CN207085901U - One kind is used for ethylene tetramerization catalyst system and catalyzing batch mixing and feed system - Google Patents
One kind is used for ethylene tetramerization catalyst system and catalyzing batch mixing and feed system Download PDFInfo
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- CN207085901U CN207085901U CN201720804781.9U CN201720804781U CN207085901U CN 207085901 U CN207085901 U CN 207085901U CN 201720804781 U CN201720804781 U CN 201720804781U CN 207085901 U CN207085901 U CN 207085901U
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Abstract
A kind of batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, batch mixing reactor；Agitating device, it is arranged in batch mixing reactor；Raw material feeder is pre-mixed, is connected with batch mixing reactor top, for the different raw materials for configuring ethylene tetramerization reaction solution to be added in batch mixing reactor；An at least vacuum nitrogen filling device of air, it is connected respectively with the connection of batch mixing reactor, premixing raw material feeder, vacuum nitrogen filling device of air takes the air in batch mixing reactor, in premixing raw material feeder away when opening vacuum extraction valve, close vacuum extraction valve and open nitrogen charge valve again, nitrogen is filled with toward batch mixing reactor, premixing raw material feeder, repetition vacuumizes, inflated with nitrogen repeatedly maintains negative pressure state up to the pressure of batch mixing reactor, and is pre-mixed in the pipeline of raw material feeder and is full of nitrogen；Side position feed pipe, it is connected to batch mixing reactor side and gos deep into batch mixing reactor bottom.
Description
Technical field
A kind of batch mixing and feed system for chemical process is the utility model is related to, particularly one kind is used for ethene
The batch mixing and charging system of Cr (III)/PNP/MAO catalyst system and catalyzings during four consor production 1- octenes.
Background technology
1- octenes can be used as LLDPE (LLDPE) copolymerization as a kind of important Organic Chemicals
Monomer, it is big as LLDPE melt extensibility prepared by comonomer by 1- octenes, have good tensile property, shock resistance and
Environmental stress crack resistance, machining property, heat resistance, flexibility and transparency of polyethylene etc. can be obviously improved.
1- octenes are mainly prepared by ethylene oligomerization method at present, and it is the wide alpha-olefin being distributed to be obtained due to ethylene oligomerization method, is needed
The methods of passing through rectifying is purified, thus cost is higher.Therefore, using ethylene tetramerization method, it is pungent that high selectivity obtains 1-
Alkene (1- Octenes selectivities are more than 65%) has very important economic implications.
Ethylene tetramerization prepares 1- octenes based on Cr (III)/PNP (PNP=Ph2P-N (R)-PPh2, diphenyl phosphine amine ligand)
Catalyst, MAO (MAO) are co-catalyst.In the presence of MAO, Cr (III) (tetrahydrofuran chromium trichloride or levulinic
Ketone chromium) with PNP formed complex compound there is high catalytic activity and selectivity.Because Cr (III)/PNP and MAO are air-sensitive
Compound, thus need special device to be mixed.Because Cr (III)/PNP/MAO catalytic activity is higher (up to 107g
Ethene/(mol Crh)), catalyst local over-concentration can cause local reaction activity too high and generate more in the reactor
Accessory substance.
The patent of ethylene tetramerization concentrates on catalyst for ethylene tetramerization composition and application aspect at present.Such as patent
CN104245640, CN104220402, CN102164936, CN102909072, CN103044181, CN105562101 are provided
Composition of four poly- catalyst of differing ethylene and preparation method thereof, above-mentioned patent is not involved with batch mixing and the charging side of catalyst
Influence of the formula to ethylene tetramerization reactivity worth.
Utility model content
Technical problem to be solved in the utility model be for catalyst for ethylene tetramerization system to air-sensitive characteristic and
Itself need to be pre-mixed that just there is the problem of high selectivity, there is provided the good mixing of reaction effect under a kind of anhydrous and oxygen-free environment
Mode, while a kind of catalyst charge mode that can effectively avoid ethylene tetramerization catalyst reactor local over-concentration is provided.
The utility model is in order to solve the above-mentioned technical problem, there is provided following technical scheme：
A kind of batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that including,
One batch mixing reactor；
One agitating device, it is arranged in the batch mixing reactor；
One premixing raw material feeder, is connected with batch mixing reactor top, for that will configure ethylene tetramerization reaction solution
Different raw materials add in batch mixing reactors；
An at least vacuum nitrogen filling device of air, connected respectively with the batch mixing reactor, the premixing raw materials dress
Put connection, the vacuum nitrogen filling device of air is provided with vacuum extraction valve, nitrogen charge valve, described in when opening the vacuum extraction valve
Vacuum nitrogen filling device of air takes the air in batch mixing reactor, in premixing raw material feeder away, closes vacuum extraction valve
Nitrogen charge valve is opened again, is filled with nitrogen toward the batch mixing reactor, described be pre-mixed in raw material feeder, repetition is taken out true
Empty, inflated with nitrogen is repeatedly until the pressure of the batch mixing reactor maintains negative pressure state, and the premixing raw material feeder
Pipeline in be full of nitrogen；
Side position feed pipe, it is connected to the batch mixing reactor side and gos deep into the batch mixing reactor bottom, to urge
Agent is fed, and catalyst is injected in batch mixing reactor in the presence of the negative pressure of the batch mixing reactor.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, the vacuum nitrogen filling device of air include one
Vacuum plant and a nitrogen device, the vacuum plant is connected by vacuum tube with the batch mixing reactor, the premixing is former
Expect feeding device connection, the nitrogen device is connected by nitrogen tube with the batch mixing reactor, the premixing raw materials
Device connects.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that the premixing raw material
Feeding device include at least two Feed lines, two solid feed pots, the two solids feed pot respectively by a feeding line with
The batch mixing reactor connection, two Feed lines directly connect with the batch mixing reactor.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that the vacuum tube, described
Nitrogen tube is drawn from the feeding line respectively, and the vacuum tube is provided with the vacuum extraction valve, and the nitrogen tube is provided with
Nitrogen charge valve, the both ends of the feeding line are provided with inlet control valve.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that side position feed pipe
For a door type pipe, provided with a charging aperture and a discharging opening, the discharging opening gos deep into the batch mixing reactor bottom.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that the charging aperture is saw
Dentation port, interior to be provided with gear piece, catalyst injects the batch mixing reactor bottom with the catalysis that scatter by gear piece rotation
Agent.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that two Feed lines
On be equipped with measuring pump and control valve, two Feed lines are respectively adding MAO and solvent.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that the batch mixing reactor
It is provided with pressure vacuum gauge.
The described batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that side position feed pipe
It is provided with valve.
The beneficial effects of the utility model：Using the solid feeding device with anhydrous and oxygen-free device, it is ensured that solid
There will not be air entrance in body charging, avoid adversely affecting catalyst；With side position feed pipe and zigzag port
Feed pipe, material can be made, into ethylene tetramerization reaction solution, to avoid the local over-concentration of catalyst by gear piece rotation drop.
Brief description of the drawings
Fig. 1 is system construction drawing of the present utility model.
Vacuum tube 01,03
Nitrogen tube 02,04
Solid feed pot 11,12
Feeding line 111,121
MAO Feed lines 13
Solvent Feed lines 14
Batch mixing reactor 21
Charging aperture 25
Agitating device 27
Embodiment
Technical solutions of the utility model are described in detail with specific embodiment below in conjunction with the accompanying drawings, with further
Understand the purpose of this utility model, method and effect, but do not limit the utility model.
A kind of batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing disclosed in the utility model, including,
One batch mixing reactor 21；
One agitating device, it is arranged in the batch mixing reactor 21；
Raw material feeder is pre-mixed, is connected with the top of batch mixing reactor 21, for ethylene tetramerization reaction solution will to be configured
Different raw materials add in batch mixing reactors 21；Furtherly, being pre-mixed raw material feeder includes at least reacting with batch mixing
Two Feed lines that kettle 21 directly connects, and two solid feed pots, two Feed lines are MAO Feed lines 13, solvent respectively
Feed lines 14, MAO Feed lines 13 are provided with valve 17 and measuring pump 18, and the solvent Feed lines 14 are provided with the He of valve 19
Measuring pump 20, described one end of MAO Feed lines 13 are connected the other end with the upper end of batch mixing reactor 21 and are connected with MAO storage tanks, solvent
The one end of Feed lines 14 is connected the other end with the upper end of batch mixing reactor 21 and is connected with solvent tank, in the present embodiment, solvent charging
Pipeline 14 feeds (MAO charging) to toluene feed, MAO Feed lines 13 to MAO.
Solid feed pot is connected with batch mixing reactor 21 by feeding line (111,121), wherein a feeding line 111
Both ends are provided with inlet control valve (15,22), and the both ends of another feeding line 121 are provided with inlet control valve (16,23), charging control
Valve (22,23) is set close to batch mixing reactor 21, inlet control valve (15,16) set close to solid feed pot (11,12), it is necessary to
It is noted that be provided with external screw thread in feeding line (111,121) one end of the solid feed pot (11,12), it is used for and batch mixing
The top thread seal connection of reactor 21.
To air-sensitive characteristic and itself need to be pre-mixed that just there is high selection for catalyst for ethylene tetramerization system
Property the problem of, batch mixing reactor 21 with premixing raw material feeder on be also connected with a vacuum nitrogen filling device of air, the device use
To protect catalyst for ethylene tetramerization system to be under anhydrous and oxygen-free environment, the vacuum nitrogen filling device of air is provided with vacuum suction
Valve, nitrogen charge valve, open during the vacuum extraction valve vacuum nitrogen filling device of air by batch mixing reactor 21, premixing
Air in raw material feeder is taken away, closes vacuum extraction valve and opens nitrogen charge valve again, toward the batch mixing reactor 21, institute
State and nitrogen is filled with premixing raw material feeder, repetition vacuumizes, inflated with nitrogen is repeatedly until the pressure of the batch mixing reactor 21
Power maintains negative pressure state, is full of nitrogen in the pipeline of the premixing raw material feeder.Batch mixing reactor 21 is provided with true
Hollow pressure gauge.
In the present embodiment, vacuum nitrogen filling device of air also includes a vacuum plant and a nitrogen device, the vacuum holding
Put connected by vacuum tube with the batch mixing reactor 21, it is described premixing raw material feeder be connected, the nitrogen device leads to
Cross nitrogen tube connected with the batch mixing reactor 21, it is described premixing raw material feeder be connected.It should be noted that premixing
Raw material feeder can individually connect a vacuum nitrogen filling device of air, can also share one with batch mixing reactor 21 and vacuumize and fill
Nitrogen device, in the present embodiment, premixing raw material feeder configures a vacuum nitrogen filling device of air, and batch mixing reactor 21 is matched somebody with somebody
Put another vacuum nitrogen filling device of air.
Specifically, in the present embodiment, the top of batch mixing reactor 21 connection vacuum tube 01 and nitrogen tube 02, vacuum tube 01 with
Vacuum plant (not shown) is connected, and nitrogen tube 02 is connected with nitrogen device (not shown), and vacuum tube 01 is provided with vacuum extraction valve
05, nitrogen tube 02 is provided with nitrogen charge valve 06.
Vacuum nitrogen filling device of air also with premixing raw material feeder be connected, vacuum nitrogen filling device of air respectively with solid
Feed pot 11,12 connect, in detail it, draw one on the feeding line 111 between inlet control valve 15 and inlet control valve 22
Vacuum tube 03, the vacuum tube 03 connect the vacuum plant, the vacuum extraction valve 07 are provided with the vacuum tube 03, are controlled in charging
A vacuum tube 03 is drawn on feeding line 121 between valve 16 and inlet control valve 22, is taken out on the vacuum tube 03 provided with vacuum
Air valve 08, in the present embodiment, two feeding lines (111,121) are connected with same nitrogen tube 04, and the nitrogen tube 04 is with being somebody's turn to do
Nitrogen device is connected, and nitrogen tube 04 is drawn from feeding line (111,121), and positioned at the inlet control valve (16 and 23 at both ends
Or 15 and 22) between, feeding line 111 is provided with nitrogen charge valve 9, and feeding line 121 is provided with nitrogen charge valve 10.
Batch mixing reactor 21 connects side position feed pipe, and to catalyst charge, side position feed pipe is connected to the batch mixing
The bottom of batch mixing reactor 21 is simultaneously goed deep into the side of reactor 21, and side position feed pipe 24 is by the first pipeline 241, the second pipeline
242 liang of by-pass lines connect the door type pipe to be formed, and the crossbeam oblique of door type is set up, and door type pipe is provided with a charging aperture 25
With a discharging opening, the charging aperture 25 is on the first pipeline 241, and the discharging opening is on the second pipeline 242, the first pipeline
241 caliber is more than the caliber of the second pipeline 242, charging aperture 25 and the ethylene tetramerization reactor (not shown) of the first pipeline 241
Upper end is connected and is suspended from above its internal liquid, and the other end is connected with the second pipeline 242, and the discharging opening of the second pipeline 242 enters
In batch mixing reactor 21 and go deep into the bottom of batch mixing reactor 21, valve 26, the charging aperture are provided with the second pipeline 242
25 lower ends are zigzag port, interior to be provided with gear piece, catalyst by gear piece rotation inject the polymerization reaction kettle bottom with
Scatter catalyst, prevents catalyst local over-concentration, the first pipeline with zigzag port, material can be made to be revolved by gear piece
Turn in ethylene tetramerization reaction solution of the drop into batch mixing reactor, avoid the local over-concentration of catalyst.When ethylene tetramerization reacts
When having pressure difference between kettle and batch mixing reactor, catalyst in the presence of the negative pressure of the batch mixing reactor 21 to will catalysis
In agent injection batch mixing reactor 21.
In order to preferably explain the technical solution of the utility model, operation principle of the present utility model described in detail below：
Quantitative Cr (III) (tetrahydrofuran trichlorine is added to solid feed pot in nitrogen protection device (such as glove box)
Change chromium or chromium acetylacetonate) or PNP (Ph2P-N (- CH (CH3) 2)-PPh2), close solid charging tank mouth inlet control valve 15 or
16, taken out from glove box, feeding line is threadedly attached on batch mixing reactor 21, close batch mixing reactor 21 and ethene
Valve between four poly- reactors, batch mixing reactor 21 vacuumize-add after nitrogen circulates three times altogether to be filled with nitrogen, to solid
The feeding line being connected between body feed pot and batch mixing reactor 21 vacuumize-add after nitrogen circulates three times altogether being filled with nitrogen
Gas, the inlet control valve on MAO Feed lines 13 is opened,
Chromium acetylacetonate (Cr (III)) and PNP is entered in batch mixing reactor 21, open on solvent Feed lines 14
Valve 19, solvent is added, starts stirring, then opened the valve 17 on MAO Feed lines 13, add MAO, stir certain time
After open into valve on the feed pipe of side position, catalyst is pressed into charging aperture 25 using nitrogen pressure, and using spiral way edge
The inwall of charging aperture 25 flows and instills reactor along the lower end sawtooth of charging aperture 25, and all catalyst enter ethylene tetramerization reactor
Valve on feeding line is closed afterwards, completes a catalyst batch mixing and fill process.
It is basic embodiment of the present utility model above, the utility model specific operation process step described in detail below
Suddenly:
Step 1,0.7kg acetyl is separately added into solid feed pot 11 and 12 in nitrogen protection device (such as glove box)
Acetone chromium and 0.9kgPNP, the inlet control valve (15,16) closed at solid feed pot (11,12) tank mouth.
Step 2 is taken out from glove box, and feeding line is threadedly attached on batch mixing reactor 21, closes batch mixing reaction
Valve 26 between kettle 21 and ethylene tetramerization reactor, close solid feed pot (11,12) entering between batch mixing reactor 21
Expect control valve (22,23), the nitrogen charge valve 06 closed in nitrogen tube 02, valve 17 and solvent enter on MAO feeding lines 13
Valve 19 on expects pipe line 14, open the vacuum extraction valve 05 on vacuum tube 01, by being evacuated in batch mixing reactor 21-
0.095MPa。
The vacuum extraction valve 05 that step 3. is closed on vacuum tube 01, the nitrogen charge valve 06 opened in nitrogen tube 02 are filled with nitrogen
Gas is then shut off nitrogen charge valve 06 to 0.1MPa, and repetition vacuumizes-and inflated with nitrogen maintains pressure in batch mixing reactor 21 afterwards three times
For 0.01MPa.
Step 4. opens the vacuum extraction valve 07 on vacuum tube 03, will be evacuated to -0.095MPa in feeding line 111,
The vacuum extraction valve 07 being then shut off on vacuum tube 03, open feeding line 111 and be filled with nitrogen extremely provided with nitrogen charge valve 09
Nitrogen charge valve 09 is closed after 0.1MPa, repeatedly vacuumize-pressure is inflated with nitrogen in maintenance batch mixing reactor 21 afterwards three times
0.01MPa, the feeding line 121 between inlet control valve 16 and inlet control valve 23 is set to be filled with nitrogen by identical operation.
Step 5, inlet control valve 22 and inlet control valve 15, inlet control valve 23 and inlet control valve 16 are opened, is made solid
Chromium acetylacetonate and PNP in body feed pot (11,12) are entered in batch mixing reactor 21, close inlet control valve (22,23).
Step 6, the valve 19 on solvent Feed lines 14 is opened, toluene 2L is added by measuring pump 20, closes valve 19
And measuring pump 20, agitating device is started, valve 17 and measuring pump 18 on MAO Feed lines 13 is opened, adds 1.0mol/L's
MAO toluene solution 100L, valve 17 and measuring pump 18 are closed, stirred 10 minutes.
Valve 26 on step 7 opening side position feed pipe 24, the nitrogen charge valve 06 in nitrogen tube 02 is opened, utilizes nitrogen
Catalyst is slowly added into batch mixing reactor 21, nitrogen charge valve 06 and valve 26 are closed after addition, is completed once
Catalyst batch mixing and fill process.
Claims (9)
- A kind of 1. batch mixing and feed system for ethylene tetramerization catalyst system and catalyzing, it is characterised in that including,One batch mixing reactor；One agitating device, it is arranged in the batch mixing reactor；One premixing raw material feeder, is connected with batch mixing reactor top, for will configure ethylene tetramerization reaction solution not Same raw material is added in batch mixing reactor；An at least vacuum nitrogen filling device of air, connected respectively with the batch mixing reactor, the premixing raw material feeder connects Connect, the vacuum nitrogen filling device of air is provided with vacuum extraction valve, nitrogen charge valve, is taken out described in when opening the vacuum extraction valve true Empty nitrogen charging device takes the air in batch mixing reactor, in premixing raw material feeder away, closes vacuum extraction valve and beats again Nitrogen charge valve is opened, is filled with nitrogen toward the batch mixing reactor, described be pre-mixed in raw material feeder, repetition is vacuumized, filled Nitrogen is repeatedly until the pressure of the batch mixing reactor maintains negative pressure state, and the pipeline of the premixing raw material feeder It is interior to be full of nitrogen；Side position feed pipe, it is connected to the batch mixing reactor side and gos deep into the batch mixing reactor bottom, to catalyst Charging, catalyst are injected in batch mixing reactor in the presence of the negative pressure of the batch mixing reactor.
- 2. it is used for the batch mixing and feed system of ethylene tetramerization catalyst system and catalyzing, the vacuum nitrogen gas as claimed in claim 1 Device includes a vacuum plant and a nitrogen device, and the vacuum plant is connected by vacuum tube with the batch mixing reactor, institute Premixing raw material feeder connection is stated, the nitrogen device is connected by nitrogen tube with the batch mixing reactor, the premix Close raw material feeder connection.
- 3. it is used for the batch mixing and feed system of ethylene tetramerization catalyst system and catalyzing as claimed in claim 2, it is characterised in that described pre- Mixed material feeding device includes at least two Feed lines, two solid feed pots, and the two solids feed pot enters by one respectively Expects pipe line is connected with the batch mixing reactor, and two Feed lines directly connect with the batch mixing reactor.
- 4. it is used for the batch mixing and feed system of ethylene tetramerization catalyst system and catalyzing as claimed in claim 3, it is characterised in that described true Blank pipe, the nitrogen tube are drawn from the feeding line respectively, and the vacuum tube is provided with the vacuum extraction valve, the nitrogen Pipe is provided with nitrogen charge valve, and the both ends of the feeding line are provided with inlet control valve.
- 5. it is used for the batch mixing and feed system of ethylene tetramerization catalyst system and catalyzing as claimed in claim 1, it is characterised in that the side Position feed pipe is a door type pipe, and provided with a charging aperture and a discharging opening, the discharging opening gos deep into the batch mixing reactor bottom.
- 6. as claimed in claim 5 be used for ethylene tetramerization catalyst system and catalyzing batch mixing and feed system, it is characterised in that it is described enter Material mouth is zigzag port, interior to be provided with gear piece, and catalyst is rotated along side position feed pipe by the gear piece and injects the batch mixing Reactor bottom.
- 7. it is used for the batch mixing and feed system of ethylene tetramerization catalyst system and catalyzing as claimed in claim 3, it is characterised in that described two It is equipped with measuring pump and control valve on Feed lines, two Feed lines are respectively adding MAO and solvent.
- 8. the batch mixing and feed system according to claim 1 for ethylene tetramerization catalyst system and catalyzing, it is characterised in that described Batch mixing reactor is provided with pressure vacuum gauge.
- 9. the batch mixing and feed system according to claim 5 for ethylene tetramerization catalyst system and catalyzing, it is characterised in that described Side position feed pipe is provided with valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201720804781.9U CN207085901U (en) | 2017-07-05 | 2017-07-05 | One kind is used for ethylene tetramerization catalyst system and catalyzing batch mixing and feed system |
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| CN201720804781.9U CN207085901U (en) | 2017-07-05 | 2017-07-05 | One kind is used for ethylene tetramerization catalyst system and catalyzing batch mixing and feed system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114259971A (en) * | 2021-12-03 | 2022-04-01 | 哈尔滨工程大学 | Device for treating cation exchange resin through carbonate oxidation and application thereof |
-
2017
- 2017-07-05 CN CN201720804781.9U patent/CN207085901U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114259971A (en) * | 2021-12-03 | 2022-04-01 | 哈尔滨工程大学 | Device for treating cation exchange resin through carbonate oxidation and application thereof |
| CN114259971B (en) * | 2021-12-03 | 2023-11-28 | 哈尔滨工程大学 | Device for oxidizing and treating cation exchange resin by carbonate and application thereof |
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