narrow meshed annular outer tube wall 49, catalyst bed 8 between annular outer barrel room 7 and catalyst bed 8
Be internally provided with some heat exchange pipelines 24, narrow meshed annular inner tube wall 50 is equipped between catalyst bed 8 and inner cylinder room 9,
The top of housing 48 is equipped with material inlet 6 and steam (vapor) outlet 26, and material inlet 6 is connected with the top of annular outer barrel room 7, and steam goes out
Mouth 26 is connected by drum 25 with the top of heat exchange pipeline 24;The bottom of housing 48 is equipped with material outlet 10, bottom admission port 22
With catalyst discharge port 47, bottom admission port 22 is connected by hydroecium 23 with the bottom of heat exchange pipeline 24, material outlet 10 with it is interior
The bottom of cylinder room 9 is connected, and catalyst discharge port 47 is connected with the bottom of catalyst bed 8;The water supply network 21 passes through pipe
Road is connected with bottom admission port 22, and steam (vapor) outlet 26 is connected by the first regulating valve 27 with steam pipe network 28, and steam pipe network 28 divides
It is not connected by pipeline with the second regulating valve 36, the 3rd regulating valve 37 and the 4th regulating valve 38, the second regulating valve 36 passes through furfural
Steam pipe coil in evaporator 5 is connected with steam condensate accumulator tank 31, the shell side that the 3rd regulating valve 37 passes through the first reboiler 29
It is connected with steam condensate accumulator tank 31, the shell side and 31 phase of steam condensate accumulator tank that the 4th regulating valve 38 passes through the second reboiler 30
Even;The shell side import of the cooler 12 is connected by the 5th regulating valve 39 with lithium bromide come grid 32, the shell of cooler 12
Journey outlet is connected with lithium bromide return pipe net 33;The shell side import of the condenser 19 by the 6th regulating valve 40 and lithium bromide come
Grid 32 is connected, and the shell-side outlet of condenser 19 is connected with lithium bromide return pipe net 33;The steam (vapor) outlet 26 and first is adjusted
Pressure gauge 46 is installed, the top of furfural evaporator 5 is provided with the first thermometer table 41, and cooler 12 is managed between section valve 27 on pipeline
Second temperature meter table 42, the installation of 15 tower reactor of first rectifying column are installed on the pipeline between journey and 2- methylfuran crude products storage tank 13
There is the 3rd thermometer table 43, the 4th thermometer table 44, the second essence are installed on the pipeline between condenser 19 and finished product storage tank 20
Evaporate 18 tower reactor of tower and the 5th thermometer table 45 is installed;The pressure gauge 46, the first thermometer table 41, second temperature meter table 42,
Three thermometer tables 43, the input terminal of the 4th thermometer table 44 and the 5th thermometer table 45 respectively with controller 53 are connected, controller
53 output terminal is adjusted with the first regulating valve 27, the second regulating valve 36, the 3rd regulating valve 37, the 4th regulating valve the 38, the 5th respectively
Valve 39 is connected with the 6th regulating valve 40.The furfural evaporator 5 is is vertically arranged, and the lower part of 5 inner cylinder of furfural evaporator is equipped with steaming
Vapour coil pipe, the top of inner cylinder is hollow.The surface of the annular outer tube wall 49 and annular inner tube wall 50 is evenly distributed with aperture.Institute
Heat exchange pipeline 24 is stated vertically to be distributed in catalyst bed 8.The heat exchange pipeline 24 is annularly distributed in catalyst bed 8.
2~4 vertical thermocouples 51 are provided with the catalyst bed 8, vertical thermocouple 51 is annularly distributed in catalyst bed 8
It is interior;Multiple temperature measuring points 52 are vertically evenly equipped with vertical thermocouple 51.It is in bulk that the internal upper part of the first rectifying column 15 is equipped with first
Packing layer 54, the internal upper part of Second distillation column 18 are equipped with the second dumped packing layer 55.First feed preheater 11 is around pipe
Formula heat exchanger.
A kind of method for the process units for preparing 2- methylfurans, this method comprises the following steps:
Step 1:From the hydrogen of hydrogen gas holder 1,25~35 DEG C of temperature, pressure 2Kpa, pressurize through hydrogen gas compressor 2
Enter after being 0.05~0.1Mpa to 70~100 DEG C, pressure in annular outer barrel room 7 through hydrogen gas buffer 3, material inlet 6;Liquid phase
25~35 DEG C of furfurals of temperature of furfural measuring tank 4 enter furfural evaporator 5 by gravity, are steamed with 5 inner cylinder of furfural evaporator
The steam heat-exchanging of 0.9~1.1MPa in vapour coil pipe, temperature rise to 160~175 DEG C of furfural gasifications, and gas phase furfural is through material inlet 6
Into in annular outer barrel room 7;
Step 2:Hydrogen and gas phase furfural are entered after entering annular outer barrel room 7 by the aperture by annular outer tube wall 49
Into catalyst bed 8, in Cu-series catalyst presence, gas phase furfural and hydrogen reaction generation gas phase 2- methylfurans are above-mentioned
Substantial amounts of reaction heat is discharged in reaction process, reaction heat exchanges heat with heat exchange pipeline 24, makes the deaerated water in heat exchange pipeline 24
Absorb heat generation saturated vapor;The Cu-series catalyst for CuO- silicon oxide catalysts, CuO- aluminium oxide catalysts or
One of CuO- sial composite oxide catalysts;
Step 3:Gas phase 2- methylfurans enter in inner cylinder room 9 through the aperture on annular inner tube wall 50, through material outlet 10
Enter 2- methyl furans after temperature is reduced to 10~15 DEG C by the first tube bank of the first feed preheater 11,12 tube side of cooler
Mutter crude product storage tank 13;
Step 4:2- methylfurans crude product in 2- methylfuran crude products storage tank 13 is pressurized to 0.2 through feed pump 14~
After 0.3MPa, restrained by the second tube bank of the first feed preheater 11 with the first tube bank in the first feed preheater 11 and the 3rd
Media for heat exchange enters in 15 tower reactor of first rectifying column to after 100~105 DEG C, into the 2- methyl furans in 15 tower reactor of first rectifying column
Crude product overflow of muttering enters in 29 tube side of the first reboiler, it gasifies after steam heat-exchanging in the first reboiler 29 with shell side, gas
The 2- methylfuran crude products of change are ascended into first rectifying column 15, by the first dumped packing layer 54, the 2- methyl furans of gasification
The heavy constituent muttered in crude product is separated, and falls into 15 tower reactor of first rectifying column, light group in the 2- methylfuran crude products of gasification
Divide and be situated between by the first dumped packing layer 54 by the gaseous phase outlet at the top of first rectifying column 15 into the first feed preheater 11 the 3rd
Heat exchange in matter tube bank, the light component after heat exchange become liquid phase and enter in pans 16;Height in 15 tower reactor of first rectifying column
Boiling thing is periodically discharged into high-boiling components collecting tank 34;
Step 5:It is back into the liquid phase light component part in pans 16 by 15 centre inlet of first rectifying column
In first rectifying column 15, another part liquid phase light component enters 18 tower reactor of Second distillation column by 17 shell side of the second feed preheater
Interior, the overflow of liquid phase light component enters in 30 tube side of the second reboiler, and with gasifying after the steam heat-exchanging of shell side, gas phase light component enters
In Second distillation column 18, by the second dumped packing layer 55, in gas phase light component, high boiling substance, which is separated, falls into second
18 tower reactor of rectifying column, gas phase 2- methylfurans by the second dumped packing layer 55 by the top of Second distillation column 18 gaseous phase outlet into
Enter 17 tube side of the second feed preheater to exchange heat, become liquid phase 2- methylfurans after heat exchange, by the tube side of condenser 19 with
Bromine cold water enters in finished product storage tank 20 after further exchanging heat;The waste water of 18 tower reactor of Second distillation column is periodically discharged into waste collection
In tank 35;
Step 6:Deaerated water in water supply network 21 is entered in heat exchange pipeline 24 by bottom admission port 22 and hydroecium 23,
The reaction heat in catalyst bed 8 is taken away into the deaerated water in heat exchange pipeline 24, and generates saturated vapor, saturated vapor is by vapour
Bag 25,26 and first regulating valve 27 of steam (vapor) outlet enter in steam pipe network 28, and the saturated vapor in steam pipe network 28 respectively enters
Heated material uses in furfural evaporator 5, the first reboiler 29 and the second reboiler 30, and the steam condensate produced after use returns to
Steam condensate accumulator tank 31 recycles;Deoxygenation water pressure in the water supply network 21 is 0.5MPa, and temperature is 105 DEG C;Institute
It is 0.9~1.1MPa to state saturated vapour pressure, and temperature is 175~184 DEG C;
Step 7:Temperature measuring point 52 on vertical thermocouple 51 monitors the temperature of catalyst bed 8 in real time, makes catalyst bed
8 temperature are 175~184 DEG C;Temperature and steam pressure in catalyst bed 8 are direct ratio;When the temperature that temperature measuring point 52 detects is high
Steam pressure raises when 184 DEG C, and the pressure that pressure gauge 46 detects is more than 1.1MPa, and pressure gauge 46 feeds back pressure signal at this time
To controller 53, signal is transmitted to the first regulating valve 27 by controller 53, and the increase of 27 aperture of the first regulating valve, is sent to steam pipe network 28
Quantity of steam increase, heat transfer increase, recovers untill 175~184 DEG C until 8 temperature of catalyst bed in radial reactor;When
Steam pressure reduces when the temperature that temperature measuring point 52 detects is less than 175 DEG C, and the pressure that pressure gauge 46 detects is less than 0.9MPa, presses at this time
Pressure signal is fed back to controller 53 by power table 46, and signal is transmitted to the first regulating valve 27 by controller 53, and the first regulating valve 27 is opened
Degree reduces, and the quantity of steam for being sent to steam pipe network 28 is reduced, and heat transfer reduces in radial reactor, until 8 temperature of catalyst bed is extensive
Again untill 175~184 DEG C;
Step 8:First thermometer table 41 of the top of furfural evaporator 5 monitors gas phase furfural temperature at 160~175 DEG C, works as temperature
When degree is less than 160 DEG C, the first thermometer table 41 transmits a signal to controller 53, and signal is transmitted to the second regulating valve by controller 53
36, the increase of 36 aperture of the second regulating valve, is sent to the quantity of steam increase of steam pipe coil in furfural evaporator 5, and heat transfer strengthens, until the
One thermometer table, 41 temperature is recovered untill 160~175 DEG C;Conversely, when temperature is higher than 175 DEG C, the first thermometer table 41 will
Signal sends controller 53 to, and signal is transmitted to the second regulating valve 36 by controller 53, and 36 aperture of the second regulating valve reduces, and is sent to chaff
The quantity of steam of steam pipe coil is reduced in aldehyde evaporator 5, and heat transfer weakens, until 41 temperature of the first thermometer table is recovered to 160~175
Untill DEG C;
Step 9:Second temperature meter table 42 between 12 tube side of cooler and 2- methylfuran crude products storage tank 13 monitors pipeline
The temperature of interior 2- methylfurans crude product is between 10~15 DEG C, and when temperature is less than 10 DEG C, second temperature meter table 42 passes signal
Controller 53 is given, signal is transmitted to the 5th regulating valve 39 by controller 53, and 39 aperture of the 5th regulating valve reduces, and is sent to cooler 12
Bromine cool water quantity reduce, heat transfer weaken, recover until 42 temperature of second temperature meter table untill 10~15 DEG C;Conversely, work as temperature
During higher than 15 DEG C, second temperature meter table 42 transmits a signal to controller 53, and signal is transmitted to the 5th regulating valve 39 by controller 53,
5th regulating valve, 39 aperture increases, and is sent to the bromine cool water quantity increase of cooler 12, heat transfer enhancing, until the temperature of second temperature meter table 42
Degree recovers untill 10~15 DEG C;
Step 10:The bottom temperature of 3rd thermometer table 43 monitoring first rectifying column 15 works as temperature between 105~110 DEG C
When degree is less than 105 DEG C, the 3rd thermometer table 43 transmits a signal to controller 53, and signal is transmitted to the 3rd regulating valve by controller 53
37, the increase of 37 aperture of the 3rd regulating valve, is sent to the quantity of steam increase of the first reboiler 29, heat transfer enhancing, until the 3rd thermometer
43 temperature of table is recovered untill 105~110 DEG C;When temperature is higher than 110 DEG C, the 3rd thermometer table 43 transmits a signal to control
Signal is transmitted to the 3rd regulating valve 37 by device 53, controller 53, and 37 aperture of the 3rd regulating valve reduces, and is sent to the steaming of the first reboiler 29
Vapour amount is reduced, and heat transfer weakens, and recovers until 43 temperature of the 3rd thermometer table untill 105~110 DEG C;
Step 11:The bottom temperature of 5th thermometer table 45 monitoring Second distillation column 18 works as temperature between 80~85 DEG C
When degree is less than 80 DEG C, the 5th thermometer table 45 transmits a signal to controller 53, and signal is transmitted to the 4th regulating valve by controller 53
38, the increase of 38 aperture of the 4th regulating valve, is sent to the quantity of steam increase of the second reboiler 30, heat transfer enhancing, until the 5th thermometer
45 temperature of table is recovered untill 105~110 DEG C;Conversely, when temperature is higher than 85 DEG C, the 5th thermometer table 45 transmits a signal to
Signal is transmitted to the 4th regulating valve 38 by controller 53, controller 53, and 38 aperture of the 4th regulating valve reduces, and is sent to the second reboiler 30
Quantity of steam reduce, heat transfer weaken, recover until 45 temperature of the 5th thermometer table untill 105~110 DEG C;
Step 12:19 tube side of condenser and 2- methylfurans in the 4th thermometer table 44 monitoring pipeline of finished product storage tank 20
Temperature between 10~15 DEG C, when temperature be less than 10 DEG C when, the 4th thermometer table 44 transmits a signal to controller 53, control
Signal is transmitted to the 6th regulating valve 40 by device 53, and 40 aperture of the 6th regulating valve reduces, and the bromine cool water quantity for being sent to cooler 12 is reduced, and is passed
Heat weakens, and recovers until 44 temperature of the 4th thermometer table untill 10~15 DEG C;Conversely, when temperature is higher than 15 DEG C, the 4th temperature
Degree meter table 44 transmits a signal to controller 53, and signal is transmitted to the 6th regulating valve 40,40 aperture of the 6th regulating valve by controller 53
Increase, is sent to the bromine cool water quantity enhancing of condenser 19, heat transfer enhancing, until 44 temperature of the 4th thermometer table is recovered to 10~15 DEG C
Untill.
For the more detailed explanation present invention, the present invention is further elaborated in conjunction with embodiment.Specific embodiment
It is as follows:
Embodiment one
A kind of method for the process units for preparing 2- methylfurans, this method comprises the following steps:
Step 1:From the hydrogen of hydrogen gas holder 1,25~35 DEG C of temperature, pressure 2Kpa, pressurize through hydrogen gas compressor 2
Enter after being 0.05~0.1Mpa to 70~100 DEG C, pressure in annular outer barrel room 7 through hydrogen gas buffer 3, material inlet 6;Liquid phase
25~35 DEG C of furfurals of temperature of furfural measuring tank 4 enter furfural evaporator 5 by gravity, are steamed with 5 inner cylinder of furfural evaporator
The steam heat-exchanging of 0.9~1.1MPa in vapour coil pipe, temperature rise to 167.5 DEG C of furfural gasifications, and gas phase furfural enters through material inlet 6
In annular outer barrel room 7;
Step 2:Hydrogen and gas phase furfural are entered after entering annular outer barrel room 7 by the aperture by annular outer tube wall 49
Into catalyst bed 8, in Cu-series catalyst presence, gas phase furfural and hydrogen reaction generation gas phase 2- methylfurans are above-mentioned
Substantial amounts of reaction heat is discharged in reaction process, reaction heat exchanges heat with heat exchange pipeline 24, makes the deaerated water in heat exchange pipeline 24
Absorb heat generation saturated vapor;The Cu-series catalyst is CuO- silicon oxide catalysts;
Step 3:Gas phase 2- methylfurans enter in inner cylinder room 9 through the aperture on annular inner tube wall 50, through material outlet 10
Enter 2- methylfurans after temperature is reduced to 12.5 DEG C by the first tube bank of the first feed preheater 11,12 tube side of cooler
Crude product storage tank 13;
Step 4:2- methylfurans crude product in 2- methylfuran crude products storage tank 13 is pressurized to 0.2 through feed pump 14~
After 0.3MPa, restrained by the second tube bank of the first feed preheater 11 with the first tube bank in the first feed preheater 11 and the 3rd
Media for heat exchange enters in 15 tower reactor of first rectifying column to after 100~105 DEG C, into the 2- methyl furans in 15 tower reactor of first rectifying column
Crude product overflow of muttering enters in 29 tube side of the first reboiler, it gasifies after steam heat-exchanging in the first reboiler 29 with shell side, gas
The 2- methylfuran crude products of change are ascended into first rectifying column 15, by the first dumped packing layer 54, the 2- methyl furans of gasification
The heavy constituent muttered in crude product is separated, and falls into 15 tower reactor of first rectifying column, light group in the 2- methylfuran crude products of gasification
Divide and be situated between by the first dumped packing layer 54 by the gaseous phase outlet at the top of first rectifying column 15 into the first feed preheater 11 the 3rd
Heat exchange in matter tube bank, the light component after heat exchange become liquid phase and enter in pans 16;Height in 15 tower reactor of first rectifying column
Boiling thing is periodically discharged into high-boiling components collecting tank 34;
Step 5:It is back into the liquid phase light component part in pans 16 by 15 centre inlet of first rectifying column
In first rectifying column 15, another part liquid phase light component enters 18 tower reactor of Second distillation column by 17 shell side of the second feed preheater
Interior, the overflow of liquid phase light component enters in 30 tube side of the second reboiler, and with gasifying after the steam heat-exchanging of shell side, gas phase light component enters
In Second distillation column 18, by the second dumped packing layer 55, in gas phase light component, high boiling substance, which is separated, falls into second
18 tower reactor of rectifying column, gas phase 2- methylfurans by the second dumped packing layer 55 by the top of Second distillation column 18 gaseous phase outlet into
Enter 17 tube side of the second feed preheater to exchange heat, become liquid phase 2- methylfurans after heat exchange, by the tube side of condenser 19 with
Bromine cold water enters in finished product storage tank 20 after further exchanging heat;The waste water of 18 tower reactor of Second distillation column is periodically discharged into waste collection
In tank 35;
Step 6:Deaerated water in water supply network 21 is entered in heat exchange pipeline 24 by bottom admission port 22 and hydroecium 23,
The reaction heat in catalyst bed 8 is taken away into the deaerated water in heat exchange pipeline 24, and generates saturated vapor, saturated vapor is by vapour
Bag 25,26 and first regulating valve 27 of steam (vapor) outlet enter in steam pipe network 28, and the saturated vapor in steam pipe network 28 respectively enters
Heated material uses in furfural evaporator 5, the first reboiler 29 and the second reboiler 30, and the steam condensate produced after use returns to
Steam condensate accumulator tank 31 recycles;Deoxygenation water pressure in the water supply network 21 is 0.5MPa, and temperature is 105 DEG C;Institute
It is 0.9~1.1MPa to state saturated vapour pressure, and temperature is 179.88 DEG C;
Step 7:Temperature measuring point 52 on vertical thermocouple 51 monitors the temperature of catalyst bed 8 in real time, makes catalyst bed
8 temperature are 175~184 DEG C;Temperature and steam pressure in catalyst bed 8 are direct ratio;Temperature measuring point 52 detect temperature be
179.88 DEG C, steam pressure 1.0MPa, the aperture of the first regulating valve 27 is constant at this time;
Step 8:First thermometer table 41 of the top of furfural evaporator 5 monitors gas phase furfural temperature at 160~175 DEG C;First
41 displays temperature of thermometer table is 167.5 DEG C, and 36 aperture of the second regulating valve is constant;
Step 9:Second temperature meter table 42 between 12 tube side of cooler and 2- methylfuran crude products storage tank 13 monitors pipeline
For the temperature of interior 2- methylfurans crude product between 10~15 DEG C, 42 displays temperature of second temperature meter table is 12.5 DEG C, and the 5th is adjusted
Valve opening is constant;
Step 10:The bottom temperature of 3rd thermometer table 43 monitoring first rectifying column 15 is between 105~110 DEG C, and the 3rd
43 displays temperature of thermometer table is 107.5 DEG C, and the aperture of the 3rd regulating valve 37 is constant;
Step 11:The bottom temperature of 5th thermometer table 45 monitoring Second distillation column 18 is between 80~85 DEG C, and the 5th
45 displays temperature of thermometer table is 82.5 DEG C, and 38 aperture of the 4th regulating valve is constant;
Step 12:19 tube side of condenser and 2- methylfurans in the 4th thermometer table 44 monitoring pipeline of finished product storage tank 20
Temperature between 10~15 DEG C, 44 displays temperature of the 4th thermometer table be 12.5 DEG C, 40 aperture of the 6th regulating valve is constant.
Embodiment two
A kind of method for the process units for preparing 2- methylfurans, this method comprises the following steps:
Step 1:From the hydrogen of hydrogen gas holder 1,25~35 DEG C of temperature, pressure 2Kpa, pressurize through hydrogen gas compressor 2
Enter after being 0.05~0.1Mpa to 70~100 DEG C, pressure in annular outer barrel room 7 through hydrogen gas buffer 3, material inlet 6;Liquid phase
25~35 DEG C of furfurals of temperature of furfural measuring tank 4 enter furfural evaporator 5 by gravity, are steamed with 5 inner cylinder of furfural evaporator
The steam heat-exchanging of 0.9~1.1MPa in vapour coil pipe, temperature rise to 158 DEG C, and it is 160 DEG C of chaffs to be adjusted by step 8 to temperature
Aldehyde gasifies, and gas phase furfural enters in annular outer barrel room 7 through material inlet 6;
Step 2:Hydrogen and gas phase furfural are entered after entering annular outer barrel room 7 by the aperture by annular outer tube wall 49
Into catalyst bed 8, in Cu-series catalyst presence, gas phase furfural and hydrogen reaction generation gas phase 2- methylfurans are above-mentioned
Substantial amounts of reaction heat is discharged in reaction process, reaction heat exchanges heat with heat exchange pipeline 24, makes the deaerated water in heat exchange pipeline 24
Absorb heat generation saturated vapor;The Cu-series catalyst is CuO- aluminium oxide catalysts;
Step 3:Gas phase 2- methylfurans enter in inner cylinder room 9 through the aperture on annular inner tube wall 50, through material outlet 10
Temperature is reduced to 8 DEG C by the first tube bank of the first feed preheater 11,12 tube side of cooler, adjusts temperature through step 9
Enter 2- methylfuran crude products storage tank 13 after to 10 DEG C;
Step 4:2- methylfurans crude product in 2- methylfuran crude products storage tank 13 is pressurized to 0.2 through feed pump 14~
After 0.3MPa, restrained by the second tube bank of the first feed preheater 11 with the first tube bank in the first feed preheater 11 and the 3rd
Media for heat exchange enters in 15 tower reactor of first rectifying column to after 100~105 DEG C, into the 2- methyl furans in 15 tower reactor of first rectifying column
Crude product overflow of muttering enters in 29 tube side of the first reboiler, it gasifies after steam heat-exchanging in the first reboiler 29 with shell side, gas
The 2- methylfuran crude products of change are ascended into first rectifying column 15, by the first dumped packing layer 54, the 2- methyl furans of gasification
The heavy constituent muttered in crude product is separated, and falls into 15 tower reactor of first rectifying column, light group in the 2- methylfuran crude products of gasification
Divide and be situated between by the first dumped packing layer 54 by the gaseous phase outlet at the top of first rectifying column 15 into the first feed preheater 11 the 3rd
Heat exchange in matter tube bank, the light component after heat exchange become liquid phase and enter in pans 16;Height in 15 tower reactor of first rectifying column
Boiling thing is periodically discharged into high-boiling components collecting tank 34;
Step 5:It is back into the liquid phase light component part in pans 16 by 15 centre inlet of first rectifying column
In first rectifying column 15, another part liquid phase light component enters 18 tower reactor of Second distillation column by 17 shell side of the second feed preheater
Interior, the overflow of liquid phase light component enters in 30 tube side of the second reboiler, and with gasifying after the steam heat-exchanging of shell side, gas phase light component enters
In Second distillation column 18, by the second dumped packing layer 55, in gas phase light component, high boiling substance, which is separated, falls into second
18 tower reactor of rectifying column, gas phase 2- methylfurans by the second dumped packing layer 55 by the top of Second distillation column 18 gaseous phase outlet into
Enter 17 tube side of the second feed preheater to exchange heat, become liquid phase 2- methylfurans after heat exchange, by the tube side of condenser 19 with
Bromine cold water enters in finished product storage tank 20 after further exchanging heat;The waste water of 18 tower reactor of Second distillation column is periodically discharged into waste collection
In tank 35;
Step 6:Deaerated water in water supply network 21 is entered in heat exchange pipeline 24 by bottom admission port 22 and hydroecium 23,
The reaction heat in catalyst bed 8 is taken away into the deaerated water in heat exchange pipeline 24, and generates saturated vapor, saturated vapor is by vapour
Bag 25,26 and first regulating valve 27 of steam (vapor) outlet enter in steam pipe network 28, and the saturated vapor in steam pipe network 28 respectively enters
Heated material uses in furfural evaporator 5, the first reboiler 29 and the second reboiler 30, and the steam condensate produced after use returns to
Steam condensate accumulator tank 31 recycles;Deoxygenation water pressure in the water supply network 21 is 0.5MPa, and temperature is 105 DEG C;Institute
It is 0.9~1.1MPa to state saturated vapour pressure, and temperature is 170.4 DEG C, is adjusted at this time by step 7 into trip temperature;
Step 7:Temperature measuring point 52 on vertical thermocouple 51 monitors the temperature of catalyst bed 8 in real time, makes catalyst bed
8 temperature are 175~184 DEG C;Temperature and steam pressure in catalyst bed 8 are direct ratio;When the temperature that temperature measuring point 52 detects is
Steam pressure reduces at 170.4 DEG C, and the pressure that pressure gauge 46 detects is 0.8MPa, and pressure gauge 46 feeds back to pressure signal at this time
Signal is transmitted to the first regulating valve 27 by controller 53, controller 53, and 27 aperture of the first regulating valve reduces, and is sent to steam pipe network 28
Quantity of steam is reduced, and heat transfer reduction, recovers untill 175 DEG C until 8 temperature of catalyst bed in radial reactor;
Step 8:First thermometer table 41 of the top of furfural evaporator 5 monitors gas phase furfural temperature at 160~175 DEG C, works as temperature
Spend for 158 DEG C when, the first thermometer table 41 transmits a signal to controller 53, and signal is transmitted to the second regulating valve by controller 53
36, the increase of 36 aperture of the second regulating valve, is sent to the quantity of steam increase of steam pipe coil in furfural evaporator 5, and heat transfer strengthens, until the
One thermometer table, 41 temperature is recovered untill 160 DEG C;
Step 9:Second temperature meter table 42 between 12 tube side of cooler and 2- methylfuran crude products storage tank 13 monitors pipeline
The temperature of interior 2- methylfurans crude product is between 10~15 DEG C, and when temperature is 8 DEG C, second temperature meter table 42 transmits a signal to
Signal is transmitted to the 5th regulating valve 39 by controller 53, controller 53, and 39 aperture of the 5th regulating valve reduces, and is sent to the bromine of cooler 12
Cool water quantity is reduced, and heat transfer weakens, and recovers until 42 temperature of second temperature meter table untill 10 DEG C;
Step 10:The bottom temperature of 3rd thermometer table 43 monitoring first rectifying column 15 works as temperature between 105~110 DEG C
Spend for 102 DEG C when, the 3rd thermometer table 43 transmits a signal to controller 53, and signal is transmitted to the 3rd regulating valve by controller 53
37, the increase of 37 aperture of the 3rd regulating valve, is sent to the quantity of steam increase of the first reboiler 29, heat transfer enhancing, until the 3rd thermometer
43 temperature of table is recovered untill 105 DEG C;
Step 11:The bottom temperature of 5th thermometer table 45 monitoring Second distillation column 18 works as temperature between 80~85 DEG C
Spend for 75 DEG C when, the 5th thermometer table 45 transmits a signal to controller 53, and signal is transmitted to the 4th regulating valve 38 by controller 53,
4th regulating valve, 38 aperture increases, and is sent to the quantity of steam increase of the second reboiler 30, heat transfer enhancing, until the 5th thermometer table 45
Temperature is recovered untill 80 DEG C;
Step 12:19 tube side of condenser and 2- methylfurans in the 4th thermometer table 44 monitoring pipeline of finished product storage tank 20
Temperature between 10~15 DEG C, when temperature be 9 DEG C when, the 4th thermometer table 44 transmits a signal to controller 53, controller
Signal is transmitted to the 6th regulating valve 40 by 53, and 40 aperture of the 6th regulating valve reduces, and the bromine cool water quantity for being sent to cooler 12 is reduced, heat transfer
Weaken, recover until 44 temperature of the 4th thermometer table untill 10 DEG C.
Embodiment three
A kind of method for the process units for preparing 2- methylfurans, this method comprises the following steps:
Step 1:From the hydrogen of hydrogen gas holder 1,25~35 DEG C of temperature, pressure 2Kpa, pressurize through hydrogen gas compressor 2
Enter after being 0.05~0.1Mpa to 70~100 DEG C, pressure in annular outer barrel room 7 through hydrogen gas buffer 3, material inlet 6;Liquid phase
25~35 DEG C of furfurals of temperature of furfural measuring tank 4 enter furfural evaporator 5 by gravity, are steamed with 5 inner cylinder of furfural evaporator
The steam heat-exchanging of 0.9~1.1MPa in vapour coil pipe, temperature rise to 177 DEG C, and it is 175 DEG C of chaffs to be adjusted by step 8 to temperature
Aldehyde gasifies, and gas phase furfural enters in annular outer barrel room 7 through material inlet 6;
Step 2:Hydrogen and gas phase furfural are entered after entering annular outer barrel room 7 by the aperture by annular outer tube wall 49
Into catalyst bed 8, in Cu-series catalyst presence, gas phase furfural and hydrogen reaction generation gas phase 2- methylfurans are above-mentioned
Substantial amounts of reaction heat is discharged in reaction process, reaction heat exchanges heat with heat exchange pipeline 24, makes the deaerated water in heat exchange pipeline 24
Absorb heat generation saturated vapor;The Cu-series catalyst is CuO- sial composite oxide catalysts;
Step 3:Gas phase 2- methylfurans enter in inner cylinder room 9 through the aperture on annular inner tube wall 50, through material outlet 10
Temperature is reduced to 16 DEG C by the first tube bank of the first feed preheater 11,12 tube side of cooler, through step 9 by temperature tune
Enter 2- methylfuran crude products storage tank 13 after whole to 15 DEG C;
Step 4:2- methylfurans crude product in 2- methylfuran crude products storage tank 13 is pressurized to 0.2 through feed pump 14~
After 0.3MPa, restrained by the second tube bank of the first feed preheater 11 with the first tube bank in the first feed preheater 11 and the 3rd
Media for heat exchange enters in 15 tower reactor of first rectifying column to after 100~105 DEG C, into the 2- methyl furans in 15 tower reactor of first rectifying column
Crude product overflow of muttering enters in 29 tube side of the first reboiler, it gasifies after steam heat-exchanging in the first reboiler 29 with shell side, gas
The 2- methylfuran crude products of change are ascended into first rectifying column 15, by the first dumped packing layer 54, the 2- methyl furans of gasification
The heavy constituent muttered in crude product is separated, and falls into 15 tower reactor of first rectifying column, light group in the 2- methylfuran crude products of gasification
Divide and be situated between by the first dumped packing layer 54 by the gaseous phase outlet at the top of first rectifying column 15 into the first feed preheater 11 the 3rd
Heat exchange in matter tube bank, the light component after heat exchange become liquid phase and enter in pans 16;Height in 15 tower reactor of first rectifying column
Boiling thing is periodically discharged into high-boiling components collecting tank 34;
Step 5:It is back into the liquid phase light component part in pans 16 by 15 centre inlet of first rectifying column
In first rectifying column 15, another part liquid phase light component enters 18 tower reactor of Second distillation column by 17 shell side of the second feed preheater
Interior, the overflow of liquid phase light component enters in 30 tube side of the second reboiler, and with gasifying after the steam heat-exchanging of shell side, gas phase light component enters
In Second distillation column 18, by the second dumped packing layer 55, in gas phase light component, high boiling substance, which is separated, falls into second
18 tower reactor of rectifying column, gas phase 2- methylfurans by the second dumped packing layer 55 by the top of Second distillation column 18 gaseous phase outlet into
Enter 17 tube side of the second feed preheater to exchange heat, become liquid phase 2- methylfurans after heat exchange, by the tube side of condenser 19 with
Bromine cold water enters in finished product storage tank 20 after further exchanging heat;The waste water of 18 tower reactor of Second distillation column is periodically discharged into waste collection
In tank 35;
Step 6:Deaerated water in water supply network 21 is entered in heat exchange pipeline 24 by bottom admission port 22 and hydroecium 23,
The reaction heat in catalyst bed 8 is taken away into the deaerated water in heat exchange pipeline 24, and generates saturated vapor, saturated vapor is by vapour
Bag 25,26 and first regulating valve 27 of steam (vapor) outlet enter in steam pipe network 28, and the saturated vapor in steam pipe network 28 respectively enters
Heated material uses in furfural evaporator 5, the first reboiler 29 and the second reboiler 30, and the steam condensate produced after use returns to
Steam condensate accumulator tank 31 recycles;Deoxygenation water pressure in the water supply network 21 is 0.5MPa, and temperature is 105 DEG C;Institute
It is 0.9~1.1MPa to state saturated vapour pressure, and temperature is 188 DEG C;Adjusted at this time by step 7 into trip temperature;
Step 7:Temperature measuring point 52 on vertical thermocouple 51 monitors the temperature of catalyst bed 8 in real time, makes catalyst bed
8 temperature are 175~184 DEG C;Temperature and steam pressure in catalyst bed 8 are direct ratio;When the temperature that temperature measuring point 52 detects is
At 188 DEG C, steam pressure rise, the pressure that pressure gauge 46 detects is 1.2MPa, and pressure gauge 46 feeds back to pressure signal at this time
Signal is transmitted to the first regulating valve 27 by controller 53, controller 53, and the increase of 27 aperture of the first regulating valve, is sent to steam pipe network 28
Quantity of steam increases, and heat transfer increase, recovers untill 184 DEG C until 8 temperature of catalyst bed in radial reactor;
Step 8:First thermometer table 41 of the top of furfural evaporator 5 monitors gas phase furfural temperature at 160~175 DEG C, works as temperature
Spend for 177 DEG C when, the first thermometer table 41 transmits a signal to controller 53, and signal is transmitted to the second regulating valve by controller 53
36,36 aperture of the second regulating valve reduces, and the quantity of steam for being sent to steam pipe coil in furfural evaporator 5 is reduced, and heat transfer weakens, until the
One thermometer table, 41 temperature is recovered untill 175 DEG C;
Step 9:Second temperature meter table 42 between 12 tube side of cooler and 2- methylfuran crude products storage tank 13 monitors pipeline
The temperature of interior 2- methylfurans crude product is between 10~15 DEG C, and when temperature is 16 DEG C, second temperature meter table 42 transmits signal
To controller 53, signal is transmitted to the 5th regulating valve 39 by controller 53, and the increase of 39 aperture of the 5th regulating valve, is sent to cooler 12
Bromine cool water quantity increase, heat transfer enhancing, recovers untill 15 DEG C until 42 temperature of second temperature meter table;
Step 10:The bottom temperature of 3rd thermometer table 43 monitoring first rectifying column 15 works as temperature between 105~110 DEG C
Spend for 115 DEG C when, the 3rd thermometer table 43 transmits a signal to controller 53, and signal is transmitted to the 3rd regulating valve by controller 53
37,37 aperture of the 3rd regulating valve reduces, and the quantity of steam for being sent to the first reboiler 29 is reduced, and heat transfer weakens, until the 3rd thermometer
43 temperature of table is recovered untill 110 DEG C;
Step 11:The bottom temperature of 5th thermometer table 45 monitoring Second distillation column 18 works as temperature between 80~85 DEG C
Spend for 86 DEG C when, the 5th thermometer table 45 transmits a signal to controller 53, and signal is transmitted to the 4th regulating valve 38 by controller 53,
4th regulating valve, 38 aperture reduces, and the quantity of steam for being sent to the second reboiler 30 is reduced, and heat transfer weakens, until the 5th thermometer table 45
Temperature is recovered untill 85 DEG C;
Step 12:19 tube side of condenser and 2- methylfurans in the 4th thermometer table 44 monitoring pipeline of finished product storage tank 20
Temperature between 10~15 DEG C, when temperature be higher than 17 DEG C when, the 4th thermometer table 44 transmits a signal to controller 53, control
Signal is transmitted to the 6th regulating valve 40 by device 53, and the increase of 40 aperture of the 6th regulating valve, is sent to the bromine cool water quantity enhancing of condenser 19, passes
Heat enhancing, recovers untill 15 DEG C until 44 temperature of the 4th thermometer table.
Experimental example:
The method of 2- methylfurans is prepared using axial adiabatic reactor and 2- is produced by the device of the invention and method
Methylfuran, the contrast of its basic condition are as follows:
Project | Axial adiabatic reactor | The present invention |
Resistance situation | 20~30KPa | 5~10KPa |
Bed temperature gradient | 175~250 DEG C | 175~184 DEG C |
Recirculated cooling water | Need | Need not |
Byproduct steam | Nothing | By-product 1.0MPa steam |
Conversion ratio | 90% | 96% |
Accessory substance | It is more | It is few |
Catalyst service life | 3 months | 5 months |
Resistance situation in upper table refers to the resistance situation of catalyst bed 8, and recirculated cooling water refers to 2- methylfurans
The type of cooling, from the content of above table, the resistance of method catalyst bed 8 of the invention is small, 8 temperature of catalyst bed
Graded is small, and the high conversion rate and quality of the product of output are good, and need not cool down, can byproduct steam, catalyst use
Long lifespan.
In the description of the present invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " connection ", " phase
Company " etc. should be interpreted broadly, for example, it may be being fixedly connected, be integrally connected or be detachably connected;Can also
It is the connection inside two elements;It can be directly connected, can also be indirectly connected by intermediary, for the general of this area
For logical technical staff, the concrete meaning of above-mentioned term in the present invention can be understood as the case may be.Above specifically
The bright feasibility embodiment only for the present invention illustrates, they are simultaneously not used to the protection model of the limitation present invention
Enclose, all equivalent implementations made without departing from skill spirit of the present invention, change and transformation should be included in the protection of the present invention
Within the scope of.
Claims (9)
1. a kind of process units for preparing 2- methylfurans, including hydrogen gas holder (1), liquid phase furfural measuring tank (4), finished product storage tank
(20) and water supply network (21), it is characterised in that:The hydrogen gas holder (1) passes through hydrogen gas compressor (2) and hydrogen gas buffer (3)
It is connected with the material inlet (6) of radial reactor, liquid phase furfural measuring tank (4) passes through furfural evaporator (5) and radial reactor
Material inlet (6) be connected, what the material outlet (10) of radial reactor passed sequentially through the first feed preheater (11) first is situated between
Matter tube bank, cooler (12) tube side, 2- methylfuran crude product storage tanks (13), feed pump (14), the first feed preheater (11)
Second medium tube bank is connected with the middle and lower part import of first rectifying column (15), first rectifying column (15) outlet at bottom respectively with high-boiling components
Collecting tank (34) is connected with the bottoms material entrance of the first reboiler (29) tube side, the top gas phase of the first reboiler (29) tube side
Outlet is connected with the lower inlet of first rectifying column (15), and the gaseous phase outlet at the top of first rectifying column (15) is pre- by the first charging
Hot the 3rd medium of device (11) tube bank is connected with the input end of pans (16), first exit end and the first rectifying of pans (16)
The middle and upper part import of tower (15) is connected, and the second outlet end of pans (16) passes through the second feed preheater (17) shell side and second
Rectifying column (18) middle and upper part import is connected, and Second distillation column (18) outlet at bottom boils again with waste collection tank (35) and second respectively
The bottoms material entrance of device (30) tube side is connected, the top gas phase outlet and Second distillation column (18) of the second reboiler (30) tube side
Lower inlet be connected, the gaseous phase outlet at the top of Second distillation column (18) passes through the second feed preheater (17) tube side and condenser
(19) tube side is connected with finished product storage tank (20);
The radial reactor includes housing (48), and housing (48) ecto-entad has annular outer barrel room (7), catalyst bed successively
(8) and inner cylinder room (9) narrow meshed annular outer tube wall (49), is equipped between annular outer barrel room (7) and catalyst bed (8), is urged
Agent bed (8) is internally provided with some heat exchange pipelines (24), is equipped between catalyst bed (8) and inner cylinder room (9) with small
The annular inner tube wall (50) in hole, the top of housing (48) are equipped with material inlet (6) and steam (vapor) outlet (26), material inlet (6) with
The top of annular outer barrel room (7) is connected, and steam (vapor) outlet (26) is connected by drum (25) with the top of heat exchange pipeline (24);Housing
(48) bottom is equipped with material outlet (10), bottom admission port (22) and catalyst discharge port (47), and bottom admission port (22) are logical
The bottom that hydroecium (23) is crossed with heat exchange pipeline (24) is connected, and material outlet (10) is connected with the bottom of inner cylinder room (9), catalyst
Discharge port (47) is connected with the bottom of catalyst bed (8);
The water supply network (21) is connected by pipeline with bottom admission port (22), and steam (vapor) outlet (26) passes through the first regulating valve
(27) it is connected with steam pipe network (28), steam pipe network (28) passes through pipeline and the second regulating valve (36), the 3rd regulating valve respectively
(37) it is connected with the 4th regulating valve (38), the second regulating valve (36) is coagulated by the steam pipe coil in furfural evaporator (5) with steam
Liquid accumulator tank (31) is connected, the shell side and steam condensate accumulator tank (31) phase that the 3rd regulating valve (37) passes through the first reboiler (29)
Even, the 4th regulating valve (38) is connected by the shell side of the second reboiler (30) with steam condensate accumulator tank (31);
The shell side import of the cooler (12) is connected by the 5th regulating valve (39) with lithium bromide come grid (32), cooler
(12) shell-side outlet is connected with lithium bromide return pipe net (33);
The shell side import of the condenser (19) is connected by the 6th regulating valve (40) with lithium bromide come grid (32), condenser
(19) shell-side outlet is connected with lithium bromide return pipe net (33);
Pressure gauge (46), furfural evaporator (5) are installed between the steam (vapor) outlet (26) and the first regulating valve (27) on pipeline
Top is provided with the first thermometer table (41), on the pipeline between cooler (12) tube side and 2- methylfuran crude product storage tanks (13)
Second temperature meter table (42) is installed, first rectifying column (15) tower reactor is provided with the 3rd thermometer table (43), condenser (19) with
4th thermometer table (44) is installed, Second distillation column (18) tower reactor is provided with the 5th temperature on the pipeline between finished product storage tank (20)
Degree meter table (45);
The pressure gauge (46), the first thermometer table (41), second temperature meter table (42), the 3rd thermometer table (43), the 4th temperature
Degree meter table (44) and input terminal of the 5th thermometer table (45) respectively with controller (53) are connected, the output terminal point of controller (53)
Not with the first regulating valve (27), the second regulating valve (36), the 3rd regulating valve (37), the 4th regulating valve (38), the 5th regulating valve
(39), the 6th regulating valve (40) is connected.
A kind of 2. process units for preparing 2- methylfurans according to claim 1, it is characterised in that:The furfural evaporation
Device (5) is is vertically arranged, and the lower part of furfural evaporator (5) inner cylinder is equipped with steam pipe coil, and the top of inner cylinder is hollow.
A kind of 3. process units for preparing 2- methylfurans according to claim 1, it is characterised in that:The annular outer barrel
The surface of wall (49) and annular inner tube wall (50) is evenly distributed with aperture.
A kind of 4. process units for preparing 2- methylfurans according to claim 1, it is characterised in that:The heat exchange pipeline
(24) vertically it is distributed in catalyst bed (8).
A kind of 5. process units for preparing 2- methylfurans according to claim 3, it is characterised in that:The heat exchange pipeline
(24) annularly it is distributed in catalyst bed (8).
A kind of 6. process units for preparing 2- methylfurans according to claim 1, it is characterised in that:The catalyst bed
2~4 vertical thermocouples (51) are provided with layer (8), vertical thermocouple (51) is annularly distributed in catalyst bed (8);
Multiple temperature measuring points (52) are vertically evenly equipped with vertical thermocouple (51).
A kind of 7. process units for preparing 2- methylfurans according to claim 1, it is characterised in that:First rectifying
The internal upper part of tower (15) is equipped with the first dumped packing layer (54), and the internal upper part of Second distillation column (18) is equipped with the second dumped packing layer
(55)。
A kind of 8. process units for preparing 2- methylfurans according to claim 1, it is characterised in that:First charging
Preheater (11) is wound tube heat exchanger.
9. a kind of method that process units using described in claim 1-8 prepares 2- methylfurans, it is characterised in that this method
Include the following steps:
Step 1:The hydrogen come from hydrogen gas holder (1), 25~35 DEG C of temperature, pressure 2Kpa, pressurize through hydrogen gas compressor (2)
Through hydrogen gas buffer (3), material inlet (6) enter annular outer barrel room (7) after being 0.05~0.1Mpa to 70~100 DEG C, pressure
It is interior;
25~35 DEG C of furfurals of temperature that liquid phase furfural measuring tank (4) comes enter furfural evaporator (5) by gravity, are steamed with furfural
The steam heat-exchanging of 0.9~1.1MPa in device (5) inner cylinder steam pipe coil is sent out, temperature rises to 160~175 DEG C of furfural gasifications, gas phase chaff
Aldehyde enters in annular outer barrel room (7) through material inlet (6);
Step 2:Hydrogen and gas phase furfural are entered after entering annular outer barrel room (7) by the aperture by annular outer tube wall (49)
In to catalyst bed (8), in Cu-series catalyst presence, gas phase furfural and hydrogen reaction generation gas phase 2- methylfurans, on
State and substantial amounts of reaction heat is discharged in reaction process, reaction heat exchanges heat with heat exchange pipeline (24), makes in heat exchange pipeline (24)
Deaerated water absorbs heat generation saturated vapor;The Cu-series catalyst is CuO- silicon oxide catalysts, CuO- alumina catalyzations
One of agent or CuO- sial composite oxide catalysts;
Step 3:Gas phase 2- methylfurans enter in inner cylinder room (9) through the aperture on annular inner tube wall (50), through material outlet
(10) enter after temperature being reduced to 10~15 DEG C by the first tube bank of the first feed preheater (11), cooler (12) tube side
2- methylfuran crude product storage tanks (13);
Step 4:The interior 2- methylfurans crude product of 2- methylfuran crude product storage tanks (13) is pressurized to 0.2 through feed pump (14)~
After 0.3MPa, by the second tube bank and the first tube bank in the first feed preheater (11) and the 3rd pipe of the first feed preheater (11)
The media for heat exchange of beam enters in first rectifying column (15) tower reactor to after 100~105 DEG C, into first rectifying column (15) tower reactor
The overflow of 2- methylfuran crude products enters in the first reboiler (29) tube side, it is changed in the first reboiler (29) with the steam of shell side
Gasifying after heat, the 2- methylfuran crude products of gasification are ascended into first rectifying column (15), by the first dumped packing layer (54),
Heavy constituent in the 2- methylfuran crude products of gasification is separated, and falls into first rectifying column (15) tower reactor, the 2- methyl of gasification
Light component in furans crude product enters the by the first dumped packing layer (54) by the gaseous phase outlet at the top of first rectifying column (15)
Heat exchange in the tube bank of the 3rd medium of one feed preheater (11), the light component after heat exchange become liquid phase and enter in pans (16);Institute
The high-boiling components stated in first rectifying column (15) tower reactor are periodically discharged into high-boiling components collecting tank (34);
Step 5:It is back into the liquid phase light component part in pans (16) by first rectifying column (15) centre inlet
In first rectifying column (15), another part liquid phase light component enters Second distillation column by the second feed preheater (17) shell side
(18) in tower reactor, the overflow of liquid phase light component enters in the second reboiler (30) tube side, with gasifying after the steam heat-exchanging of shell side, gas phase
Light component enters in Second distillation column (18), and by the second dumped packing layer (55), high boiling substance is divided in gas phase light component
From getting off to fall into Second distillation column (18) tower reactor, gas phase 2- methylfurans are by the second dumped packing layer (55) by Second distillation column
(18) gaseous phase outlet at the top of exchanges heat into the second feed preheater (17) tube side, becomes liquid phase 2- methyl furans after heat exchange
Mutter, by the tube side of condenser (19) with entering after bromine cold water further heat exchange in finished product storage tank (20);The Second distillation column
(18) waste water of tower reactor is periodically discharged into waste collection tank (35);
Step 6:Deaerated water in water supply network (21) enters heat exchange pipeline (24) by bottom admission port (22) and hydroecium (23)
It is interior, the reaction heat in catalyst bed (8) is taken away into the deaerated water in heat exchange pipeline (24), and saturated vapor is generated, saturation
Steam is entered in steam pipe network (28) by drum (25), steam (vapor) outlet (26) and the first regulating valve (27), in steam pipe network (28)
Saturated vapor respectively enter heated material in furfural evaporator (5), the first reboiler (29) and the second reboiler (30) and use,
The steam condensate produced after use returns to steam condensate accumulator tank (31) recycling;Deaerated water in the water supply network (21)
Pressure is 0.5MPa, and temperature is 105 DEG C;The saturated vapour pressure is 0.9~1.1MPa, and temperature is 175~184 DEG C;
Step 7:Temperature measuring point (52) on vertical thermocouple (51) monitors the temperature of catalyst bed (8) in real time, makes catalyst bed
Layer (8) temperature is 175~184 DEG C;Temperature and steam pressure in catalyst bed (8) are direct ratio;When temperature measuring point (52) detects
Temperature be higher than 184 DEG C when steam pressure raise, pressure gauge (46) detection pressure be more than 1.1MPa, at this time pressure gauge (46) general
Pressure signal feeds back to controller (53), and signal is transmitted to the first regulating valve (27) by controller (53), and the first regulating valve (27) is opened
Degree increase, the quantity of steam for being sent to steam pipe network (28) increase, heat transfer increase in radial reactor, until catalyst bed (8) temperature
Degree recovers untill 175~184 DEG C;When the temperature of temperature measuring point (52) detection is less than 175 DEG C, steam pressure reduces, pressure gauge
(46) pressure of detection is less than 0.9MPa, and pressure signal is fed back to controller (53), controller (53) by pressure gauge (46) at this time
Signal is transmitted to the first regulating valve (27), the first regulating valve (27) aperture reduces, and the quantity of steam for being sent to steam pipe network (28) is reduced,
Heat transfer reduces in radial reactor, and until catalyst bed (8), temperature is recovered untill 175~184 DEG C;
Step 8:The first thermometer table (41) monitors gas phase furfural temperature at 160~175 DEG C at the top of furfural evaporator (5), works as temperature
When degree is less than 160 DEG C, the first thermometer table (41) transmits a signal to controller (53), and signal is transmitted to second by controller (53)
Regulating valve (36), the increase of the second regulating valve (36) aperture, is sent to the quantity of steam increase of furfural evaporator (5) interior steam pipe coil, passes
Heat enhancing, recovers untill 160~175 DEG C until first thermometer table (41) temperature;Conversely, when temperature is higher than 175 DEG C, the
One thermometer table (41) transmits a signal to controller (53), and signal is transmitted to the second regulating valve (36) by controller (53), and second
Regulating valve (36) aperture reduces, and the quantity of steam for being sent to furfural evaporator (5) interior steam pipe coil is reduced, and heat transfer weakens, until first
Thermometer table (41) temperature is recovered untill 160~175 DEG C;
Step 9:Second temperature meter table (42) monitoring pipe between cooler (12) tube side and 2- methylfuran crude product storage tanks (13)
The temperature of 2- methylfurans crude product is between 10~15 DEG C in road, and when temperature is less than 10 DEG C, second temperature meter table (42) will be believed
Number sending controller (53) to, signal is transmitted to the 5th regulating valve (39) by controller (53), and the 5th regulating valve (39) aperture reduces,
The bromine cool water quantity for being sent to cooler (12) is reduced, and heat transfer weakens, until second temperature meter table (42) temperature is recovered to 10~15 DEG C
Untill;Conversely, when temperature is higher than 15 DEG C, second temperature meter table (42) transmits a signal to controller (53), controller (53)
Signal is transmitted to the 5th regulating valve (39), the increase of the 5th regulating valve (39) aperture, is sent to the bromine cool water quantity increase of cooler (12),
Heat transfer enhancing, until second temperature meter table (42), temperature is recovered untill 10~15 DEG C;
Step 10:The bottom temperature of 3rd thermometer table (43) monitoring first rectifying column (15) works as temperature between 105~110 DEG C
When degree is less than 105 DEG C, the 3rd thermometer table (43) transmits a signal to controller (53), and signal is transmitted to the 3rd by controller (53)
Regulating valve (37), the increase of the 3rd regulating valve (37) aperture, is sent to the quantity of steam increase of the first reboiler (29), and heat transfer strengthens, directly
Recover to the 3rd thermometer table (43) temperature untill 105~110 DEG C;When temperature is higher than 110 DEG C, the 3rd thermometer table (43)
Controller (53) is transmitted a signal to, signal is transmitted to the 3rd regulating valve (37), the 3rd regulating valve (37) aperture by controller (53)
Reduce, be sent to the first reboiler (29) quantity of steam reduce, heat transfer weaken, until the 3rd thermometer table (43) temperature recover to
Untill 105~110 DEG C;
Step 11:The bottom temperature of 5th thermometer table (45) monitoring Second distillation column (18) works as temperature between 80~85 DEG C
When degree is less than 80 DEG C, the 5th thermometer table (45) transmits a signal to controller (53), and signal is transmitted to the 4th by controller (53)
Regulating valve (38), the increase of the 4th regulating valve (38) aperture, is sent to the quantity of steam increase of the second reboiler (30), and heat transfer strengthens, directly
Recover to the 5th thermometer table (45) temperature untill 105~110 DEG C;Conversely, when temperature is higher than 85 DEG C, the 5th thermometer table
(45) controller (53) is transmitted a signal to, signal is transmitted to the 4th regulating valve (38), the 4th regulating valve (38) by controller (53)
Aperture reduces, and the quantity of steam for being sent to the second reboiler (30) is reduced, and heat transfer weakens, until the 5th thermometer table (45) temperature is recovered
Untill 80~85 DEG C;
Step 12:Condenser (19) tube side and 2- methyl furans in the 4th thermometer table (44) the monitoring pipeline of finished product storage tank (20)
The temperature muttered is between 10~15 DEG C, and when temperature is less than 10 DEG C, the 4th thermometer table (44) transmits a signal to controller
(53), signal is transmitted to the 6th regulating valve (40) by controller (53), and the 6th regulating valve (40) aperture reduces, and is sent to cooler (12)
Bromine cool water quantity reduce, heat transfer weaken, recover until the 4th thermometer table (44) temperature untill 10~15 DEG C;Conversely, when temperature
When degree is higher than 15 DEG C, the 4th thermometer table (44) transmits a signal to controller (53), and signal is transmitted to the 6th by controller (53)
Regulating valve (40), the increase of the 6th regulating valve (40) aperture, is sent to the bromine cool water quantity enhancing of condenser (19), and heat transfer strengthens, until
4th thermometer table (44) temperature is recovered untill 10~15 DEG C.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711379256.8A CN107973763A (en) | 2017-12-08 | 2017-12-08 | A kind of process units and method for preparing 2- methylfurans |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711379256.8A CN107973763A (en) | 2017-12-08 | 2017-12-08 | A kind of process units and method for preparing 2- methylfurans |
Publications (1)
Publication Number | Publication Date |
---|---|
CN107973763A true CN107973763A (en) | 2018-05-01 |
Family
ID=62006763
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201711379256.8A Pending CN107973763A (en) | 2017-12-08 | 2017-12-08 | A kind of process units and method for preparing 2- methylfurans |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107973763A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108863995A (en) * | 2018-06-18 | 2018-11-23 | 苏州盖德精细材料有限公司 | The high-efficiency environment friendly preparation method of 2- methylfuran |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU4213785A (en) * | 1984-03-27 | 1985-11-01 | Schick, J.H. | Vorrichtung zum warme- und stoffaustausch zwischen zwei oder mehr stromungsfahigen medien |
CN1467188A (en) * | 2002-07-10 | 2004-01-14 | 中国石油化工股份有限公司 | Cooling and heat recovery method for high temperature discharging of ethyl benzene dehydrogenation system |
CN1915943A (en) * | 2005-08-15 | 2007-02-21 | 中国石油化工股份有限公司 | Method for producing dimethylbenzene and benzene through dismutation of toluene and transference of alkyl |
WO2009135384A1 (en) * | 2008-05-05 | 2009-11-12 | Zhou Xiangjin | A process for preparing purified isophthalic acid |
CN102766118A (en) * | 2011-12-22 | 2012-11-07 | 江苏清泉化学有限公司 | Preparation method of 2-methyl furan |
CN203484134U (en) * | 2013-09-10 | 2014-03-19 | 张立军 | Water pipe type reaction device with steam pockets |
CN203916626U (en) * | 2014-05-08 | 2014-11-05 | 田晓良 | A kind of inner/outer drum structure the radial reactor with interpolation pipe heat exchanger |
CN105642197A (en) * | 2014-09-24 | 2016-06-08 | 楼韧 | Large-sized reactor, and device and process thereof |
CN205288361U (en) * | 2015-11-23 | 2016-06-08 | 河南心连心化肥有限公司 | Production heat transfer device for furfuryl alcohol |
CN105833802A (en) * | 2016-05-27 | 2016-08-10 | 成都赛普瑞兴科技有限公司 | Steam rising type catalyst bed reactor |
-
2017
- 2017-12-08 CN CN201711379256.8A patent/CN107973763A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU4213785A (en) * | 1984-03-27 | 1985-11-01 | Schick, J.H. | Vorrichtung zum warme- und stoffaustausch zwischen zwei oder mehr stromungsfahigen medien |
CN1467188A (en) * | 2002-07-10 | 2004-01-14 | 中国石油化工股份有限公司 | Cooling and heat recovery method for high temperature discharging of ethyl benzene dehydrogenation system |
CN1915943A (en) * | 2005-08-15 | 2007-02-21 | 中国石油化工股份有限公司 | Method for producing dimethylbenzene and benzene through dismutation of toluene and transference of alkyl |
WO2009135384A1 (en) * | 2008-05-05 | 2009-11-12 | Zhou Xiangjin | A process for preparing purified isophthalic acid |
CN102766118A (en) * | 2011-12-22 | 2012-11-07 | 江苏清泉化学有限公司 | Preparation method of 2-methyl furan |
CN203484134U (en) * | 2013-09-10 | 2014-03-19 | 张立军 | Water pipe type reaction device with steam pockets |
CN203916626U (en) * | 2014-05-08 | 2014-11-05 | 田晓良 | A kind of inner/outer drum structure the radial reactor with interpolation pipe heat exchanger |
CN105642197A (en) * | 2014-09-24 | 2016-06-08 | 楼韧 | Large-sized reactor, and device and process thereof |
CN205288361U (en) * | 2015-11-23 | 2016-06-08 | 河南心连心化肥有限公司 | Production heat transfer device for furfuryl alcohol |
CN105833802A (en) * | 2016-05-27 | 2016-08-10 | 成都赛普瑞兴科技有限公司 | Steam rising type catalyst bed reactor |
Non-Patent Citations (1)
Title |
---|
韩建多: "糠醛气相加氢制2-甲基呋喃的研讨", 辽宁化工 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108863995A (en) * | 2018-06-18 | 2018-11-23 | 苏州盖德精细材料有限公司 | The high-efficiency environment friendly preparation method of 2- methylfuran |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN204303368U (en) | Fixed gas retracting device in a kind of radioactive liquid waste evaporation process | |
CN104864734A (en) | Condenser and condensation method | |
CN107973763A (en) | A kind of process units and method for preparing 2- methylfurans | |
CN104864376B (en) | Heat-pipe type falling film evaporation low-temperature waste heat utilization and water recovery equipment | |
CN203869554U (en) | High-temperature-resistant single-tube-pass heat exchanger | |
CN206783619U (en) | A kind of waste heat of coke oven crude gas retracting device | |
CN203123608U (en) | Vertical type three-section condensation cooler | |
CN207671958U (en) | A kind of process units preparing 2- methylfurans | |
CN115975664A (en) | Delayed coking coke tower heat control process | |
CN107869857A (en) | One kind is based on the second kind absorption type mixing heat pump | |
CN204806354U (en) | Heat pipe formula falling film evaporation low temperature waste heat utilization and water -recovery apparatus | |
CN207671959U (en) | It is a kind of can flexible modulation prepare the process units of 2- methylfurans or furfuryl alcohol | |
CN207585140U (en) | One kind is based on the second kind absorption type mixing heat pump | |
CN216538373U (en) | Final stage water transfer heat bed layer ammonia synthesis reactor | |
CN105169734B (en) | Vacuum rectifying apparatus and its rectificating method | |
CN103567197B (en) | Washing device and process of PET (polyethylene terephthalate) liquid-phase tackifying kettle | |
CN105135907A (en) | High-temperature-resistant single-tube-pass heat exchange method and heat exchanger | |
CN207079195U (en) | A kind of new tar distillation device | |
CN106370028A (en) | Coking raw gas waste heat recovery method and apparatus | |
CN212214643U (en) | A liquid heat transfer economizer system that boils for ethanol is retrieved | |
CN104826348B (en) | A kind of steam condensed water waste heat that recycles processes the method extracting mixed liquor | |
CN204987932U (en) | Coking raw coke oven gas waste heat recovery device | |
CN203271829U (en) | Double-power ORC power generation system | |
CN202945072U (en) | Liquid evaporator | |
CN202105448U (en) | Multi-stage heat exchange distillation apparatus for dirty organic materials |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
CB02 | Change of applicant information |
Address after: 453731 Xinxiang Economic Development Zone, Henan Province (Xiaoji Town) Applicant after: Henan Xinlianxin Chemical Industry Group Co.,Ltd. Address before: 453731 Henan Xinxiang Economic Development Zone Xiaoji Town Henan Xinlianxin Chemical Fertilizer Co., Ltd. Applicant before: HENAN XINLIANXIN FERTILIZER Co.,Ltd. |
|
CB02 | Change of applicant information | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180501 |
|
WD01 | Invention patent application deemed withdrawn after publication |