CN112500509A - System and process for strengthening ethylene polymerization - Google Patents

System and process for strengthening ethylene polymerization Download PDF

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Publication number
CN112500509A
CN112500509A CN201910867780.2A CN201910867780A CN112500509A CN 112500509 A CN112500509 A CN 112500509A CN 201910867780 A CN201910867780 A CN 201910867780A CN 112500509 A CN112500509 A CN 112500509A
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ethylene
catalyst
gas
feeding
micro
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CN112500509B (en
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张志炳
李磊
周政
张锋
孟为民
王宝荣
杨高东
罗华勋
杨国强
田洪舟
曹宇
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Nanjing Institute of Microinterface Technology Co Ltd
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Nanjing Institute of Microinterface Technology Co Ltd
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Priority to PCT/CN2019/120188 priority patent/WO2021047049A1/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F10/02—Ethene
    • 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
    • B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • 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
    • B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B01J10/002—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor carried out in foam, aerosol or bubbles
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/14—Production of inert gas mixtures; Use of inert gases in general
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/02—Ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
    • C08F218/02—Esters of monocarboxylic acids
    • C08F218/04—Vinyl esters
    • C08F218/08—Vinyl acetate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • 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
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Abstract

The present invention relates to a system and process for enhancing ethylene polymerization, comprising: a feed unit; a reaction unit connected with the feeding unit; a micro-interface generator disposed within the feed unit; and the discharging unit is connected with the reaction unit. According to the invention, ethylene is crushed to form micron-scale bubbles, the micron-scale bubbles of the ethylene are mixed with a solvent to form a gas-liquid emulsion, meanwhile, the thickness of a liquid film is reduced, and the mass transfer resistance is reduced, so that the micron-scale bubbles of the ethylene are formed by crushing an initiator, and the micron-scale bubbles of the initiator are mixed with the gas-liquid emulsion to form a mixed material, thereby achieving the effect of strengthening mass transfer within a lower preset operating condition range; meanwhile, each micron-sized bubble can be fully mixed with a solvent to form a gas-liquid emulsion, and the gas-liquid two phases are fully mixed, so that ethylene and an initiator in the system can be fully contacted with the solvent alkene, and the polymerization efficiency of the system is further improved.

Description

System and process for strengthening ethylene polymerization
Technical Field
The invention relates to the technical field of polymer preparation, in particular to a system and a process for strengthening ethylene polymerization.
Background
Polyethylene (PE) is the most commonly used plastic polymer in the world, with annual rates of consumption exceeding 500 billion pounds per year. More than 70% of Porex products use polyethylene. In units of the repeating linear molecular structure-CH 2-CH2-, PE is a semi-crystalline polymer whose toughness is enhanced prior to tensile failure. In general, PE is a strong, lightweight thermoplastic material possessing excellent chemical resistance. The glass fiber has excellent corrosion resistance and electrical insulation (especially high-frequency insulation), can be chloridized and modified by irradiation, and can be reinforced by glass fiber. The low-pressure polyethylene has higher melting point, rigidity, hardness and strength, small water absorption, and good electrical property and radiation resistance; the high-pressure polyethylene has good flexibility, elongation, impact strength and permeability, and the ultra-high molecular weight polyethylene has high impact strength, fatigue resistance and wear resistance. The low-pressure polyethylene is suitable for manufacturing corrosion-resistant parts and insulating parts; the high-pressure polyethylene is suitable for manufacturing films and the like; the ultra-high molecular weight polyethylene is suitable for manufacturing shock-absorbing, wear-resisting and transmission parts.
Chinese patent publication No.: CN101754987A discloses a method for preparing polyethylene and the prepared polyethylene, comprising the following steps: a process for producing a polyethylene or polypropylene polymer or copolymer thereof comprising contacting a medium comprising monomer with polymerization catalyst particles in at least one high shear mixing device to form a dispersion. The monomer is selected from the group consisting of ethylene, propylene, and combinations thereof. It can be seen that the method and system have the following problems:
first, the system crushes the catalyst in a stirring manner, although the contact area between the catalyst and the material is increased, the ethylene gas still has large bubbles, and the ethylene cannot be in full contact with the catalyst, so that the reaction of the system is not uniform, and the polymerization efficiency of the system is low.
Secondly, the system mixes the raw materials of each component together for stirring, and a plurality of raw materials cannot be fully mixed in a mixing device.
Thirdly, the tail gas after reaction in the system is directly discharged, so that the utilization rate of the ethylene raw material is low, and the operation cost of the system is increased.
Disclosure of Invention
Therefore, the invention provides a system and a process for strengthening ethylene polymerization, which are used for overcoming the problem of low polymerization efficiency caused by insufficient mixing of materials in the prior art.
In one aspect, the present invention provides a system for enhancing ethylene polymerization, comprising:
a feeding unit for separately feeding a raw material and a liquid-phase catalyst;
the reaction unit is connected with the feeding unit and is used for receiving the mixed solution of the raw materials and the catalyst output by the feeding unit so as to enable the ethylene in the mixed solution to generate a polymerization reaction in the reaction unit;
the micro-interface generator is arranged in the feeding unit, converts the pressure energy of gas and/or the kinetic energy of liquid into the surface energy of bubbles and transmits the surface energy to the gas-phase raw material, so that the gas-phase raw material is crushed into micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm to improve the mass transfer area of a phase boundary, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the materials are mixed to form a gas-liquid emulsion after being crushed so as to strengthen the mass transfer efficiency and the reaction efficiency between the phase boundaries within the range of preset operating conditions;
and the discharging unit is connected with the reaction unit and used for receiving the polymerized material output by the reaction unit and carrying out post-treatment on the polymerized material.
Further, the feed unit comprises:
the raw material feeding pipeline is connected with the micro-interface generator and is used for conveying the gas-phase raw material to the micro-interface generator so that the micro-interface generator breaks the raw material into micron-sized bubbles;
a catalyst feed conduit connected to the reaction unit for delivering catalyst to the interior of the reaction unit;
a viscosity reducing agent feed conduit connected to the reaction unit for delivering a viscosity reducing agent to the interior of the reaction unit.
Further, the raw material feed conduit comprises:
a feed tube to deliver a gas phase feedstock to the gas phase feed conduit;
the compressor is connected with the feeding pipe and used for providing power for conveying materials;
the cooler is connected with the compressor and used for cooling the material output by the compressor;
a solvent feed line connected to the feed line and disposed downstream of the comonomer feed line for delivering solvent to the interior of the gas phase feed line;
a comonomer feed connected to said feed and disposed at the outlet of said cooler for delivering comonomer to the interior of said gas phase feed conduit;
an initiator feed line connected to the feed line and disposed downstream of the solvent feed line for delivering initiator to the interior of the gas phase feed conduit.
Further, the micro-interface generator includes:
the first micro-interface generator is arranged at a confluence position between the feeding pipe and the solvent feeding pipe and is used for crushing ethylene to form micron-scale micro-scale bubbles so as to be mixed with a solvent to form a gas-liquid emulsion;
and the second micro-interface generator is arranged at the confluence position of the feeding pipe and the initiator feeding pipe and is used for crushing the initiator to form micron-scale bubbles and mixing the micron-scale bubbles with the gas-liquid emulsion containing the comonomer output by the first micro-interface generator to form a mixed material.
Further, the catalyst feed conduit comprises:
a catalyst feeder for storing and transporting a liquid phase catalyst;
and the catalyst feeding valve is arranged at the outlet of the catalyst feeder and is used for controlling the flow of the catalyst.
Further, the reaction unit is a reactor for providing a reaction space for the micro bubbles, and includes:
the material feeding hole is formed in the bottom of the reactor and connected with the material feeding pipeline, so that the material feeding pipeline outputs materials to the inside of the reactor;
the catalyst feeding hole is formed in the side wall of the reactor and is connected with the catalyst feeding pipeline, so that the catalyst feeding pipeline outputs the catalyst to the inside of the reactor;
the viscosity reducing agent feeding port is formed in the side wall of the reactor and is connected with the viscosity reducing agent feeding pipeline, so that the viscosity reducing agent feeding pipeline outputs the viscosity reducing agent to the inside of the reactor;
the material outlet is formed in the side wall of the lower part of the reactor, is connected with the discharging unit and is used for outputting the reacted mixture to the discharging unit;
and the tail gas outlet is arranged at the top of the reactor and used for discharging tail gas generated after reaction out of the system.
Furthermore, a return pipe is arranged between the reaction unit and the material feeding pipeline and used for returning unreacted ethylene in the reaction unit to the material feeding unit so as to reuse the ethylene.
Further, the discharging unit comprises:
the discharging intermediate tank is connected with the reaction unit and is used for carrying out gas-liquid separation on the materials output by the reaction unit;
and the product bin is arranged at the bottom of the discharging intermediate tank, is connected with the discharging intermediate tank and is used for receiving the liquid-phase material output by the discharging intermediate tank, drying the material and granulating the polyethylene in the material.
Further, tail gas output by the reaction unit and the discharge unit can enter a torch, and the torch can burn the tail gas to prevent the tail gas from polluting the environment.
In another aspect, the present invention provides a process for enhancing the polymerization of ethylene, comprising:
step 1: introducing nitrogen into the material feeding pipeline, allowing the nitrogen to flow through the system to replace moisture and oxygen in the system, and after replacement is finished, introducing ethylene into the material feeding pipeline to continue replacement;
step 2: after replacement, introducing a liquid-phase catalyst into the catalyst feeding pipeline, outputting the catalyst into the reaction unit through the catalyst feeding pipeline, introducing a viscosity reducer into the viscosity reducer feeding pipeline, outputting the viscosity reducer into the reaction unit through the viscosity reducer feeding pipeline, and introducing the viscosity reducer into the viscosity reducer feeding pipeline;
and step 3: the compressor starts to operate, so that ethylene flows in the feeding pipe along a specified direction, when the ethylene is conveyed, the solvent is conveyed through the solvent feeding pipe, the comonomer is conveyed through the comonomer feeding pipe, and the initiator is conveyed through the initiator feeding pipe;
and 4, step 4: the first micro-interface generator is used for crushing ethylene to form micron-scale micro-scale bubbles, mixing the micron-scale ethylene bubbles with a solvent to form a gas-liquid emulsion, and the second micro-interface generator is used for crushing an initiator to form micron-scale micro-scale bubbles, mixing the micron-scale bubbles with the gas-liquid emulsion containing a comonomer to form a mixed material and conveying the mixed material into the reaction unit;
and 5: ethylene in the mixed material is subjected to polymerization reaction under the action of a catalyst, a comonomer and an initiator to generate polyethylene, the mixed material containing the polyethylene is conveyed to the discharging unit, and the viscosity reducer can prevent the polyethylene from being solidified;
step 6: tail gas remaining in the polymerization process enters a torch through the tail gas outlet for treatment, unpolymerized ethylene flows back to the feeding pipe through the return pipe, and is conveyed to flow through the cooler through the compressor, and the cooler cools the ethylene to a specified temperature for reuse;
and 7: the polymerized material is conveyed to the discharging intermediate tank through the discharging port, the discharging intermediate tank can carry out gas-liquid separation on the polymerized material, the residual gas in the polymerized material is separated and conveyed to a torch for treatment, and the separated discharging intermediate tank conveys the material to the product bin;
and 8: and after separation, the discharging intermediate tank conveys the material to the product bin, the product bin dries the material to remove the viscosity reducer, the polyethylene is granulated after drying, and the polyethylene is output to the system after the granulation is finished.
Compared with the prior art, the invention has the beneficial effects that the micron-scale bubbles are formed by crushing ethylene, the micron-scale bubbles of ethylene are mixed with the solvent to form the gas-liquid emulsion, the micron-scale bubbles of ethylene are formed by crushing the initiator, the micron-scale bubbles of initiator are mixed with the gas-liquid emulsion to form the mixed material, and the phase interface area of gas and liquid phases is increased, the thickness of a liquid film is reduced, and the mass transfer resistance is reduced, so that the effect of strengthening mass transfer within a lower preset operation condition range is achieved; meanwhile, each micron-sized bubble can be fully mixed with a solvent to form a gas-liquid emulsion, and the gas-liquid two phases are fully mixed, so that ethylene and an initiator in the system can be ensured to be fully contacted with the solvent, and the polymerization efficiency of the system is further improved.
In addition, the range of the preset operation condition can be flexibly adjusted according to different product requirements or different catalysts, so that the full and effective reaction is further ensured, the reaction rate is further ensured, and the purpose of strengthening the reaction is achieved.
Furthermore, a plurality of confluence pipelines are respectively arranged in the raw material feeding pipelines, and the raw materials can be mixed with ethylene in sequence by adding the specified raw materials into the ethylene in sequence, so that the mixing efficiency among the raw materials in the feeding unit is improved.
Particularly, the first micro-interface generator is arranged at the confluence position of the feeding pipe and the solvent feeding pipe, and when the system operates, the first micro-interface generator can crush ethylene to form micron-sized bubbles so as to fully mix the ethylene and the solvent, thereby improving the mixing efficiency among materials in the system.
Particularly, the second micro-interface generator is arranged at the confluence position of the feeding pipe and the initiator feeding pipe, and when the system operates, the second micro-interface generator can crush the initiator to form micron-sized bubbles so as to fully mix the micron-sized bubbles of the initiator and the gas-liquid emulsion, so that the mixing efficiency of materials in the system is further improved.
Furthermore, a viscosity reducer feeding pipeline is further arranged in the feeding unit, and the viscosity reducer is conveyed into the material, so that the fluidity of the polyethylene after reaction can be kept, the phenomenon of solidification caused by excessive polymerization can be avoided, and the polymerization efficiency of the system is improved.
Furthermore, a catalyst feeding valve is arranged in the catalyst feeding pipe, and the polymerization rate of ethylene in the system is controlled by adjusting the flow of the catalyst, so that the reaction rate in the system is more stable, the product distribution is more uniform, and the polymerization efficiency of the system is further improved.
Furthermore, a return pipe is arranged between the reaction unit and the feeding pipe, when the system runs, unreacted ethylene can flow back to the feeding pipe through the return pipe, and the running cost of the system is saved by fully utilizing the ethylene.
Further, when the system is operated, tail gas generated in the reaction process can be conveyed to a torch for treatment, so that the tail gas is prevented from polluting the environment when being discharged out of the system.
Furthermore, the system respectively uses nitrogen and ethylene to replace moisture and oxygen in the system before operation, and the purity of a system product can be effectively improved by removing the moisture and the oxygen in the system, so that the polymerization efficiency of the system is further improved.
Drawings
FIG. 1 is a schematic view of the system for enhancing ethylene polymerization according to the present invention.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Fig. 1 is a schematic structural diagram of a system for enhancing ethylene polymerization according to the present invention, which includes a feeding unit 1, a reaction unit 2, a micro-interface generator 3, and a discharging unit 4. Wherein the feeding unit 1 is connected with the reaction unit 2 for conveying materials to the reaction unit 2. The micro-interface generator 3 is arranged in the feeding unit 1 and is used for crushing gas-phase materials to form micron-scale micro-bubbles. The discharging unit 4 is connected with the reaction unit 2 and is used for processing the polymerized material output by the reaction unit 2. When the system operates, the feeding unit 1 can convey the material to the reaction unit 2, in the conveying process, the micro-interface generator 3 can respectively crush the gas-phase material to form micron-sized bubbles with micron scale, the micron-sized bubbles and the liquid-phase material are mixed to form a gas-liquid emulsion, after the mixing is completed, the feeding unit 1 can convey the mixed material to the inside of the reaction unit 2 for reaction, the reaction unit 2 can carry out polymerization reaction on the material inside, the polymerized material is output to the discharging unit 4 after the reaction, and the discharging unit 4 carries out gas-liquid separation and drying treatment on the polymerized material and then carries out granulation to prepare polyethylene particles. It will be appreciated by those skilled in the art that the system can be used not only for the polymerization of ethylene, but also for the polymerization of polyvinyl chloride, propylene or other types of organic matter, provided that the system is capable of achieving its specified operating conditions.
With continued reference to FIG. 1, the feed unit 1 of the present invention includes a feedstock feed line 11, a catalyst feed line 12, and a viscosity depressant feed line 13. Wherein, the raw material feeding pipeline 11 is connected with the bottom of the reaction unit 2 and used for conveying mixed materials. The catalyst feed pipe 12 is connected to the side wall of the reaction unit 2 to convey a liquid phase catalyst. The viscosity reducing agent feed pipe 13 is connected to the side wall of the reaction unit 2 to feed the viscosity reducing agent. When the system is in operation, the raw material feeding pipeline 11 fully mixes gas-phase materials and liquid-phase materials, and conveys the mixed materials to the reaction unit 2, and the catalyst feeding pipeline 12 conveys liquid-phase catalyst into the reaction unit 2. The viscosity reducing agent feed pipe 13 feeds viscosity reducing agent to the reaction unit 2.
Specifically, the raw material feed line 11 includes a feed line 111, a compressor 112, a cooler 113, a solvent feed line 114, a comonomer feed line 115, and an initiator feed line 116. Wherein the compressor 112 is disposed on the feeding pipe 111 to provide power for the transportation of the material. The cooler 113 is disposed on the feeding pipe 111 and located downstream of the compressor 112, so as to cool the ethylene conveyed by the feeding pipe 111. The solvent feed pipe 114 is connected to the feed pipe 111 and located downstream of the cooler 113 to feed the solvent into the feed pipe 111. The comonomer 115 is connected to the feed line 111 and is located downstream of the solvent feed line 114 for feeding comonomer into feed line 111. The initiator feed line 116 is connected to the feed line 111 and is located downstream of the comonomer feed line 115 for feeding initiator thereto.
When raw materials charge-in pipeline 11 moves, ethylene can be carried to inlet pipe 111, compressor 112 can move and carry ethylene along the direction of designation in the inlet pipe 111, and ethylene is flowing through during cooler 113, cooler 113 can cool down ethylene, after the cooling, solvent inlet pipe 114 can carry the solvent to inlet pipe 111, solvent and ethylene intensive mixing form the gas-liquid emulsion, mixes the back, comonomer inlet pipe 115 carries comonomer to inlet pipe 111, and after comonomer and gas-liquid emulsion mixed, initiator inlet pipe 116 carried the initiator to inlet pipe 111 in, and the initiator mixes with the gas-liquid emulsion that mixes comonomer, forms the misce metal, inlet pipe 111 carries the misce metal to after the completion of mixing reaction unit 2.
Specifically, the catalyst feed line 12 includes a catalyst doser 121 and a catalyst feed valve 122. The catalyst feeder 121 is a tank for storing a liquid catalyst. The catalyst feeding valve 122 is a valve disposed at the outlet of the catalyst feeder 121 for controlling the flow rate of the catalyst outputted from the catalyst feeder 121. When the system is operated, the opening of the catalyst feed valve is adjusted to control the flow rate of the catalyst from the catalyst doser 121 to output a specified amount of catalyst to the reaction unit.
With continued reference to fig. 1, the reaction unit 2 of the present invention is a reaction tank connected to the feeding unit 1 for receiving the mixture, the catalyst and the viscosity reducer, respectively, and providing a reaction site for the polymerization of ethylene in the mixture. The bottom of the reaction unit 2 is provided with a material feeding hole, and the material feeding hole is connected with the raw material feeding pipeline 11 and used for receiving the mixed material output by the material feeding pipeline 11. The side wall of the reaction unit 2 is provided with a catalyst feed inlet, and the catalyst feed inlet is connected with the catalyst feed pipeline 12 and used for receiving the catalyst output by the catalyst feed pipeline. The side wall of the reaction unit 2 is also provided with a viscosity reducing agent feed inlet, and the viscosity reducing agent feed inlet is connected with the viscosity reducing agent feed pipeline 13 and used for receiving the viscosity reducing agent output by the viscosity reducing agent feed pipeline 13. The side wall of the reaction unit is also provided with a discharge port, and the discharge port is connected with the discharge unit 4 and used for outputting polymerized materials after polymerization to the discharge unit 4. The top of the reaction unit 2 is provided with a tail gas outlet for outputting tail gas generated in the reaction to a torch. The top of the reaction unit 2 is also provided with a return pipe, and the return pipe is connected with the feed pipe 111 and is used for returning unpolymerized ethylene in the reaction unit 2 to the feed pipe 111 so as to reuse the ethylene.
When the system is in operation, the reaction unit 2 receives a mixed material through the material feed inlet, receives a liquid-phase catalyst through the catalyst feed inlet, receives a viscosity reducer through the viscosity reducer feed inlet, mixes the three raw materials, controls the temperature and pressure in the reaction unit, enables ethylene in the material to undergo polymerization reaction, outputs the polymerized material after the reaction to the discharge unit 4 through the discharge outlet, outputs tail gas generated during the reaction to a torch through the tail gas outlet for treatment, and returns unpolymerized ethylene to the material pipe 111 through the return pipe during the reaction process, and is cooled by the cooler 113 for reuse. It is understood that the size and material of the reaction unit 2 are not particularly limited in this embodiment, as long as the reaction unit 2 can achieve the specified operation state.
Referring to fig. 1, the micro-interface generator 3 of the present invention includes a first micro-interface generator 31 and a second micro-interface generator 32. Wherein the first micro-interfacial surface generator 31 is disposed at the confluence of the feeding pipe 111 and the solvent feeding pipe 114, for breaking the ethylene to form micron-scale ethylene micro-bubbles. The second micro-interfacial surface generator 32 is disposed at the confluence of the feed pipe 111 and the initiator feed pipe 116 to break the initiator into micron-sized initiator micro-bubbles. When the raw material feeding pipeline 11 is used for conveying materials, the first micro-interface generator 31 may crush ethylene to form micron-scale ethylene micron-scale bubbles, and mix the ethylene micron-scale bubbles with a solvent to form a gas-liquid emulsion, the second micro-interface generator 32 may crush an initiator to form micron-scale initiator micron-scale bubbles, mix the initiator micron-scale bubbles with the gas-liquid emulsion mixed with a comonomer to form a mixed material, and output the mixed material to the reaction unit 2 for a polymerization reaction. It is understood that the micro-interface generator 3 of the present invention can also be used in other multi-phase reactions, such as multi-phase fluid formed by micro-scale particles, micro-nano-scale particles, micro-bubble fluid, micro-bubble fluid, micro-bubble fluid, micro-bubble fluid, micro-foam, micro-bubble fluid, micro-nano-emulsion fluid, micro-phase micro-structure fluid, micro-liquid-solid micro-mixed fluid, micro-liquid-solid micro-nano fluid, micro-liquid-solid emulsion fluid, micro-liquid, micro-bubble fluid, micro-dispersed fluid, two micro-mixed fluid, micro-turbulent fluid, micro-bubble fluid, micro-bubble fluid, micro-nano-bubble fluid, and micro-bubble fluid, by using micro-mixing, micro-fluidization, micro-bubble fermentation, micro-bubble bubbling, micro-bubble mass, Or multiphase fluid (micro interface fluid for short) formed by micro-nano-scale particles, thereby effectively increasing the phase boundary mass transfer area between the gas phase and/or the liquid phase and/or the solid phase in the reaction process.
With continued reference to fig. 1, the discharge unit 4 of the present invention includes a discharge tundish 41 and a product bin 42. The discharge intermediate tank 41 is connected with a discharge port in the reaction unit 2, and is used for receiving the polymerized material output by the reaction unit 2 and performing gas-liquid separation on the polymerized material. The product bin 42 is connected to the discharge intermediate tank 41, and is configured to dry and granulate the material output from the discharge intermediate tank 41 to generate a polyethylene product. When reaction unit 2 polymerization is accomplished the back, reaction unit 2 will polymerize the back material output extremely ejection of compact intermediate tank 41, ejection of compact intermediate tank 41 can carry out gas-liquid separation to the material after polymerization, will separate the back gas output to the torch in order to handle, and will separate the back liquid phase material and carry extremely product feed bin 42, after the material got into product feed bin 42, product feed bin 42 can dry the material, evaporates its inside viscosity reducer, makes the polyethylene in the material solidify to accomplish the preparation of polyethylene.
Specifically, ejection of compact intermediate tank 41 is a jar body, its with reaction unit 2 links to each other for carry out gas-liquid separation to the post polymerization material, ejection of compact intermediate tank 41 top is equipped with the gas vent, is used for exporting the gas after the separation to the torch, ejection of compact intermediate tank 41 bottom is equipped with the discharge gate, be used for with the post separation material output extremely product feed bin 42. When the polymerized material is conveyed to the inside of the discharge intermediate tank 41, the discharge intermediate tank 41 performs gas-liquid separation on the polymerized material, and outputs the separated gas to a torch through the exhaust port, and outputs the liquid-phase material to the product bin 42.
Specifically, the product bin 42 is a tank for drying the separated material and granulating the polyethylene. After the discharge intermediate tank 41 finishes gas-liquid separation, the separated material in the liquid phase is conveyed to the product bin 42, and the product bin 42 dries the separated material to remove viscosity reducer in the material, so that polyethylene in the material is solidified, and the polyethylene is granulated, thereby completing the preparation of the polyethylene.
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A process for enhancing the polymerization of ethylene comprising the steps of:
step 1: introducing nitrogen into the material feeding pipeline, allowing the nitrogen to flow through the system to replace moisture and oxygen in the system, and after replacement is finished, introducing ethylene into the material feeding pipeline to continue replacement;
step 2: after replacement, introducing a liquid-phase catalyst into the catalyst feeding pipeline, outputting the catalyst into the reaction unit through the catalyst feeding pipeline, introducing a viscosity reducer into the viscosity reducer feeding pipeline, outputting the viscosity reducer into the reaction unit through the viscosity reducer feeding pipeline, and introducing the viscosity reducer into the viscosity reducer feeding pipeline;
and step 3: the compressor starts to operate, so that ethylene flows in the feeding pipe along a specified direction, when the ethylene is conveyed, the solvent is conveyed through the solvent feeding pipe, the comonomer is conveyed through the comonomer feeding pipe, and the initiator is conveyed through the initiator feeding pipe;
and 4, step 4: the first micro-interface generator is used for crushing ethylene to form micron-scale micro-scale bubbles, mixing the micron-scale ethylene bubbles with a solvent to form a gas-liquid emulsion, and the second micro-interface generator is used for crushing an initiator to form micron-scale micro-scale bubbles, mixing the micron-scale bubbles with the gas-liquid emulsion containing a comonomer to form a mixed material and conveying the mixed material into the reaction unit;
and 5: ethylene in the mixed material is subjected to polymerization reaction under the action of a catalyst, a comonomer and an initiator to generate polyethylene, the mixed material containing the polyethylene is conveyed to the discharging unit, and the viscosity reducer can prevent the polyethylene from being solidified;
step 6: tail gas remaining in the polymerization process enters a torch through the tail gas outlet for treatment, unpolymerized ethylene flows back to the feeding pipe through the return pipe, and is conveyed to flow through the cooler through the compressor, and the cooler cools the ethylene to a specified temperature for reuse;
and 7: the polymerized material is conveyed to the discharging intermediate tank through the discharging port, the discharging intermediate tank can carry out gas-liquid separation on the polymerized material, the residual gas in the polymerized material is separated and conveyed to a torch for treatment, and the separated discharging intermediate tank conveys the material to the product bin;
and 8: and after separation, the discharging intermediate tank conveys the material to the product bin, the product bin dries the material to remove the viscosity reducer, the polyethylene is granulated after drying, and the polyethylene is output to the system after the granulation is finished.
Specifically, in the step 2, one or more of titanium tetrachloride and diethyl aluminum monochloride are selected as the catalyst.
And 2, the viscosity reducer in the step 2 is n-hexane.
In the step 3, the comonomer is selected from one of short-chain alpha-olefin, vinyl acetate and acrylate.
In the step 3, oxygen is selected as an initiator, and the content of the initiator is 0.003-0.007% of the ethylene content.
The polymerization temperature in the step 5 is 230 ℃ to 260 ℃, and the reaction pressure is 140MPa to 200 MPa.
It can be understood that the range of the preset operation conditions can be flexibly adjusted according to different product requirements or different catalysts, so as to ensure the full and effective reaction, further ensure the reaction rate and achieve the purpose of strengthening the reaction. Meanwhile, in the present embodiment, the kind of the catalyst is not particularly limited as long as the strengthening reaction can be smoothly performed.
Example one
The preparation of polyethylene is carried out by using the system and the process, wherein the catalyst in the step 2 is titanium tetrachloride.
And 2, the viscosity reducer in the step 2 is n-hexane.
In the step 3, the comonomer is short-chain alpha-olefin.
Oxygen is selected as an initiator in the step 3, and the content of the initiator is 0.003 percent of the content of ethylene.
In the step 5, the polymerization temperature is 230 ℃, and the reaction pressure is 140 MPa.
The prepared polyethylene was examined, and found that the product polyethylene had a PDI of 1.93 and an ethylene conversion of 93.5%.
Example two
The preparation of polyethylene is carried out by using the system and the process, wherein, in the step 2, the catalyst is diethyl aluminum chloride.
And 2, the viscosity reducer in the step 2 is n-hexane.
And vinyl acetate is selected as the comonomer in the step 3.
In the step 3, oxygen is selected as an initiator, and the content of the initiator is 0.004% of the ethylene content.
In the step 5, the polymerization temperature is 245 ℃, and the reaction pressure is 160 MPa.
The prepared polyethylene was examined, and found that the product polyethylene had a PDI of 1.81 and an ethylene conversion of 94.8%.
EXAMPLE III
The preparation of polyethylene is carried out by using the system and the process, wherein in the step 2, the catalyst is selected from a mixed solvent of titanium tetrachloride and diethyl aluminum monochloride.
And 2, the viscosity reducer in the step 2 is n-hexane.
In the step 3, the comonomer is acrylate.
Oxygen is selected as an initiator in the step 3, and the content of the initiator is 0.006 percent of the ethylene.
In the step 5, the polymerization temperature is 255 ℃, and the reaction pressure is 180 MPa.
The prepared polyethylene was examined, and found that the product polyethylene had a PDI of 1.55 and an ethylene conversion of 96.7%.
Example four
The preparation of polyethylene is carried out by using the system and the process, wherein in the step 2, the catalyst is selected from a mixed solvent of titanium tetrachloride and diethyl aluminum monochloride.
And 2, the viscosity reducer in the step 2 is n-hexane.
In the step 3, the comonomer is short-chain alpha-olefin.
In the step 3, oxygen is selected as an initiator, and the content of the initiator is 0.007% of the ethylene content.
In the step 5, the polymerization temperature is 260 ℃ and the reaction pressure is 200 MPa.
The prepared polyethylene was examined, and found that the product polyethylene had a PDI of 1.26 and an ethylene conversion of 98.1%.
Comparative example
The preparation of polyethylene was carried out using a system of the prior art and the preparation process was the same as in example four.
The polyethylene produced was examined, and the PDI of the product polyethylene was found to be 2.19 and the ethylene conversion was found to be 89.94%.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A system for enhancing ethylene polymerization, comprising:
a feeding unit for separately feeding a raw material and a liquid-phase catalyst;
the micro-interface generator is arranged in the feeding unit, converts the pressure energy of gas and/or the kinetic energy of liquid into the surface energy of bubbles and transmits the surface energy to the gas-phase raw material, so that the gas-phase raw material is crushed into micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm to improve the mass transfer area of a phase boundary, reduce the thickness of a liquid film and reduce the mass transfer resistance, and the materials are mixed to form a gas-liquid emulsion after being crushed so as to strengthen the mass transfer efficiency and the reaction efficiency between the phase boundaries within the range of preset operating conditions;
the reaction unit is connected with the feeding unit and is used for receiving the mixed solution of the raw materials and the catalyst output by the feeding unit so as to enable the ethylene in the mixed solution to generate a polymerization reaction in the reaction unit;
and the discharging unit is connected with the reaction unit and used for receiving the polymerized material output by the reaction unit and carrying out post-treatment on the polymerized material.
2. The system for enhancing ethylene polymerization of claim 1, wherein the feed unit comprises:
the raw material feeding pipeline is connected with the micro-interface generator and is used for conveying the gas-phase raw material to the micro-interface generator so that the micro-interface generator breaks the raw material into micron-sized bubbles;
a catalyst feed conduit connected to the reaction unit for delivering catalyst to the interior of the reaction unit;
a viscosity reducing agent feed conduit connected to the reaction unit for delivering a viscosity reducing agent to the interior of the reaction unit.
3. The system for enhancing ethylene polymerization of claim 2, wherein the feed conduit comprises:
a feed tube to deliver a gas phase feedstock to the gas phase feed conduit;
the compressor is connected with the feeding pipe and used for providing power for conveying materials;
the cooler is connected with the compressor and used for cooling the material output by the compressor;
a solvent feed line connected to the feed line and disposed downstream of the comonomer feed line for delivering solvent to the interior of the gas phase feed line;
a comonomer feed connected to said feed and disposed at the outlet of said cooler for delivering comonomer to the interior of said gas phase feed conduit;
an initiator feed line connected to the feed line and disposed downstream of the solvent feed line for delivering initiator to the interior of the gas phase feed conduit.
4. The system for enhancing ethylene polymerization of claim 3, wherein the micro-interface generator comprises:
the first micro-interface generator is arranged at a confluence position between the feeding pipe and the solvent feeding pipe and is used for crushing ethylene to form micron-scale micro-scale bubbles so as to be mixed with a solvent to form a gas-liquid emulsion;
and the second micro-interface generator is arranged at the confluence position of the feeding pipe and the initiator feeding pipe and is used for crushing the initiator to form micron-scale bubbles and mixing the micron-scale bubbles with the gas-liquid emulsion containing the comonomer output by the first micro-interface generator to form a mixed material.
5. The system for enhancing ethylene polymerization of claim 3, wherein the catalyst feed conduit comprises:
a catalyst feeder for storing and transporting a liquid phase catalyst;
and the catalyst feeding valve is arranged at the outlet of the catalyst feeder and is used for controlling the flow of the catalyst.
6. The system for enhancing ethylene polymerization as claimed in claim 2, wherein the reaction unit is a reactor for providing a reaction space for the micro bubbles, comprising:
the material feeding hole is formed in the bottom of the reactor and connected with the material feeding pipeline, so that the material feeding pipeline outputs materials to the inside of the reactor;
the catalyst feeding hole is formed in the side wall of the reactor and is connected with the catalyst feeding pipeline, so that the catalyst feeding pipeline outputs the catalyst to the inside of the reactor;
the viscosity reducing agent feeding port is formed in the side wall of the reactor and is connected with the viscosity reducing agent feeding pipeline, so that the viscosity reducing agent feeding pipeline outputs the viscosity reducing agent to the inside of the reactor;
the material outlet is formed in the side wall of the lower part of the reactor, is connected with the discharging unit and is used for outputting the reacted mixture to the discharging unit;
and the tail gas outlet is arranged at the top of the reactor and used for discharging tail gas generated after reaction out of the system.
7. The system for enhancing ethylene polymerization as claimed in claim 6, wherein a return pipe is provided between the reaction unit and the material feeding pipeline for returning unreacted ethylene in the reaction unit to the material feeding unit for reuse of ethylene.
8. The system for enhancing ethylene polymerization as claimed in claim 1, wherein the discharging unit comprises:
the discharging intermediate tank is connected with the reaction unit and is used for carrying out gas-liquid separation on the materials output by the reaction unit;
and the product bin is arranged at the bottom of the discharging intermediate tank, is connected with the discharging intermediate tank and is used for receiving the liquid-phase material output by the discharging intermediate tank, drying the material and granulating the polyethylene in the material.
9. The system for enhancing ethylene polymerization as claimed in claim 1, wherein the tail gas output from the reaction unit and the discharge unit enters a torch, and the torch burns the tail gas to prevent the tail gas from polluting the environment.
10. A process for enhancing the polymerization of ethylene, comprising:
step 1: introducing nitrogen into the material feeding pipeline, allowing the nitrogen to flow through the system to replace moisture and oxygen in the system, and after replacement is finished, introducing ethylene into the material feeding pipeline to continue replacement;
step 2: after replacement, introducing a liquid-phase catalyst into the catalyst feeding pipeline, outputting the catalyst into the reaction unit through the catalyst feeding pipeline, introducing a viscosity reducer into the viscosity reducer feeding pipeline, outputting the viscosity reducer into the reaction unit through the viscosity reducer feeding pipeline, and introducing the viscosity reducer into the viscosity reducer feeding pipeline;
and step 3: the compressor starts to operate, so that ethylene flows in the feeding pipe along a specified direction, when the ethylene is conveyed, the solvent is conveyed through the solvent feeding pipe, the comonomer is conveyed through the comonomer feeding pipe, and the initiator is conveyed through the initiator feeding pipe;
and 4, step 4: the first micro-interface generator is used for crushing ethylene to form micron-scale micro-scale bubbles, mixing the micron-scale ethylene bubbles with a solvent to form a gas-liquid emulsion, and the second micro-interface generator is used for crushing an initiator to form micron-scale micro-scale bubbles, mixing the micron-scale bubbles with the gas-liquid emulsion containing a comonomer to form a mixed material and conveying the mixed material into the reaction unit;
and 5: ethylene in the mixed material is subjected to polymerization reaction under the action of a catalyst, a comonomer and an initiator to generate polyethylene, the mixed material containing the polyethylene is conveyed to the discharging unit, and the viscosity reducer can prevent the polyethylene from being solidified;
step 6: tail gas remaining in the polymerization process enters a torch through the tail gas outlet for treatment, unpolymerized ethylene flows back to the feeding pipe through the return pipe, and is conveyed to flow through the cooler through the compressor, and the cooler cools the ethylene to a specified temperature for reuse;
and 7: the polymerized material is conveyed to the discharging intermediate tank through the discharging port, the discharging intermediate tank can carry out gas-liquid separation on the polymerized material, the residual gas in the polymerized material is separated and conveyed to a torch for treatment, and the separated discharging intermediate tank conveys the material to the product bin;
and 8: and after separation, the discharging intermediate tank conveys the material to the product bin, the product bin dries the material to remove the viscosity reducer, the polyethylene is granulated after drying, and the polyethylene is output to the system after the granulation is finished.
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