CN115260347B - Production system and method of high-isotacticity polypropylene - Google Patents
Production system and method of high-isotacticity polypropylene Download PDFInfo
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- CN115260347B CN115260347B CN202211061206.6A CN202211061206A CN115260347B CN 115260347 B CN115260347 B CN 115260347B CN 202211061206 A CN202211061206 A CN 202211061206A CN 115260347 B CN115260347 B CN 115260347B
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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
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/06—Propene
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/417—Polyolefins
Abstract
The invention provides a production system of high isotacticity polypropylene, which is sequentially connected with the following process units in series: the catalyst comprises a catalyst prepolymerization unit, a catalyst washing unit, at least one liquid phase bulk reaction kettle, an active polymer powder treatment unit, at least one gas phase fluidized bed reactor, a degassing bin unit and a drying bin unit. The invention realizes the elimination of low isotactic components and fine powder components by adding the washing pretreatment of the prepolymerized catalyst and the intermediate treatment of the active powder in the polymerization process in the traditional Hypol polypropylene process, realizes the production of high isotactic low ash polypropylene, and ensures the stable and consistent product performance in industrialized continuous production; the film product prepared by the material has relatively high melting point, better film puncture strength and fewer surface crystal points and gels after film formation.
Description
Technical Field
The invention relates to the technical field of polypropylene preparation, in particular to a polypropylene production process technology with high isotacticity.
Background
The lithium ion battery is one of key components of the current energy storage product, wherein the lithium ion battery is used as a key component for separating the anode and the cathode of the battery, one of key materials for ensuring the stable operation of the battery is a diaphragm, the diaphragm material for mass production at present is a wet polyethylene diaphragm, the diaphragm is produced by utilizing a solvent, the dissolution capacity of the solvent can be utilized, and the unnecessary large particles and low molecular components in the product are separated by mechanical forces such as filtration or centrifugal separation, but the production process speed is slower due to the existence of the solvent, the solvent recovery treatment cost is higher, and the solvent is not suitable for the requirements of safety and environmental protection more and more; meanwhile, compared with a polypropylene product, the melting point of polyethylene is lower, after the polyethylene is made into a battery, the separator can be quickly melted through after an exothermic phenomenon occurs, and the risk of ignition exists. In contrast, polypropylene has a melting point at least 20 ℃ higher than that of polyethylene, and can leave the reaction treatment time for the user in combination with an efficient temperature control alarm system, thereby essentially improving the safety level.
At present, newly built polypropylene devices in China are more and more, but most of the newly built polypropylene devices in China select a loop process or a fluidized bed process, and the polypropylene device is characterized by large single-kettle yield, short flow, space saving and few movable equipment, and the existing Hypol process devices in China only comprise early introduction devices such as Lanzhou petrochemical devices, daqing petrochemical devices, yanzi petrochemical devices, yanshan petrochemical devices and the like, and particularly after the devices are improved by Japanese Sanjing corporation, the combined process of the original reaction kettle and the fluidized bed is changed into the loop and fluidized bed process, and the type of devices are not newly built. The process flow is long, the reaction unit and other auxiliary units are arranged in parallel, the occupied area is large, the tank towers are more, the movable equipment is also more, the material residence time is long, the polymerization is more sufficient, and the catalyst pretreatment unit is arranged, so that the production of high-rigidity products is facilitated, and the production of high-isotacticity products can be realized by matching with novel external electron donors.
Disclosure of Invention
The invention aims to provide a production method and a production system of high isotacticity polypropylene, so as to realize the production of high isotacticity polypropylene products with low ash content, high rigidity, narrow particle size distribution and high relative molecular weight.
The invention is realized by adopting the following technical scheme:
the invention provides a production system of high isotacticity polypropylene, which is sequentially connected with the following process units in series: the catalyst comprises a catalyst prepolymerization unit, a catalyst washing unit, at least one liquid phase bulk reaction kettle, an active polymer powder treatment unit, at least one gas phase fluidized bed reactor, a degassing bin unit and a drying bin unit.
The catalyst prepolymerization unit is used for the prepolymerization reaction of propylene and a catalyst.
The catalyst washing unit is used for removing the fine powder, the low isotactic part and a small amount of catalyst shedding carrier formed after the prepolymerization, and the catalyst system after washing is pressurized and injected into the first liquid phase body reaction kettle.
The liquid phase bulk reaction kettle is used for realizing liquid phase bulk polymerization reaction of propylene, and preferably two liquid phase bulk reaction kettles are connected in series.
The purpose of the active polymer powder treatment unit is to remove a small amount of low isotacticity polymer and propylene liquid phase bulk in the liquid phase bulk polymerization reaction product. The active polymer powder treatment unit consists of a filtering mechanism and/or a cyclone separation mechanism.
The gas-phase fluidized bed reactor is mainly used for further realizing the synthesis of polypropylene with required molecular weight, and can of course also realize the copolymerization reaction of propylene, ethylene and the like, thereby realizing the switching of different polypropylene brands. The addition of ethylene is optional and is not an essential component of the target product of the present invention. Preferably two gas phase fluidized bed reactors in series.
The degassing bin unit and the drying bin unit are respectively used for removing unreacted monomers and drying powder; the powder deactivation storage unit is treated with nitrogen containing a small amount of water vapor to substantially remove the activity of the unconsumed cocatalyst.
The inventor surprisingly found that by adding a pretreatment unit for the pre-polymerized catalyst and an intermediate treatment unit for active powder in the polymerization process in the traditional Hypol polypropylene process, the removal of low-isotactic components and fine powder components is realized, and the high-isotacticity low-ash polypropylene production can be realized by matching with a catalyst system with higher activity, compared with the original process, and the stable and consistent product performance can be ensured in industrialized continuous production. The inventors completed the present invention based on the above findings.
Preferably, hydrogen is used to adjust the relative molecular mass of the product in the liquid phase bulk reactor and/or the gas phase fluidized bed reactor.
And the powder inactivation storage unit can be sequentially connected with a processing aid metering and feeding unit and a granulating unit in series.
The invention also provides a production method of the high isotacticity polypropylene, which comprises the following steps:
s1, injecting a catalyst, a cocatalyst and an external electron donor into a catalyst prepolymerization reaction kettle (namely a catalyst prepolymerization unit), wherein the kettle temperature of the catalyst prepolymerization reaction kettle is 5-15 ℃, and injecting polymerization-grade propylene into the catalyst prepolymerization reaction kettle in a liquid phase bulk form for prepolymerization reaction, wherein the pressure is controlled to be 3.0-3.6Mpa;
s2, after prepolymerization, the catalyst system enters a catalyst washing unit, fine powder, a low isotactic part and a small amount of catalyst shedding carriers formed after prepolymerization are removed, and the washed catalyst system is pressurized and injected into a first liquid phase bulk reaction kettle;
s3, controlling the total pressure of the first liquid phase bulk reaction kettle to be 2.9-3.3Mpa, the average residence time of the materials to be 40-80min, and the material level to be 35-75%;
s4, sequentially feeding the polymer materials into a second liquid phase bulk reaction kettle for continuous polymerization, controlling the total pressure of the second liquid phase bulk reaction kettle to be 2.5-2.8Mpa, controlling the average material residence time to be 40-80min and the material level to be 35-75%;
s5, the polymer material enters an active polymer powder treatment unit, a small amount of low isotacticity polymer is dissolved or swelled in liquid propylene, and the liquid propylene containing the low isotacticity polymer is removed by filtration and cyclone separation;
s6, sequentially entering the treated polymer powder into a first gas-phase fluidized bed reactor and a second gas-phase fluidized bed reactor to continue to react, wherein the total pressure is controlled to be 1.9-2.4Mpa and 1.4-1.8Mpa respectively, and the average residence time of the materials is 45-90min;
and S7, the powder discharged from the second gas-phase fluidized bed reactor enters a degassing tower (namely a degassing bin unit) and a drying tower (namely a drying bin unit) to remove unreacted monomers, then enters an inactivation treatment unit, is treated by nitrogen containing a small amount of water vapor to fully remove the activity of the unconsumed cocatalyst, and finally obtains the high-isotacticity polypropylene powder.
In step S1, the degree of prepolymerization is controlled to 5 to 50, preferably 15 to 35. The ratio (molar ratio) of the total amount of propylene to the total amount of catalyst fed into the catalyst prepolymerization reactor was taken as the prepolymerization degree.
In the step S1, the dosages of the catalyst, the cocatalyst and the external electron donor are respectively as follows: the molar ratio of cocatalyst to catalyst is 10-200:1, preferably 30-80:1, a step of; the molar ratio of the external electron donor to the catalyst is 5-30:1, preferably 8-20:1.
Preferably, the catalyst uses active Ti as a catalytic center and uses ether or ester compounds as internal electron donors, including but not limited to cyclobutyl-1, 1-dimethanol dimethyl ether, 1, 3-diethers, 1, 3-propanediol dimethyl ether, 2-diisobutyl-1, 3-propanediol dimethyl ether, cyclopentyl-1, 1-dimethanol dimethyl ether, 1, 3-diol ester compounds, di-n-butyl phthalate, diisobutyl phthalate, ethyl benzoate, dibutyl phthalate and the like, and the catalyst preferably uses the internal electron donors as ether compounds, and also can use a mixture of ether and ester compounds.
The cocatalyst includes, but is not limited to, organoaluminum compounds such as triethylaluminum, triisobutylaluminum, diisobutylaluminum monochloride, and the like, preferably triethylaluminum.
The external electron donor includes, but is not limited to, phenyltriethoxysilane, diphenyldimethoxysilane, diisobutyldimethoxysilane, dicyclopentyldimethoxysilane, diisopropyldimethoxysilane, isopropylisobutyldimethoxysilane, cyclopentyibutyldimethoxysilane, cyclohexylmethyldimethoxysilane and the like, preferably diisobutyldimethoxysilane, dicyclopentyldimethoxysilane.
In step S3, depending on the characteristics of the final product, ethylene may be used to adjust the melting point and crystallization temperature, and hydrogen may be used to adjust the MFR and relative molecular mass and distribution thereof, with the level of the feed being preferably controlled at 50-55% by controlling the feed procedure in the polymer level.
In the step S4, ethylene and/or hydrogen can be added or not added into the second liquid phase bulk reaction kettle, and the material level is preferably controlled to be 50-55% by controlling a feeding program through a polymerization material level.
In step S6, the first gas-phase fluidized bed reactor and the second gas-phase fluidized bed reactor may be supplemented with or without ethylene and/or hydrogen, and further adjust physical properties such as melting point, crystallization temperature, MFR, relative molecular mass, and distribution thereof of the product.
Preferably, the high isotacticity polypropylene powder can be further added with an auxiliary agent and then enters a granulator for granulation.
The invention also provides application of the high-isotacticity polypropylene prepared by the method in preparation of lithium battery diaphragms.
The high isotacticity polypropylene prepared by the invention has better crystallization performance, the products prepared from the raw materials generally have better rigidity and higher glass transition temperature, and the products have better dimensional stability when heated and sterilized in boiling water; meanwhile, the high isotacticity polypropylene of the invention also has the characteristic of low ash content, and a film product prepared by adopting the material has relatively high melting point, better film puncture strength and fewer surface crystal points and gels after film formation.
The invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of the process flow of the present invention.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and are not intended to limit the scope of the invention, as other obvious variations will occur to those skilled in the art. The basic principles of the invention defined in the following description may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
The apparatus, industrial equipment or reagents in the embodiments of the present invention are not manufacturer-specific, and are conventional commercial apparatus, industrial equipment or reagents. Wherein propylene is polymer grade propylene.
As shown in fig. 1, the production system of the high isotacticity polypropylene of the invention is sequentially connected with the following process units in series: the catalyst comprises a catalyst prepolymerization unit, a catalyst washing unit, a first liquid phase bulk reaction kettle, a second liquid phase bulk reaction kettle, an active polymer powder treatment unit, a first gas phase fluidized bed reactor, a second gas phase fluidized bed reactor, a degassing bin unit, a drying bin unit, a powder inactivation storage unit, a processing aid metering and feeding unit and a granulating unit. Wherein the processing aid metering and charging unit and the granulating unit are optional units, and can also be directly packaged in powder form.
Of course, it is known in the art that a catalyst deployment unit, a propylene refining unit, and optionally hydrogen production systems, feed transport systems, etc. during polymerization are also required prior to the catalyst pre-polymerization unit. The combination of each process unit can be carried out according to actual needs by a person skilled in the art, and the process units, the connection mode between the process units and the process units provided by the invention, the process parameters and the like can all adopt conventional means in the art, and the invention is not repeated.
The invention relates to a production method of high isotacticity polypropylene, which comprises the following steps:
s1, injecting a catalyst, a cocatalyst and an external electron donor into a catalyst prepolymerization reaction kettle (namely a catalyst prepolymerization unit), wherein the kettle temperature of the catalyst prepolymerization reaction kettle is 5-15 ℃, and injecting polymerization-grade propylene into the catalyst prepolymerization reaction kettle in a liquid phase bulk form for prepolymerization reaction, wherein the pressure is controlled to be 3.0-3.6Mpa;
s2, after prepolymerization, the catalyst system enters a catalyst washing unit, fine powder, a low isotactic part and a small amount of catalyst shedding carriers formed after prepolymerization are removed, and the washed catalyst system is pressurized and injected into a first liquid phase bulk reaction kettle;
s3, the average residence time of the materials in the first liquid phase bulk reaction kettle is 40-80min;
s4, sequentially feeding the polymer materials into a second liquid phase bulk reaction kettle for continuous polymerization, wherein the average residence time of the materials in the second liquid phase bulk reaction kettle is 40-80min;
s5, the polymer material enters an active polymer powder treatment unit, a small amount of low isotacticity polymer is dissolved or swelled in liquid propylene, and the liquid propylene containing the low isotacticity polymer is removed by filtration and cyclone separation;
s6, sequentially entering the treated polymer powder into a first gas-phase fluidized bed reactor and a second gas-phase fluidized bed reactor to continue to react, wherein the average residence time of the materials is 45-90min;
and S7, the powder discharged from the second gas-phase fluidized bed reactor enters a degassing tower (namely a degassing bin unit) and a drying tower (namely a drying bin unit) to remove unreacted monomers, then enters an inactivation treatment unit, is treated by nitrogen containing a small amount of water vapor to fully remove the activity of the unconsumed cocatalyst, and finally obtains the high-isotacticity polypropylene powder.
The process parameters of the polymerization section are shown in table 1:
table 1 process parameters of the reactor section
| Polymeric unit | Temperature (DEG C) | Pressure Mpa | Level% |
| First liquid phase body reaction kettle | 70±1.0 | 2.9-3.2 | 45-65 |
| Second liquid phase body reaction kettle | 68±1.0 | 2.5-2.8 | 45-65 |
| First gas-phase fluidized bed reactor | 84±1.0 | 2.1-2.4 | 45-75 |
| Second gas-phase fluidized bed reactor | 80±1.0 | 1.6-2.0 | 45-75 |
Example 1
The catalyst is a Z-N catalyst containing lipid internal electron donor, triethyl aluminum is matched as a cocatalyst, diisobutyl dimethoxy silane is used as an external electron donor, the Al/Si/Ti molar ratio is 75/9/1, the prepolymerization temperature is 8 ℃, and the prepolymerization degree is 10.
Example 2
The catalyst is a Z-N catalyst containing an ether internal electron donor, and is matched with triethylaluminum as a cocatalyst, diisobutyldimethoxy silane is used as an external electron donor, the Al/Si/Ti molar ratio is 70/8/1, the prepolymerization temperature is 10 ℃, and the prepolymerization degree is 10.
Example 3
The catalyst is a Z-N catalyst containing an ether internal electron donor, and is matched with triethylaluminum as a cocatalyst, dicyclopentyl dimethoxy silane is used as an external electron donor, the Al/Si/Ti molar ratio is 70/9/1, the prepolymerization temperature is 12 ℃, and the prepolymerization degree is 15.
Comparative example 1
The catalyst washing unit and the corresponding catalyst washing step S2 were not employed, otherwise as in example 1.
Comparative example 2
The catalyst washing unit and the corresponding catalyst washing step S2 and the living polymer powder treatment unit and the corresponding living powder treatment step S5 were not used, and the same as in example 1 was followed.
The powder products obtained in each example and comparative example were granulated by adding antioxidant 1010, 168 and zinc stearate (at 2500ppm, ratio of 1:2:2), respectively, and then tested for each property, and the results are shown in tables 2 and 3:
table 2 sample test results 1
TABLE 3 sample test results 2
Wherein, MFR is tested according to GB/T3682.1-2018, tensile strength is tested according to GB/T1040.2-2006, flexural modulus and flexural strength are tested according to GB/T9341-2008, impact strength at normal temperature is tested according to GB/T1043.1-2008, ash is tested according to GB/T9345.1-2008, melting point and crystallization temperature are tested according to GB/T19466.3-2004, and isotacticity is tested according to GB/T2412-2008.
Gel Permeation Chromatography (GPC) analysis: the gel was tested by using a PL-220 type gel permeation chromatograph (1, 2, 4-trichlorobenzene as solvent, elution temperature 150 ℃ C., flow rate 1.0 mL/min) from America Polymer Laboratories.
As can be seen from the detection data in tables 1 and 2, the isotacticity of the polypropylene material prepared by the method and the production system is improved by 12.8% -14.1% compared with the comparative example, the ash content is reduced by 44.4% -83.3% compared with the comparative example, the molecular weight distribution is narrow, the mechanical strength is improved to different degrees, unexpected technical effects are generated, and the catalyst washing unit, the corresponding catalyst washing step, the active polymer powder processing unit and the corresponding active powder processing step are shown, so that the isotacticity of the polypropylene material and the ash content are unexpectedly and obviously improved. Therefore, the invention is suitable for preparing lithium battery diaphragm products, has relatively high melting point, better film puncture strength and fewer surface crystal points and gels after film formation.
It will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are by way of example only and are not limiting. The objects of the present invention have been fully and effectively achieved. The functional and structural principles of the present invention have been shown and described in the examples and embodiments of the invention may be modified or practiced without departing from the principles described.
Claims (9)
1. A production system of high isotacticity polypropylene is characterized in that the following process units are connected in series in sequence: the catalyst comprises a catalyst prepolymerization unit, a catalyst washing unit, at least one liquid phase bulk reaction kettle, an active polymer powder treatment unit, at least one gas phase fluidized bed reactor, a degassing bin unit, a drying bin unit and a powder inactivation storage unit; the active polymer powder treatment unit consists of a filtering mechanism and/or a cyclone separation mechanism.
2. The system for producing high isotacticity polypropylene according to claim 1, further comprising a processing aid dosing unit and a pelletization unit in series after the powder deactivation storage unit.
3. The production method of the high isotacticity polypropylene is characterized by comprising the following steps of:
s1, injecting a catalyst, a cocatalyst and an external electron donor into a catalyst prepolymerization reaction kettle, wherein the kettle temperature of the catalyst prepolymerization reaction kettle is 5-15 ℃, and polymerization-grade propylene is injected into the catalyst prepolymerization reaction kettle in a liquid phase body form for prepolymerization reaction, and the pressure is controlled at 3.0-3.6Mpa;
s2, after prepolymerization, the catalyst system enters a catalyst washing unit, fine powder, a low isotactic part and a small amount of catalyst shedding carriers formed after prepolymerization are removed, and the washed catalyst system is pressurized and injected into a first liquid phase bulk reaction kettle;
s3, controlling the total pressure of the first liquid phase bulk reaction kettle to be 2.9-3.3Mpa, the average residence time of the materials to be 40-80min, and the material level to be 35-75%;
s4, sequentially feeding the polymer materials into a second liquid phase bulk reaction kettle for continuous polymerization, controlling the total pressure of the second liquid phase bulk reaction kettle to be 2.5-2.8Mpa, controlling the average material residence time to be 40-80min and the material level to be 35-75%;
s5, the polymer material enters an active polymer powder treatment unit, a small amount of low isotacticity polymer is dissolved or swelled in liquid propylene, and the liquid propylene containing the low isotacticity polymer is removed by filtration and cyclone separation;
s6, sequentially entering the treated polymer powder into a first gas-phase fluidized bed reactor and a second gas-phase fluidized bed reactor to continue to react, wherein the total pressure is controlled to be 1.9-2.4Mpa and 1.4-1.8Mpa respectively, and the average residence time of the materials is 45-90min;
s7, the powder discharged from the second gas-phase fluidized bed reactor enters a degassing tower and a drying tower to remove unreacted monomers, then enters an inactivation treatment unit, and is treated by nitrogen containing a small amount of water vapor to fully remove the activity of the unconsumed cocatalyst, and finally the high-isotacticity polypropylene powder is obtained.
4. A method according to claim 3, wherein in step S1, the degree of prepolymerization is controlled in the range of 5 to 50; the mole ratio of the cocatalyst to the catalyst is 10-200:1, a step of; the molar ratio of the external electron donor to the catalyst is 5-30:1.
5. A method according to claim 3, wherein in step S1, the degree of prepolymerization is controlled in the range of 35 to 45; the molar ratio of the cocatalyst to the catalyst is 50-125:1, a step of; the molar ratio of the external electron donor to the catalyst is 8-15:1.
6. The method of claim 3, wherein the catalyst is an ether or ester compound as an internal electron donor with active Ti as a catalytic center; the cocatalyst is at least one selected from triethylaluminum, triisobutylaluminum and diisobutylaluminum monochloride; the external electron donor is at least one selected from phenyl triethoxy silane, diphenyl dimethoxy silane, diisobutyl dimethoxy silane, dicyclopentyl dimethoxy silane, diisopropyl dimethoxy silane, isopropyl isobutyl dimethoxy silane, cyclopentyl isobutyl dimethoxy silane and cyclohexyl methyl dimethoxy silane.
7. The method of claim 6, wherein the internal electron donor is an ether compound.
8. A highly isotactic polypropylene produced according to the process of any one of claims 3 to 7.
9. Use of the highly isotactic polypropylene prepared according to any one of claims 3 to 7 in the preparation of lithium battery separator.
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