CN106166469A - A kind of environmental protection hydrocarbon solvent low-voltage hydrogenation takes off arylation reaction device and catalyst filling method - Google Patents
A kind of environmental protection hydrocarbon solvent low-voltage hydrogenation takes off arylation reaction device and catalyst filling method Download PDFInfo
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- CN106166469A CN106166469A CN201610774424.2A CN201610774424A CN106166469A CN 106166469 A CN106166469 A CN 106166469A CN 201610774424 A CN201610774424 A CN 201610774424A CN 106166469 A CN106166469 A CN 106166469A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J8/04—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 passing successively through two or more beds
- B01J8/0446—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 passing successively through two or more beds the flow within the beds being predominantly vertical
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/44—Hydrogenation of the aromatic hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00752—Feeding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00761—Discharging
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00769—Details of feeding or discharging
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/02—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles
- B01J2208/023—Details
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/18—Solvents
Abstract
The present invention provides a kind of environmental protection hydrocarbon solvent low-voltage hydrogenation to take off arylation reaction device and catalyst filling method, use different-grain diameter porcelain ball and different-grain diameter, difformity catalyst layering collocation packing method, can prevent material from walking " short-circuit " or bed sink, the fluid distrbution being effectively improved in beds and pressure drop, strengthen distribution and the mixed effect of cold hydrogen system, reaction medium is made to contact with catalyst uniformly, in reactor, the flowing of medium is homogeneous, entirety reduces reactor size, to ensure the optimum depth of hydrogenation dearomatization reaction, speed and the yield of raising ideal composition, reduce equipment investment and Product processing cost, improve light hydrocarbon feedstocks comprehensive utilization added value.It is high that the present invention has reaction efficiency, and production capacity is big, manufactures the advantages such as easy to maintenance, temperature control intelligent, and alkane product is fractionated into rear purity and reaches more than 99%.
Description
Technical field:
The present invention relates to technical field of petrochemical industry, especially a kind of environmental protection hydrocarbon solvent low-voltage hydrogenation takes off arylation reaction device and catalysis
Agent loading method.
Background technology:
The hydrocarbon organic solvent of environmental protection low volatility is typically by preparing through rectification after the refined de-virtue of high-pressure hydrogenation again at present.Hydrogenation essence
The purpose of the de-virtue of system is the impurity such as sulfur, nitrogen, oxygen, chlorine, alkene and aromatic hydrocarbons in removing material, and some olefin generates through additive reaction
Corresponding paraffins, increases alkane yield, reduces the benzene content of product, reduces the extra organic emission during product uses, with
Reach environment protection emission index request.High-pressure hydrogenation takes off arylation reaction device and is not suitable for the light hydrocarbon feedstocks done less than less than 200 DEG C raw
Produce environmentally friendly solvent: first high-pressure hydrogenation takes off the reaction pressure height of arylation reaction device, and hydrogen consumption height, crack materials becomes the deep of gas phase；
Secondly high-pressure hydrogenation easily causes catalysqt deactivation, mechanical strength reduces, and loads knot in catalyst particle size collocation and reactor in addition
Structure design is unreasonable, causes the catalyst first saturated pulverizing on reactor top to be hardened, makes recycle hydrogen gas by reactor flow process
It is obstructed, it is impossible to ensure that reaction medium contacts uniformly with catalyst, it is impossible to realize the flowing of medium in reactor homogeneous, cause turnover
Mouth pressure reduction increases, and reaction temperature is out of control, so that cannot be properly functioning, device is forced to stop production, and carries out catalyst regeneration or renewal；Its
Sub-high pressure hydrogenation dearomatization catalyst requires to reach certain mechanical strength, and selects a certain amount of noble metal, and cost is higher, and one
Secondary property input ratio is relatively big, and unit product processing cost is high, and the market competitiveness is little.And the low-voltage hydrogenation applied now takes off arylation reaction device
Kind also compares many, and weak point is that structure is the simplest, and the gas flow characteristic not focusing on inside reactor processes, it is impossible to make
Reaction medium and catalyst uniform contact, hydrofinishing is inefficient, is unfavorable for popularization and application.
Catalyst packing operational approach is critically important, not only affects loaded catalyst, relevant with unit capacity, more important
Be that if density is uneven during filling, it is easy to make material walk " short-circuit " or bed sink, cause in reactor material with
Temperature distributing disproportionation, the phenomenon that material and catalyst contact time do not wait, have influence on the quality of product and the life-span of catalyst.As
Really the granularity of porcelain ball and the blending powder of catalyst are improper, are likely to result in the migration of catalyst.Therefore, the dress to catalyst
Fill out and must pay much attention to, carry out in strict accordance with requiring.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency, it is provided that with lighter hydrocarbons be raw material production pentane, normal hexane, hexane, petroleum ether,
A kind of environmental protection hydrocarbon solvent low-voltage hydrogenation of the hydrocarbon solvent such as heptane, benzene takes off arylation reaction device, and its technical scheme is: manhole flange group
Part is made up of bolt, nut and pad, is fixedly mounted on manhole connecting pipe, and manhole connecting pipe is welded on upper cover, and feed pipe leads to
Crossing feed pipe flange assembly connect mother tube and weld with manhole flange, its underpart is welded mutually with feed pipe heteromorphic connector, charging
In pipe heteromorphic connector, welding A-frame is in order to fixing rotating metallic blade, and feed distributor is solid by bolt, nut and pad
Dingan County is contained on feed pipe heteromorphic connector, and upper cover is oval, and its top is manhole, and bottom is welded with reactor shell, the
Four nozzle for thermometer are fixedly mounted on the sidewall outside cylinder, and hanger is welded on below the 4th nozzle for thermometer on barrel, catalysis
Being provided with the 3rd nozzle for thermometer on agent discharge duct II adjacent position, catalyst discharge duct II is arranged on a support plate top, catalysis
Agent discharge duct II flange assembly is made up of blind flange, bolt, nut and pad, is fixedly mounted on catalyst discharge duct II,
Support plate (is arranged on I-steel and bearing, cold hydrogen intake assembly adjacent position is provided with the second nozzle for thermometer, in the second temperature
Degree meter adapter is provided with the first nozzle for thermometer on adjacent position, and cold hydrogen intake assembly is arranged on below I-steel and bearing, cold
In the form of a ring, cold hydrogen nozzle is the most just to the fan blades being fixed on cold hydrogen tube, and removable insulation bracing ring is provided with multiple for hydrogen pipe,
Being welded on barrel outer surface, low head top is welded with reactor shell, and bottom is welded with skirt cylinder II, bottom low head
Being provided with discharging opening catcher, discharge nozzle overcoat discharging opening reinforced tube, top is connected with discharging opening catcher, is fixedly mounted on lower envelope
Communicate on head bottom center position outer wall and with cylinder, then by discharge nozzle elbow, discharging adapter, reactant is caused reactor
Outward, discharging adapter Socket welding is connected on skirt cylinder II, and interior welds discharging adapter gripper shoe is by fixing for discharging adapter, and discharging connects
Pipe flange assembly is made up of bolt, nut and pad, is fixedly mounted in discharging adapter, and steam vent adapter is welded on skirt cylinder
On II, it is following that catalyst discharge duct I sleeve pipe is positioned at steam vent adapter, is welded on skirt cylinder II, and interior welds catalyst unloads
Material pipe I gripper shoe fixed catalyst discharge duct I, catalyst discharge duct I be fixedly mounted on the outer wall of cylinder low head and with cylinder
Body communicates, and root is made up of bolt, nut and pad, by catalyst reinforcement sleeve pipe reinforcement, catalyst discharge duct I flange assembly
Discharge duct I blind flange is fixedly mounted on catalyst discharge duct I, and nameplate base is welded on skirt cylinder I, checks that eyelet welding is connected on skirt
On seat cylinder I, bottom foundation bolt seat welding skirt cylinder I, electrostatic grounding plate is welded on foundation bolt seat.
Catalyst filling method comprises the steps: that (1), catalyst filling must be carried out at fine day, and first installing periphery must
Want accessory device, carry out reactor, reactor internals, instrument, safety equipment, catalyst, porcelain ball preparation and every safety
Check work, verification catalyst and porcelain ball specifications and models, implement every safety measure；(2), according to reactor volume and catalyst
Amount, calculates filling ratio, determines each layer catalyst, the particle diameter of porcelain ball and filling height；(3), filling personnel wear safety
Cap, wears long tube respiratory organ, puts on dustproof clothes, marking pen on band, fastens seat belts in entrance pre-hydrogenator tower, enters
Within first 1 hour, carry out oxygen analysis qualified, according to the calculating of step 2, carry out each layer filling number of altitude, tower at reactor wall
Interior personnel must stand on plank, does not allow to stand directly on catalyst, in order to avoid stepping on broken catalyst, carrying out splicing and preparing, (4),
At the good Catalyst packing equipment of reactor head stage+module, be generally made up of three parts: hopper, under connect metal straight
Pipe, then be connected with a canvas hose, depending on metal tube and canvas duct diameter visual response device top opening size, general control exists
15～20cm, respectively set a gate valve with metal tube and metal tube with canvas duct junction at hopper, toward hopper apparatus with catalyst inside
Time close top gate valve, and bottom gate valve is for controlling the packing speed of catalyst, for preventing catalyst free-falling speed mistake
Hurry up, produce electrostatic and catalyst breakage, or " bridge formation ", preferably control the canvas mouth of pipe and be less than 1m away from charge level, (5), by canvas hose (on
Mouth is fixed on tower top manhole) put into tower, with crane, the inert ceramic balls of φ 15mm is hung tower top platform by loadings, porcelain ball
Pour hopper into, be sent in tower by canvas hose, after installing, porcelain ball carefully taken off flat, spread above by filling height the most successively
φ 8mm, φ 6mm inert ceramic balls, then at the stainless steel cloth of φ 6mm porcelain ball upper berth two-layer 20 mesh, run into installation thermometer and connect
The place of pipe, installs nozzle for thermometer, highly spreads φ 4mm, φ the most successively above by filling at the stainless steel silk completed
2mm, φ 4mm catalyst, after the catalyst of each layer of particle diameter installs, carefully takes off flat, after three layers of Catalyst packing, at φ
The stainless steel cloth of two-layer 20 mesh is spread on 4mm catalyst, the most again at paving φ 6mm, the inert ceramic balls of φ 8mm the most successively,
So far, lower bed layer filling is complete；(6), cold hydrogen intake assembly, I-steel and bearing, nozzle for thermometer, support plate, 10 mesh are installed
Stainless steel cloth, when installing these assemblies, assembly and reactor wall contact portion add girth sheets and asbestos seal with anti-leak, installation
After, remove foreign material in time, (7), according to step 5,6, successively filling upper bed layer porcelain ball, catalyst, install the temperature of bed
The internals such as degree meter adapter and feeding assembly, seal manhole.
Beneficial effects of the present invention: practicality reasonable in design, uses different-grain diameter porcelain ball and different-grain diameter, difformity catalyst to divide
Layer collocation packing method, can prevent material from walking " short-circuit " or bed and sink, the fluid distrbution being effectively improved in beds with
Pressure drop, strengthens distribution and the mixed effect of cold hydrogen system, makes reaction medium contact with catalyst uniformly, medium in reactor
Flowing homogeneous, entirety reduces reactor size, to ensure optimum depth, speed and raising ideal composition that hydrogenation dearomatization reacts
Yield, reduces equipment investment and Product processing cost, improves light hydrocarbon feedstocks comprehensive utilization added value.There is reaction efficiency high, raw
Production capacity power is big, manufactures the advantages such as easy to maintenance, temperature control intelligent, can be used for hydrogenation dearomatization produce high-purity pentane, normal hexane,
The environmental protection hydrocarbon solvents such as hexane, petroleum ether, heptane, benzene, alkane product is fractionated into rear purity and reaches more than 99%.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
Fig. 2 is the Catalyst packing method schematic diagram of a diameter of 1600mm of reactor shell of the present invention.
Detailed description of the invention
As it is shown in figure 1, shown in Fig. 1, a kind of environmental protection hydrocarbon solvent low-voltage hydrogenation takes off arylation reaction device, mainly by manhole flange assembly 1,
Manhole connecting pipe 2, feed pipe flange assembly 3, feed pipe 4, feed pipe heteromorphic connector 5, feed distributor 6, upper cover 7, reactor
Cylinder the 8, the 4th nozzle for thermometer 9, hanger the 10, the 3rd nozzle for thermometer 11, catalyst discharge duct II 12, catalyst discharge duct II
Flange assembly 13, a support plate 14, I-steel and bearing 15, cold hydrogen intake assembly the 16, second nozzle for thermometer 17, removable insulation are propped up
Support ring the 18, first nozzle for thermometer 19, low head 20, skirt cylinder II 21, discharging opening catcher 22, discharging opening reinforced tube 23,
Discharge nozzle 24, discharge nozzle elbow 25, discharging adapter sleeve pipe 26, discharging adapter gripper shoe 27, discharging adapter 28, discharging pipe connecting flange
Assembly 29, steam vent adapter 30, catalyst discharge duct I sleeve pipe 31, catalyst discharge duct I gripper shoe 32, catalyst discharge duct I
33, catalyst discharge duct I flange assembly 34, catalyst discharge duct I blind flange 35, nameplate base 36, inspection hole 37, skirt cylinder I
38, foundation bolt seat 39, electrostatic grounding plate 40 are constituted；Manhole flange assembly 1 is made up of bolt, nut and pad, fixed installation
On manhole connecting pipe 2, manhole connecting pipe 2 is welded on upper cover 7, and feed pipe 4 connects mother tube also by feed pipe flange assembly 3
Welding with manhole flange, its underpart is welded with feed pipe heteromorphic connector 5 phase, and in feed pipe heteromorphic connector 5, welding A-frame is used
With fixing rotating metallic blade, feed distributor 6 is fixedly mounted on feed pipe heteromorphic connector 5 by bolt, nut and pad,
Upper cover 7 is oval, and its top is manhole, and bottom is welded with reactor shell 8, and the 4th nozzle for thermometer 9 is fixedly mounted on
On sidewall outside cylinder, hanger 10 is welded on the 4th nozzle for thermometer 9 barrel below, catalyst discharge duct II 12 adjacent position
On the 3rd nozzle for thermometer 11 is installed, catalyst discharge duct II 12 is arranged on support plate 14 top, catalyst discharge duct II method
Blue assembly 13 is made up of blind flange, bolt, nut and pad, is fixedly mounted on catalyst discharge duct II 12, and a support plate 14 is pacified
It is contained on I-steel and bearing 15, cold hydrogen intake assembly 16 adjacent position is provided with the second nozzle for thermometer 17, in the second temperature
Degree meter is provided with the first nozzle for thermometer 19 on adapter 17 adjacent position, and cold hydrogen intake assembly 16 is arranged on I-steel and bearing 15
Below, in the form of a ring, cold hydrogen nozzle is the most just to the fan blades being fixed on cold hydrogen tube, removable insulation bracing ring 18 for cold hydrogen tube
Being provided with multiple, be welded on barrel outer surface, low head 20 top is welded with reactor shell 8, bottom and skirt cylinder II 21
Welding, is provided with discharging opening catcher 22, discharge nozzle 24 overcoat discharging opening reinforced tube 23 bottom low head 20, top is received with discharging opening
Storage 22 connects, and is fixedly mounted on low head 20 bottom center position outer wall and communicates with cylinder, then by discharge nozzle elbow
25, reactant is caused outside reactor by discharging adapter 28, and discharging adapter sleeve pipe 26 is welded on skirt cylinder II 21, interior welds
Discharging adapter 28 is fixed by discharging adapter gripper shoe 27, and discharging pipe connecting flange assembly 29 is made up of bolt, nut and pad, fixing
Being arranged in discharging adapter 28, steam vent adapter 30 is welded on skirt cylinder II 21, and catalyst discharge duct I sleeve pipe 31 is positioned at row
Below pore adapter 30, being welded on skirt cylinder II 21, interior welds catalyst discharge duct I gripper shoe 32 fixed catalyst unloads
Material pipe I 33, catalyst discharge duct I 33 is fixedly mounted on the outer wall of cylinder low head 20 and communicates with cylinder, and root is by reinforcement
Sleeve pipe reinforcement, catalyst discharge duct I flange assembly 34 is made up of bolt, nut and pad, by catalyst discharge duct I blind flange 35
Being fixedly mounted on catalyst discharge duct I 33, nameplate base 36 is welded on skirt cylinder I 38, checks that hole 37 is welded on skirt cylinder
On body I 38, foundation bolt seat 39 welds bottom skirt cylinder I 38, and electrostatic grounding plate 40 is welded on foundation bolt seat 39.
Catalyst filling method comprises the steps: that (1), catalyst filling must be carried out at fine day, and first installing periphery must
Want accessory device, carry out reactor, reactor internals, instrument, safety equipment, catalyst, porcelain ball preparation and every safety
Check work, verification catalyst and porcelain ball specifications and models, implement every safety measure；(2), according to reactor volume and catalyst
Amount, calculates filling ratio, determines each layer catalyst, the particle diameter of porcelain ball and filling height；(3), filling personnel wear safety
Cap, wears long tube respiratory organ, puts on dustproof clothes, marking pen on band, fastens seat belts in entrance pre-hydrogenator tower, enters
Within first 1 hour, carry out oxygen analysis qualified, according to the calculating of step 2, carry out each layer filling number of altitude, tower at reactor wall
Interior personnel must stand on plank, does not allow to stand directly on catalyst, in order to avoid stepping on broken catalyst, carrying out splicing and preparing, (4),
At the good Catalyst packing equipment of reactor head stage+module, be generally made up of three parts: hopper, under connect metal straight
Pipe, then be connected with a canvas hose, depending on metal tube and canvas duct diameter visual response device top opening size, general control exists
15～20cm, respectively set a gate valve with metal tube and metal tube with canvas duct junction at hopper, toward hopper apparatus with catalyst inside
Time close top gate valve, and bottom gate valve is for controlling the packing speed of catalyst, for preventing catalyst free-falling speed mistake
Hurry up, produce electrostatic and catalyst breakage, or " bridge formation ", preferably control the canvas mouth of pipe and be less than 1m away from charge level, (5), by canvas hose (on
Mouth is fixed on tower top manhole) put into tower, with crane, the inert ceramic balls of φ 15mm is hung tower top platform by loadings, porcelain ball
Pour hopper into, be sent in tower by canvas hose, after installing, porcelain ball carefully taken off flat, spread above by filling height the most successively
φ 8mm, φ 6mm inert ceramic balls, then at the stainless steel cloth of φ 6mm porcelain ball upper berth two-layer 20 mesh, run into installation thermometer and connect
The place of pipe, installs nozzle for thermometer, highly spreads φ 4mm, φ the most successively above by filling at the stainless steel silk completed
2mm, φ 4mm catalyst, after the catalyst of each layer of particle diameter installs, carefully takes off flat, after three layers of Catalyst packing, at φ
The stainless steel cloth of two-layer 20 mesh is spread on 4mm catalyst, the most again at paving φ 6mm, the inert ceramic balls of φ 8mm the most successively,
So far, lower bed layer filling is complete；(6), cold hydrogen intake assembly, I-steel and bearing, nozzle for thermometer, support plate, 10 mesh are installed
Stainless steel cloth, when installing these assemblies, assembly and reactor wall contact portion add girth sheets and asbestos seal with anti-leak, installation
After, remove foreign material in time, (7), according to step 5,6, successively filling upper bed layer porcelain ball, catalyst, install the temperature of bed
The internals such as degree meter adapter and feeding assembly, seal manhole.
Present invention process flow process: in feed pipe heteromorphic connector, welding A-frame is in order to fixing rotating metallic blade, and blade is by former
Material promotes and rotates, and makes raw material liquid phase change flow direction with gas phase, is more once sufficiently mixed, and is also beneficial to maintain charging point
In cloth device, gas phase, liquid phase fully combine, and make feed distributor respectively spray a gas-liquid flow rate evenly, in effectively preventing reactor
The formation of channel, improves reaction efficiency.The present invention is for processing the light hydrocarbon feedstocks doing less than 200 DEG C, uses gas, liquid mistake
Filter mixed feeding, therefore without designing gas distributor and rust deposite basket, by the inert catalyst protection porcelain ball of collocation different-grain diameter
Carry out substitutional theorem device and realize being uniformly distributed of liquid and gas in reactor.Disk hole limit is supported with upper bed layer for reducing porcelain ball cambered surface
Edge is in close contact and blocks the probability of happening of support disk hole event, as preferably, a support plate opens a width of 10mm, a length of 16mm,
It is spaced apart the strip hole of 10mm.Thickness according to a support plate and material, preferably supporting disc thickness 1/4 is that radius is to towards charging side
To limit, hole carry out rounding, to increase the gap between porcelain ball and support plate, it is achieved air-liquid run-off maximizes.Adding of hydro carbons
Hydrogen takes off virtue and belongs to exothermic reaction, and for many bed reactors, oil and hydrogen are after a upper bed reaction, and temperature will raise, for
It is suitable for next bed and continues the needs of hydrogenation dearomatization, it is necessary to the mode adding cold hydrogen in the middle of using controls reaction temperature: reaction
Temperature is the lowest the most favourable to aromatic hydrogenation reaction, and can make more benzene, toluene conversion is saturated hexamethylene and hexahydrotoluene.
Reaction temperature accelerates the forward and inverse response speed of aromatic hydrocarbons, in relatively low temperature range, the influence degree to positive reaction while raising
Much larger than the impact of back reaction, so it is favourable to the aromatic hydrogenation generation saturated hydrocarbons in lighter hydrocarbons to control relatively low reaction temperature.
As preferably, cold hydrogen intake assembly is arranged on below I-steel and bearing, and in the form of a ring, cold hydrogen nozzle is one to cold hydrogen tube
Determining angle just to the fan blades being fixed on cold hydrogen tube, hydrogen promotes fan blades high-speed rotation, makes the reaction fallen from upper support plate
Thing and hydrogen mixed aerosol, can improve flowing and the distribution of mixture, reduces temperature of charge, and intensified response thing air-fuel mixture is imitated
Really, the reaction for next bed provides preference temperature and the mixed uniformly advantage of reaction medium.As preferably, hydrogenation dearomatization
Reactor is made up of two beds, and each bed respectively sets a nozzle for thermometer, and built-in thermocouple can be to temperature of reactor
Monitor in real time, be conducive to regulating reaction temperature, to ensure the optimal degree of depth, speed and the raising ideal composition of hydrogenation dearomatization
Yield.
Preferably having the palladium of higher hydrogenation dearomatization activity, molybdenum, Raney nickel, its active center is Metal Palladium, molybdenum, nickel, profile
For spherical (φ 2.0-4.0mm-2.0-6.0mm), bulk density is 800-820Kg/m3, crushing strength ＞ 90N/cm, pore volume ＞
0.3cm3/100g.In order to reduce reactor pressure decrease, the catalyst of different-grain diameter takes different shapes filling of arranging in pairs or groups.Preferably
The high intensity porcelain ball such as corundum, mullite (φ 3.0-15.0mm).Porcelain ball is as the support of catalyst in reactor and covering
Material, available buffer enters the liquids and gases impact to catalyst in reactor, guard catalyst.Along feedstock direction from bed
Top starts the middle part to bed, and porcelain ball is gradually reduced with catalyst particle size, and liquids and gases distributed points gradually increases, and is respectively distributed
Point raw material forms a plurality of stable runoff due to gravity and intermolecular graviational interaction, and in being effectively improved reactor, liquid is gentle
The distribution of body, makes the flowing of medium in reactor homogeneous, and reaction medium contacts with catalyst uniformly, can prevent material from walking " short-circuit "
Or bed sink, it is ensured that reaction effect；To bottom bed in the middle part of bed, porcelain ball is gradually increased with catalyst particle size, liquid and
Gas distributed points gradually decreases, and reactant flow path resistance gradually decreases, and is favorably improved reaction efficiency.
As in figure 2 it is shown, preferably lower bed layer porcelain ball particle diameter is 15.0mm, 8.0mm, 6.0mm.From low head bottom center grain
Footpath 15.0mm porcelain ball upwards fills out 300.0mm, upwards fills out 100.0mm with particle diameter 8.0mm porcelain ball, with particle diameter 6.0mm porcelain ball the most upwards
Fill out 100.0mm；More than particle diameter 6.0mm porcelain ball filling out catalyst, catalyst top is porcelain ball protective layer: catalyst top particle diameter
6.0mm porcelain ball upwards fills out 100.0mm, upwards fills out 150.0mm with particle diameter 8.0mm porcelain ball.Lower bed layer is in addition to porcelain ball is taken up space, surplus
Complementary space is used for loading catalyst.Preferably lower bed layer catalyst particle size is 4mm, 2mm, from top to bottom large and small by particle diameter, fill greatly
Fill out, in the case of filling gross mass is certain, load in 2:5:3-1.5:6:2.5 ratio from top to bottom.
As in figure 2 it is shown, according to feedstock property, upper bed layer top preferable appendix molybdenum, nickel, the porous porcelain of cobalt isoreactivity component
Ball, it is simple to the impurity not filtered out in absorption raw material, to prevent carbon distribution coking and the poisoning of catalyst.Preferably upper bed layer porcelain ball grain
Footpath is 13.0mm, 8.0mm, 6.0mm.First it is layered on a support plate by the stainless steel cloth of barrel diameter two 10 circular mesh of cutting
On, upwards fill out 100.0mm with particle diameter 8.0mm porcelain ball at stainless (steel) wire, upwards fill out 150.0mm, particle diameter with particle diameter 6.0mm porcelain ball
More than 6.0mm porcelain ball filling out catalyst, catalyst top is porcelain ball protective layer: catalyst top particle diameter 6.0mm porcelain ball is upwards filled out
100.0mm, upwards fills out 150.0mm with particle diameter 8.0mm appendix molybdenum, nickel, the porous porcelain ball of cobalt isoreactivity component, uses particle diameter 13.0mm
Appendix molybdenum, nickel, the porous porcelain ball of cobalt isoreactivity component the most upwards fill out 150.0mm.Upper bed layer is in addition to porcelain ball is taken up space, and residue is empty
Between be used for loading catalyst.Preferably upper bed layer catalyst particle size is 4mm, 2mm, from top to bottom large and small by particle diameter, load greatly,
In the case of filling gross mass is certain, load in 2.5:4.5:3-1.5:6:2.5 ratio from top to bottom.
Do the raw oil of less than 200 DEG C heated after jointly enter reactor with hydrogen, elder generation is different through feed pipe, feed pipe
Shape joint, promotes the blade being fixed on feed pipe heteromorphic connector to rotate, and air-liquid is biphase tentatively to be mixed through feed distributor
Orifice plate also spreads to surrounding.First liquid phase, gas phase mixture fall in upper bed layer ground floor porous porcelain ball, through porous porcelain ball
Absorption, carries out raw material the most overanxious again, and four scatters by resistance shelves, friction and the swabbing action in each gap, is formed
Multiple feed distribution points, each distributed points raw material forms a plurality of stable runoff due to gravity and intermolecular graviational interaction, all
Even fall on next layer of porcelain ball, until catalyst layer.Along with porcelain ball, the reducing of catalyst particle size, void count increases, space away from
From reducing, the distributed points, the footpath fluxion that are formed increase the most accordingly, when arriving minimum grain size catalyst layer, formed distributed points,
Footpath fluxion reaches maximum, it is achieved reaction medium contacts uniformly with catalyst, prevents material from walking " short-circuit " or bed sink, it is ensured that
Reaction effect；More connect bottom bed, the particle diameter of catalyst and support the particle diameter of porcelain ball and be gradually increased, distributed points and footpath fluxion by
The fewest, footpath flow resistance is gradually reduced, and run-off is increasing, is conducive to improving reaction efficiency.Upper bed layer behind rounding angle props up
Support plate hole also contributes to reduce reagent flow resistance and dirty, and the design of this support disk hole is more conducive to supporting catalyst and is easy to
The derivation of reactant.The blade atomization that the reactant that upper bed layer flows down blows regularly on cold hydrogen tube through cold hydrogen tube nozzle
After, it is sufficiently mixed with cold hydrogen, uniformly falls into next bed, then arrive catalyst layer by porcelain ball protective layer, repeat a upper bed
Course of reaction, to ensure the optimum depth of hydrogenation dearomatization, speed and the yield of raising ideal composition.Final reaction product is through going out
Mouth catcher, discharge nozzle go out reactor.
Claims (2)
1. an environmental protection hydrocarbon solvent low-voltage hydrogenation takes off arylation reaction device and catalyst filling method, it is characterised in that: manhole flange
Assembly (1) is made up of bolt, nut and pad, is fixedly mounted on manhole connecting pipe (2), and manhole connecting pipe (2) is welded on upper cover
(7), on, feed pipe (4) connects mother tube by feed pipe flange assembly (3) and welds with manhole flange, its underpart and feed pipe
Heteromorphic connector (5) welds mutually, and in feed pipe heteromorphic connector (5), welding A-frame is in order to fixing rotating metallic blade, charging point
Cloth device (6) is fixedly mounted on feed pipe heteromorphic connector (5) by bolt, nut and pad, and upper cover (7) is oval, its
Top is manhole, and bottom is welded with reactor shell (8), and the 4th nozzle for thermometer (9) is fixedly mounted on the sidewall outside cylinder,
Hanger (10) is welded on the 4th nozzle for thermometer (9) barrel below, and catalyst discharge duct II (12) is provided with on adjacent position
3rd nozzle for thermometer (11), catalyst discharge duct II (12) is arranged on support plate (14) top, catalyst discharge duct II flange
Assembly (13) is made up of blind flange, bolt, nut and pad, is fixedly mounted on catalyst discharge duct II (12), a support plate
(14) it is arranged on I-steel and bearing (15), cold hydrogen intake assembly (16) adjacent position is provided with the second nozzle for thermometer
(17), the second nozzle for thermometer (17) adjacent position is provided with the first nozzle for thermometer (19), cold hydrogen intake assembly (16)
Being arranged on I-steel and bearing (15) below, in the form of a ring, cold hydrogen nozzle is the most just to being fixed on cold hydrogen tube for cold hydrogen tube
Fan blades, removable insulation bracing ring (18) is provided with multiple, is welded on barrel outer surface, low head (20) top and reactor cylinder
Body (8) welds, and bottom is welded with skirt cylinder II (21), and low head (20) bottom is provided with discharging opening catcher (22), discharge nozzle
(24) overcoat discharging opening reinforced tube (23), top is connected with discharging opening catcher (22), is fixedly mounted on low head (20) bottom surface
Communicate on the outer wall of center and with cylinder, then by discharge nozzle elbow (25), discharging adapter (28), reactant is caused reaction
Outside device, discharging adapter sleeve pipe (26) is welded on skirt cylinder II (21), and interior welds discharging adapter gripper shoe (27) is by discharging
Adapter (28) is fixed, and discharging pipe connecting flange assembly (29) is made up of bolt, nut and pad, is fixedly mounted on discharging adapter (28)
On, steam vent adapter (30) is welded on skirt cylinder II (21), and catalyst discharge duct I sleeve pipe (31) is positioned at steam vent adapter
(30) below, it is welded on skirt cylinder II (21), interior welds catalyst discharge duct I gripper shoe (32) fixed catalyst discharging
Pipe I (33), catalyst discharge duct I (33) is fixedly mounted on the outer wall of cylinder low head (20) and communicates with cylinder, root by
Reinforcement sleeve pipe reinforcement, catalyst discharge duct I flange assembly (34) is made up of bolt, nut and pad, by catalyst discharge duct I method
Blue lid (35) is fixedly mounted on catalyst discharge duct I (33), and nameplate base (36) is welded on skirt cylinder I (38), checks hole
(37) it is welded on skirt cylinder I (38), foundation bolt seat (39) welding skirt cylinder I (38) bottom, electrostatic grounding plate (40)
It is welded on foundation bolt seat (39).
A kind of environmental protection hydrocarbon solvent low-voltage hydrogenation the most according to claim 1 takes off arylation reaction device and catalyst filling method,
It is characterized in that: catalyst filling method comprises the steps: that (1), catalyst filling are carried out at fine day, first install peripheral necessary
Accessory device, carries out reactor, reactor internals, instrument, safety equipment, catalyst, porcelain ball preparation and every safety inspection
Look into work, verification catalyst and porcelain ball specifications and models, implement every safety measure；(2), according to reactor volume and catalyst
Amount, calculates filling ratio, determines each layer catalyst, the particle diameter of porcelain ball and filling height；(3), filling personnel wear safety
Cap, wears long tube respiratory organ, puts on dustproof clothes, marking pen on band, fastens seat belts in entrance pre-hydrogenator tower, enters
Within first 1 hour, carry out oxygen analysis qualified, according to the calculating of step 2, carry out each layer filling number of altitude, tower at reactor wall
Interior personnel stand on plank, carry out splicing and prepare, (4), at the good Catalyst packing equipment of reactor head stage+module, generally
Be made up of three parts: hopper, under connect metal straight pipe, then be connected with a canvas hose, metal tube regards with canvas duct diameter
Depending on reactor head opening size, control 15～20cm, in hopper and metal tube and metal tube and canvas duct junction
Respectively setting a gate valve, toward closing top gate valve during hopper apparatus with catalyst inside, and bottom gate valve is for controlling the filling speed of catalyst
Degree, prevents catalyst free-falling excessive velocities, produces electrostatic and catalyst breakage, or " bridge formation ", controls the canvas mouth of pipe away from material
Face is less than 1m, (5), canvas hose (suitable for reading be fixed on tower top manhole) is put into tower, with crane the inert ceramic balls of φ 15mm
Hang tower top platform by loadings, porcelain ball is poured into hopper, be sent in tower by canvas hose, after installing, porcelain ball carefully taken off
Flat, spread φ 8mm, φ 6mm inert ceramic balls above, then at φ 6mm porcelain ball upper berth two-layer 20 mesh by filling height the most successively
Stainless steel cloth, run into install nozzle for thermometer place, install nozzle for thermometer, depend on the net at the stainless steel silk completed
Secondary by filling height spread φ 4mm, φ 2mm, φ 4mm catalyst above, after the catalyst of each layer of particle diameter installs, carefully take off
Flat, after three layers of Catalyst packing, φ 4mm catalyst is spread the stainless steel cloth of two-layer 20 mesh, the most again above
Paving φ 6mm, the inert ceramic balls of φ 8mm successively, so far, lower bed layer filling is complete；(6), install cold hydrogen intake assembly, I-steel and
Bearing, nozzle for thermometer, support plate, 10 mesh stainless steel cloths, assembly and reactor wall contact portion add girth sheets and asbestos seal,
After installing, remove foreign material, (7), according to step 5,6, successively filling upper bed layer porcelain ball, catalyst, install the temperature of bed
Degree meter adapter and feeding assembly internals, seal manhole.
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| CN107551959A (en) * | 2017-10-28 | 2018-01-09 | 上海迅凯新材料科技有限公司 | A kind of hydrogenation catalyst packing method |
| CN107815331A (en) * | 2017-12-13 | 2018-03-20 | 中冶焦耐(大连)工程技术有限公司 | A kind of organic sulfur removal reactor |
| CN108014720A (en) * | 2017-12-13 | 2018-05-11 | 青岛聚力科创信息技术有限公司 | A kind of hydrogenation reactor for petroleum and petrochemical industry |
| CN108554323A (en) * | 2018-06-28 | 2018-09-21 | 钦州学院 | Duct type liquid-phase catalysis reaction unit |
| CN109304133A (en) * | 2018-11-21 | 2019-02-05 | 爱润森德（天津）能源科技有限公司 | A kind of hydrogenator device for hydrogenation reaction |
| CN109985573A (en) * | 2017-12-29 | 2019-07-09 | 中国石油化工股份有限公司 | A kind of hydrogenator improving even in liquid phase degree |
| CN111249999A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Fixed bed reactor for catalytic reduction of hexavalent uranium by hydrazine nitrate and application |
| CN114653311A (en) * | 2022-03-22 | 2022-06-24 | 武汉氢能与燃料电池产业技术研究院有限公司 | Dehydrogenation reactor for liquid organic hydrogen storage material |
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| CN114653311A (en) * | 2022-03-22 | 2022-06-24 | 武汉氢能与燃料电池产业技术研究院有限公司 | Dehydrogenation reactor for liquid organic hydrogen storage material |
| CN117225298A (en) * | 2023-11-09 | 2023-12-15 | 北京拓川科研设备股份有限公司 | Solid raw material feeding system based on moving bed reactor |
| CN117225298B (en) * | 2023-11-09 | 2024-03-22 | 北京拓川科研设备股份有限公司 | Solid raw material feeding system based on moving bed reactor |
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