CN109395668A - A kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol - Google Patents
A kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol Download PDFInfo
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- B01J8/025—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 vertical in a cylindrical shaped bed
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- B01J8/0453—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 in two or more cylindrical beds the beds being superimposed one above the other
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
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- C07C29/147—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of carboxylic acids or derivatives thereof
- C07C29/149—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of carboxylic acids or derivatives thereof with hydrogen or hydrogen-containing gases
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- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
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Abstract
本发明涉及一种用于草酸烷基酯加氢合成乙二醇的耦合反应器，包括上封头、下封头以及设置在上封头与下封头之间的反应器壳体，所述的上封头设有反应气体进口、冷媒出口以及人孔，所述的下封头设有反应气体出口、冷媒进口以及催化剂卸料口，所述的反应器壳体内部由上而下依次设有第一气体分布器、绝热反应段、第二气体分布器以及轴径向反应段。与现有技术相比，本发明整体结构简单、紧凑，经济实用性好，安全稳定，具有反应气体分布均匀、床层温度分布合理、乙二醇选择性高，且能在不增加反应器直径的前提下大幅度提高反应器的生产能力等优点，工业应用前景好。
The invention relates to a coupling reactor for synthesizing ethylene glycol by hydrogenation of alkyl oxalate, comprising an upper head, a lower head and a reactor shell arranged between the upper head and the lower head. The upper head is provided with a reaction gas inlet, a refrigerant outlet and a manhole, the lower head is provided with a reaction gas outlet, a refrigerant inlet and a catalyst discharge port, and the inside of the reactor shell is sequentially arranged from top to bottom. There are a first gas distributor, an adiabatic reaction section, a second gas distributor, and an axial-radial reaction section. Compared with the prior art, the present invention has the advantages of simple and compact overall structure, good economical practicability, safety and stability, uniform reaction gas distribution, reasonable bed temperature distribution, high ethylene glycol selectivity, and can reduce the diameter of the reactor without increasing. Under the premise of greatly improving the production capacity of the reactor, the industrial application prospect is good.
Description
Technical field
The invention belongs to chemical process technology fields, are related to a kind of coupled reactor, are used for oxalic acid more particularly, to one kind
The coupled reactor of Arrcostab hydrogenation synthesizing of ethylene glycol.
Background technique
Ethylene glycol is a kind of important Organic Chemicals, and it is poly- to benzene that it can react generation with terephthalic acid (TPA) (PTA)
Naphthalate (PET), i.e. polyester resin, can be used as the raw material of polyester fiber and polyester plastics, this is current ethylene glycol
Main purposes.Ethylene glycol can also react generation with polyacids such as phthalic acid, maleic acid and fumaric acid
Corresponding polymer is referred to as alkyd resin.Secondly, ethylene glycol can also be directly used as antifreezing agent and prepare the coolant of engine,
The dinitrate of ethylene glycol can be used as explosive, while be also production plasticizer, paint, adhesive, surfactant, explosive and electricity
The indispensable substance of the products such as container electrolyte.
Coal based synthetic gas preparing ethylene glycol is from synthesis gas by CO gas-phase catalytic coupling synthesis of oxalic acid Arrcostab, then plus
Hydrogen prepares ethylene glycol, and the dependence to petroleum resources is got rid of from raw material, actively complies with ethylene glycol production technology trend, meets
The development strategy of China's energy development.
The key technology of coal based synthetic gas preparing ethylene glycol first is that oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol reactor is opened
Hair.Currently, commercial plant medium-height grass acid alkyl ester hydrogenation synthesizing of ethylene glycol uses shell and tube reactor, which belongs to axial direction
Type, for catalyst loaded in tubulation, shell walks refrigerant, and separate unit reactor tubulation number reaches 4000-5000 root, and about 4 meters of reactor outer diameter,
About 7.5 ten thousand tons/year of separate unit reactor ethylene glycol production capacity.Since by being limited in terms of transporting, reactor diameter cannot be excessive, one
As control at 4 meters or so, thus using shell and tube reactor cannot achieve the enlargement of separate unit oxalic acid Arrcostab hydrogenator.
In addition, existing shell and tube reactor exchange capability of heat is limited, hot(test)-spot temperature is higher, causes hydrogenation products production quantity more, ethylene glycol
Selectivity can not further increase.
Compared with axial flow reactor, have fluid flow area big in radial reactor, catalyst bed is thin, bed pressure
Small advantage drops, and radial reactor is at home and abroad applied in a variety of chemical fields in recent years.Patent CN202876771U is public
A kind of radial reactor applied to oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol has been opened, has from top to bottom successively included being located at input end
Reactor inlet pipe, inlet gas distributor, Heat Room, upper end inert filler layer, intermediate radial reaction bed, lower end inertia
Packing layer, exit gas distributor and reactor outlet pipe；The intermediate radial reaction bed, successively include from outside to inside with it is upper
Annular space, outer distributing barrel, catalyst bed, inside distributor between the reactor shell inner wall and outer distributing barrel of holding inert filler layer to connect
With center gas collecting tube.Reactor catalyst packing factor is high in the patent, and pressure drop is small, and production capacity is big, but this is radially reacted
For device since fluid flow area is very big, catalyst bed is relatively thin, and there are the axially distributed non-uniform possibilities of fluid.In addition, by
Containing the impurity for having destruction to catalyst in the DMO supplied materials of upstream, lack guard bed, relatively thin radial bed not can guarantee
The service life of catalyst.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of gases to be evenly distributed,
Bed temperature is reasonably distributed, glycol selectivity is high, adapt to single series enlargement production for oxalic acid Arrcostab hydrogenation synthesis
The coupled reactor of ethylene glycol.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol, including upper cover, lower head and set
Set the reactor shell between upper cover and lower head, the upper cover be equipped with reacting gas inlet, refrigerant exit and
Manhole, the lower head is equipped with reaction gas outlet, refrigerant inlet and catalyst discharge port, in the reactor enclosure body
Portion is from top to bottom successively arranged first gas distributor, adiabatic reaction section, second gas distributor and axis radial direction conversion zone.
The first gas distributor, second gas distributor are diffusion type mixed distribution device or injecting type mixed distribution
Device.
The adiabatic reaction section is using dismountable whole frame structure, including refractory porcelain disposed in parallel one on the other
Layers of balls and the adiabatic section catalyst layer being arranged between two refractory porcelain layers of balls.
The axis radial direction conversion zone includes the isocon being axially arranged in reactor shell, is laid in from inside to outside
Interior porous distributing barrel and outer porous distributing barrel on the outside of isocon are set between the interior porous distributing barrel and outer porous distributing barrel
There are heat exchanger plates pair and heat-exchange system, is filled with catalyst layer between the heat exchanger plates pair.
Header is equipped between the outer porous distributing barrel and reactor shell, the isocon is located at interior porous point
The inside of cloth cylinder, and be located at the center of reactor shell.
The position of opening of the outer porous distributing barrel is lower than the position of opening of interior porous distributing barrel.
In actual design, the position of opening of outer porous distributing barrel and the difference in height of the position of opening of interior porous distributing barrel are wanted
It can ensure that most short residence time of the reaction gas in this high catalytic oxidant layer not less than reaction gas in axis radial direction conversion zone
Mean residence time.
In actual application, when reaction gas enters catalyst layer by isocon, outer porous distributing barrel aperture position
The air stream axle of top is set radially across catalyst layer, the air-flow below outer porous distributing barrel position of opening is radially across catalyst
Layer, two parts air-flow converge in header, flow downward along header into reaction gas outlet and flow out.
The heat-exchange system include the refrigerant inlet pipeline being connected with refrigerant inlet, successively with refrigerant inlet pipeline phase
Refrigerant distributor, refrigerant collector and the refrigerant exit pipeline of connection, the refrigerant exit pipeline are connected with refrigerant exit.
The refrigerant distributor is located at the bottom of heat exchanger plates pair, and the refrigerant collector is located at the top of heat exchanger plates pair
Portion, the refrigerant distributor are connected by heat exchanger plates pair with refrigerant collector.
The heat exchanger plates are to using isocon as the fan-shaped arrangement of center axis, and the spacing between adjacent two heat exchanger plates pair
For 20-180mm.
The heat exchanger plates are welded to by two pieces of heat exchanger plates, and heat exchanger plates inner surface sides are equipped with flow-disturbing fin strip, this is disturbed
Intersect between stream fin strip and heat exchanger plates pair in 30 ° of angles, the flow direction phase of the opening direction of the intersection and refrigerant in reactor
Instead, for ensuring that the internal refrigerant of heat exchanger plates is in turbulence state, enhancing moves thermal effect, hot(test)-spot temperature is effectively reduced, is subtracted with reaching
Lack hydrogenation products, and improves the purpose of glycol selectivity.
The oxalic acid Arrcostab is one of dimethyl oxalate, diethy-aceto oxalate or dibutyl oxalate.
Catalyst in coupled reactor of the present invention is Cu/SiO2Or with Cu/SiO2Based on modified catalyst, and
The height of the adiabatic reaction section is the 5%-20% of axis radial direction conversion zone height.
Compared with prior art, the invention has the characteristics that:
1) at reactor inlet, equally distributed diffusion type (or injecting type) mixed distribution device is set, while in catalyst
Inertia alumina ball is loaded in the top of bed, is uniformly distributed reaction gas, prevents gas bias current, guarantees axial in reactor
The load of catalyst bed is consistent everywhere；
2) in order to increase reaction bed temperature, reach and react required temperature, improve catalyst bed utilization rate,
Adiabatic reaction section is set in the upper surface of axis radial direction conversion zone, thus also brings a benefit, which can effectively keep away
Exempt from influence of the poisonous substances such as sulphur, phosphorus, arsenic, chlorine, water to catalyst in the axis radial direction conversion zone of main body, and then significantly improves catalyst
Whole service life；
3) flow-disturbing fin strip is set in heat exchanger plates inner surface sides, it is ensured that the internal refrigerant of heat exchanger plates is in turbulence state, enhancing
Shifting thermal effect, effectively reduces hot(test)-spot temperature, reduced hydrogenation products to reach, improve the purpose of glycol selectivity；
4) overall structure is simple, compact, and economic and practical is good, safety and stability, there is reaction gas to be evenly distributed, bed temperature
Degree is reasonably distributed, glycol selectivity is high, and the life of reactor can be increased substantially under the premise of not increasing reactor diameter
The advantages that production capacity power, prospects for commercial application are good.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention；
Description of symbols in figure:
1, upper cover, 2, refrigerant exit, 3, gas reactor import, 4, manhole, 5, adiabatic reaction section, 61, first gas
Distributor, 62, second gas distributor, 7, refractory porcelain layers of balls, 8, adiabatic section catalyst layer, 9, refrigerant exit pipeline, 10, refrigerant
Collector, 11, heat exchanger plates pair, 12, shell, 13, axis radial direction conversion zone, 14, outer porous distributor cylinder, 15, interior porous distributor
Cylinder, 16, header, 17, isocon, 18, catalyst layer, 19, refrigerant distributor, 20, refrigerant inlet pipeline, 21, catalyst unloads
Material mouth, 22, reaction gas outlet, 23, refrigerant inlet, 24, lower head.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment:
As shown in Figure 1, a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol, including upper cover 1, under
End socket 24 and the reactor shell 12 being arranged between upper cover 1 and lower head 24, upper cover 1 be equipped with reacting gas inlet 3,
Refrigerant exit 2 and manhole 4, lower head 24 are equipped with reaction gas outlet 22, refrigerant inlet 23 and catalyst discharge port 21, instead
Answer from top to bottom be successively arranged inside device shell 12 first gas distributor 61, adiabatic reaction section 5, second gas distributor 62 with
And axis radial direction conversion zone 13.
Wherein, adiabatic reaction section 5 is using dismountable whole frame structure, including refractory porcelain disposed in parallel one on the other
Layers of balls 7 and the adiabatic section catalyst layer 8 being arranged between two refractory porcelain layers of balls 7.
Axis radial direction conversion zone 13 includes the isocon 17 being axially arranged in reactor shell 12, is laid in from inside to outside
The interior porous distributing barrel 15 and outer porous distributing barrel 14 in the outside of isocon 17, interior porous distributing barrel 15 and outer porous distributing barrel 14 it
Between be equipped with heat exchanger plates to 11 and heat-exchange system, heat exchanger plates are filled with catalyst layer between 11.Outer porous distributing barrel 14 with react
Header 16 is equipped between device shell 12, isocon 17 is located at the inside of interior porous distributing barrel 15, and is located at reactor shell 12
Center at.The position of opening of outer porous distributing barrel 14 is lower than the position of opening of interior porous distributing barrel 15.Heat-exchange system include with
It is refrigerant inlet pipeline 20 that refrigerant inlet 23 is connected, the refrigerant distributor 19 being successively connected with refrigerant inlet pipeline 20, cold
Matchmaker's collector 10 and refrigerant exit pipeline 9, the refrigerant exit pipeline 9 are connected with refrigerant exit 2.Refrigerant distributor 19 is located at
For heat exchanger plates to 11 bottom, refrigerant collector 10 is located at heat exchanger plates to 11 top, and refrigerant distributor 19 is by heat exchanger plates to 11
It is connected with refrigerant collector 10.
Heat exchanger plates to 11 with isocon 17 for the fan-shaped arrangement of center axis, and adjacent two heat exchanger plates are to the spacing between 11
For 20-180mm.Heat exchanger plates are equipped with flow-disturbing fin strip, the flow-disturbing fin strip and heat exchanger plates to being in 30 ° of angles between 11 to 11 medial surfaces
Intersect, the flow direction of refrigerant is on the contrary, for ensuring that the internal refrigerant of heat exchanger plates is in the opening direction and reactor of the intersection
Turbulence state, enhancing move thermal effect, hot(test)-spot temperature are effectively reduced, reduced hydrogenation products to reach, and improve glycol selectivity
Purpose.
In the present embodiment, first gas distributor 61, second gas distributor 62 are diffusion type mixed distribution device or injection
Formula mixed distribution device.In actual design, the position of opening of the position of opening of outer porous distributing barrel 14 and interior porous distributing barrel 15
Difference in height can ensure that most short residence time of the reaction gas in this high catalytic oxidant layer not less than reaction gas in the diameter of axle
To the mean residence time of conversion zone.Catalyst in the present embodiment coupled reactor is Cu/SiO2Or with Cu/SiO2Based on
Modified catalyst, and the height of adiabatic reaction section 5 be 13 height of axis radial direction conversion zone 5%-20%.
In actual application, when reaction gas enters catalyst layer by isocon 17, outer porous distributing barrel 14 is opened
Air stream axle above hole site is radially across catalyst layer, and air-flow below outer porous 14 position of opening of distributing barrel is radially across urging
Agent layer, two parts air-flow converge in header 16, flow downward along header 16 into reaction gas outlet and flow out.
The present embodiment is used for insulation-axis radial direction coupled reactor of hydrogenation of dimethyl oxalate to synthesizing ethylene glycol, separate unit diameter
It is 4.0 meters, loads with Cu/SiO2Based on modified catalyst 90m3, ethylene glycol production capacity is 150,000 tons/year, in hot(test)-spot temperature
195 degree, pressure 3.0MPa, oxalic acid alkyl ester conversion rate is 100%, glycol selectivity 98%.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol, including upper cover (1), lower head (24) with
And the reactor shell (12) being arranged between upper cover (1) and lower head (24), the upper cover (1) are equipped with reaction gas
Import (3), refrigerant exit (2) and manhole (4), the lower head (24) are equipped with reaction gas outlet (22), refrigerant inlet
(23) and catalyst discharge port (21), which is characterized in that is from top to bottom successively arranged inside the reactor shell (12)
First gas distributor (61), adiabatic reaction section (5), second gas distributor (62) and axis radial direction conversion zone (13).
2. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 1, feature
It is, the first gas distributor (61), second gas distributor (62) are that diffusion type mixed distribution device or injecting type are mixed
Close distributor.
3. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 1, feature
It is, the adiabatic reaction section (5) is using dismountable whole frame structure, including refractory porcelain disposed in parallel one on the other
Layers of balls (7) and the adiabatic section catalyst layer (8) being arranged between two refractory porcelain layers of balls (7).
4. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 1, feature
It is, the axis radial direction conversion zone (13) includes the isocon (17) being axially arranged in reactor shell (12), by interior
Interior porous distributing barrel (15) and the outer porous distributing barrel (14) being laid on the outside of isocon (17) outward, the interior porous distribution
Heat exchanger plates are equipped between cylinder (15) and outer porous distributing barrel (14) to (11) and heat-exchange system, the heat exchanger plates are between (11)
It is filled with catalyst layer.
5. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 4, feature
It is, is equipped with header (16) between the outer porous distributing barrel (14) and reactor shell (12), the isocon
(17) it is located at the inside of interior porous distributing barrel (15), and is located at the center of reactor shell (12).
6. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 5, feature
It is, the position of opening of the outer porous distributing barrel (14) is lower than the position of opening of interior porous distributing barrel (15).
7. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 4, feature
Be, the heat-exchange system include the refrigerant inlet pipeline (20) being connected with refrigerant inlet (23), successively with refrigerant inlet
Refrigerant distributor (19), refrigerant collector (10) and the refrigerant exit pipeline (9) that pipeline (20) is connected, the refrigerant exit pipe
Road (9) is connected with refrigerant exit (2).
8. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 7, feature
It is, the refrigerant distributor (19) is located at heat exchanger plates to the bottom of (11), and the refrigerant collector (10) is located at heat exchange
Plate is connected to the top of (11), the refrigerant distributor (19) by heat exchanger plates to (11) with refrigerant collector (10).
9. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 8, feature
Be, the heat exchanger plates to (11) with isocon (17) for the fan-shaped arrangement of center axis, and adjacent two heat exchanger plates are to (11)
Between spacing be 20-180mm.
10. a kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol according to claim 9, feature
It is, the heat exchanger plates are equipped with flow-disturbing fin strip to (11) medial surface, and the flow-disturbing fin strip and heat exchanger plates are between (11)
30 ° of angles intersect, and the opening direction of the intersection is opposite with the flow direction of refrigerant in reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710712702.6A CN109395668A (en) | 2017-08-18 | 2017-08-18 | A kind of coupled reactor for oxalic acid Arrcostab hydrogenation synthesizing of ethylene glycol |
Applications Claiming Priority (1)
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| CN113856567A (en) * | 2021-11-05 | 2021-12-31 | 华东理工大学 | A kind of ethylene carbonate hydrogenation reactor and its application |
| CN113967408A (en) * | 2021-11-26 | 2022-01-25 | 西安绿鼎环保科技有限公司 | Dry desulfurization and denitrification reactor |
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