CN209010425U - A kind of tetrahydrofuran reaction separating device - Google Patents
A kind of tetrahydrofuran reaction separating device Download PDFInfo
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- CN209010425U CN209010425U CN201821556556.9U CN201821556556U CN209010425U CN 209010425 U CN209010425 U CN 209010425U CN 201821556556 U CN201821556556 U CN 201821556556U CN 209010425 U CN209010425 U CN 209010425U
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- reactor tank
- metal film
- butanediol
- outlet
- film membrane
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Abstract
The utility model relates to a kind of tetrahydrofuran reaction separating devices, are made of reactor tank, rectifying column.Rectifying column is located at the top of reactor tank, reacts and is successively arranged discharge outlet, 1,4-butanediol feed opening, purified liquor outlet, catalyst charging hole, steam inlet, recoil mouth, condensate outlet on tank skin from top to bottom;Reactor tank interior bottom portion is equipped with 1,4-butanediol distributor, and middle part middle position is equipped with blender, the periphery of blender is equipped with heating coil, the periphery of heating coil is equipped with guide shell, and the periphery of guide shell is equipped with metal film membrane stack, and reactor tank internal upper part is equipped with catalyst addition tube.Rectifying column tower wall is equipped with cooler cold source inlet and outlet, gaseous phase outlet, and middle part is equipped with filler, and top is equipped with cooler.The utility model can be improved the conversion ratio and yield of reaction, solve the separation problem of catalyst, realizes being carried out continuously for Reaction Separation.
Description
Technical field
The utility model relates to a kind of chemical reaction equipment, especially a kind of tetrahydrofuran reaction separating device, belonging to
Reacting and separating device in work production.
Background technique
Tetrahydrofuran (abbreviation THF) is that one kind is colourless, miscible with water, has the organic of smaller viscosity at normal temperatures and pressures
Liquid is a kind of middle polarity non-protonic solvent.It is mainly used for make the precursor of high molecular polymer, THF itself can
It is polycondensed into polytetramethylene ether diol (PTMEG), PTMEG can be made into the high extraordinary rubber of wear-resisting, oil resistant, low temperature performance well, intensity
Glue, block polyether polyester elastic materials, polyurethane elastomeric fiber and some specific use coating raw material.In organic synthesis side
Face, THF can be used for producing thiophane, 1.2- dichloroethanes, 2.3- dichloro tetrahydrofuran, valerolactone, butyrolactone and pyrrolidines
Ketone etc..In terms of medical industry, THF is for synthesizing carbetapentane citrate, sharp pluramycin, progesterone and some hormone drugs.THF is through hydrogen sulfide
Processing generates tetrahydro thiophenol, can make the stink agent (identification additive) in fuel gas.THF can be used as the surface treatment of synthetic leather
Agent, chromatography reagent, organic solvent etc..
The prior art is prepared in the technical process of THF using 1,4-butanediol cyclodehydration method, and 1,4-butanediol is dehydrated ring
Change reactor and use reactive distillation column, temperature in control tower, side border ring is distilled, and the tetrahydrofuran distillated is sent at subsequent handling
Reason, reaction solution are collected after the piping filter filtering through installing in reactive distillation tower wall, recycle unreacted 1 after processing,
4- butanediol, as raw material for standby, catalyst is trapped within the cyclodehydration that 1,4-butanediol is continued to participate in reactive distillation column
Reaction.In this technical process, catalyst is urged due to being filtered using the piping filter installed in reactive distillation tower wall
Agent is easily collected at around filter, causes filter net jam, it is often necessary to which maintenance down is influenced normally to produce, and also be will cause
Catalyst is unbalanced in reaction system, and the conversion ratio of 1,4-butanediol is about 90%, has about 10% 1,4-butanediol not carry out
Cyclodehydration reaction can be reused after needing further progress removal of impurities to handle by as the residual discharge of kettle, energy consumption is caused to increase,
Product yield is low, in order to solve the separation problem of catalyst in tetrahydrofuran production process, improves the conversion ratio of 1,4-butanediol,
Energy consumption is reduced, improves the yield of product tetrahydrofuran, it is necessary to change to existing tetrahydrofuran Reaction Separation rectifier unit
Into.
Summary of the invention
The purpose of the utility model is to provide a kind of tetrahydrofuran reaction separating devices, to solve tetrahydrofuran production process
The separation problem of middle catalyst improves the conversion ratio of reaction raw materials 1,4-butanediol, the yield of product tetrahydrofuran, reduces energy
Consumption.
The technical scheme in the invention for solving the technical problem is such.A kind of tetrahydrofuran Reaction Separation dress
Set, including reactor tank, rectifying column, rectifying column is located at the top of reactor tank, react be successively arranged from top to bottom on tank skin discharge outlet,
1,4- butanediol feed opening, purified liquor outlet, catalyst charging hole, steam inlet, recoil mouth, condensation-water drain.Bottom in reactor tank
Portion is equipped with 1,4-butanediol distributor, and middle part middle is equipped with blender, and the periphery of blender is equipped with heating coil, heating coil
Periphery be equipped with guide shell, the periphery of guide shell is equipped with metal film membrane stack, and reactor tank internal upper part is equipped with catalyst addition tube, rectifying
Tower tower wall is equipped with cooler cold source inlet and outlet, gaseous phase outlet, and middle part is equipped with filler, and top is equipped with cooler;
The guide shell upper end level is higher than metal film membrane stack upper end level.
The 1,4- butanediol feed opening is connected with 1,4- butanediol distributor.
The 1,4-butanediol distributor is ring-shaped round pipe, and the upper side wall of ring-shaped round pipe is equipped with equally distributed aperture.
The outlet of the catalyst addition tube is located on the inside of guide shell.
The metal film membrane stack is evenly arranged on the inside of reactor tank with annular, is located among metal film membrane stack and is equipped with 1 gold
Belong to film membrane component, is disposed with 2~4 circle metal film membrane components, the material of metal film membrane component in the metal film membrane component peripheral annular
Matter is 316L, and filtering accuracy is 0.5~3 μm.
The metal film membrane stack and metal film membrane component are easily to purchase product in the market.Metal film membrane stack is according to the processing of feed liquid
Amount is designed, and under normal circumstances, metal film membrane stack is designed to circle, allows for the flowing of material, and circle will not obstacle
The flowing of material.
The working principle of the utility model is as follows:
Raw material 1,4-butanediol enters reactor tank through feed opening, flows through 1,4-butanediol feed opening, 1,4-butanediol distribution
Device, is added on the inside of the guide shell in reactor tank from aperture equally distributed on 1,4-butanediol distributor, and catalyst flows through
On the inside of guide shell in catalyst charging hole, catalyst addition tube to reactor tank, on the inside of guide shell, in the effect of blender
Under, 1,4-butanediol and catalyst come into full contact with, and cyclodehydration occurs and reacts to obtain tetrahydrofuran, and the temperature for controlling reaction is
110~120 DEG C, pressure is 0.25~0.35MPa, 60~100min of residence time, during the reaction, the high temperature the case where
Under, the water that boiling point only has 66 DEG C of tetrahydrofuran and boiling point is 100 DEG C, which is vaporized, rises to rectifying column, in rectifier temperature
Control is 70~80 DEG C, and water is condensed, and the gaseous phase outlet that gaseous state tetrahydrofuran continues to rise through rectifying column overflows, and is sent into
Subsequent handling is further processed to obtain tetrahydrofuran product;When liquid level is more than the height of guide shell, it flow to guide shell outside
Outside, under the driving of pressure, mixed liquor is through the isolated clear liquid containing a small amount of 1,4-butanediol of metal film membrane stack, through clear
Reactor tank is sent out in liquid outlet, and the clear liquid containing a small amount of 1,4-butanediol continues to use after subsequent processing as raw material, catalyst
It is trapped to tower bottom reactor tank, is recycled on the inside of guide shell and continues to participate in instead under the power of blender from guide shell outside
It answers, it is primary every 10~50s recoil by automatic control means in metal film membrane stack separation process, each recoil time is 2~
5s。
Pass through the diameter of height, reactor tank to guide shell and the optimization design of height, and control raw material 1,4-butanediol
Charging rate, can control optimal reaction time, improve the conversion ratio of 1,4-butanediol.It detects by analysis, Isosorbide-5-Nitrae-
The conversion ratio of butanediol can reach 96% or more.
It during the reaction, can be by discharge outlet discharge unit catalyst, then from catalysis when the activity of catalyst reduces
Agent feed opening adds catalyst, realizes the persistence of reaction.
In the utility model, 1,4-butanediol be added quality, catalyst add quality sum and overflow gaseous state tetrahydro
The sum of the quality of furans, the quality that clear liquid is isolated through metal film membrane stack, the catalyst quality being discharged from discharge outlet are equal, thus
Realize the continuity of Reaction Separation.
The beneficial effect that the utility model obtains is:
(1) the utility model, due to being additionally arranged metal film membrane stack, guide shell, stirring and 1,4-butanediol in reactor tank
Distributor, can make 1,4-butanediol and catalyst is sufficiently mixed the conversion ratio for uniformly improving 1,4-butanediol;
(2) back-flushing technique for passing through metal film and automatic control, solves the separation problem of catalyst, realizes the company of Reaction Separation
Continuous property;
(3) for the filtering accuracy of metal membrane component compared with piping filter height, it is preferable to isolate clear liquid quality, reduces subsequent processing
Difficulty;
(4) practical new using this, the conversion ratio of 1,4-butanediol can reach 96% or more, compared with prior art, tetrahydro
The conversion ratio of furans can be improved 6%;
(5) content for isolating 1,4-butanediol in clear liquid through metal film membrane stack is about 4%, reduces by 6 hundred than the prior art
Branch, energy consumption can substantially reduce in subsequent processing.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model.
Fig. 2 is the top view of reactor tank.
Fig. 3 is the top view of single metal film membrane stack.
Figure label meaning is as follows:
1,1,4- butanediol feed opening 2, purified liquor outlet 3, metal film membrane stack 4, guide shell 5, reactor tank 6,
Catalyst charging hole 7, filler 9, cooler 10, gaseous phase outlet 11, catalyst addition tube 12, adds rectifying column 8
Hot coil 13, steam inlet 14, recoil mouth 15, condensation-water drain 16,1,4- butanediol distributor 17, discharge outlet
18, blender 19, metal film membrane component.
Specific embodiment
With reference to the accompanying drawing and the specific embodiment that provides of attached drawing is further described the utility model.
As shown in Figure 1, Figure 2, Figure 3 shows, a kind of tetrahydrofuran reaction separating device, including reactor tank 5, rectifying column 7, rectifying column
7 are located at the top of reactor tank 5.Discharge outlet 17,1,4- butanediol feed opening 1, clear liquid are successively arranged on 5 wall of reactor tank from top to bottom
Outlet 2, catalyst charging hole 6, steam inlet 13, recoil mouth 14, condensation-water drain 15.Bottom is equipped with annular circle in reactor tank 5
The upper side wall of the 1,4-butanediol distributor 16 of tubulose, ring-shaped round pipe is equipped with equally distributed aperture.Middle part is intermediate in reactor tank 5
Equipped with blender 18, the periphery of blender is equipped with heating coil 12, and the periphery of heating coil 12 is equipped with guide shell 4, guide shell 4
Periphery is equipped with metal film membrane stack 3, and 5 internal upper part of tower bottom reactor tank is equipped with catalyst addition tube 11.7 wall of rectifying column is equipped with cooler
9 cold sources inlet and outlet, gaseous phase outlet 10, bosom are equipped with filler 8, and top is equipped with cooler 9.4 upper end level of guide shell is higher than
3 upper end level of metal film membrane stack.1,4- butanediol feed opening 1 is connected with 1,4- butanediol distributor 16.Catalyst addition tube
11 outlet is located at 4 inside of guide shell.
As shown in Figure 1, Figure 3, metal film membrane stack is evenly arranged on the inside of reactor tank with annular, is located among metal film membrane stack
Equipped with 1 metal film membrane component, 2~4 circle metal film membrane components, metal film film are disposed in the metal film membrane component peripheral annular
The material of element is 316L, and filtering accuracy is 0.5~3 μm.
Claims (6)
1. a kind of tetrahydrofuran reaction separating device, including reactor tank (5), rectifying column (7), rectifying column (7) are located at reactor tank (5)
Top, it is characterised in that be successively arranged from top to bottom on reactor tank (5) wall discharge outlet (17), 1,4-butanediol feed opening (1),
Purified liquor outlet (2), catalyst charging hole (6), steam inlet (13), recoil mouth (14), condensation-water drain (15);Reactor tank (5)
Interior bottom is equipped with 1,4-butanediol distributor (16), and middle part is intermediate in reactor tank (5) is equipped with blender (18), the periphery of blender
Equipped with heating coil (12), the periphery of heating coil (12) is equipped with guide shell (4), and the periphery of guide shell (4) is equipped with metal film film
Heap (3), reactor tank (5) internal upper part be equipped with catalyst addition tube (11), rectifying column (7) tower wall be equipped with cooler (9) cold source into
Outlet, gaseous phase outlet (10), middle part are equipped with filler (8), and top is equipped with cooler (9).
2. reaction separating device according to claim 1, it is characterised in that guide shell (4) upper end level is higher than metal film film
Heap (3) upper end level.
3. reaction separating device according to claim 1, it is characterised in that 1,4-butanediol feed opening (1) and Isosorbide-5-Nitrae-fourth two
Alcohol distributor (16) is connected.
4. reaction separating device according to claim 1, it is characterised in that 1,4-butanediol distributor (16) is annular circle
The upper side wall of pipe, ring-shaped round pipe is equipped with equally distributed aperture.
5. reaction separating device according to claim 1, it is characterised in that the outlet of catalyst addition tube (11), which is located at, to be led
On the inside of flow cartridge (4).
6. reaction separating device according to claim 1, it is characterised in that metal film membrane stack is on the inside of reactor tank with annular
It is evenly arranged, is located among metal film membrane stack and is equipped with 1 metal film membrane component, arrange 2 in the metal film membrane component peripheral annular
~4 circle metal film membrane components, the material of metal film membrane component are 316L, and filtering accuracy is 0.5~3 μm.
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CN201821556556.9U CN209010425U (en) | 2018-09-25 | 2018-09-25 | A kind of tetrahydrofuran reaction separating device |
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CN201821556556.9U CN209010425U (en) | 2018-09-25 | 2018-09-25 | A kind of tetrahydrofuran reaction separating device |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111318236A (en) * | 2020-03-02 | 2020-06-23 | 宁夏美邦寰宇化学有限公司 | Device and method for preparing tetrahydrofuran |
CN114702465A (en) * | 2022-03-15 | 2022-07-05 | 宿迁市盈科新材料有限公司 | Method for synthesizing and converting tetrahydrofuran by using 1, 4-butanediol |
-
2018
- 2018-09-25 CN CN201821556556.9U patent/CN209010425U/en active Active
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111318236A (en) * | 2020-03-02 | 2020-06-23 | 宁夏美邦寰宇化学有限公司 | Device and method for preparing tetrahydrofuran |
CN114702465A (en) * | 2022-03-15 | 2022-07-05 | 宿迁市盈科新材料有限公司 | Method for synthesizing and converting tetrahydrofuran by using 1, 4-butanediol |
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