Manufacturing process of separated ultra-high molecular weight isotactic polypropylene

Abstract

The present invention relates to a method for producing separated ultra-high molecular weight isotactic polypropylene. The separated ultra-high molecular weight isotactic polypropylene of the present invention has low entanglement density, low bulk density, and a spherical shape. Furthermore, the separated ultra-high molecular weight isotactic polypropylene of the present invention does not require costly and energy-consuming post-production processing to reduce entanglement density.

Description

Technology Field

[0001] The present invention relates to a manufacturing process for separated ultra-high molecular weight isotactic polypropylene. Background Technology

[0002] The background information below is related to the present invention but is not necessarily prior art.

[0003] Ultra-high molecular weight polymers are used in engineering applications such as ballistics, medical prosthetics, and high-strength tapes. Ultra-high molecular weight isotactic polypropylene (UHMWiPP) has low density, good heat resistance, high stiffness, inherent biocompatibility, and excellent fatigue resistance. It can potentially be used in high-fatigue applications in the biomedical, aerospace, and automotive sectors.

[0004] The properties of UHMWiPP are closely related to its molecular weight (M). Processing of UHMWiPP is generally performed in a molten state, where polymer chains interact with each other to form entanglements. These entanglements are defined as physical constraints or friction points that hinder the fluidity of the polymer. Consequently, at high molecular weights, such as in the case of UHMWiPP, the likelihood of forming entanglements also increases. Melt viscosity ( η 0 ) The relationship between and molecular weight is defined using the following equation.

[0005] η 0 ∝ M 3.4

[0006] Due to the relationship between the molecular weight and melt viscosity of UHMWiPP, processing UHMWiPP via conventional routes becomes impossible. Consequently, alternative processing methods have been studied to reduce the entanglement density of UHMWiPP while maintaining high mechanical properties. Conventional methods used to reduce entanglement density to date are costly and energy-consuming.

[0007] Therefore, there is a need to provide a process for manufacturing separated ultra-high molecular weight isotactic polypropylene that mitigates the aforementioned disadvantages. The problem to be solved

[0008] Some of the objectives of the present invention satisfied by one or more embodiments are as follows.

[0009] The objective of the present invention is to improve upon one or more problems of the prior art or at least provide a useful alternative.

[0010] Another objective of the present invention is to provide a method for producing separated ultra-high molecular weight isotactic polypropylene having low entanglement density, low bulk density, and a spherical shape.

[0011] However, another objective of the present invention is to provide a separated ultra-high molecular weight isotactic polypropylene having low entanglement density, low bulk density, and a spherical shape.

[0012] Other objects and advantages of the present invention will become more apparent from the following description, but this is not intended to limit the scope of the invention. means of solving the problem

[0013] The present invention relates to a method for producing separated ultra-high molecular weight isotactic polypropylene. In the above process, at least one scavenger is added to and mixed in a reactor containing at least one hydrocarbon solvent maintained under an inert atmosphere to form a mixture. The mixture is stirred under a first predetermined condition to obtain a first solution. Then, propylene gas in a pressure range of 1 bar to 3 bar is introduced into the reactor, and a second predetermined condition is maintained to obtain a second solution. A predetermined amount of a pre-activated catalyst species is added to the second solution. The pre-activated catalyst species is obtained by reacting a catalyst with an activator, and the catalyst has a structural formula represented by the following structural formula 1.

[0014] [Structural Formula 1]

[0015]

[0016] Here, R 1, R 2, R3 is isopropyl.

[0017] The reactor is maintained under a third predetermined condition to obtain a third solution containing unpurified separated ultra-high molecular weight isotactic polypropylene (UHMWiPP). The third solution is quenched inside the reactor to obtain a quenched third solution containing an unpurified UHMWiPP precipitate. The quenched third solution containing the unpurified UHMWiPP precipitate is removed from the reactor and filtered to obtain a wet unpurified UHMWiPP residue. The wet unpurified UHMWiPP residue is washed with ethanol and dried to obtain separated UHMWiPP.

[0018] The present invention relates to a pre-activated catalyst species for use in the manufacture of UHMWiPP. The pre-activated catalyst species comprises a catalyst compound of the following structural formula 1 and an activator in a range of 1:1 to 1:10. The catalyst has a structural formula represented by structural formula 1.

[0019] In addition, the present invention relates to a separated ultra-high molecular weight isotactic polypropylene characterized by comprising the following.

[0020] ● Molecular weight in the range of 500,000 to 4,000,000 g / mol

[0021] ● Bulk density is 0.07 g / cm³ 3 Up to 0.7g / cm² 3 range

[0022] ● Spherical shape having a diameter in the range of 300㎛ to 600㎛

[0023] ● Melting temperature in the range of 155℃ to 160℃

[0024] ● Stored as a function of time during oscillating shear time sweep experiments at 190°C, 10 rad / s, and axial forces in the range of 0.1 N to 1 N in the viscoelastic region ( G’ ) and loss(G” ) gradually increases by at least 20%

[0025] ● Processing temperature below the melting point of separated ultra-high molecular weight isotactic polypropylene

[0026] ● And compression forming and rolling temperatures in the range of 125℃ to 150℃ Effects of the invention

[0027] The process of the present invention described above has various technical advantages, including (but not limited to) realizing the following.

[0028] Manufacturing process of separated ultra-high molecular weight isotactic polypropylene characterized by having low entanglement density, low bulk density, and spherical shape.

[0029] Separated ultra-high molecular weight isotactic polypropylene has a low entanglement density, so post-production processing to reduce entanglement density is not required. Brief explanation of the drawing

[0030] The present invention is described below through the attached drawings. Figure 1a shows the bulk density measurement of UHMWiPP prepared according to Example 1 of the present invention. Figure 1b shows the bulk density measurement of UHMWiPP prepared according to Example 2 of the present invention. Figure 1c shows the bulk density measurement of UHMWiPP prepared according to Example 3 of the present invention. Figure 1d shows the bulk density measurement of UHMWiPP prepared using a Ziegler-Natta catalyst system (Comparative Example). Figure 2 shows a scanning electron microscope image (reference: 500 microns) of UHMWiPP prepared according to Example 2 of the present invention. Figure 3 shows the proton separation of UHMWiPP prepared according to Example 2 of the present invention. 13 This represents the C NMR measurement. Figure 4a shows differential scanning calorimetry of UHMWiPP prepared according to Example 2 of the present invention to study the effect of entanglement density on isothermal crystallization. Figure 4b shows dynamic vibration rheology (time sweep), i.e., storage factor versus time measurement, for UHMWiPP prepared according to Examples 1, 2, and 3 of the present invention to study the effect of the residence time of the melt on entanglement formation. Figure 4c shows dynamic vibration rheology (time sweep), i.e., loss factor versus time measurement, for UHMWiPP prepared according to Examples 1, 2, and 3 of the present invention to study the effect of the residence time of the melt on entanglement formation. Figure 5a shows dynamic vibration rheology (frequency sweep) measurements to obtain the estimated molecular weight of UHMWiPP prepared according to Example 1 of the present invention. Figure 5b shows dynamic vibration rheology (frequency sweep) measurements to obtain the estimated molecular weight of UHMWiPP prepared according to Example 2 of the present invention. Figure 5c shows dynamic vibration rheology (frequency sweep) measurements to obtain the estimated molecular weight of UHMWiPP prepared according to Example 3 of the present invention. Figure 5d shows dynamic vibration rheology (frequency sweep) measurements to obtain the estimated molecular weight of UHMWiPP prepared according to Examples 1, 2, and 3 of the present invention. And Figure 6 shows dynamic vibration rheology (frequency sweep) measurements to obtain the estimated molecular weight of UHMWiPP prepared according to Example 4 of the present invention. Specific details for implementing the invention

[0031] As used in the present invention, the following terms generally have the following meanings, except where otherwise indicated by the context in which they are used.

[0032] Isotactic polypropylene: It is polypropylene in which all methyl groups are stereochemically oriented along the same plane of the polymer backbone chain.

[0033] Storage and Loss Factors: In viscoelastic materials such as polymers, the storage factor is related to the elastic component and measures the material's ability to elastically store energy. The storage factor can be defined as the ratio of the elastic component of stress to the strain. The loss factor is related to the viscous component of the material and measures the material's ability to dissipate stress through heat. The loss factor can be defined as the ratio of the viscous component of stress to the strain.

[0034] Vibration rheology: It is used to study the properties of both viscous and elastic materials at different time scales. It is a valuable tool for understanding the structural and dynamic properties of viscous and elastic materials. The basic principle of a viscous rheometer is to induce sinusoidal shear deformation in a sample and measure the resulting stress response. The time scale investigated is determined by the vibrational frequency (ω) of the shear deformation.

[0035] Separation polymer: It is a polymer that resists the tendency of polymer chains to form entanglements with each other.

[0036] Embodiments of the present invention will now be described with reference to the enclosed drawings.

[0037] Examples are provided to convey the scope of the invention to the reader thoroughly and completely. Numerous details regarding specific components and methods are presented to provide a complete understanding of the embodiments of the invention. It will be apparent to the reader that the details provided in the examples should not be interpreted as limiting the scope of the invention. In some embodiments, well-known processes, well-known device structures, and well-known techniques are not described in detail.

[0038] The terms used in this invention are for the purpose of describing specific embodiments only and should not be construed as limiting the scope of this invention. As used in this invention, various forms of “one” may also be intended to include plural forms unless the context clearly indicates otherwise. The terms “include” and “have” are open-ended transitional phrases that specify the presence of a stated function, integer, step, operation, element, module, unit, and / or component, but do not prohibit the presence or addition of one or more other functions, integers, steps, operations, elements, components, and / or groups thereof. The order of specific steps disclosed in the methods and processes of this invention is not to be interpreted as necessarily being performed as described or illustrated. It should also be understood that additional or alternative steps may be applied.

[0039] The properties of UHMWiPP depend on their molecular weight. When the molten state of UHMWiPP is achieved during the process, the polymer chains of UHMWiPP tend to form entanglements with each other, which impedes the fluidity of the polymer. In the case of ultra-high molecular weight polyolefins such as isotactic polypropylene, the probability of entanglement formation increases as the molecular weight increases; therefore, as the molecular weight of UHMWiPP increases, the melt viscosity rises exponentially.

[0040] Due to the relationship between the molecular weight and melt viscosity of UHMWiPP, processing of UHMWiPP through conventional routes becomes impossible. Therefore, other processing methods are required to reduce the entanglement density of UHMWiPP while maintaining high mechanical properties.

[0041] Recently, gelation, crystallization, and gel-like spherical press (GSP) methods have been commercialized to produce ultra-high molecular weight polyethylene (UHMWPE) fibers with low entanglement density. However, these methods are primarily post-production processes and are costly and energy-consuming.

[0042] The present invention provides a manufacturing process for separated UHMWiPP characterized by having low entanglement density, low bulk density, and a spherical shape. The separated UHMWiPP of the present invention does not require costly and time-consuming post-production processing to reduce entanglement density.

[0043] In the first aspect of the present invention, a process for manufacturing separated ultra-high molecular weight isotactic polypropylene is provided.

[0044] The process is explained in detail below.

[0045] First, a reactor containing at least one hydrocarbon solvent is maintained under an inert atmosphere, at least one scavenger is added and mixed to form a mixture, and said mixture is stirred under a first predetermined condition to obtain a first solution.

[0046] According to an embodiment of the present invention, the hydrocarbon solvent is one or more selected from toluene and heptane. In an embodiment, the hydrocarbon solvent is heptane.

[0047] According to an embodiment of the present invention, the scavenger is selected from methylalumonic acid (MAO) and tri-isobutylaluminum (TiBA). In one embodiment, the scavenger is tri-isobutylaluminum (TiBA).

[0048] Typically, scavengers perform the function of removing impurities. Examples of these include oligomeric or polymeric alumonic acids such as methylalumonic acid (MAO) and metal alkylated species such as triisobutylaluminum (TiBA).

[0049] The manufacturing process of separated ultra-high molecular weight isotactic polypropylene is carried out in an inert atmosphere. In the examples, the inert atmosphere is maintained using nitrogen gas.

[0050] According to an embodiment of the present invention, under a first predetermined condition, 10 to obtain a first solution o C to 70o It includes a time range of 10 to 30 minutes under a temperature in the C range and a stirring speed in the range of 150 rpm to 350 rpm. In the examples, the temperature is 40 o C, the time is 20 minutes, and the stirring speed is 250 rpm.

[0051] In the next step, propylene gas in a pressure range of 1 bar to 3 bar is introduced into the reactor, and a second predetermined condition is maintained to obtain a second solution. In the example, the pressure of the propylene gas is 1.1 bar.

[0052] It was found that propylene pressure conditions can improve the form of separated UHMWiPP.

[0053] According to an embodiment of the present invention, under the second predetermined condition, 10 o C to 70 o It includes a temperature in the C range and a stirring speed in the range of 650 rpm to 850 rpm. In the example, the temperature is 40 o C and the stirring speed is 750 rpm.

[0054] Next, a predetermined amount of pre-activated catalyst species is added to the second solution. Then, the reactor is maintained under third predetermined conditions to obtain a third solution containing unpurified separated ultra-high molecular weight isotactic polypropylene (UHMWiPP).

[0055] The above-mentioned pre-activated catalyst species is obtained by reacting a catalyst with an activator, and the catalyst has the structure of the following structural formula 1.

[0056] [Structural Formula 1]

[0057]

[0058] In an embodiment of the present invention, alkyl group R 1, R2 and R3 are isopropyl. For the polymerization of propylene, the use of R3=hydrogen atom (H) was evaluated, and the thermal properties of the obtained polymer are lower compared to R3=isopropyl.

[0059] According to an embodiment of the present invention, the activator is one or more selected from N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate, trityl tetrakis(pentafluorophenyl) borate, tris(substituted aryl) borane, and derivatives thereof. In an embodiment, the activator is N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate.

[0060] According to an embodiment of the present invention, the ratio of the catalyst to the activator is in the range of 1:1 to 1:10. In an example, the ratio is 1:1. In another example, the ratio is 1:2.

[0061] According to an embodiment of the present invention, under a third predetermined condition, 10 o C to 70 o It includes a time range of 1 hour to 3 hours under a temperature in the range of C and a stirring speed in the range of 650 rpm to 850 rpm. In the examples, the temperature is 40 o C, the time is 1 hour, and the stirring speed is 750 rpm. In another embodiment, the time is 2 hours. In yet another embodiment, the time is 3 hours.

[0062] For the production of ultra-high molecular weight propylene, reduced entanglement density, and the fabrication of microspherical forms, catalysts based on hafnium complexes require an activation step. Generally, a combination with a suitable activator leads to the formation of a pre-activated catalyst, which completes the activation step in the presence of a propylene monomer. Typically, a wide range of activators, such as alumoxic acid, Lewis acid, Brønsted acid, and possible combinations, are used. Preferably, the activator species is M(C6F5)4 - It must contain non-weak coordination anions such as (M:B, Al) and cations (Brønsted acid) capable of breaking H-Me bonds through easy proton disintegration.

[0063] According to an embodiment of the present invention, the ratio of catalyst to scavenger is in the range of 1:50 to 1:100. In an example, the ratio is 1:70.

[0064] The above third solution is quenched inside the reactor to obtain a quenched third solution containing an unpurified separated UHMWiPP precipitate. In the example, quenching is performed using ethanol.

[0065] The quenched third solution containing the precipitate of the unpurified separated UHMWiPP is removed from the reactor and filtered to obtain the residue of the wet unpurified UHMWiPP. The residue of the wet unpurified separated UHMWiPP is washed and dried to obtain the separated UHMWiPP.

[0066] Furthermore, the present invention relates to a pre-activated catalyst species for use in the manufacture of UHMWiPP. The pre-activated catalyst species comprises a catalyst having the structure of Structural Formula 1 and an activator in the ranges of 1:1 and 1:10. The catalyst has the structure of Structural Formula 1.

[0067] [Structural Formula 1]

[0068]

[0069] In the example, the activator is N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate, and the ratio of the catalyst to the activator is 1:1.

[0070] In the examples, the manufacturing process of separated ultra-high molecular weight isotactic polypropylene includes the following steps.

[0071] First, one or more scavengers are added to and mixed in a reactor containing one or more hydrocarbon solvents maintained under an inert atmosphere to form a mixture, and this is 40 o The first solution is obtained by stirring at a speed of 250 rpm for 20 minutes at a temperature of C. Then, at a pressure of 1.1 and a temperature of 40 oPropylene gas is introduced into the reactor of C, and stirring is maintained at a speed of 750 rpm to obtain a second solution. A predetermined amount of a pre-activated catalyst species is added to the second solution. The pre-activated catalyst species is obtained by reacting a catalyst with an activator, and the catalyst has a structural formula represented by the following structural formula 1.

[0072] [Structural Formula 1]

[0073]

[0074] Here, R 1, R 2, R3 is isopropyl.

[0075] Next, the reactor is heated to a stirring speed of 750 rpm for a time ranging from 1 to 3 hours for 40 o A third solution containing unpurified separated ultra-high molecular weight isotactic polypropylene (UHMWiPP) is obtained by maintaining at C. The third solution is quenched inside a reactor to obtain a quenched third solution containing an unpurified UHMWiPP precipitate. The quenched third solution containing the unpurified UHMWiPP precipitate is removed from the reactor and filtered to obtain a wet unpurified UHMWiPP residue. The wet unpurified UHMWiPP residue is washed with ethanol and dried to obtain separated UHMWiPP.

[0076] According to an embodiment of the present invention, the average molecular weight of the separated ultra-high molecular weight isotactic polypropylene falls within the range of 500,000 to 4,000,000 g / mol. In an example, the average molecular weight is 800,000 g / mol. In another example, the average molecular weight is 2,400,000 g / mol. However, in yet another example, the average molecular weight is 3,000,000 g / mol.

[0077] According to an embodiment of the present invention, the bulk density of the separated ultra-high molecular weight isotactic polypropylene is 0.05 g / cm³ 3 Up to 0.12 g / cm² 3It is a range. In the example, the bulk density is 0.065 g / cm³. 3 is. In another embodiment, the bulk density is 0.095 g / cm³. 3 is. In another embodiment, the bulk density is 0.105 g / cm³. 3 am.

[0078] According to an embodiment of the present invention, the separated ultra-high molecular weight isotactic polypropylene is in the form of spherical particles with a diameter ranging from 300 μm to 600 μm. In an example, the diameter is 500 μm. In another example, the diameter is 600 μm.

[0079] According to an embodiment of the present invention, the storage factor of separated ultra-high molecular weight isotactic polypropylene ( G' The storage factor and loss factor exhibit a gradual increase of at least 20% as a function of time. This was revealed during viscoelastic shear time sweep experiments within the viscoelastic region at 190°C, 10 rad / s, and axial forces ranging from 0.1N to 1N. In an example, the storage factor and loss factor exhibit a gradual increase of 20% as a function of time. This was revealed during viscoelastic shear time sweep experiments within the viscoelastic region at 190°C, 10 rad / s, and 0.1N axial forces. In another example, the storage factor and loss factor exhibit a gradual increase of 36% and 39%, respectively, as a function of time. This was revealed during viscoelastic shear time sweep experiments within the viscoelastic region at 190°C, 10 rad / s, and 1N axial forces. In yet another example, the storage factor and loss factor exhibit a gradual increase of 31% and 32%, respectively, as a function of time. This was revealed during the viscoelastic shear time sweep experiment within the viscoelastic region at 190°C, 10 rad / s, and 1 N axial force.

[0080] According to an embodiment of the present invention, the melting temperature of the separated ultra-high molecular weight isotactic polypropylene is in the range of 155°C to 160°C. In an example, the melting temperature is 158°C. In another example, the melting temperature is 159°C. In yet another example, the melting temperature is 160°C.

[0081] According to an embodiment of the present invention, the process temperature of the separated UHMWiPP is below the melting point of the ultra-high molecular weight polypropylene.

[0082] According to an embodiment of the present invention, the compression forming and rolling temperature is in the range of 125°C to 150°C. In an embodiment, the forming and rolling temperature is 135°C. In another embodiment, the forming and rolling temperature is 130°C.

[0083] The present invention also provides a separated ultra-high molecular weight isotactic polypropylene characterized by comprising the following:

[0084] ● The molecular weight ranges from 500,000 to 4,000,000 g / mol and

[0085] ● Bulk density is 0.09 g / cm³ 3 Up to 0.12 g / cm² 3 It is a range.

[0086] ● The diameter of the sphere is in the range of 300㎛ to 600㎛ and

[0087] ● The melting temperature is in the range of 155℃ to 160℃ and

[0088] ● Provides a separated ultra-high molecular weight isotactic polypropylene characterized by the storage factor and loss factor exhibiting a gradual increase of at least 20% as a function of time. This is within the viscoelastic region at 190°C, 10 rad / s, and axial force in the range of 0.1N to 1N.

[0089] ● The processing temperature is below the melting point of the above ultra-high molecular weight polypropylene and

[0090] ● The compression forming and rolling temperatures are in the range of 125℃ to 150℃.

[0091] In the examples, the separated ultra-high molecular weight isotactic polypropylene is characterized by having the following.

[0092] ● Molecular weight is 800,000 g / mol

[0093] ● Bulk density is 0.065 g / cm³ 3

[0094] ● Particle size is 600 microns, melting temperature is 159 o It is C

[0095] ● The storage and loss factors show a gradual increase of 20% as a function of time. This is at 190°C,

[0096] ● Within the viscoelastic region at an axial force of 10 rad / s and 1 N, and

[0097] ● The processing temperature is below the melting point of the above ultra-high molecular weight polypropylene and

[0098] ● The compression forming and rolling temperature is 130℃.

[0099] In another embodiment, the isolated ultra-high molecular weight isotactic polypropylene is characterized by the following:

[0100] ● Molecular weight is 2,400,000 g / mol

[0101] ● Bulk density is 0.095 g / cm³ 3

[0102] ● Particle size is 500 microns

[0103] ● The melting temperature is 158 o It is C

[0104] ● The storage factor and the loss factor show a gradual increase of 36% and 39%, respectively, as a function of time.

[0105] ● This is within the viscoelastic region at 190°C, 10 rad / s, and an axial force of 1 N, and

[0106] ● The processing temperature is below the melting point of the above ultra-high molecular weight polypropylene and

[0107] ● The compression forming and rolling temperature is 130℃.

[0108] In another embodiment, the molecular weight is 3,000,000 g / mol and the bulk density is 0.105 g / cm³ 3 The particle size is 500 microns, and the melting temperature is 158 o C, and the storage factor and loss factor show a gradual increase of 31% and 32%, respectively, as a function of time. This was revealed during a vibratory shear time sweep experiment in which the process is within the viscoelastic region at 190°C, 10 rad / s, and 1 N axial force, the processing temperature is below the melting point of the ultra-high molecular weight polypropylene, and the compression molding and rolling temperature is 130°C.

[0109] The present invention provides a manufacturing process for separated UHMWiPP characterized by having low entanglement density, low bulk density, and a spherical shape. The separated UHMWiPP of the present invention does not require costly and time-consuming post-production processing to reduce entanglement density.

[0110] The description of the foregoing embodiments is provided for illustrative purposes only and is not intended to limit the scope of the invention. The individual components of a particular embodiment are generally not limited to that particular embodiment but are interchangeable. Such variations are not deemed to be out of the invention, and all such variations are considered to be included within the scope of the invention.

[0111] The present invention is further explained in light of the following experiment, which is presented merely for illustrative purposes and should not be interpreted as limiting the scope of the invention. The following experiment can be tested and scaled up to an industrial / commercial scale, and the results obtained can be inferred for an industrial scale.

[0112] Experiment Details

[0113] Manufacturing process and characterization of separated ultra-high molecular weight isotactic polypropylene according to the present invention

[0114] The separated ultra-high molecular weight isotactic polypropylene of the present invention is characterized by using the following method / procedure.

[0115] Bulk density measurement: 0.2 g of isolated UHMWiPP was weighed and placed in a 5 mL graduated cylinder. Density was calculated by determining the ratio of the amount of polymer (g) to the volume occupied in the cylinder (ml).

[0116] Percentage measurement of isotactic characteristics: The percentage of isotactic traits is a pentad percentage (% mmm) It was expressed as 13 It was determined by 3C NMR spectroscopy. Proton separation 13 C{ 1 H} NMR measurements were performed on a Bruker Avance Neo 400 NMR spectrometer, and chemical changes were observed at concentrations below 21.85 ppm for isotactic pentads ( mmmm The methyl signal of ) was internally referenced. Generally, 50 to 60 mg of UHMWiPP samples were dissolved in C6D5Br at high temperature. %mmm It was quantified by the integration of the methyl region between 22.0 and 19.7 ppm and reported as a mole fraction (%). All polymers synthesized by the proposed route were confirmed to exhibit an isotactic state (>90%).

[0117] Crystallinity measurement: The percentage of crystallinity was measured using Differential Scanning Calorimetry (DSC). The percentage of crystallinity was determined using commercial DSC equipment, such as the TA Instruments Q250 equipped with TRIOS software. The percentage of crystallinity was calculated using the normalized heat of fusion (ΔH) of the sample, utilizing the first melting endothermic (100–180°C) and a heating rate of 10°C / min. f The ratio of the theoretical value difference for ) and 100% crystalline iPP (204 J / g) was obtained by calculating.

[0118] DSC (Differential Scanning Calorimeter):

[0119] 1. Manufactured according to the present invention separation Characterization of UHMWiPP Entanglement Density:Differential scanning calorimetry was performed using commercially available equipment (e.g., TA Instruments Q250 DSC) to determine the effect of residence time in the melt on crystallization kinetics under isothermal conditions (related to entanglement formation when annealing the sample in the melt). Samples were prepared using Tzero® aluminum pans and lids. A 1.5 mg polymer sample was placed inside the pan and sealed using a commercially available micropress (TA Instruments). Once the pan was sealed, a specific thermal protocol ( Liu, K.; De Boer, E.L.; Yao, Y.; Romano, D.; Ronca, S.; Rastogi, S.,Macromolecules 2016 , 49 (19), 7497-7509 The method was applied to the sample according to the method, which is presented here for reference. The sample was equilibrated at 50°C under a nitrogen atmosphere and then heated at a constant rate of 10°C / min up to a maximum of 200°C. At 200°C, different isothermal times (3 min, 1 hour, and 24 hours) were applied to evaluate the effect of entanglement density. After this time, the sample was cooled at a constant rate of 10°C / min to 135°C. The residence time under the isothermal condition (135°C) was set to 3 hours. Finally, the sample was cooled to 50°C at a constant rate of 10°C / min.

[0120] 2. Melting point measurement of separated UHMWiPP: DSC was also used to determine the melting point of the separated UHMWiPP prepared according to the present invention. The melting point was in the range of 150 to 160°C depending on the polymerization conditions.

[0121] Vibration rheology measurement: Characterization of entanglement density was performed using vibration rheology measurements, and dynamic frequency and time sweep experiments were performed using commercial equipment (Anton-Par MCR 702 Multi Drive Rheometer, etc.) to determine the effects of time, temperature, frequency, and combinations thereof on loss and storage factors (which affected entanglement formation).

[0122] Generally, 0.5 g of isolated UHMWiPP was placed in a circular stainless steel mold with a diameter of 25 mm and then compressed at 125°C for 30 minutes using a maximum load of 30 bar. The sample was cooled at 10°C / min under a constant pressure of 30 bar. Subsequently, the sample was placed between rheometer plates at a temperature of 110°C and heated at a constant rate to 190 or 220°C. Then, a vibration amplitude sweep was performed at a constant value of frequency (ω=10 rad / s) and an axial force ranging from 0.25 N to 4 N. Finally, a vibration frequency sweep was performed at constant values ​​of strain (selected in the previous step), frequency (ω=10 rad / s), and axial force (0.25 N).

[0123] In addition, the present invention evaluated the effect of residence time in the melt on entanglement formation using dynamic vibration rheology (time sweep experiment). As described above, separated UHMWiPP was high-temperature compressed below its melting point to create a rheological sample. The sample was then heated to 110 to 190°C (10°C / min). After maintaining the sample in equilibrium for 3 minutes, a vibration time experiment was performed in the linear viscoelastic region (10 rad / s and 0.1% strain).

[0124] The storage and loss factors were calculated from the dynamic vibration rheology (time sweep experiment) described above. The storage factor of the separated UHMWiPP is the entanglement of the equilibrium rubbery flat zone according to the following: M e It is related to the molecular weight between ). G n 0 = g N ρRT / <M e > , here g N is a numeric coefficient (1 or 4 / 5 depending on convection), and ρ is density, R N is the gas constant, and T is the absolute temperature. Low entanglement densityM e Considering that it is converted to a high value, the resulting elastic response (non-equilibrium) is, since the other terms of the previous formula are usually constant G' <G n 0 is. Therefore, the storage coefficient as a function of time in the melt G' The gradual increase of suggested a gradual increase in entanglement density (low M e ).

[0125] According to the results of the vibration shear time sweep experiment of the present invention, storage during a vibration shear time sweep experiment in a viscoelastic region at 190°C, 10 rad / s, and an axial force in the range of 0.1 N to 1 N ( G’ ) and loss( G” UHMWiPP was classified as isolated when the coefficient showed a gradual increase of at least 20% as a function of time. .

[0126] Molecular weight measurement: Mass average molecular weight (M) of separated UHMWiPP samples w ) and polyvariance(M w / M n The ) value was evaluated through dynamic vibration rheology experiments and gel permeation chromatography. M of the present invention w The isolated UHMWiPP was found to be in the range of 800,000 to 4,000,000. The polydispersity of the isolated UHMWiPP of the present invention was in the range of 2.0 to 15.0.

[0127] The preparation of reagents for the production of separated ultra-high molecular weight isotactic polypropylene according to the present invention is characterized by using the following procedure.

[0128] The preparation of activator and scavenger reagent solutions was carried out using standard Schlenk techniques under a purified nitrogen atmosphere inside a glove box. All solvents used were anhydrous, deoxygenated, and purified using a solvent purification system (SPS).

[0129] Preparation of activator reagent solution:Inside the glove box, N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate (10 μmol, 8.16 mg) was weighed using an anti-static funnel. The compound was transferred to a 25 mL glass Schlenk vial and dissolved using a magnetic bar with 5 mL of dry toluene from SPS. The compound was continuously stirred at 20°C for 1 hour.

[0130] Preparation of Scavenger Reagent Solution: 0.55 mL of tri-isobutyl aluminum (TiBA) solution (25 wt.% in toluene) was placed in a 25 mL Schlenk vial inside a glove box. The TiBA solution (700 μmol, 0.55 mL) was transferred from the original solution container to the vial using a 1 mL plastic syringe and needle.

[0131] Preparation of separated ultra-high molecular weight polypropylene:

[0132] Example 1 :

[0133] Propylene polymerization was carried out in a 1.5 L Buch Glaster batch reactor equipped with a 3-blade propeller, thermocouple, and oil temperature control. The reactor was flushed by applying 7 cycles of dry nitrogen (P: 2.5 bar) and vacuum (-1.0 bar). Subsequently, the flushed reactor was filled with nitrogen and heated continuously to 125°C. After temperature equalization, a high vacuum was applied continuously for at least 8 to 12 hours to remove nitrogen and residual moisture. Then, the reactor temperature was set to the desired value, and the polymerization reaction was started at 40°C. Once the temperature stabilized, 750 mL of heptane was loaded into the reactor. The reactor was continuously stirred at 250 rpm under a dry nitrogen atmosphere. Once the temperature stabilized, 700 μmol (0.55 mL) of the scavenger reagent prepared above, namely a TiBA solution, was injected into the reactor under a continuous nitrogen flow and stirred at 250 rpm for 20 minutes to obtain the first solution. The ratio of catalyst to scavenger was 1:70. Then, stirring was stopped and a high vacuum was applied until the reactor pressure reached -0.9 bar. Once the pressure stabilized, the vacuum was stopped, and propylene monomer was introduced into the mixture in the reactor with continuous stirring (750 rpm) and a constant absolute pressure of 1.1 bar to obtain the second solution.

[0134] Separately, 10 μmol (7.19 mg) of N-[2,6-Bis(1-methylethyl)phenyl]-α-[2-(1-methylethyl)-phenyl]-6-(1-naphthalenyl-κC2)-2-pyridintanaminato(2-)-κN1,κN2]dimethylhanium catalyst (compound of Formula 1) was quantified inside a glove box using an antistatic funnel. The catalyst was dissolved in a Schlenk flask using 4 mL of dry toluene from a solvent purification system (SPS) and a magnetic bar. After continuous mixing for 1 minute, 5 mL of N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate solution (10 μmol, 8.16 mg) as prepared above was reacted with the catalyst solution to obtain a solution containing the pre-activated catalyst species. The ratio of catalyst to activator was maintained at 1:1. A solution containing pre-activated catalyst species was continuously stirred for 5 minutes.

[0135] 9 mL of a solution containing a pre-activated catalyst species was added to a second solution for 10 minutes under a continuous propylene monomer flow and constant stirring (750 rpm) to start the polymerization reaction. The reaction was carried out for 1 hour to obtain a third solution containing unpurified separated ultra-high molecular weight isotactic polypropylene (UHMWiPP).

[0136] The third solution was prepared by injecting 5 mL (70% v / v) of ethanol into the third solution in the reactor and releasing the residual propylene monomer inside the reactor to obtain a quenched third solution containing the precipitate of the crude separated UHMWiPP. After quenching the polymerization, the temperature inside the reactor was set to 23°C. Once the temperature stabilized, the reactor was opened, and the quenched third solution containing the precipitate of the crude separated UHMWiPP was recovered. The quenched third solution containing the precipitate of the crude separated UHMWiPP was washed twice with excess ethanol and filtered under reduced pressure to obtain wet crude UHMWiPP. Subsequently, the wet crude UHMWiPP was dried at room temperature for at least 7 days. The wet crude UHMWiPP may also be dried at 40°C under reduced pressure for 12 hours to obtain UHMWiPP.

[0137] Example 2 Example 2 was carried out in a manner similar to Experiment 1, except that the polymerization reaction was performed for 2 hours.

[0138] Example 3 Example 3 was carried out in a manner similar to Experiment 1, except that the polymerization reaction was performed for 3 hours.

[0139] The properties of the separated UHMWiPP obtained in Examples 1, 2, and 3 are presented in Table 1 below.

[0140] Table 1: Properties of UHMWiPP prepared according to Examples 1, 2, and 3

[0141] condition: Examples 1 2 3 Catalyst (mg) 7.31 7.26 7.20 Polymerization time (h) 1 2 3 Active agent (mg) 8.5 8.24 8.52 Scavenger concentration (mL) 0.55 0.55 0.55 Yield (g) 22 50 42 Activity (Kg polymerization / mol 30 min·bar) 1833 2083 1165 M w rheology (g / mol) 800000 2400000 3000000 polyvariance 2.0 4.5 7.2 %mmmm(%isotactic state) >90% >90% >90% polymer form nine nine nine Bulk density (g / mL) 0.065 0.095 0.105 Average particle size (μm) 600 500 500 % increase in storage factor as a function of time during viscoelastic shear time sweep experiments at 190°C, 10 rad / s, and axial forces in the range of 0.1N to 1N 20% (Axial force: 0.1N) 36% (Axial force: 1N) 31% (Axial force: 1N) % increase in loss factor as a function of time during viscoelastic shear time sweep experiments at 190°C, 10 rad / s, and axial forces in the range of 0.1 N to 1 N 20% (Axial force: 0.1N) 39% (Axial force: 1N) 32% (Axial force: 1N) Forming and rolling temperatures 130°C 130°C 130°C

[0142] The bulk density measurements of the isolated UHMWiPP prepared according to Examples 1, 2, and 3 are shown in Figures 1-a, 1-b, and 1-c. As shown in Figure 1-d, the bulk density of the UHMWiPP prepared using the Ziegler-Natta catalyst system is 0.669 g / cm³. 3As such, it was higher than the bulk density of the isolated UHMWiPP prepared according to the present invention. The size of the isolated UHMWiPP measured using a scanning electron microscope as shown in Figure 2. The size of the isolated UHMWiPP prepared according to Example 2 was reported to be 500 microns. The proportion of the isotactic state of the isolated UHMWiPP prepared according to the present invention was calculated using proton separation carbon NMR as shown in Figure 3 (Example 2). In the case of the isolated UHMWiPP prepared according to the above examples, the percentage of the isotactic state was found to be 90% or higher. The molecular weight of the isolated UHMWiPP obtained in Examples 1, 2, and 3 was measured using dynamic vibrational rheology measurements as shown in Figures 5-a, 5-b, and 5-c, respectively. Figure 5-d shows the superposition of vibrational rheology measurements of the isolated UHMWiPP obtained in Examples 1, 2, and 3. Various frequency sweep measurements were recorded and analyzed to obtain estimated molecular weight and polydispersity.

[0143] As shown in Figure 4-a, differential scanning calorimetry was performed on the separated UHMWiPP obtained in Example 2 to evaluate the entanglement density. The effect of the residence time of the melt on the crystallization time under isothermal conditions is summarized in Table 2 below.

[0144] Table 2: Effect of residence time in melt (200°C) on isothermal crystallization of separated UHMWiPP at 135°C (Example 2)

[0145] Time @ 200 Crystallization maximum enthalpy Initiation crystallization time 3 minutes 23.0 minutes 6.4 minutes 1 hour 45.0 minutes 12.0 minutes 24 hours 78.0 minutes 14.5 minutes

[0146] As shown in Figure 4-a, the residence times in the melt (200°C) were 3 minutes, 1 hour, and 24 hours. The relatively low melting time of 3 minutes (black curve) leads to rapid nucleation and crystal growth, indicated by the curve start (~1 minute) and maximum height (~20 minutes), respectively. Conversely, the time in the melt ( for exampleAs time (1 hour and 24 hours) increased, the onset time (5 minutes and 10 minutes) clearly lengthened, and the width of the overall curve shape (red and blue curves, respectively) widened. These results indicated the presence of low entanglement density in the separated UHMWiPP prepared according to Example 2 of the present invention. As the sample was kept in the melt for a long time, chain recombination occurred slowly. Entanglement acted as a mobility limiting factor that hindered nucleation and consequently extended the crystallization process of the material. As shown in Table 2, as time in the melt increased, nucleation (onset) was delayed, and crystal growth, determined by the maximum enthalpy value as a function of time, was delayed.

[0147] As shown in Figures 4-b and 4-c, the entanglement density of separated UHMWiPP prepared according to Examples 1, 2, and 3 was evaluated using dynamic vibration rheology, and the storage factor and loss factor were measured as a function of time, respectively. Figure 4-b showed that the storage factor of separated UHMWiPP prepared according to Examples 1, 2, and 3 of the present invention increased by at least 20% by the end of the experiment. Similarly, Figure 4-c showed that the loss factor of separated UHMWiPP prepared according to Examples 1, 2, and 3 of the present invention increased by at least 20% by the end of the experiment. These results were attributed to the heterogeneous (non-equilibrium) distribution of entanglement in the molten state. Therefore, Figures 4-b and 4-c show that the UHMWiPP prepared according to Examples 1, 2, and 3 had low entanglement density at the beginning of the experiment, and the gradual increase in the storage and loss factor as a function of time in the melt suggests a gradual increase in entanglement density. The lowest curve in Figures 4b and 4c (the green curve—point indicated by the inverted triangle) also indicated that the UHMWiPP prepared using the Ziegler-Natta catalyst system (comparative example) was not separated compared to the UHMWiPP prepared according to Examples 1, 2, and 3 of the present invention, as the UHMWiPP prepared using the Ziegler-Natta catalyst system showed only an increase in the storage and loss factor as a function of time.

[0148] Example 4 Example 4 was performed similarly to Experiment 2, except that 20 μmol of N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate was used. The ratio of catalyst to activator was maintained at 1:2. The polymerization results are shown in Table 3 below.

[0149] Table 3: Comparison of properties of separated UHMWiPP prepared according to Examples 1 and 4.

[0150] condition: Examples 1 4 Catalyst (mg) 7.26 7.26 Metal:activator 1:1 1:2 Polymerization time (h) 2 2 Active agent (mg) 8.24 16.28 Scavenger concentration (mL) 0.55 0.55 Yield (g) 50 29 Activity (Kg polymerization / mol 30 min·bar) 2083 1183 M w rheology (g / mol) 2400000 3000000 polyvariance 2.0 2.6 %mmmm >90% >90% polymer form rectangle Gel type Bulk density (g / mL) 0.095 Not applicable Average particle size (μm) 500 Not applicable

[0151] Table 3 shows that isolated UHMWiPP synthesized with a catalyst-to-activator ratio of 1:2 produced a gel-like form, whereas the 1:1 sample showed a fine spherical form.

[0152] As shown in Figure 5-d, the molecular weight and polydispersity of the separated UHMWiPP prepared according to Examples 1, 2, and 3 were calculated using vibrational rheology measurements.

[0153] In addition, the thermal properties of the separated UHMWiPP prepared according to Examples 1, 2, 3, and 4 were measured using DSC as summarized in Table 4 below.

[0154] Table 4: Comparison of separated UHMWiPP prepared in Examples 1-4

[0155] Examples Polymerization time (h) Catalyst: Activator T m (°C) ΔH f (J / g) catalyst(%) a T c (°C) ΔH c (J / g) 1 1 1:1 159 116 57 125 105 2 2 1:1 158 117 57 118 107 3 3 1:1 158 119 58 119 112 4 2 1:2 160 119 58 125 98

[0156] a) ΔH0 = 204 J / g

[0157] As can be seen from the table above, the melting temperature of the separated UHMWiPP of the present invention is 158 o C to 160 o The crystallinity of the separated UHMWiPP prepared according to Examples 1, 2, 3 and 4 is in the range of C, and is in the range of 55 to 60%.

[0158] The present invention provides a method for manufacturing separated UHMWiPP having low entanglement density, low bulk density, and spherical shape, and does not require post-processing to reduce entanglement density.

[0159] The embodiments, various features, and beneficial details described above are explained in the following description with reference to non-limiting embodiments.

[0160] Throughout this specification, the word “constitutes” or variations such as “constitutes” or “constituting” are understood to mean the inclusion of specified elements, integers or steps or groups of elements, integers or steps, but not the exclusion of other elements, integers or steps or groups of elements, integers or steps.

[0161] Using the expressions “at least” or “at least one” implies the use of one or more elements, components, or amounts. This is because such use may be employed in embodiments of the invention to obtain one or more desired purposes or results.

[0162] Because the description of the specific embodiments mentioned above is sufficient to reveal the general characteristics of the embodiments, others may easily modify and / or adapt the specific embodiments without departing from the general concept by applying current knowledge. Therefore, such adaptations and modifications should be understood and intended to be within the equivalent meaning and scope of the disclosed embodiments. It should be understood that the language and terminology used herein are for illustrative purposes only and are not limiting. Accordingly, while the embodiments described herein have been described in terms of preferred embodiments, those skilled in the art will recognize that these embodiments may be modified and practiced within the spirit and scope of the embodiments described herein. Furthermore, it should be clearly understood that the foregoing should be interpreted merely as an example of the invention and not as a limitation.

[0163] Although the principles of the invention have been explained and illustrated in relation to the described embodiments, it will be recognized that the described embodiments may be modified in arrangement and details without departing from the scope of such principles.

[0164] Although significant emphasis has been placed on the components and parts of the preferred embodiment in this document, it will be understood that many embodiments can be made and many modifications can be made to the preferred embodiment without departing from the principles of the invention. Since such and other modifications of the preferred embodiment as well as other embodiments of the invention will be apparent to those skilled in the art, it should be clearly understood that the foregoing description should be interpreted merely as illustrative of the invention and not as restrictive.

Claims

Claim 1 A process for manufacturing separated ultra-high molecular weight isotactic polypropylene comprising the following steps: a) in a reactor maintained under an inert atmosphere, containing at least one hydrocarbon solvent, adding at least one scavenger, and mixing and stirring the mixture thus formed under a first predetermined condition to obtain a first solution; b) injecting propylene gas into the reactor at a pressure in the range of 1 bar to 3 bar and maintaining a second predetermined condition to obtain a second solution; c) adding a predetermined amount of a pre-activated catalyst species to the second solution (wherein the pre-activated catalyst species is formed by reacting a catalyst having Structural Formula 1 with an activator to obtain the pre-activated catalyst species); [Structural Formula 1] In the above structural formula 1, R 1, R 2, R3 is isopropyl, and the molar ratio of the catalyst to the activator is 1:1; d) maintaining the reactor under a third predetermined condition to obtain a third solution containing unpurified separated ultra-high molecular weight isotactic polypropylene (UHMWiPP); e) quenching the third solution within the reactor to obtain a quenched third solution containing a precipitate of the unpurified separated UHMWiPP; f) removing the quenched third solution containing the precipitate from the reactor and filtering the quenched third solution to obtain a residue of wet unpurified separated UHMWiPP; and g) washing and drying the residue of wet unpurified separated UHMWiPP to obtain the separated UHMWiPP. Claim 2 A process for producing separated ultra-high molecular weight isotactic polypropylene, wherein the activator is at least one selected from N,N'-dimethylanilinium tetrakis(pentafluorophenyl) borate, trityl tetrakis(pentafluorophenyl) borate, tris(substituted aryl) borane, and derivatives thereof. Claim 3 In claim 1, the first predetermined condition is 10 o C to 70 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene selected from a temperature in the range of C, a stirring speed in the range of 150 rpm to 350 rpm, and a time cycle in the range of 10 minutes to 30 minutes. Claim 4 In claim 3, the first predetermined condition is 40 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene comprising a temperature of C, a stirring speed of 250 rpm, and a time of 20 minutes. Claim 5 In claim 1, the second predetermined condition is 10 o C to 70 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene selected from a temperature in the C range and a stirring speed in the range of 650 rpm to 850 rpm. Claim 6 In claim 5, the second predetermined condition is 40 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene including a temperature of C and a stirring speed of 750 rpm. Claim 7 In claim 1, the third predetermined condition is 10 o C to 70 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene selected from a temperature in the range of C, a stirring speed in the range of 650 rpm to 850 rpm, and a time period in the range of 1 hour to 3 hours. Claim 8 In claim 7, the third predetermined condition is 40 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene comprising a temperature of C, a stirring speed of 750 rpm, and a time cycle of 1 hour. Claim 9 In claim 7, the third predetermined condition is 40 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene comprising a temperature of C, a stirring speed of 750 rpm, and a time cycle of 2 hours. Claim 10 In claim 7, the third predetermined condition is 40 o A manufacturing process for separated ultra-high molecular weight isotactic polypropylene comprising a temperature of C, a stirring speed of 750 rpm, and a time cycle of 3 hours. Claim 11 A process for producing separated ultra-high molecular weight isotactic polypropylene, wherein the scavenger is one or more scavengers selected from the group consisting of methylalumonic acid (MAO) and tri-isobutylaluminum (TiBA). Claim 12 A process for producing separated ultra-high molecular weight isotactic polypropylene according to claim 1, wherein the molar ratio of the catalyst and the scavenger reacted to form a pre-activated catalyst species is in the range of 1:100 to 1:

50. Claim 13 A process for producing separated ultra-high molecular weight isotactic polypropylene according to claim 1, wherein the molar ratio of the catalyst and the scavenger reacted to form a pre-activated catalyst species is 1:

70. Claim 14 A process for manufacturing separated ultra-high molecular weight isotactic polypropylene, wherein the hydrocarbon solvent is one or more selected from toluene and heptane. Claim 15 In claim 1, a process for manufacturing separated ultra-high molecular weight isotactic polypropylene comprising the following steps: a) in a reactor maintained under an inert atmosphere, containing at least one hydrocarbon solvent, adding at least one scavenger, and the mixture thus formed 40 o a) mixing and stirring at a temperature of C, and stirring at a speed of 250 rpm for a time cycle of 20 minutes to obtain a first solution; b) injecting propylene gas at a pressure of 1.1 bar into the reactor and a temperature of 40 o c) a step of obtaining a second solution by maintaining C and stirring at a speed of 750 rpm; d) a step of adding a predetermined amount of a pre-activated catalyst species to the second solution (wherein the pre-activated catalyst species is formed by reacting a catalyst having Structural Formula 1 with an activator to obtain the pre-activated catalyst species); [Structural Formula 1] In the above structural formula 1, R 1, R 2, R3 is isopropyl, and d) the reactor at a stirring speed of 750 rpm for a time ranging from 1 to 3 hours, 40 o a) a step of obtaining a third solution containing unpurified separated ultra-high molecular weight isotactic polypropylene (UHMWiPP) by maintaining at C; e) a step of quenching the third solution in the reactor to obtain a quenched third solution containing a precipitate of the unpurified separated UHMWiPP; f) a step of removing the quenched third solution containing the precipitate from the reactor and filtering the quenched third solution to obtain a residue of wet unpurified separated UHMWiPP; and g) a step of washing and drying the wet unpurified separated UHMWiPP to obtain the separated UHMWiPP. Claim 16 Separated ultra-high molecular weight isotactic polypropylene having the following characteristics obtained by a process described in any one of claims 1 to 15: ● Molecular weight in the range of 500,000 to 4,000,000 g / mol ● 0.05 g / cm³ 3 Up to 0.12 g / cm² 3 Bulk density in the range ● Spherical with a diameter of 300μm to 600μm ● Melting temperature in the range of 155°C to 160°C ● Storage ( G' ) and loss( G'' The modulus exhibits a gradual increase of at least 20% as a function of time during viscoelastic shear time sweep experiments in the viscoelastic region of 190°C, 10 rad / s, and axial force in the range of 0.1N to 1N ● Process temperature below the melting point of the ultra-high molecular weight polypropylene ● Compression molding and rolling temperatures in the range of 125°C to 150°C. Claim 17 delete Claim 18 delete Claim 19 delete Claim 20 delete

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