CN104607112A - Multistage enhanced fixed bed reactor and use method thereof - Google Patents
Multistage enhanced fixed bed reactor and use method thereof Download PDFInfo
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- CN104607112A CN104607112A CN201510001986.9A CN201510001986A CN104607112A CN 104607112 A CN104607112 A CN 104607112A CN 201510001986 A CN201510001986 A CN 201510001986A CN 104607112 A CN104607112 A CN 104607112A
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- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 91
- 239000003054 catalyst Substances 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 47
- 239000013067 intermediate product Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000005728 strengthening Methods 0.000 claims description 67
- 239000007788 liquid Substances 0.000 claims description 23
- 230000008676 import Effects 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 230000002301 combined effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 14
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- FUDNBFMOXDUIIE-UHFFFAOYSA-N 3,7-dimethylocta-1,6-diene Chemical compound C=CC(C)CCC=C(C)C FUDNBFMOXDUIIE-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- XSNQECSCDATQEL-UHFFFAOYSA-N dihydromyrcenol Chemical compound C=CC(C)CCCC(C)(C)O XSNQECSCDATQEL-UHFFFAOYSA-N 0.000 description 3
- 229930008394 dihydromyrcenol Natural products 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 101100412856 Mus musculus Rhod gene Proteins 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000005341 cation exchange Methods 0.000 description 2
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- -1 isobornyl isopropyl ether Chemical compound 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 1
- YZUPZGFPHUVJKC-UHFFFAOYSA-N 1-bromo-2-methoxyethane Chemical compound COCCBr YZUPZGFPHUVJKC-UHFFFAOYSA-N 0.000 description 1
- JECYNCQXXKQDJN-UHFFFAOYSA-N 2-(2-methylhexan-2-yloxymethyl)oxirane Chemical compound CCCCC(C)(C)OCC1CO1 JECYNCQXXKQDJN-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- DTGKSKDOIYIVQL-MRTMQBJTSA-N Isoborneol Natural products C1C[C@@]2(C)[C@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-MRTMQBJTSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
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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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- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses a multistage enhanced fixed bed reactor and a use method thereof, wherein the multistage enhanced fixed bed reactor comprises a raw material forced mixing kettle, an intermediate product forced mixing kettle and several horizontally placed reactor tubes; each reactor tube comprises several independent enhanced reaction units, each enhanced reaction unit is connected with the raw material forced mixing kettle by a reactor feed manifold and is connected with the intermediate product forced mixing kettle by a reactor discharge manifold; the intermediate product forced mixing kettle is further connected to several reactor feed manifolds by several circulation lines. According to the invention, a liquid phase is forced into a catalyst bed layer by a raw material transferring pump so that the liquid phase forms turbulent flow; the raw materials and intermediate products are forcedly mixed by the combined effect of the raw material transferring pump and a jet mixer, so as to ultimately enhance the reaction process, accelerate the reaction process and improve the utilization efficiency of materials and energies.
Description
Technical field
The present invention relates to multistage strengthening fixed bed reactors and using method thereof.
Background technology
Fixed bed reactors are one of current industrial most widely used chemical reactors, also known as making packed bed reactor, its inside is the certain thickness bed piled up by granular filler (being generally catalyst or the inert carrier material containing catalyst).Bed transfixion, material then flows through bed and reacts, to realize heterogeneous reaction process, as industrial ethylene prepares oxirane, ethyl benzene dehydrogenation preparation of styrene etc.
Catalytic mechanical wearing and tearing in fixed bed reactors are little, can be used continuously by the long period; Fluid back-mixing in bed is less, can be counted as desirable displacement stream, effectively can contact, be conducive to the carrying out of chemical reaction with catalyst; The time of staying of material in bed and Temperature Distribution also can be conditioned control effectively, improve feed stock conversion and product selectivity to a certain extent.In addition, fixed bed reactors structure is simple, does not have harsh requirement to operating condition, and operate conveniently, operating flexibility is also larger.But fixed bed reactors are due to the existence of bed, and material flow can be larger through the resistance of beds, flow velocity is comparatively slow, easily causes the phase-splitting between non soluble liquids, makes material fully contact and to react, cause reaction efficiency low, and material consumption, energy consumption are high.Further, conduct heat between material and beds and to become difficulty along with the increase of thickness of bed layer, temperature is wayward.
In order to solve the problem, be badly in need of innovating traditional fixed bed reactors structure and technological principle and space mounting, arrangement.For this reason, the present invention proposes a kind of new multistage strengthening fixed bed reactors and space arrangement thereof
,to meet the needs that modern industry is produced.
Summary of the invention
The present invention is intended at least to solve one of technical problem existed in prior art.
To achieve these goals, propose a kind of multistage strengthening fixed bed reactors according to embodiments of the invention, comprise the raw material Forced Mixing still and the intermediate product Forced Mixing still being connected product discharge pipe that connect feed pipe; The reactor tube of several horizontal positioned, each described reactor tube includes several and independently strengthens reaction member, the import of each strengthening reaction member all connects a reactor feed house steward by a feed-inputing branched pipe, reactor feed house steward is equipped with feedstock transportation pump, several reactor feeds house steward connects the outlet of described raw material Forced Mixing still; The outlet of each strengthening reaction member all connects a reactor discharge header pipe by a discharging arm, and reactor discharge header pipe is equipped with heat exchanger, and several reactor discharge header pipe connect described intermediate product Forced Mixing still; Described reactor feed house steward, feed-inputing branched pipe and circulation line are equipped with flowmeter and valve, described discharging arm is also provided with valve; The outlet of described intermediate product Forced Mixing still also connects several circulation lines, several circulation lines described and described several reactor feeds house steward one_to_one corresponding, and before being connected to the feedstock transportation pump on reactor feed house steward, after valve and flowmeter.
Whole conversion zone according to multistage strengthening fixed bed reactors of the present invention is divided into L layer, every layer containing M root reactor tube, horizontal setting, and every root fixed bed reactors are divided into again and N number ofly independently strengthen reaction member, therefore total L × M × N number of independently strengthens reaction member.Each independent strengthening reaction member is all independently strengthen fixed bed reactors, and its fluid flow controls by valve and flowmeter, can select used numbe rof reactor unit and uninterrupted according to needs of production.During reaction, choose the independent reaction unit of suitable quantity according to need of production, reaction mass is sent in each reaction member by delivery pump after the mixing fully of raw material Forced Mixing still, and the liquid after reacted imports discharge header pipe, and enters intermediate product Forced Mixing still.By feedstock transportation pump, press-in beds is forced to liquid phase, make it in turbulent flow, and by the synergy of feedstock transportation pump and jet mixer, Forced Mixing is carried out to raw material and intermediate product, the strengthening of final realization response process, accelerated reaction process, improves material and efficiency of energy utilization.
Multistage strengthening fixed bed reactors according to the embodiment of the present invention can also have following additional technical feature:
Preferably, described raw material Forced Mixing still comprises the first mixing kettle and the first mixed pipe line, the two ends of described first mixed pipe line connect upper end import and the lower end outlet of described first mixing kettle respectively, and the first mixed pipe line is provided with the first mixed pipe line pump, first-class gauge and the first valve; Described intermediate product Forced Mixing still includes the second mixing kettle and the second mixed pipe line, the two ends of described second mixed pipe line connect upper end import and the lower end outlet of described second mixing kettle respectively, second mixed pipe line is provided with the second mixed pipe line pump, second gauge and the second valve, and described product discharge pipe is located on the second mixed pipe line.
Preferably, the space arrangement of several reactor tubes described is: horizontal alignment is provided with multilayer, and every layer is set side by side with multiple reactor tube.
Preferably, Flange joint is passed through between described strengthening reaction member and adjacent strengthening reaction member.
Preferably, described strengthening reaction member comprises housing, is provided with beds in housing, and the housing at the two ends of beds is respectively equipped with described import and outlet.
Preferably, described strengthening reaction member housing is also provided with the catalyst inlet corresponding with described beds and catalyst outlet.
Preferably, described beds is monoblock type, and its external diameter is less than the internal diameter of housing, and beds is also connected with catalyst stop.
Preferably, described feed-inputing branched pipe is connected to the left end of described fixed bed interval, and described discharging arm is connected to the right-hand member of described fixed bed interval.
Preferably, liquid forced jet blender is also provided with in described mixing kettle.
The present invention also provides a kind of using method adopting above-mentioned multistage strengthening fixed bed reactors, comprises the steps:
(1) material enters raw material Forced Mixing still by feed pipe, mixing through raw material Forced Mixing still makes material fully mix, close the valve on circulation line, open the valve on reactor feed house steward, and by flowmeter and valve co-controlling uninterrupted, send into each strengthening reaction member respectively by feedstock transportation pump, import reactor discharge header pipe through abundant reacted liquid through each discharging arm, and after heat exchanger heat exchange, enter intermediate product Forced Mixing still respectively; In the process, how many according to raw material Forced Mixing still rate of discharge, filled into the raw material of respective amount to raw material Forced Mixing still by feed pipe;
(2) after a period of time, through intermediate product Forced Mixing still mixed material, open the valve on some circulation lines gradually and reduce the aperture of the valve on reactor feed house steward, the flow that the flow that intermediate product Forced Mixing still is increased and raw material Forced Mixing still reduce is suitable, until the valve on reactor feed house steward is closed completely;
(3) after testing, if the product in intermediate product Forced Mixing still conforms to requirement, then stop the mixing of intermediate product Forced Mixing still, and close the valve on circulation line, product is exported by discharge nozzle; Otherwise the material mixed in intermediate product Forced Mixing still, under the effect of feedstock transportation pump, is circulated in each strengthening reaction member and continues to participate in reaction, until complete.
Preferably, described raw material Forced Mixing still and intermediate product Forced Mixing still are respectively by the first mixed pipe line and the mixing of the second mixed pipe line.
Major advantage of the present invention is:
1, be applicable to large-scale production, reaction efficiency is high, administration measure.
2, for the system that course of reaction heat release is more, heat can be walked by fast fetching, avoid bed " temperature runaway ".
3, operating flexibility is high, can open or close some reaction member at any time, can not form impact to other reaction member.
4, catalyst bed layer height is low, and resistance is little, and in bed, the fast and liquid stream of flow velocity is evenly distributed, and is conducive to the control to product quality.
5, catalyst can be changed at any time, maintenance and convenience thereof.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is multistage strengthening fixed bed reactors front view of the present invention;
Fig. 2 is multistage strengthening fixed bed reactors top view of the present invention;
Fig. 3 is multistage strengthening fixed bed reactors side view of the present invention;
Fig. 4 (a) is for independently strengthening the block diagram example one of reaction member;
Fig. 4 (b) is for independently strengthening the block diagram example two of reaction member.
Detailed description of the invention
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Being exemplary below by the embodiment be described with reference to the drawings, only for explaining the present invention, and can not limitation of the present invention being interpreted as.
embodiment 1
Referring to Fig. 1-4(b) describe according to the multistage strengthening fixed bed reactors of the embodiment of the present invention and using method thereof.
A kind of multistage strengthening fixed bed reactors, it forms primarily of with lower part: feed pipe (Material pipeline) G1, reactor feed house steward G2, reactor discharge header pipe G3, product discharge pipe G4, feed-inputing branched pipe I1, I2, I(N-1), I(N), discharging arm O1, O2, O(N-1), O(N), second valve F, raw material Forced Mixing still V1, intermediate product Forced Mixing still V2, feedstock transportation pump P(1, 1), P(2, 1), P(L, 1), reactor tube T(1, 1), T(2, 1), T(L, 1), beds n1, n2, n(N-1), n(N), heat exchanger E(1, 1) ... E(1, M), E(2, 1), E(2, M) E(L, 1) E(L, M), first mixed pipe line pump P1 and the second mixed pipe line pump P2.
Feed pipe G1 connects raw material Forced Mixing still V1, and product discharge pipe G4 connects intermediate product Forced Mixing still V2.
The reactor tube T(1 of whole conversion zone, 1), T(2,1) ..., T(L, 1) and be divided into L layer (L >=1, depending on real space and Production requirement) every layer of reactor tube T(1,1), T(2,1) ..., T(L, 1) structure all similar.Every layer containing M root reactor tube, horizontal setting, and every root fixed bed reactors are divided into again and N number ofly independently strengthen reaction member, therefore total L × M × N number of independently strengthens reaction member.Each independent strengthening reaction member is all independently strengthen fixed bed reactors, and its fluid flow controls by valve and flowmeter, can select used numbe rof reactor unit and uninterrupted according to needs of production.The beds n1 of horizontally-arranged column reactor, n2, n(N-1), n(N) N number of independently reaction member is divided into, and parallel with one another, they can be adjusted flow and unlatching at any time by the valve of feed-inputing branched pipe and flowmeter or be closed corresponding reaction member according to reaction needed, make production have elasticity.
The import of each strengthening reaction member all connects a reactor feed house steward G2 by a feed-inputing branched pipe, reactor feed house steward G2 is equipped with feedstock transportation pump P(1,1), P(2,1) ... P(L, 1), several reactor feeds house steward G2 connects the outlet of raw material Forced Mixing still V1; The outlet of each strengthening reaction member all connects a reactor discharge header pipe G3 by a discharging arm, reactor discharge header pipe G3 is equipped with heat exchanger E(1,1), E(2,1) ... E(L, 1), several reactors discharge header pipe G3 connects intermediate product Forced Mixing still V2; Reactor feed house steward G2, feed-inputing branched pipe I1, I2 ..., I(N-1), I(N) and circulation line on be equipped with flowmeter and valve, discharging arm O1, O2 ..., O(N-1), O(N) on be also provided with valve; The outlet of intermediate product Forced Mixing still V2 also connects several circulation lines, several circulation lines and several reactor feeds house steward G2 one_to_one corresponding, and the feedstock transportation pump P(1 be connected on reactor feed house steward G2,1), P(2,1) ... P(L, 1) before, after valve and flowmeter.
Raw material Forced Mixing still V1 comprises the first mixing kettle and the first mixed pipe line, the two ends of the first mixed pipe line connect upper end import and the lower end outlet of the first mixing kettle respectively, and the first mixed pipe line is provided with the first mixed pipe line pump P1, first-class gauge and the first valve; Intermediate product Forced Mixing still V2 includes the second mixing kettle and the second mixed pipe line, the two ends of the second mixed pipe line connect upper end import and the lower end outlet of the second mixing kettle respectively, second mixed pipe line is provided with the second mixed pipe line pump P2, second gauge and the second valve F, and product discharge pipe G4 is located on the second mixed pipe line.Liquid forced jet blender is provided with in the tank body of raw material Forced Mixing still V1 and intermediate product Forced Mixing still V2.Operationally, under the first mixed pipe line pump P1 or the second mixed pipe line pump P2 and the effect of liquid forced jet blender, being able to Forced Mixing even emulsification between liquid-liquid, reaching well-mixed effect, the phase-splitting possibility effectively avoiding material when entering reactor can being made.
Every root reactor tube T(1,1), T(2,1) ..., T(L, 1) and be divided into again N number of strengthening reaction member (N >=2, depending on real space and Production requirement).The structure of each strengthening reaction member is all similar, and adjacent between reaction member by Flange joint.Shown in Fig. 4 (a) is reactor T(1,1) and, it comprises housing, is provided with beds n1 in housing, and the housing at the two ends of beds n1 is respectively equipped with the import being positioned at left section of fixed bed interval and the outlet being positioned at fixed bed interval right-hand member.Each beds n1 place pipe diameter size independently strengthening reaction member is generally 10-1000mm, and for industrial-scale production, beds n1 place pipe diameter size is preferably 100-600mm; Beds n1 height dimension is generally 50-1000mm, and for industrial-scale production, beds n1 place diameter dimension is preferably 200-600mm.Import connects feed-inputing branched pipe, and feed-inputing branched pipe is provided with flowmeter 1 and inlet valve 2, and discharging arm is provided with outlet valve 3.The upper end of housing is provided with catalyst outlet 4, and lower end is provided with catalyst inlet 5.Fluid enters beds n1 after flowing into housing, and mass flow is controlled by inlet valve 2.After catalyst participates in reaction repeatedly, activity declines to some extent, now, can be withdrawn from the catalyst of inefficacy by catalyst outlet 4, and add new catalyst from catalyst inlet 5 and change.Beds n1 also can be prefabricated into monoblock type, and its external diameter is slightly less than the internal diameter of this section of reaction member pipeline, loads from one end, left side entirety of this unit, and as shown in Figure 4 (b), wherein, beds n1 is also connected with catalyst stop 6 to concrete structure.The replacing of traditional reactor catalyst generally need stop production and carry out, and the replacing of catalyst of the present invention with produce and can carry out simultaneously, as long as the arm valve closing of catalyst place independent reaction unit changed will be needed, and independent reaction unit pulled down change.
The present invention also provides a kind of using method adopting above-mentioned multistage strengthening fixed bed reactors, comprises the steps:
(1) during reaction, material enters raw material Forced Mixing still V1 by feed pipe G1, until inconsistent liquid after the first mixed pipe line pump P1 fully mixes, close the valve on circulation line, open the valve on reactor feed house steward G2, and by flowmeter and valve co-controlling uninterrupted, by feedstock transportation pump P(1, 1), P(2, 1), P(L, 1) each strengthening reaction member is sent into respectively, reactor discharge header pipe G3 is imported through each discharging arm through abundant reacted liquid, and respectively through heat exchanger E(1, 1), E(2, 1), E(L, 1) intermediate product Forced Mixing still V2 is entered after heat exchange, in the process, how many according to raw material Forced Mixing still V1 rate of discharge, filled into the raw material of respective amount to raw material Forced Mixing still V1 by feed pipe G1.Wherein, reactor tube T(1, 1), T(2, 1), T(L, 1) structure is all similar, with T(1, 1) be example, enter the material of house steward G2 through being in charge of I1, I2, I(N-1), I(N) each section of beds n1 is entered, n2, n(N-1), n(N) in (fluid enters beds flow after flowing into and being in charge of is controlled by valve 2), liquid after abundant haptoreaction is in charge of O1 through each section, O2, O(N-1), O(N) import in discharge header pipe G3, and respectively through heat exchanger E(1, 1), E(1, 2), E(1, M) intermediate product Forced Mixing still V2 is entered after heat exchange.
(2) after a period of time, through intermediate product Forced Mixing still V2 mixed material (opening the second valve F to mix), open the valve on some circulation lines gradually and reduce the aperture of the valve on reactor feed house steward G2, the flow that the flow that intermediate product Forced Mixing still V2 is increased and raw material Forced Mixing still V1 reduce is suitable, until the valve on reactor feed house steward G2 is closed completely;
(3) after testing, if the product in intermediate product Forced Mixing still V2 conforms to requirement, then stop the mixing of intermediate product Forced Mixing still V2, and close the valve on circulation line, product is exported by discharge nozzle; Otherwise, the material mixed in intermediate product Forced Mixing still V2 at feedstock transportation pump P(1,1), P(2,1) ..., P(L, 1) effect under, be circulated in each strengthening reaction member continue participate in reaction, until complete.Catalyst repeatedly participates in reacting rear activity and declines to some extent, now, can be withdrawn from the catalyst of inefficacy by outlet 4, and adds new catalyst from entrance 5 and change; If beds is monoblock type, then direct one end, left side from this unit entirety draws off and loads new catalyst.
here is the embody rule of multistage strengthening fixed bed reactors to the embodiment of the present invention 1 and using method.
embodiment 1: the annual production that certain factory's dihydromyrcene hydration reaction produces dihydromyrcenol is 8600t, employing the present invention designs, independently strengthening numbe rof reactor unit is that 3 × 3 × 3(3 represents the number of plies, 3 represent every layer contained by reactor tube radical, every root reactor tube establishes 3 individual catalyst beds in parallel), reactor tube internal diameter is 60mm, catalyst bed layer height 500mm, and catalyst bed entirety loads.Catalyst is sulfonic acid ion exchange resin Amberlyst 15, and Rhom and Hass of the U.S. produces.
Send in the house steward of every root reactor through delivery pump after raw material (dihydromyrcene: water: isobutanol=1:1:2, mass ratio) mixes, and enter each reaction member of independently strengthening by arm and react.Wherein, feed-inputing branched pipe flow is controlled by valve and flowmeter.It is 83 DEG C that temperature of reactor controls, and raw material total mass flow rate is 34.5t/h, and each independently strengthening reaction member inlet amount is 1.5m
3/ h.Reacted liquid is exported by discharge nozzle, enters middle storage tank respectively through heat exchanger heat exchange, enters circulation line and continue to participate in reaction after liquid agitation is even under the effect of delivery pump.Through 4h reaction, dihydromyrcene conversion ratio is 39.5%, and the selective of dihydromyrcenol reaches 91.8%.
embodiment 2: the annual production that certain factory's amphene hydration reaction produces isoborneol is 6200t, employing the present invention designs, independently strengthening numbe rof reactor unit is that 2 × 2 × 3(2 represents the number of plies, 2 represent every layer contained by reactor tube radical, every root reactor tube establishes 3 individual catalyst beds in parallel), reactor tube internal diameter is 50mm, catalyst bed layer height 400mm, and catalyst bed entirety loads.Catalyst is strong acid ion exchange resin Lewatit 2620, and German Lanxess Corporation produces.
Send in the house steward of every root reactor through delivery pump after raw material (amphene: water: Y solvent=1:0.2:2, mass ratio) stirs, and enter each reaction member of independently strengthening by arm and react.Wherein, charging is in charge of flow and is controlled by valve and flowmeter.It is 65 DEG C that temperature of reactor controls, and raw material total mass flow rate is 20.4t/h, and each independently strengthening reaction member inlet amount is 2m
3/ h.Reacted liquid is exported by discharge nozzle, enters middle storage tank respectively through heat exchanger heat exchange, enters circulation line and continue to participate in reaction after liquid agitation is even under the effect of delivery pump.Through 5h reaction, dihydromyrcene conversion ratio is 94%, and the selective of dihydromyrcenol reaches 82.5%.
embodiment 3: the annual production that certain factory's amphene and isopropanol reaction produce isobornyl isopropyl ether is 9800t, employing the present invention designs, independently strengthening numbe rof reactor unit is that 2 × 3 × 4(2 represents the number of plies, 3 represent every layer contained by reactor tube radical, every root reactor tube establishes 4 individual catalyst beds in parallel), reactor tube internal diameter is 100mm, catalyst bed layer height 600mm, and catalyst bed entirety loads.Catalyst is strongly acidic cation-exchange CT-482, and Piao Laite company of the U.S. produces.
Send in the house steward of every root elementary reaction device through delivery pump after raw material (amphene: isopropyl alcohol=1:2, mass ratio) stirs, and enter each reaction member of independently strengthening by arm and react.Wherein, charging is in charge of flow and is controlled by valve and flowmeter.It is 85 DEG C that temperature of reactor controls, and raw material total mass flow rate is 63.1t/h, and each independently strengthening reaction member inlet amount is 3.1m
3/ h.Reacted liquid is exported by discharge nozzle, enters middle storage tank respectively through heat exchanger heat exchange, enters circulation line and continue to participate in reaction after liquid agitation is even under the effect of delivery pump.Through 6.5h reaction, amphene conversion ratio is 80.3%, and the selective of isobornyl isopropyl ether reaches 94%.
embodiment 4: the annual production that certain factory's cyclohexene hydration reaction produces cyclohexanol is 17000t, employing the present invention designs, independently strengthening numbe rof reactor unit is that 4 × 3 × 4(4 represents the number of plies, 3 represent every layer contained by reactor tube radical, every root reactor tube establishes 4 individual catalyst beds in parallel), reactor tube internal diameter is 60mm, catalyst bed layer height 500mm, and catalyst bed entirety loads.Catalyst is sulfonic acid ion exchange resin Amberlyst 35, and Rhom and Hass of the U.S. produces.
Send in the house steward of every root reactor through delivery pump after raw material (cyclohexene: water=1:3, mass ratio) stirs, and enter each reaction member of independently strengthening by arm and react.Wherein, charging is in charge of flow and is controlled by valve and flowmeter.It is 120 DEG C that temperature of reactor controls, and raw material total mass flow rate is 160t/h, and every section feeding amount is each independently strengthening reaction member inlet amount is 4m
3/ h.Reacted liquid is exported by discharge nozzle, enters middle storage tank respectively through heat exchanger heat exchange, enters circulation line and continue to participate in reaction after liquid agitation is even under the effect of delivery pump.Through 4h reaction, cyclohexene conversion rate is 24%, and the selective of cyclohexanol reaches 99.6%
embodiment 5: the annual production that certain factory β-carypohyllene hydration reaction produces β-caryophyllenol is about 14000t, employing the present invention designs, independently strengthening numbe rof reactor unit is that 3 × 4 × 3(3 represents the number of plies, 4 represent every layer contained by reactor tube radical, every root reactor tube establishes 3 individual catalyst beds in parallel), reactor tube internal diameter is 80mm, catalyst bed layer height 600mm, and catalyst bed entirety loads.Catalyst is strongly acidic cation-exchange NKC-9, and Chemical Plant of Nankai Univ. produces.
Send in the house steward of every root reactor through delivery pump after raw material (β-carypohyllene: water=1:1.2, mass ratio) stirs, and enter each reaction member of independently strengthening by arm and react.Wherein, charging is in charge of flow and is controlled by valve and flowmeter.It is 90 DEG C that temperature of reactor controls, and raw material total mass flow rate is 163.8t/h, and every section feeding amount is each independently strengthening reaction member inlet amount is 5.1m
3/ h.Reacted liquid is exported by discharge nozzle, enters middle storage tank respectively through heat exchanger heat exchange, enters circulation line and continue to participate in reaction after liquid agitation is even under the effect of delivery pump.Through 1h reaction, β-carypohyllene conversion ratio is that the selective of 34%, β-caryophyllenol reaches 98%.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.
Claims (11)
1. multistage strengthening fixed bed reactors, is characterized in that, comprise the raw material Forced Mixing still and the intermediate product Forced Mixing still being connected product discharge pipe that connect feed pipe; The reactor tube of several horizontal positioned, each described reactor tube includes several and independently strengthens reaction member, the import of each strengthening reaction member all connects a reactor feed house steward by a feed-inputing branched pipe, reactor feed house steward is equipped with feedstock transportation pump, several reactor feeds house steward connects the outlet of described raw material Forced Mixing still; The outlet of each strengthening reaction member all connects a reactor discharge header pipe by a discharging arm, and reactor discharge header pipe is equipped with heat exchanger, and several reactor discharge header pipe connect described intermediate product Forced Mixing still; Described reactor feed house steward, feed-inputing branched pipe and circulation line are equipped with flowmeter and valve, described discharging arm is also provided with valve; The outlet of described intermediate product Forced Mixing still also connects several circulation lines, several circulation lines described and described several reactor feeds house steward one_to_one corresponding, and before being connected to the feedstock transportation pump on reactor feed house steward, after valve and flowmeter.
2. multistage strengthening fixed bed reactors according to claim 1, it is characterized in that, described raw material Forced Mixing still comprises the first mixing kettle and the first mixed pipe line, the two ends of described first mixed pipe line connect upper end import and the lower end outlet of described first mixing kettle respectively, and the first mixed pipe line is provided with the first mixed pipe line pump, first-class gauge and the first valve; Described intermediate product Forced Mixing still includes the second mixing kettle and the second mixed pipe line, the two ends of described second mixed pipe line connect upper end import and the lower end outlet of described second mixing kettle respectively, second mixed pipe line is provided with the second mixed pipe line pump, second gauge and the second valve, and described product discharge pipe is located on the second mixed pipe line.
3. multistage strengthening fixed bed reactors according to claim 1, is characterized in that, the space arrangement of several reactor tubes described is: horizontal alignment is provided with multilayer, and every layer is set side by side with multiple reactor tube.
4. multistage strengthening fixed bed reactors according to claim 1, is characterized in that, pass through Flange joint between described strengthening reaction member and adjacent strengthening reaction member.
5. multistage strengthening fixed bed reactors according to claim 1, is characterized in that, described strengthening reaction member comprises housing, is provided with beds in housing.
6. multistage strengthening fixed bed reactors according to claim 5, it is characterized in that, described beds can be the bulk type by catalyst inlet, and now, strengthening reaction member housing is provided with the catalyst inlet corresponding with described beds and catalyst outlet.
7. multistage strengthening fixed bed reactors according to claim 5, it is characterized in that, described beds can be monoblock type, and its external diameter is less than the internal diameter of housing, and beds is also connected with catalyst stop.
8. multistage strengthening fixed bed reactors according to claim 5, is characterized in that, described feed-inputing branched pipe is connected to the left end of described fixed bed interval, and described discharging arm is connected to the right-hand member of described fixed bed interval.
9. multistage strengthening fixed bed reactors according to claim 2, is characterized in that, are also provided with liquid forced jet blender in described mixing kettle.
10. a using method for the multistage strengthening fixed bed reactors described in any one of claim 1-8, is characterized in that, comprise the steps:
(1) material enters raw material Forced Mixing still by feed pipe, mixing through raw material Forced Mixing still makes material fully mix, close the valve on circulation line, open the valve on reactor feed house steward, and by flowmeter and valve co-controlling uninterrupted, send into each strengthening reaction member respectively by feedstock transportation pump, import reactor discharge header pipe through abundant reacted liquid through each discharging arm, and after heat exchanger heat exchange, enter intermediate product Forced Mixing still respectively; In the process, how many according to raw material Forced Mixing still rate of discharge, filled into the raw material of respective amount to raw material Forced Mixing still by feed pipe;
(2) after a period of time, through intermediate product Forced Mixing still mixed material, open the valve on some circulation lines gradually and reduce the aperture of the valve on reactor feed house steward, the flow that the flow that intermediate product Forced Mixing still is increased and raw material Forced Mixing still reduce is suitable, until the valve on reactor feed house steward is closed completely;
(3) after testing, if the product in intermediate product Forced Mixing still conforms to requirement, then stop the mixing of intermediate product Forced Mixing still, and close the valve on circulation line, product is exported by discharge nozzle; Otherwise the material mixed in intermediate product Forced Mixing still, under the effect of feedstock transportation pump, is circulated in each strengthening reaction member and continues to participate in reaction, until complete.
11. usings method according to claim 9, is characterized in that, described raw material Forced Mixing still and intermediate product Forced Mixing still are respectively by the first mixed pipe line and the mixing of the second mixed pipe line.
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