CN102399332A - Propylene polymerization production technology by loop reactor batch liquid bulk method - Google Patents
Propylene polymerization production technology by loop reactor batch liquid bulk method Download PDFInfo
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Abstract
The invention relates to a propylene polymerization production technology by a loop reactor batch liquid bulk method. With combination of a loop reactor and a batch liquid bulk reaction vessel, materials cycle between the loop reactor and the batch liquid bulk reaction vessel by an axial-flow pump of the loop reactor or with the addition of a pump, thus solving poor heat removing performance of the batch liquid bulk reaction vessel, controlling the pressure of the batch liquid bulk reaction vessel to be higher than the saturation pressure of the materials in the loop reactor, maintaining completely full state of the loop reactor and stabilizing the reaction pressure. In comparison with present production technologies, according to the invention, a reactor vacuum tank is canceled, the production capacity of devices is expanded, the utilization rate of a catalyst is raised, and a plurality of functions of production equipment is fully performed. The improved process is simple and easy to operate and the construction cycle is short; therefore, the production technology provided by the invention has a great economic benefit.
Description
Technical field
The present invention proposes a kind of annular-pipe reactor liquid phase noumenal method and produce polyacrylic process modification method; Adopt annular-pipe reactor and the interconnected array mode of liquid phase body still, reach the purpose of expansion instrument throughput, raising catalyst utilization, increase product grade.The invention belongs to field of olefin polymerisation.
Technical background
Produce in the polyacrylic polyreaction workshop section at the annular-pipe reactor liquid phase noumenal method, the propylene liquid monomer that transports from propylene tank gets into pre-polymerization reactor, annular-pipe reactor respectively.Catalyst system gets into pre-polymerization reactor, respond activity and get into annular-pipe reactor of the material web after the prepolymerization; At last, the product material is from the continuous discharging of annular-pipe reactor, and the degassing of entering polymkeric substance and propylene recycle section.
In this technology, use the Ziegler-Natta catalyst system usually; This catalyzer is by a large amount of open and widely-used; The catalyzer that preferably has high stereoselective, " Ziegler-Natta catalyst of high stereoselective " described herein are meant and can prepare isotactic index greater than 95% alfon.This type of catalyzer contains (1) active solid catalyst component usually, is preferably titaniferous solid catalyst active ingredient; (2) organo-aluminium compound cocatalyst component; (3) and randomly add the external electron donor component.
The specific examples that operational this type contains the active solid catalyst component is disclosed in Chinese patent CN85100997, CN98126383.6, CN98111780.5, CN98126385.2, CN93102795.0, CN00109216.2, CN99125566.6, CN99125567.4, CN02100900.7.
Organo-aluminium compound preferred alkyl aluminum compound as the catalyzer cocatalyst component more preferably comprises trialkylaluminium, as: triethyl aluminum, triisobutyl aluminium, three n-butylaluminum etc.
Can be silicoorganic compound, diether, diol ester etc. as the external electron donor of catalyst component randomly.
In this polymerization process, annular-pipe reactor is full still operation, and in order to reduce the pressure surge of annular-pipe reactor, existing technology has connected reactor drum buffer tank (or being called the reactor drum surge tank) on annular-pipe reactor, shown in frame of broken lines in the accompanying drawing 1.With the propylene feed at steam heating reactor drum buffer tank top, make the pressure of reactor drum buffer tank internal pressure and annular-pipe reactor be higher than the saturation pressure 0.3～0.5MPa of material in the endless tube.If the import and export material of annular-pipe reactor is uneven or pressure surge, disappearance perhaps exceeds the quata in the additional perhaps buffering ring pipe reactor of the reactor drum buffer tank meeting very first time material and pressure, thus the full still of assurance annular-pipe reactor is operated and pressure-stabilisation.
The effect ten minutes of reactor drum buffer tank is important in the existing technology, but its huge volume had not both been participated in polyreaction, reduced the potential security of device again.
Carrying out polyreaction if the reactor drum buffer tank is transformed into the series connection of liquid phase bulk reaction still, is feasible technically.But because bulk propylene polymerization is a strong exothermal reaction, removing of liquid phase bulk reaction still is hot relatively poor.The liquid phase reaction still is removed heat problem when volume ratio is less not serious, and it is hot not enough often under the bigger situation of volume, only to adopt jacket water (J.W.) to remove, and must adopt inner cool tube, gas phase outer circulation, liquid phase outer circulation etc. to strengthen and remove heat.And adopt these measures must increase investment.Maximize at poly-unit, liquid phase bulk reaction still is removed under the big situation of heat, and the measure that heat is removed in these reinforcements also often can not meet the requirements of removes heat.
Patent CN1926159A has described a kind of technology of interconnected annular-pipe reactor.This technical description is a kind of in the poly technology of endless tube, through this technology material is circulated between two endless tubes, produces the Vilaterm of bimodal or wide molecular weight distribution.This technology has adopted recycle ratio between the endless tube that in reaction time, is lower than twice for reducing the mixing of liquid phase component between two endless tubes.Therefore round-robin material removing heat affecting and almost can ignore between two endless tubes to two endless tubes.On this endless tube device, still must use bulky reactor drum buffer tank.
At present, domestic have a large amount of employing monocycle pipe polypropylene plants to need capacity expansion revamping, and the quantity that merely increases annular-pipe reactor obviously can be appended huge investment to improve throughput.The polypropylene product of wide molecular weight distribution is because its good processing properties and mechanical property are that market is accepted extensively.But monocycle pipe polypropylene plant product is more single, is difficult to produce the polypropylene product with wide molecular weight distribution.
Summary of the invention
The present invention adopts annular-pipe reactor and the interconnected mode of liquid phase body still, not only increases considerably the throughput of poly-unit, has improved the utilization ratio of catalyzer; And saved reactor drum buffer tank and relevant pipeline thereof, equipment, the facility investment that existing apparatus is transformed is few.What have more positive effect is, for the device of monocycle pipe, has increased the polypropylene product that the body still can the production wide molecular weight distribution.
A kind of annular-pipe reactor liquid phase noumenal method of the present invention propylene polymerization production technique, this process using annular-pipe reactor and the interconnected mode of liquid phase bulk reaction still, catalyst system gets into annular-pipe reactor after through pre-polymerization reactor; Rely on the propeller pump of annular-pipe reactor or on annular-pipe reactor and pipeline that liquid phase bulk reaction still is connected pump of increase, material is circulated between annular-pipe reactor and liquid phase bulk reaction still; Reactor drum buffer tank in the existing production technique of cancellation; The saturation pressure that the reaction pressure of control liquid phase bulk reaction still is higher than the annular-pipe reactor material is 0.1MPa at least, guarantees that annular-pipe reactor is in full state, makes the running of endless tube propeller pump stable; Material after the polymerization comprises that Vestolen PP 7052 and propylene liquid monomer get into the polymkeric substance degassing and propylene recycle section.
The present invention produces in the polyacrylic technology about the unitary improvement of polymerization technology to the annular-pipe reactor liquid phase noumenal method.This technique unit comprises equipment such as prepolymerization reaction kettle, annular-pipe reactor, liquid phase bulk reaction still.The propylene liquid monomer that transports from propylene tank gets into pre-polymerization reactor, annular-pipe reactor and liquid phase bulk reaction still respectively.Catalyst system gets into annular-pipe reactor after through pre-polymerization reactor; The material of being discharged by annular-pipe reactor gets into the polymerization of liquid phase bulk reaction still; A part of material under the effect of propeller pump in the liquid phase bulk reaction still loops back annular-pipe reactor; Reactor drum buffer tank in the existing production technique of cancellation; Material after the polymerization comprises that Vestolen PP 7052 and propylene liquid monomer get into the polymkeric substance degassing and propylene recycle section by liquid phase bulk reaction still.
If the uneven perhaps pressure surge of the import and export material of annular-pipe reactor, liquid phase bulk reaction still can in time replenish or the interior disappearance of buffering ring pipe reactor perhaps exceeds the quata material and pressure.This improves one's methods and not only makes liquid phase bulk reaction still participate in polyreaction; And the full still that has guaranteed annular-pipe reactor is operated and pressure-stabilisation; Can replace reactor drum buffer tank device in the existing technology fully, simplify technical process, give full play to the multinomial function of liquid phase bulk reaction still.
In the interconnected Vestolen PP 7052 production technique of described annular-pipe reactor and liquid phase bulk reaction still, the prepolymer of catalyzer can get into annular-pipe reactor, also can get into liquid phase body still; The preferred annular-pipe reactor that gets into.Material after the polymerization comprises that Vestolen PP 7052 and propylene liquid monomer can get into the polymkeric substance degassing and propylene recycle section by liquid phase bulk reaction still, also can get into the polymkeric substance degassing and propylene recycle section from annular-pipe reactor; Preferably get into the polymkeric substance degassing and propylene recycle section from liquid phase bulk reaction still.
In the interconnected Vestolen PP 7052 production technique of described annular-pipe reactor and liquid phase bulk reaction still; Rely on the endless tube propeller pump that material is circulated between endless tube and reaction kettle; The temperature of control liquid phase bulk reaction still is higher than annular-pipe reactor, withdraws from most of heat of polymerization that liquid phase bulk reaction still produces through recycle stock; Liquid phase bulk reaction still through with endless tube round-robin mass flow and jacket water (J.W.) controlled temperature.
In the interconnected Vestolen PP 7052 production technique of described annular-pipe reactor and liquid phase bulk reaction still; Also can material be circulated between endless tube and reaction kettle without the endless tube propeller pump; But on annular-pipe reactor and pipeline that liquid phase bulk reaction still is connected, increase a pump, use this pump that material is circulated between annular-pipe reactor and liquid phase bulk reaction still.The temperature of control liquid phase bulk reaction still is higher than annular-pipe reactor, withdraws from most of heat of polymerization that liquid phase bulk reaction still produces through recycle stock; Liquid phase bulk reaction still through with endless tube round-robin mass flow and jacket water (J.W.) controlled temperature.
In the interconnected Vestolen PP 7052 production technique of above-described annular-pipe reactor and liquid phase body still; Temperature through control liquid phase bulk reaction still is come control pressure; Make the reaction pressure of liquid phase bulk reaction still be higher than the saturation pressure 0.1～1.0MPa of annular-pipe reactor material, preferred 0.3～0.6MPa all the time.This need make the temperature of liquid phase bulk reaction still higher 2～10 ℃ than the temperature of annular-pipe reactor usually.Can improve the polymerization velocity of liquid phase bulk reaction still in this case, improve activity of such catalysts.
The present invention has made full use of endless tube through annular-pipe reactor and the interconnected mode of liquid phase body still and has removed the high and tank reactor gas-phase space equilibrium pressure advantage of thermo-efficiency.Improve the utilization ratio of catalyzer through the residence time that has prolonged reactant, improved the throughput of device, alleviated the deficiency that simple annular-pipe reactor exists to a certain extent.
According to the present invention the monocycle pipe unit is increased an interconnected liquid phase bulk reaction still, polypropylene product that just can the production wide molecular weight distribution.High hydrogen regulation performance in catalyzer of the present invention has than annular-pipe reactor under the higher temperature of reaction of liquid phase bulk reaction still usually; Though therefore contain close density of hydrogen, in liquid phase body still reactor drum, the Vestolen PP 7052 of producing had lower molecular weight at annular-pipe reactor and liquid phase bulk reaction still internal reaction device.Thereby can obtain the polypropylene product of wide molecular weight distribution.Because the circulation of polymkeric substance in annular-pipe reactor and liquid phase bulk reaction still, the broad molecular weight distribution polypropylene through explained hereafter of the present invention has the uniform especially characteristics of quality.
In the interconnected Vestolen PP 7052 production technique of described annular-pipe reactor and liquid phase bulk reaction still, annular-pipe reactor can be single loop reactors or multiple loop reactors series connection.If multiple loop reactors series connection; Liquid phase bulk reaction still can be interconnected on any annular-pipe reactor; But preferably be interconnected on the annular-pipe reactor of final discharging; The higher temperature of reaction of liquid phase bulk reaction still helps improving catalyst activity, improves catalyzer and prolongs and the situation of decay of activity with the residence time.
In the interconnected Vestolen PP 7052 production technique of annular-pipe reactor of the present invention and liquid phase body still; After annular-pipe reactor and the interconnected system of liquid phase bulk reaction still; Can continue series connection liquid phase bulk reaction still according to usual method, perhaps make the Gas-phase reactor of connecting after the slurries flash separation.
Above-described annular-pipe reactor liquid phase noumenal method is produced in the polyacrylic process modification method, and the polymerizing condition of annular-pipe reactor is: 50～130 ℃ of polymerization temperatures, polymerization pressure are 2.5～5.5Mpa; The polymerizing condition of liquid phase bulk reaction still is: 52～135 ℃ of polymerization temperatures, polymerization pressure are 2.5～5.5Mpa.
Adopt above-mentioned improving one's methods, not only enlarged the throughput of device, improved the utilization ratio of catalyzer, and given full play to the multinomial function of production unit, reduced facility investment.Improve this improvement and make the polypropylene product that monocycle pipe polypropylene plant can the production wide molecular weight distribution.The enforcement of improving one's methods is simple, is a kind of simple and practical improving one's methods.
Description of drawings
Accompanying drawing 1: single loop reactors and the interconnected technical process of liquid phase bulk reaction still, 1 is pre-polymerization reactor; 2 is the reactor drum buffer tank in original production technique; 3 is annular-pipe reactor; 4 is liquid phase bulk reaction still;
Accompanying drawing 2: double loop reactor and the interconnected technical process of liquid phase bulk reaction still, 1 is pre-polymerization reactor; 2 is first annular-pipe reactor; 3 is the reactor drum buffer tank in original production technique; 4 is second annular-pipe reactor; 5 is liquid phase bulk reaction still;
Accompanying drawing be annular-pipe reactor and liquid phase bulk reaction still interconnected the polymerization technique schematic flow sheet.
The present invention produces in the polyacrylic polymerization technique improvement about polyreaction workshop section to the annular-pipe reactor liquid phase noumenal method, wherein accompanying drawing 1 be single loop reactors and liquid phase bulk reaction still interconnected technical process; Accompanying drawing 2 be double loop reactor and liquid phase bulk reaction still interconnected technical process.
The reactor drum of liquid phase bulk reaction still 4 for increasing newly cancelled the reactor drum buffer tank 2 in original production technique.In former polymerization technique technology; Reaction mass through behind the annular-pipe reactor 3 just discharging got into next workshop section; The present technique invention proposes liquid phase bulk reaction still 4 is interconnected on the annular-pipe reactor 3; Throughput that can expansion instrument, thus the residence time that prolongs reactant improve activity of such catalysts.
Complete full state and minimizing pressure surge for retaining ring pipe reactor 3.Former polymerization technique is that reactor drum buffer tank 2 is connected on the annular-pipe reactor 3, and shown in frame of broken lines in the accompanying drawing 1: propylene monomer is pressed in the jar from reactor drum buffer tank 2 tops through short steam heating back, and makes pressure for it.All the time the saturation pressure 0.3～0.5MPa that is higher than annular-pipe reactor 3 materials with the pressure that guarantees reactor drum buffer tank 2.
The present invention is interconnected at liquid phase bulk reaction still 4 on the annular-pipe reactor 3; Utilize with endless tube round-robin mass flow and add the temperature of reaction that cover recirculated water is controlled liquid phase bulk reaction still 4, make the reaction pressure of liquid phase bulk reaction still 4 be higher than the reaction pressure 0.3～0.5MPa of annular-pipe reactor 3 all the time.
The present invention utilizes annular-pipe reactor 3 to solve the heat problem of removing of liquid phase bulk reaction still 4.The present invention makes liquid phase bulk reaction still 4 when participating in polyreaction, can play the effect of stopping reaction pressure again, has replaced the reactor drum buffer tank device 2 in the former polymerization technique fully.
With YO is that 70,000 tons/year monocycle pipe polypropylene plant is an example; Adopt improvement technology like accompanying drawing 1 scheme; Use and the sizable liquid phase bulk reaction of reactor drum buffer tank still, the throughput of device can increase by 20～50%, and activity of such catalysts also can improve 20～50%.Transform the polypropylene product that the back device can the production wide molecular weight distribution.
With YO is that 100,000 tons/year dicyclo pipe polypropylene plant is an example; Adopt improvement technology like accompanying drawing 2 schemes; Use and the sizable liquid phase bulk reaction of reactor drum buffer tank still, the throughput of device can increase by 20～30%, and activity of such catalysts also can improve 20～30%.
Claims (7)
1. an annular-pipe reactor liquid phase noumenal method propylene polymerization production technique is characterized in that, this process using annular-pipe reactor and the interconnected mode of liquid phase bulk reaction still, and catalyst system gets into annular-pipe reactor after through pre-polymerization reactor; Rely on the propeller pump of annular-pipe reactor or on annular-pipe reactor and pipeline that liquid phase bulk reaction still is connected pump of increase, material is circulated between annular-pipe reactor and liquid phase bulk reaction still; Reactor drum buffer tank in the existing production technique of cancellation; The saturation pressure that the reaction pressure of control liquid phase bulk reaction still is higher than the annular-pipe reactor material is 0.1MPa at least, guarantees that annular-pipe reactor is in full state, makes the running of endless tube propeller pump stable; Material after the polymerization comprises that Vestolen PP 7052 and propylene liquid monomer get into the polymkeric substance degassing and propylene recycle section.
2. annular-pipe reactor liquid phase noumenal method propylene polymerization production technique according to claim 1 is characterized in that, the round-robin material between annular-pipe reactor and liquid phase bulk reaction still at reaction time internal recycle number of times greater than twice.
3. annular-pipe reactor liquid phase noumenal method propylene polymerization production technique according to claim 1 is characterized in that annular-pipe reactor randomly is single loop reactors or multiple loop reactors.
4. annular-pipe reactor liquid phase noumenal method propylene polymerization production technique according to claim 1 is characterized in that, after liquid phase body still, and one or more liquid phase body stills of randomly connecting, or one or more gas-phase polymerization reactors of randomly connecting.
5. annular-pipe reactor liquid phase noumenal method propylene polymerization production technique according to claim 1, it is characterized in that the polymerizing condition of annular-pipe reactor is: 50～130 ℃ of polymerization temperatures, polymerization pressure are 2.5～5.0Mpa; The polymerizing condition of liquid phase bulk reaction still is: 52～135 ℃ of polymerization temperatures, polymerization pressure are 2.8～5.5Mpa.
6. annular-pipe reactor liquid phase noumenal method propylene polymerization production technique according to claim 1 is characterized in that the reaction pressure of liquid phase bulk reaction still is higher than the saturation pressure 0.1～1.0MPa of annular-pipe reactor material all the time.
7. annular-pipe reactor liquid phase noumenal method propylene polymerization production technique according to claim 1 is characterized in that the reaction pressure of liquid phase bulk reaction still is higher than the saturation pressure 0.3～0.6MPa of annular-pipe reactor material all the time.
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Cited By (7)
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| CN103788272A (en) * | 2012-10-31 | 2014-05-14 | 中国石油化工股份有限公司 | Hydrogenation method of polymer containing olefin unsaturated bonds |
| CN104383862A (en) * | 2014-11-22 | 2015-03-04 | 山东阳谷华泰化工股份有限公司 | Production equipment for synthesizing rubber accelerator NS and application |
| CN107537408A (en) * | 2016-06-23 | 2018-01-05 | 中国石油化工股份有限公司 | A kind of method of catalyst pre-contact device and catalyst pre-contact for alkene continuous polymerization |
| CN109456428A (en) * | 2017-09-06 | 2019-03-12 | 中国石油化工股份有限公司 | A kind of liquid phase autoclave method polypropylene manufacturing process and its application |
| CN109456430A (en) * | 2017-09-06 | 2019-03-12 | 中国石油化工股份有限公司 | A kind of liquid phase method polypropylene manufacturing process and its application |
| CN109456427A (en) * | 2017-09-06 | 2019-03-12 | 中国石油化工股份有限公司 | A kind of liquid phase endless tube method polypropylene manufacturing process and its application |
| CN114797989A (en) * | 2022-05-30 | 2022-07-29 | 卫星化学股份有限公司 | Supported catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109456427A (en) * | 2017-09-06 | 2019-03-12 | 中国石油化工股份有限公司 | A kind of liquid phase endless tube method polypropylene manufacturing process and its application |
| CN109456427B (en) * | 2017-09-06 | 2021-05-11 | 中国石油化工股份有限公司 | Liquid phase ring pipe method polypropylene production method and application thereof |
| CN109456430B (en) * | 2017-09-06 | 2021-05-11 | 中国石油化工股份有限公司 | Liquid phase method polypropylene production method and application thereof |
| CN109456428B (en) * | 2017-09-06 | 2021-05-11 | 中国石油化工股份有限公司 | Liquid-phase kettle type polypropylene production method and application thereof |
| CN114797989A (en) * | 2022-05-30 | 2022-07-29 | 卫星化学股份有限公司 | Supported catalyst and preparation method and application thereof |
| CN114797989B (en) * | 2022-05-30 | 2024-02-23 | 卫星化学股份有限公司 | Supported catalyst and preparation method and application thereof |
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