CN104190330A - Jet flow fluidized bed reaction device and olefin polymerization method thereof - Google Patents
Jet flow fluidized bed reaction device and olefin polymerization method thereof Download PDFInfo
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Abstract
The invention discloses a jet flow fluidized bed reaction device which comprises two units, namely a polymerization reactor unit and a particle gas cycle conveying unit, wherein the polymerization reactor unit comprises a lower vertical cylinder (1), a middle variable-diameter enlargement section (2) and an upper enlargement section (3); and the particle gas cycle conveying unit comprises a primary cyclone separator (19) and a secondary cyclone separator (22). By utilizing the device disclosed by the invention, C1-C6 olefin feed gas is subjected to an olefin polymerization reaction by using a known addition polymerization catalyst. The jet flow fluidized bed reaction device has the advantages of simple structure, low cost and capability of performing large-scale polyolefin production.
Description
Technical field
The invention belongs to a kind of method for olefin polymerization and device, be specifically related to a kind of method of jet fluidized-bed reaction unit and olefinic polymerization thereof.
Background technology
Gas-phase polymerization is the known method for the preparation of polymer.Gas-phase fluidized bed polymerization process causes the concern of polyolefin industry with its simple synthesis process.The production capacity of gas-phase polymerization reactor is generally taking space-time yield as index, and this is the key parameter of reactor design, except relevant with the characteristic of polymerization catalyst, is mainly limited by the exchange capability of heat of system.In gas-phase fluidized bed polymer reactor, the heat-transfer capability that the heat-transfer capability of system is mainly had by fluid bed unit volume determines, the heat that polymerisation produces needs a large amount of circulating air and adds part condensate liquid and take away.But because reactor operates near the softening temperature of polymer, if the temperature of bed interpolymer powder reaches its softening temperature point, free-pouring polymer powder will start to reunite and be attached on wall and inner member, if and these aggregates are broken not in time or remove, the fluidization quality of bed will further be destroyed, occur to lose fluidization phenomenon, will force fluidized-bed reactor to stop.If can prevent the generation of large aggregate or can remove in time large aggregate, will play vital effect to polyolefinic safety and steady production.Mostly gas-phase fluidized bed polymerization process is periodic discharging, and periodically discharging meeting produces larger interference to fluid bed, if can successional discharge product, will be conducive to gas-phase fluidized-bed continous-stable operation.
In the different polyolefin productions of multiple exploitation, the heat of polymerization producing in gas-phase fluidized-bed reactor is taken away by a large amount of recyclegas, has strengthened the needed gas flow of fluidisation, increases the production cost of olefin polymerization.
How to realize the production cost that reduces olefin polymerization, prevent the generation of large aggregate, once produce large aggregate, how can remove in time large aggregate, and the discharging of continous-stable, the olefin polymerization reactor of developing structure optimization is most important to the development of polymerization technique.
Summary of the invention
First object of the present invention is that design is a kind of simple in structure, and cost is low, can produce polyolefinic jet fluidized-bed reaction unit.
Second object of the present invention is to provide one can be suitable for the polyolefinic jet fluidized-bed polymerization of large-scale production.
Design a kind of jet fluidized-bed reaction unit in order to realize the present invention.
Jet fluidized-bed reaction unit of the present invention comprises polymer reactor unit, two unit of granular gas circulation supply unit, described polymer reactor unit comprises lower vertical cylinder, middle part reducing expanding reach and top expanding reach, side discharge gate is positioned at the bottom of lower vertical cylinder, on side discharge gate, there are successively feed pipe and circulating granular carrier pipe, lower loading hopper is connected with feed pipe, on lower loading hopper, it is upper loading hopper, in lower vertical cylinder under side discharge gate, there is the conical distribution plate that is inverted cone shape, on conical distribution plate, there is equally distributed gas vent, conical distribution plate lower end is connected with taper reducing pipe top, conical distribution plate upper end is connected with lower vertical cylinder inner wall, taper reducing pipe lower end is connected with annular release pipe top, jet pipe is arranged in annular release pipe, and be positioned on axis, jet pipe outlet is positioned at same level with taper reducing pipe top, the import of jet pipe is connected with jet pipe air inlet pipe, annular release pipe bottom is provided with annular release pipe air inlet pipe, jet pipe air inlet pipe is arranged at annular release pipe top, lower vertical cylinder below conical distribution plate is provided with distribution grid air inlet pipe, annular release pipe bottom is connected with lower hopper with upper hopper successively, and there is gas discharge outlet on the top of top expanding reach.
Primary cyclone in described granular gas circulation supply unit is connected with gas discharge outlet, the bottom of primary cyclone connects one-level vertical circulating pipes, the lower end of one-level vertical circulating pipes is connected with circulating granular carrier pipe, the top of primary cyclone is connected with secondary cyclone, the bottom of secondary cyclone connects secondary vertical circulating pipes, secondary vertical circulating pipes is connected with one-level vertical circulating pipes, the top of secondary cyclone and recycle gas compressor, heat recovery boiler, circulating air pipeline is connected successively, circulating air pipeline is connected with annular release pipe air inlet pipe with distribution grid air inlet pipe.
The diameter of described top expanding reach is with the diameter of lower vertical cylinder than being 2-4, and the aspect ratio of the height of top expanding reach and lower vertical cylinder is 0.5-1; The height of middle part reducing expanding reach is 0.02-0.2 with lower vertical cylinder heights ratio.
The percent opening of described conical distribution plate is 0.3%-9%, aperture is 0.1-2mm, the bus of conical distribution plate and the angle of central shaft are 20 °-70 °, taking 55 ° as good, the gas vent of conical distribution plate is vertical with conical distribution plate bus, and the height of conical distribution plate is 0.12-0.92 with the diameter ratio of lower vertical cylinder.
The described element of cone of taper reducing pipe and the angle of central shaft are 3 °-12 °, and the height of taper reducing pipe is 0.1-1.5 with the diameter ratio of lower vertical cylinder.
The method of jet fluidized-bed device olefin polymerization of the present invention comprises the steps:
(1) polymerization
From jet pipe air inlet pipe, annular release pipe air inlet pipe, distribution grid air inlet pipe passes into unstripped gas, adds continuously catalyst from feed pipe, sets up gradually material bed in reactor, controls the bed pressure drop of material in reactor at 2-10KPa; In jet pipe air inlet pipe, pass into fresh unstripped gas, in jet pipe air inlet pipe, the speed of gas is 10-60m/s; The air inflow of distribution grid air inlet pipe is 2-8 with the air inflow ratio of annular release pipe air inlet pipe; Reactor operating pressure 0-10MPa (optimum range 0.5-5MPa), operating temperature 30-120 ° (optimum range 40-100 DEG C); For controlling the temperature of reactor, in jet pipe air inlet pipe, pass into condensed fluid simultaneously, the pressure of strengthening polymer reactor moves heat energy power, and the mass ratio of the quality of condensate liquid and overall reaction unstripped gas is 0.05-0.15; The mass ratio of catalyst and unstripped gas is 1-1000, unstripped gas is the alkene of C1-C6, optimum unstripped gas is ethene or propylene, catalyst is known addition polymerization catalyst, comprise by make containing magnesium, titanium, halogen and ingredient of solid catalyst to electronics and organo-aluminum compound component with contact the Ziegler-Natta catalyst forming to electronics component, metallocene catalyst, non-cyclopentadienyl single site catalyst, also can be used in combination these catalyst.
(2) separation of products
In polymerization process, regulate annular separator tube gas speed at 0.5-8m/s, by adjusting annular separator tube gas speed, control and discharge polyolefin amount, make material in jet fluidized-bed reactor keep bed pressure drop at 2-10KPa; In the time that product granularity area requirement is strictly controlled, regulating annular separator tube gas speed to make annular release pipe gas speed and the ratio of the corresponding particle terminal velocity of average grain diameter of product is 1-1.25; In the time of urgent discharge, open side discharge gate simultaneously;
(3) purification of circulating air and Waste Heat Recovery
Unreacted unstripped gas is discharged from gas discharge outlet, separates with secondary cyclone through primary cyclone, and the fine grained of trapping, through vertical circulating pipes, circulating granular carrier pipe, is sent to dense-phase fluidized bed section, again participates in polymerisation; Separated unreacted unstripped gas is sent to annular release pipe air inlet pipe and distribution grid air inlet pipe through recycle gas compressor, heat recovery boiler, circulating air conveyance conduit, and the ratio that enters the circulating flow rate in circulating flow rate in distribution grid air inlet pipe and annular release pipe air inlet pipe is 1-6;
(4) reactor shutdowns
When orderly shutdown, stop adding catalyst; The place's emptying of circulating air pipeline, is progressively depressurized to normal pressure; Reduce the discharge rate that annular release pipe gas speed strengthens product, after product is drained, stop air inlet, final system nitrogen blowing one time.
Tool of the present invention has the following advantages:
(1) fluidized gas that conical distribution plate passes into makes bed in good fluidized state, produce jet air pocket (jetting bubble) by annular release pipe and jet pipe simultaneously, air pocket flows and causes an interior strong stirring, increase the efficiency of gas-solid contact, ensured good mass-and heat-transfer efficiency;
(2) by the adjusting to annular release pipe gas speed, the polyolefin particles generating in continuous discharge reactor that can effective as selective: the one, can discharge aggregate larger in reactor, prevent that large aggregate from further increasing, will produce vital effect to polyolefinic safety and steady production; The 2nd, can optionally discharge polyolefin particles, can accurately control product quality, ensure the size distribution of polyolefin particles;
(3) in jet pipe, can pass into condensate liquid, the pressure of strengthening polymer reactor moves heat energy power, thereby realizes the target that increases substantially reactor space-time yield.
Brief description of the drawings
Fig. 1 is a kind of jet fluidized-bed structure of reactor schematic diagram.
Brief description of the drawings, the 1st, lower vertical cylinder, the 2nd, middle part reducing expanding reach, the 3rd, top expanding reach, the 4th, lower loading hopper, the 5th, upper loading hopper, the 6th, feed pipe, the 7th, conical distribution plate, the 8th, taper reducing pipe, the 9th, jet pipe, the 10th, cylindrical chamber's housing, the 11st, annular release pipe, the 12nd, annular release pipe air inlet pipe, the 13rd, jet pipe air inlet pipe, the 14th, distribution grid air inlet pipe, the 15th, upper hopper, the 16th, lower hopper, the 17th, side discharge gate, the 18th, gas discharge outlet, the 19th, primary cyclone, the 20th, one-level vertical circulating pipes, the 21st, circulating granular carrier pipe, the 22nd, secondary cyclone, the 23rd, secondary vertical circulating pipes, the 24th, recycle gas compressor, the 25th, heat recovery boiler, the 26th, circulating air pipeline, the 27th, condensate liquid pipeline, the 28th, olefinic monomer import pipe.
Detailed description of the invention
In embodiment, provide for the method at one or more alkene of Gas-phase reactor polymerization, this Gas-phase reactor is jet fluidized-bed, and jet fluidized-bed is the one of fluid bed: the fluidized gas that conical distribution plate passes into enters bed, makes bed in good fluidized state; The gas simultaneously passing into by annular release pipe and jet pipe forms larger jet in bed bottom, jet does not penetrate bed, jet fully develops rear disengaging fluerics, produce larger bubble, jet and air pocket mobile causes an interior strong stirring, increase the efficiency of gas-solid contact, ensured good mass-and heat-transfer efficiency.
Olefine polymerizing process of the present invention and special equipment accompanying drawings thereof are as follows:
Jet fluidized-bed reaction unit comprises polymer reactor unit, two unit of granular gas circulation supply unit, described polymer reactor unit comprises lower vertical cylinder 1, middle part reducing expanding reach 2 and top expanding reach 3, side discharge gate 17 is positioned at the bottom of lower vertical cylinder 1, on side discharge gate 17, there are successively feed pipe 6 and circulating granular carrier pipe 21, lower loading hopper 4 is connected with feed pipe 6, it on lower loading hopper 4, is upper loading hopper 5, in lower vertical cylinder 1 under side discharge gate 17, there is the conical distribution plate 7 that is inverted cone shape, on conical distribution plate 7, there is equally distributed gas vent, conical distribution plate 7 lower ends are connected with taper reducing pipe 8 tops, conical distribution plate 7 upper ends are connected with lower vertical cylinder 1 inwall, taper reducing pipe 8 lower ends are connected with annular release pipe 11 tops, jet pipe 9 is arranged in annular release pipe 11, and be positioned on axis, jet pipe 9 outlets are positioned at same level with taper reducing pipe 8 tops, the import of jet pipe 9 is connected with jet pipe air inlet pipe 13, annular release pipe 11 bottoms are provided with annular release pipe air inlet pipe 12, jet pipe air inlet pipe 13 is arranged at annular release pipe 11 tops, lower vertical cylinder 1 below conical distribution plate 7 is provided with distribution grid air inlet pipe 14, annular release pipe 11 bottoms are connected with lower hopper 16 with upper hopper 15 successively, and there is gas discharge outlet 18 on the top of top expanding reach 3.
Primary cyclone 19 in described granular gas circulation supply unit is connected with gas discharge outlet 18, the bottom of primary cyclone 19 connects one-level vertical circulating pipes 20, the lower end of one-level vertical circulating pipes 20 is connected with circulating granular carrier pipe 21, the top of primary cyclone 19 is connected with secondary cyclone 22, the bottom of secondary cyclone 22 connects secondary vertical circulating pipes 23, secondary vertical circulating pipes 23 is connected with one-level vertical circulating pipes 20, the top of secondary cyclone 22 and recycle gas compressor 24, heat recovery boiler 25, circulating air pipeline 26 is connected successively, circulating air pipeline 26 is connected with annular release pipe air inlet pipe 12 with distribution grid air inlet pipe 14.
The diameter of lower vertical cylinder 1 is D, is highly H; The diameter of top expanding reach 3 is 2D-4D, is highly 0.5H-H; The height of middle part reducing expanding reach 2 is 0.02H-0.2H.
The percent opening of described conical distribution plate 7 is 0.3%-9%, and aperture is 0.1-2mm, and the height of conical distribution plate 7 is 0.12D-0.92D, and the bus of conical distribution plate 7 and the angle of central shaft are 20 °-70 °.
The described element of cone of taper reducing pipe 8 and the angle of central shaft are 3 °-12 °, and the height of taper reducing pipe 8 is 0.1D-1.5D.
Concrete olefinic polymerization is implemented as follows:
Pack olefin polymerization catalysis into upper loading hopper 5 and lower loading hopper 4, filling seed bed, the temperature and pressure of reactor is adjusted to technological requirement value, unstripped gas by olefinic monomer import pipe 28 respectively through annular release pipe air inlet pipe 12, jet pipe air inlet pipe 13, distribution grid air inlet pipe 14 enters in jet fluidized-bed reactor; Enter by primary cyclone 19 from gas discharge outlet 18, one-level vertical circulating pipes 20, circulating granular carrier pipe 21, secondary cyclone 22, secondary vertical circulating pipes 23, recycle gas compressor 24, heat recovery boiler 25, the granular gas circulation supply unit that circulating air pipeline 26 forms, in granular gas circulation supply unit, through gas solid separation, the unreacting gas after compression and heat exchange enters in jet fluidized-bed reactor once again through circulating air pipeline 26, annular release pipe air inlet pipe 12 and distribution grid air inlet pipe 14.On circulating air pipeline 26, need to add olefinic polymerization monomer, comonomer or hydrogen through olefinic monomer import pipe 28 according to technique, in jet pipe air inlet pipe 13, pass into fresh unstripped gas or cooling medium, cooling medium can be straight chain or branched alkane or the cycloalkane that carbon number is greater than 4.Catalyst injects from feed pipe 6 continuously, constantly grows up thereby make olefinic monomer participate in reaction polyolefin particles, and polymer product can, continuously from reactor bottom, be discharged through annular release pipe 11, or off and on from reactor bottom, through side material row mouthful 17 discharges; Thus, jet fluidized-bed polymerization reaction system starts stable operation.
The olefin polymerization catalysis using in the present invention can be the known addition polymerization catalyst using in olefinic polymerization, comprise by make containing magnesium, titanium, halogen and ingredient of solid catalyst to electronics and organo-aluminum compound component with contact the Ziegler-Natta catalyst forming to electronics component, metallocene catalyst, non-cyclopentadienyl single site catalyst, also can be used in combination these catalyst.The Harmonic average grain diameter of catalyst is generally 5 to 150 μ m, particularly in gas jet fluidized-bed reactor, be distributed to outside reactor in order to suppress particle, prevent the elutriation of catalyst granules, the pressure that reduces the fine powder recovery of cycle gas system, the Harmonic average grain diameter of preferred catalyst is greater than 10 μ m.
Jet fluidized-bed polymer reactor in the present invention can carry out under common olefinic polymerization condition, polymerization pressure is less than 10MPa conventionally, preferably 0.5 to 5MPa, polymerization temperature is according to monomer type, molecular weight of product and other factors and change, but must be lower than the fusing point of polymer, and preferably at least than the temperature of low at least 10 DEG C of fusing point, particularly, polymerization temperature is less than 120 DEG C conventionally, preferably 40 to 100 DEG C.
Use jet fluidized-bed polymer reactor provided by the invention, the vigorous agitation that the jet air pocket that annular release pipe 11 and jet pipe 9 produce will bring bed, in bed, gas, solid phase are in fierce turbulence state, gas-solid interphase exchange coefficient is higher, conduct heat, mass-transfer efficiency is higher, gas short circuit is few, operates comparatively steady.Simultaneously, in polymerisation, pass through the adjusting to annular release pipe 11 gas speed, the polyolefin particles generating in discharge reactor that can effective as selective: the one, can discharge aggregate larger in reactor, prevent that large aggregate from further increasing, will produce vital effect to polyolefinic safety and steady production; The 2nd, can optionally discharge polyolefin particles, can accurately control product quality, ensure the size distribution of polyolefin particles.In jet pipe 9, can pass into reactor feed gas, can also in gas-phase polymerization reactor, inject condensate liquid through jet pipe air inlet pipe 13 by condensate liquid pipeline 27, the pressure of strengthening polymer reactor moves heat energy power, thereby increases substantially the target of reactor space-time yield.
Embodiment
Adopt the jet fluidized-bed polymerizing reactor of the present invention as shown in Figure 1, carried out cold conditions operation and computer simulation in laboratory, on hot device, carried out hot operation, investigated jet fluidized-bed polymerization effect.
1) laboratory cold conditions operating data
Material: wide particle diameter distribution polyethylene particle, air/nitrogen (adopting nitrogen in pressurization experiment).
The major parameter of cold experimental is listed in table 1, table 2, table 3.
Service data: adopt the present invention as the jet fluidized-bed reactor of Fig. 1, the major parameter of experimental provision is as shown in table 1, table 2, table 3, utilize ultrahigh speed image analyzers, particle dynamic imaging analytical system, optical fiber particle tachymeter, differential pressure pickup, research finds that reactor Bian Bi district movement of particles is all right, and then will can not lump in reactor Bian Bi district, in the time that operating pressure is greater than 1.6MPa, by regulating the gas speed of jet pipe, still can obtain larger jet bubble.
The major parameter of table 1 cold experimental
The major parameter of table 2 cold experimental
The major parameter of table 3 cold experimental
2) computer simulation operating data
Utilize cfdrc to adopting the jet fluidized-bed polymer reactor of the present invention as shown in Fig. 1 and table 1, table 2, table 3 to carry out digital simulation, wall place, limit granule density, particle velocity and internal circulating load are mainly investigated, research finds that wall place, limit particle is all the time in concentrated phase area, movement of particles is all right, in bed, solids circulation is enough high, show that bed operating is good, will can not form larger aggregate.
3) hot operation on hot device
Material: Z-N the 5th generation catalyst, propylene, heptane
Mainly to adopting jet fluidized-bed operation the as shown in Fig. 1 and table 1, concrete operations parameter is as shown in table 4, table 5, table 6, on pilot-plant, move 72 hours continuously, there is not high temperature dot in the temperature sensor at reactor bottom in service and wall place, limit, stop reacting wall place, back and do not find larger caking, from table 4, table 5 and table 6, reactor is in service there is not a large amount of larger particles aggregates, annular release pipe 11 can be realized the Continuous Selection of material and discharge, stable.
Pilot plant test operation result under table 4 different condition
| ? | Pilot scale 1 | Pilot scale 2 | Pilot scale 3 | Pilot scale 4 | Pilot scale 5 |
| Operating pressure, MPa | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
| Operating temperature, DEG C | 70 | 70 | 65 | 65 | 60 |
| Reaction time, h | 1.5 | 1.5 | 1.2 | 1 | 1 |
| Bed pressure drop, KPa | 6 | 6 | 4.5 | 4 | 4 |
| The ratio of conical distribution plate air inflow and endless tube air inflow | 7.5 | 7.5 | 6.5 | 6 | 5 |
| The mass ratio of the quality of condensate liquid and overall reaction unstripped gas | 0.06 | 0.06 | 0.05 | 0.05 | 0.04 |
| Jet pipe gas speed | 50 | 50 | 45 | 45 | 40 |
| Whether annular release pipe continuous pulp discharge | Be | Be | Be | Be | Be |
| Bulky grain aggregate quantity | 3 | 0 | 0 | 0 | 1 |
| Can annular release pipe discharge bulky grain aggregate | Be | - | - | - | Be |
Pilot plant test operation result under table 5 different condition
| ? | Pilot scale 6 | Pilot scale 7 | Pilot scale 8 | Pilot scale 9 | Pilot scale 10 |
| Operating pressure, MPa | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 |
| Operating temperature, DEG C | 70 | 70 | 65 | 65 | 60 |
| Reaction time, h | 1.6 | 1.5 | 1.2 | 1 | 1 |
| Bed pressure drop, KPa | 6 | 5.5 | 4.5 | 4 | 4 |
| The ratio of conical distribution plate air inflow and endless tube air inflow | 8 | 8 | 7 | 6.5 | 6 |
| The mass ratio of the quality of condensate liquid and overall reaction unstripped gas | 0.08 | 0.08 | 0.07 | 0.07 | 0.06 |
| Jet pipe gas speed | 45 | 45 | 40 | 40 | 37 |
| Whether annular release pipe continuous pulp discharge | Be | Be | Be | Be | Be |
| Bulky grain aggregate quantity | 5 | 3 | 1 | 1 | 1 |
| Can annular release pipe discharge bulky grain aggregate | Be | Be | Be | Be | Be |
Pilot plant test operation result under table 6 different condition
| ? | Pilot scale 11 | Pilot scale 12 | Pilot scale 13 | Pilot scale 14 | Pilot scale 15 |
| Operating pressure, MPa | 2.5 | 2.5 | 2.5 | 2.5 | 2.5 |
| Operating temperature, DEG C | 70 | 65 | 65 | 60 | 60 |
| Reaction time, h | 1.4 | 1.3 | 1.1 | 1 | 1 |
| Bed pressure drop, KPa | 5.5 | 5.5 | 4.5 | 4 | 4 |
| The ratio of conical distribution plate air inflow and endless tube air inflow | 8 | 8 | 7 | 6.5 | 6 |
| The mass ratio of the quality of condensate liquid and overall reaction unstripped gas | 0.13 | 0.13 | 0.11 | 0.11 | 0.09 |
| Jet pipe gas speed | 43 | 40 | 35 | 35 | 32 |
| Whether annular release pipe continuous pulp discharge | Be | Be | Be | Be | Be |
| Bulky grain aggregate quantity | 8 | 5 | 3 | 3 | 1 |
| Can annular release pipe discharge bulky grain aggregate | Be | Be | Be | Be | Be |
Claims (10)
1. a jet fluidized-bed reaction unit comprises polymer reactor unit, two unit of granular gas circulation supply unit, it is characterized in that described polymer reactor unit comprises lower vertical cylinder (1), middle part reducing expanding reach (2) and top expanding reach (3), side discharge gate (17) is positioned at the bottom of lower vertical cylinder (1), on side discharge gate (17), there are successively feed pipe (6) and circulating granular carrier pipe (21), lower loading hopper (4) is connected with feed pipe (6), on lower loading hopper (4), be upper loading hopper (5), in lower vertical cylinder (1) under side discharge gate (17), there is the conical distribution plate (7) that is inverted cone shape, conical distribution plate has equally distributed gas vent on (7), conical distribution plate (7) lower end is connected with taper reducing pipe (8) top, conical distribution plate (7) upper end is connected with lower vertical cylinder (1) inwall, taper reducing pipe (8) lower end is connected with annular release pipe (11) top, jet pipe (9) is arranged in annular release pipe (11), and be positioned on axis, jet pipe (9) outlet is positioned at same level with taper reducing pipe (8) top, the import of jet pipe (9) is connected with jet pipe air inlet pipe (13), annular release pipe (11) bottom is provided with annular release pipe air inlet pipe (12), jet pipe air inlet pipe (13) is arranged at annular release pipe (11) top, lower vertical cylinder (1) in conical distribution plate (7) below is provided with distribution grid air inlet pipe (14), annular release pipe (11) bottom is connected with lower hopper (16) with upper hopper (15) successively, and there is gas discharge outlet (18) on the top of top expanding reach (3),
Primary cyclone (19) in described granular gas circulation supply unit is connected with gas discharge outlet (18), the bottom of primary cyclone (19) connects one-level vertical circulating pipes (20), the lower end of one-level vertical circulating pipes (20) is connected with circulating granular carrier pipe (21), the top of primary cyclone (19) is connected with secondary cyclone (22), the bottom of secondary cyclone (22) connects secondary vertical circulating pipes (23), secondary vertical circulating pipes (23) is connected with one-level vertical circulating pipes (20), the top of secondary cyclone (22) and recycle gas compressor (24), heat recovery boiler (25), circulating air pipeline (26) is connected successively, circulating air pipeline (26) is connected with annular release pipe air inlet pipe (12) with distribution grid air inlet pipe (14).
2. the jet fluidized-bed reaction unit of one as claimed in claim 1, it is characterized in that the described diameter of top expanding reach (3) and the diameter ratio of lower vertical cylinder (1) are 2-4, the aspect ratio of the height of top expanding reach (3) and lower vertical cylinder (1) is 0.5-1; Height and lower vertical cylinder (1) aspect ratio of middle part reducing expanding reach (2) are 0.02-0.2.
3. the jet fluidized-bed reaction unit of one as claimed in claim 1, the percent opening that it is characterized in that described conical distribution plate (7) is 0.3%-9%, aperture is 0.1-2mm, the bus of conical distribution plate (7) and the angle of central shaft are 20 °-70 °, and the gas vent of conical distribution plate (7) is vertical with conical distribution plate (7) bus.
4. the jet fluidized-bed reaction unit of one as claimed in claim 3, is characterized in that the bus of described conical distribution plate (7) and the angle of central shaft are 55 °.
5. the jet fluidized-bed reaction unit of one as claimed in claim 1, is characterized in that the height of described conical distribution plate (7) and the diameter of lower vertical cylinder (1) than being 0.12-0.92.
6. the jet fluidized-bed reaction unit of one as claimed in claim 1, it is characterized in that the described element of cone of taper reducing pipe (8) and the angle of central shaft are 3 °-12 °, the diameter of the height of taper reducing pipe (8) and lower vertical cylinder (1) is than being 0.1-1.5.
7. a method for jet fluidized-bed device olefin polymerization, is characterized in that comprising the steps:
(1) polymerization
From jet pipe air inlet pipe, annular release pipe air inlet pipe, distribution grid air inlet pipe passes into unstripped gas, adds continuously catalyst from feed pipe, sets up gradually material bed in reactor, controls the bed pressure drop of material in reactor at 2-10KPa; In jet pipe air inlet pipe, pass into fresh unstripped gas, in jet pipe air inlet pipe, the speed of gas is 10-60m/s; The air inflow of distribution grid air inlet pipe is 2-8 with the air inflow ratio of annular release pipe air inlet pipe; Reactor operating pressure 0-10MPa, 30-120 ° of operating temperatures for controlling the temperature of reactor, pass into condensed fluid simultaneously in jet pipe air inlet pipe, the pressure of strengthening polymer reactor moves heat energy power, and the mass ratio of the quality of condensate liquid and overall reaction unstripped gas is 0.05-0.15; The mass ratio of catalyst and unstripped gas is 1-1000, and unstripped gas is the alkene of C1-C6, and catalyst is addition polymerization catalyst;
(2) separation of products
In polymerization process, regulate annular separator tube gas speed at 0.5-8m/s, by adjusting annular separator tube gas speed, control and discharge polyolefin amount, make material in jet fluidized-bed reactor keep bed pressure drop at 2-10KPa; In the time that product granularity area requirement is strictly controlled, regulating annular separator tube gas speed to make annular release pipe gas speed and the ratio of the corresponding particle terminal velocity of average grain diameter of product is 1-1.25; In the time of urgent discharge, open side discharge gate simultaneously;
(3) purification of circulating air and Waste Heat Recovery
Unreacted unstripped gas is discharged from gas discharge outlet, separates with secondary cyclone through primary cyclone, and the fine grained of trapping, through vertical circulating pipes, circulating granular carrier pipe, is sent to dense-phase fluidized bed section, again participates in polymerisation; Separated unreacted unstripped gas is sent to annular release pipe air inlet pipe and distribution grid air inlet pipe through recycle gas compressor, heat recovery boiler, circulating air conveyance conduit, and the ratio that enters the circulating flow rate in circulating flow rate in distribution grid air inlet pipe and annular release pipe air inlet pipe is 1-6;
(4) reactor shutdowns
When orderly shutdown, stop adding catalyst; The place's emptying of circulating air pipeline, is progressively depressurized to normal pressure; Reduce the discharge rate that annular release pipe gas speed strengthens product, after product is drained, stop air inlet, final system nitrogen blowing one time.
8. the method for a kind of jet fluidized-bed device olefin polymerization as claimed in claim 7, is characterized in that in step (1), reactor operating pressure is 0.5-5MPa, and operating temperature is 40-100 DEG C.
9. the method for a kind of jet fluidized-bed device olefin polymerization as claimed in claim 7, is characterized in that the alkene of C1-C6 in step (1) is ethene or propylene.
10. the method for a kind of jet fluidized-bed device olefin polymerization as claimed in claim 7, it is characterized in that catalyst in step (1) be comprise by make containing magnesium, titanium, halogen and ingredient of solid catalyst to electronics and organo-aluminum compound component with contact the Ziegler-Natta catalyst forming to electronics component, metallocene catalyst, the catalyst of non-cyclopentadienyl single site catalyst or its combination.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107531827A (en) * | 2015-04-17 | 2018-01-02 | 尤尼威蒂恩技术有限责任公司 | Method and system for olefinic polymerization |
| CN110709428A (en) * | 2017-06-20 | 2020-01-17 | 博里利斯股份公司 | Method and device for producing polymers and use of the device |
| WO2020078444A1 (en) * | 2018-10-19 | 2020-04-23 | 清华大学 | Method and device for producing nano-scale clad material |
| CN111655364A (en) * | 2016-12-16 | 2020-09-11 | 埃姆皮瑞欧有限公司 | Apparatus with annular spouted fluidized bed and method of operating the same |
| CN114761118A (en) * | 2019-12-18 | 2022-07-15 | Ifp 新能源公司 | Gas/liquid oligomerization reactor with continuous zones of varying diameter |
| CN115790229A (en) * | 2023-02-13 | 2023-03-14 | 成都天保节能环保工程有限公司 | Structure and method suitable for fluidized bed heat storage |
| CN116020573A (en) * | 2021-10-26 | 2023-04-28 | 中国石油化工股份有限公司 | Device and method for regulating and controlling particle size distribution of fluidized bed catalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85104124A (en) * | 1985-05-31 | 1986-11-26 | 联合碳化公司 | Reduce the method that thin slice generates in the alpha-olefine polymerizing process |
| US4666999A (en) * | 1983-09-01 | 1987-05-19 | Mobil Oil Corporation | Method and reactor system for rapid kill gas injection to gas phase polymerization reactors |
| CN1030918A (en) * | 1987-07-31 | 1989-02-08 | Bp化学有限公司 | Method with gas phase polymerisation of olefins in fluidised bed reactor |
| CN1322152A (en) * | 1998-08-10 | 2001-11-14 | 英国石油化学品有限公司 | Continuous process for gas phase coating of polymerisation catalyst |
| CN103212346A (en) * | 2013-03-01 | 2013-07-24 | 浙江大学 | Spouted bed reactor and olefin polymerization method thereof |
-
2014
- 2014-08-29 CN CN201410436134.8A patent/CN104190330B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4666999A (en) * | 1983-09-01 | 1987-05-19 | Mobil Oil Corporation | Method and reactor system for rapid kill gas injection to gas phase polymerization reactors |
| CN85104124A (en) * | 1985-05-31 | 1986-11-26 | 联合碳化公司 | Reduce the method that thin slice generates in the alpha-olefine polymerizing process |
| CN1030918A (en) * | 1987-07-31 | 1989-02-08 | Bp化学有限公司 | Method with gas phase polymerisation of olefins in fluidised bed reactor |
| CN1322152A (en) * | 1998-08-10 | 2001-11-14 | 英国石油化学品有限公司 | Continuous process for gas phase coating of polymerisation catalyst |
| CN103212346A (en) * | 2013-03-01 | 2013-07-24 | 浙江大学 | Spouted bed reactor and olefin polymerization method thereof |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107531827A (en) * | 2015-04-17 | 2018-01-02 | 尤尼威蒂恩技术有限责任公司 | Method and system for olefinic polymerization |
| US10711072B2 (en) | 2015-04-17 | 2020-07-14 | Univation Technologies, Llc | Methods and systems for olefin polymerization |
| CN107531827B (en) * | 2015-04-17 | 2021-04-23 | 尤尼威蒂恩技术有限责任公司 | Process and system for olefin polymerization |
| US11384164B2 (en) | 2015-04-17 | 2022-07-12 | Univation Technologies, Llc | Methods and systems for olefin polymerization |
| CN111655364A (en) * | 2016-12-16 | 2020-09-11 | 埃姆皮瑞欧有限公司 | Apparatus with annular spouted fluidized bed and method of operating the same |
| CN110709428A (en) * | 2017-06-20 | 2020-01-17 | 博里利斯股份公司 | Method and device for producing polymers and use of the device |
| CN110709428B (en) * | 2017-06-20 | 2022-01-04 | 博里利斯股份公司 | Method and device for producing polymers and use of the device |
| WO2020078444A1 (en) * | 2018-10-19 | 2020-04-23 | 清华大学 | Method and device for producing nano-scale clad material |
| CN114761118A (en) * | 2019-12-18 | 2022-07-15 | Ifp 新能源公司 | Gas/liquid oligomerization reactor with continuous zones of varying diameter |
| CN114761118B (en) * | 2019-12-18 | 2023-11-07 | Ifp 新能源公司 | Gas/liquid oligomerization reactor having continuous zones of varying diameter |
| CN116020573A (en) * | 2021-10-26 | 2023-04-28 | 中国石油化工股份有限公司 | Device and method for regulating and controlling particle size distribution of fluidized bed catalyst |
| CN115790229A (en) * | 2023-02-13 | 2023-03-14 | 成都天保节能环保工程有限公司 | Structure and method suitable for fluidized bed heat storage |
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